GLP10-01-02; Interim Repoil 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

GLP10-01-02. Interim Report 13: Analysis of PFBS. PFHS. and PFOS in Groundwater 

Samples Collected at tire IWorqan County Landfill located in Decatur. AL in November 2010 

Study Title 

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

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

Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone: 610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

Maplewood, MN 55144 

Project Identification 

GLP10-01-02-13 

Total Number of Pages 

67 

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

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

the A2I ^ Certificate #2052.01. Testing that complies with this Intematlonal Standard also 

operate In accordance with ISO 9001:2000. 

Certificate #2052.01 

Page 1 of 67 
GLP10-01-02: Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

This page has been reserved for specific country requirements. 

Page 2 of 67 
GLP10-01-02; Interim Repoil 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

GLP COMPLIANCE STATEMENT 

Report Title: GLP10-01-02, Interim Report 13. Analysis of PFBS, PFHS, and PFOS in Groundwater 

Samples Collected at the Morgan County Landfill located in Decatur, AL in November 2010 

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

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

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

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

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

system and no dosing of a test system. 

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

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

Gary Hohenstein, Sponsor Representative Date 

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

Page 3 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-02, Interim Report 13. Analysis of PFBS, PFHS, and PFOS in Groundwater 

Samples Collected at the Morgan County Landfill located in Decatur, AL in November 2010 

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

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

This report and the accompanying data were audited by the 3M Environmental Laboratory Quality 

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

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

Inspection Dates 

1/5/11-1/7/11 

Phase 

Data / Final Report 

Date Reported to 

Testing Facility 

Management 

1/20/11 

Study Director 

1/20/11 

QAU Representative 

iJMtl 

Date 

Page 4 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infonnation 8 

2 Summary 9 

3 Introduction 10 

4 Test & Control Substances 10 

5 Reference Substances 11 

6 Test System 13 

7 Method Summary 13 

7.1 Methods 13 

7.2 Sample Collection 13 

7.3 Sample Preparation 13 

7.4 Analysis 13 

8 Analytical Results 15 

8.1 Calibration 15 

8.2 System Suitability 15 

8.3 Limit of Quantitation (LOQ) 15 

8.4 Continuing Calibration 15 

8.5 Blanks 15 

8.6 Lab Control Spikes (LCSs) 16 

8.7 Analytical Method Uncertainty 20 

8.8 Field Matrix Spikes (FMS) 20 

Page 5 of 67 
GLP10-01-02: Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

9 Data Summary and Discussion 20 

10 Conclusion 29 

11 Data/Sample Retention 29 

12 Attachments 29 

13 Signatures 30 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Morgan County Landfill Groundwater, 

Decatur, AL, November 2010) 9 

Table 2. Instnjment Parameters 14 

Table 3. Liquid Chromatography Conditions 14 

Table 4. Mass Transitions 14 

Table 5. Limit of Quantitation (LOQ) 15 

Table 6. Laboratory Control Spike Recovery 17 

Table 7. Analytical Uncertainty 20 

Table 8. Field Matrix Spike Levels 20 

Table9. DALGWMCLMWIB 101110 21 

Table 10. DAL GWMCLMW I1101110 21 

Table 11. DAL GWMCLMW IS 101110 22 

Table 12. DALGWMCLMW2B 101110 22 

Table 13. DAL GWMCLMW 21101110 23 

Table 14. DAL GWMCLMW3B 101110 23 

Table 15. DAL GWMCLMW 31101110 24 

Table 16. DAL GWMCLMW3S 101110 24 

Table 17. DAL GWMCLMW 4B 101110 25 

Table 18. DALGWMCLMW41101110 25 

Table 19. DAL GW MCL MW 43 101110 26 

Table 20. DAL GW MCL MW13B 101111 26 

Page 6 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 21. DAL GWMCLMW 131101111 27 

Table 22. DAL GW MCL MW13S 101111 27 

Table 23. Trip Blank 28 

Table 24. DAL GW 602S RB 101029 28 

Page 7 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Kevin Eich; Analyst 

Chelsie Grochow; Analyst 

Jonathan Steege; Analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim Report 13 Experimental Tennination: December 15,2010 

Interim Report Completion: Date of Interim Report Signing 

Location of Arcliives 

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

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

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

Page 8 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

2 Summary 

The 3M Environmental Laboratory received groundwater samples from wells located at the Morgan 

County Landfill located in Decatur, AL, representing fourteen different sampling locations. A total of 

sixty sample bottles were received at the 3M Environmental Laboratory for perfluorooctane sulfonate 

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

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

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

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

prepared for detennination of PFBS, PFHS, and PFOS recovery. The groundwater samples, trip 

blanks and one equipment rinseate blank were collected by Weston personnel on November 10-11, 

2010 and received on November 12, 2010. All of the samples were prepared and analyzed for PFBS, 

PFHS, and PFOS following 3M Environmental Laboratory Method ETS-8-044.0 and conducted under 

3M project GLP-10-01-02-13. The average measured PFBS, PFHS, and PFOS concentrations are 

summarized in Table 1. The equipment rinseate and the trip blank were below the lower limit of 

quantitation (LLOQ), indicating adequate control of sample contamination during shipping and sample 

collections. The PFBS concentration results for all ground waters ranged from <0.0250 ng/mL to 2.26 

ng/mL. The PFHS concentration results for all ground waters ranged from <0.0250 ng/mL to 3.28 

ng/mL. The PFOS concentration results for all ground waters ranged from <0.0250 ng/mL to 14.8 

ng/mL. The method uncertainty for PFBS is ± 16%, PFHS ± 13%, and PFOS ± 30%. 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Morgan County Landfill 

Groundwater, Decatur, AL, November 2010) 

Sample ID 

DAL GW MCL MW1B 101110 

DAL GW MCL MW11101110 

DAL GWMCLMW IS 101110 

DAL GW MCL MW2B 101110 

DAL GWMCLMW 21101110 

DAL GW MCL MW3B 101110 

DAL GWMCLMW 31101110 

DAL GW MCL MW3S 101110 

DAL GW MCL MW4B 101110 

DAL GWMCLMW 41101110 

DAL GW MCL MW4S 101110 

DAL GW MCL MW13B 101111 

DAL GW MCL MW131 101111 

DAL GW MCL MW13S 101111 

Trip Blank (Milli-QTM Water) 

Equipment rinseate blanks 

Avg. PFBS 

Concentration 

(ng/mL) ± RPD 

2.26 ±25% [a] 

0.493 ±11% 

1.77 ±19% 

1.24 ±1.6% 

2.06 ±3.4% 

0.0381 ± 12% 

0.0279 ± 0.72% 

<0.0250 

<0.0250 

<0.0250 

<0.0250 

0.0987 ±4.7% 

0.0843 ±7.6% 

0.0957 ±4.2% 

< 0.0250 

< 0.0250 

Avg. PFHS 

Concentration 

(ng/mL) ± RPD 

3.28 ±22% [a] 

0.966 ±9.1% 

2.23 ± 20% 

1.38 ±2.2% 

1.38 ±2.2% 

0.0326 ± 3.7% 

0.0324 ± 8.0% 

<0.0250 

<0.0250 

<0.0250 

<0.0250 

0.0717 ±1.5% 

0.0526 ±4.4% 

0.0559 ± 8.4% 

< 0.0250 

< 0.0250 

Avg. PFOS 

Concentration 

(ng/mL) ± RPD 

7.40 ± 30% [a] 

1.47 ±13% 

6.42 ± 20% 

14.8 ± 2.0% [b] 

5.20 ±16% 

0.283 ± 7.4% 

0.262 ± 0.38% 

0.0306 ±16% 

0.0475 ±15% 

0.144 ±4.9% 

0.256 ± 5.9% 

< 0.0250 

< 0.0250 

< 0.0250 

< 0.0250 

< 0.0250 

N/A; not applicable 

[a] The sample/sample duplicate RPD was S20%. 

[b] Analytical uncertainty has been adjusted for FMS recovery for PFOS to ±35%. 

Page 9 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

3 Introduction 

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

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

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

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

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

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

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

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

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

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

samples. Each empty container for groundwater samplings was marked with a "fill to here" line to 

produce a final sample volume of 200 mL. Containers designated for field matrix samples were fortified 

with an appropriate matrix spike solution containing PFBS, PFHS, and PFOS prior to being sent to the 

field for sample collection. All sample bottles also included the addition of internal standards ^^OaPFBS, ^^Oa-PFHS, and "C4-PFOS at a nominal concentration of 1 ng/mL. All sample bottles also 

included the addition of surrogate spike ^^CA-PFOS at a nominal concentration of 0.1 ng/mL. See 

section 8.8 of the report for field matrix spike levels. 

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

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

Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

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

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

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

report. 

4 Test & Control Substances 

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

was purely analytical in nature. 

Page 10 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

5 Reference Substances 

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

Reference Substance 

Chemical Name 

Chemical Fonnula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfluorobutane sulfonate 

C4F9S03' 

Potassium Salt 

3M 

1/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

PFHS 

(linear) 

Perfluorohexane sulfonate 

C6F13SO3" 

Sodium Salt 

Wellington 

4/2/2013 

Frozen 

LPFHxSAM08 

TCR08-0018 

Crystalline 

98% 

Reference Substance 

Chemical Name 

Chemical Fonnula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

CgFiySOs 

Potassium Salt 

CAS # 2795-39-3 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + branched) 

Perfluorooctane sulfonate 

CgFiySOs 

Potassium Salt 

CAS # 2795-39-3 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

Page 11 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Reference Substance 

Chemical Name 

Chemical Fonnula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"O2-PFBS 

Labeled - Perfluorobutane 

sulfonate 

C4F9S[''02]0-

Ammonium Salt 

RTI International 

3/9/2015 

Frozen 

11546-107-2 

TCR-1022, TCR-1028, TCR1033, and TCR-1038 

Liquid 

99% 

"O2-PFHS 

Labeled - Perfluorohexane 

sulfonate 

CeFiaSf^'Ozj^'OSodium Salt 

Wellington 

04/29/2013 

Frozen 

MPFC-C-0410 

TCR10-0037 

Liquid 

NA'^' 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

"C,-PFOS 

Perfluorooctane sulfonate 

^'CaFiySOa 

Sodium Salt 

Wellington 

04/29/2013 

Frozen 

MPFC-C-0410 

TCR10-0037, TCR10-0044, and 

TCR09-0076 

Liquid 

NA<^' 

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

Page 12 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

6 Test System 

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

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

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

Sample Description Key Code. 

string Number 

Example 

1 

2 

3 

4 

5 

6 

7 

String Desaiptor Example 

DAL GWMCL MW4S 0101110 

Sample Location 

Sample Type 

Well Location 

Well ID 

Well Level 

Sample Type 

Sampling Date 

DAL= Decatur, Alabama 

GW= Groundwater 

MCL = Morgan County Landnil 

Example: MW4 

S = Shallow well 

1 = Interface well 

B = Bedrock well 

0=primary sample 

DB = duplicate sample 

LS = low spike 

RB = Rinseate Blank 

101110 = November 11, 2010 

7 Method Summar y 

7.1 Methods 

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

"Detennination of Perfluorinated Compounds In Water by High Perfonnance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

_TM , 

7.2 Sample Collection 

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

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

November 12, 2010. Samples were stored refrigerated at the laboratory after receipt. A set of 

laboratory prepared Trip Blank and Trip Blank field matrix spike samples were sent with the sample 

collection bottles. 

7.3 Sample Preparation 

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

analysis. 

7.4 Analysis 

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

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

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

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

Table 2, Table 3 and Table 4. 

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

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 2. Instrument Parameters. 

instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograpti 

Guard column 

Analytical column 

InjecUon Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETS MaryAnn 

ETS-8-044.0 

11/23/10 

Agilent 1200 

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

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

10 nL 

Applied Biosystems API 5000 

Turtx) Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

ETS Ginger 

ETS-8-044.0 

12/15/10 

Agilent 1100 

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

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

10 nL 

Applied Biosystems API 5000 

Turbo Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

Table 3. Liquid Chiromatograpiiy Conditions. 

Step 

Number 

Total Time 

(min) 

Flow Rate 

(ftUmin) 

Percent A 

(2 mM ammonium acetate) 

PercentB 

(MethanoO 

ETS-8-044.0 -11 /23/10 Analysis 

0 

1 

2 

3 

4 

5 

0 

2.0 

14.5 

15.5 

16.5 

20.0 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

ETS-8-044.0-12/15/10 Analysis 

0 

1 

2 

3 

4 

5 

0 

1.0 

11.0 

13.5 

14.0 

17.0 

300 

300 

300 

300 

300 

300 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Table 4. IVIass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

"CrPFOS Surrogate 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/99 

399/80 

499/99 

499/80 

499/130 

503/80 

Internal Standard 

C'OJPFBS 

f'OJPFHS 

("CJPFOS 

f'CJPFOS 

Mass Transition 

Q1/Q3 

303/84 

403/84 

507/80 

507/80 

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

(TIC), which vi«s used for quantitation. 

Page 14 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

8 Analytical Results 

8.1 Calibration 

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

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

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

total of thirteen spiked standards ranging from 0.025 ng/mL to 50 ng/mL (nominal) analyzed on 11/23/10 

and ten spiked standards ranging from 0.025 ng/mL to 5.0 ng/mL (nominal) analyzed on 12/15/10. Low 

curve points were disabled for PFOS on 11/23/10 to meet method blank criteria. Aquadratic, 1/x 

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

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

the peak area confinned accuracy of each curve point. 

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

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

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

8.2 System Suitability 

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

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

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

RSD was met for PFBS, PFHS, PFOS, and ^^C4-PF0S. 

8.3 Limit of Quantitation (LOQ) 

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

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

blanks. The nominal LOQ for all analytes can be found in Table 5. 

Table 5. Limit of Quantitation (LOQ). 

Analysis Date 

11/23/10 

12/15/10 

PFBS 

LOQ, ng/mL 

0.0250 

N/A 

PFHS 

LOQ, ng/mL 

0.0250 

N/A 

PFOS 

LOQ, ng/mL 

0.250 

0.0250 

N/A - Not Applicable 

8.4 Continuing Calibration 

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

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

reported sample results were bracketed by CCVs that met method criteria of 100% ± 25% with the 

exception of sampling location DAL GW MCL 21101110, which was bracketed by a CCV for PFOS that 

had a recovery of 149%. 

8.5 Blanks 

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

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

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

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

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

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

Page 15 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - november 2010 

8.6 Lab Control Spikes (LCSs) 

11/23/10 Analysis: Lab control spikes were prepared and analyzed in triplicate at three levels for PFBS, 

PFHS, and PFOS, and at two levels for ^^C4-PF0S. LCSs were prepared by spiking known amounts of 

the target analytes into 10 mL of laboratory prepared synthetic groundwater to produce the desired 

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

method acceptance criteria, average of LCS at each level within 100% + 20% with an RSD <20%, were 

met for PFBS and PFHS. The low level LCS for PFOS could not be calculated as the detected 

concentration was below the limit of quantitation. The mid and high level LCS met method acceptance 

crteria. 

12/15/10 Analysis: Lab control spikes were prepared and analyzed in triplicate at two levels for PFOS. 

LCSs were prepared by spiking known amounts of the target analytes into 10 mL of laboratory prepared 

synthetic groundwater to produce the desired concentration. The spiked water samples were then 

analyzed in the same manner as the samples. The method acceptance criteria, average of LCS at each 

level within 100% ± 20% with an RSD <20%, were met for PFOS. 

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

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

and branched PFOS were prepared at a minimum of two concentrations to evaluate the potential for 

analytical bias. 

11 /23/10 Analysis: Three LCS levels were prepared an anizyed in tripcalte. The low level linear and 

branched LCS could not be calcualted as the detected concentration was below the limit of quantitation. 

The mid level linear and branched LCS had an average recovery of 136% and the high level had an 

average recovery of 133%. A new set of linear and branched stock standards were prepared, with new 

LCS prepared at the same three concentration levels. The new LCS were analyzed at the end of the 

analytical ain. Two of the low level linear and branched LCS could not be calcualted as the detected 

concentration was below the limit of quantitation. One replicate at the low level had a recovery of 152%, 

while both the new mid and high level linear and branched LCS met method acceptance criteria with 

average recvoeries of 114%. The mid and high level LCS concentrations were more appropriate as 

compared to the sample concentrations reported from this run. A method deviation is included in the 

raw data. 

12/15/10 Analysis: Two LCS levels were prepared and aniyzed in triplicate. Both LCS level of linear 

and branched PFOS met method acceptance criteria. 

All LCS results were used in the determination of method analytical uncertainty in section 8.7. 

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

1 ^or, . D Calculated Concentration ..„„„, 

LCS Percent Recovery = * 100% 

Spike Concentration 

LCS% RSD = standard deviation LCS replicates . ^QQ„/^ 

average LCS recovery 

Page 16 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 6. Laboratory Control Spil<e Recovery. 

ETS-8-W4.0 

Lab ID 

LCS-101115-1 

LCS-101115-2 

LCS-101115-3 

Average + %RSD 

LCS-101115-4 

LCS-101115-5 

LCS-101115-6 

Average ±%RSD 

"CrPFOS 

Spiked 

ConcerrtraOon 

(ng/mL) 

0.0948 

0.0948 

0.0948 

Calculated 

Concentration 

(ng/mL) 

0.114 

0.112 

0.110 

%Recovery 

120 

118 

116 

118% ±1.7% 

0.940 

0.940 

0.940 

0.990 

1.03 

1.02 

105 

109 

109 

108%+ 2.1% 

ETS-8-044.0 

Analyzed 11/23/10 

Lab ID 

LCS-101115-1 

LCS-101115-2 

LCS-101115-3 

Average ±%RSD 

LCS-101115-4 

LCS-101115-5 

LCS-101115-6 

Average ±%RSD 

LCS-101115-7 

LCS-101115-8 

LCS-101115-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

PFBS 

Calculated 

Concentration 

(ng/mL) 

0.168 

0.205 

0.212 

%Recovery 

84.6 

103 

107 

98.2% ±12% 

1.96 

1.96 

1.96 

1.85 

2.13 

2.04 

94.2 

109 

104 

102% ±7.4% 

9.94 

9.94 

9.94 

9.10 

10.8 

10.5 

91.5 

108 

106 

102% ±8.8% 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

PFHS 

Calculated 

Concentration 

(ng/mLj 

0.189 

0.219 

0.229 

VoRecovery 

95.5 

111 

116 

108% ±9.9% 

1.97 

1.97 

1.97 

2.01 

2.37 

2.27 

102 

120 

115 

112%+ 8.3% 

9.95 

9.95 

9.95 

10.1 

12.0 

11.9 

101 

120 

119 

113% ±9.4% 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

PFOSOineai) 

Calculated 

Concentration 

(ng/mL) 

<0.250 

<0.250 

<0.250 

YcRecovery 

N/A 

N/A 

N/A 

N/A''' 

1.96 

1.96 

1.96 

1.96 

2.31 

2.18 

100 

118 

111 

110% ±8.3% 

9.94 

9.94 

9.94 

10.4 

12.0 

12.3 

105 

121 

123 

116% ±8.5% 

(1) N/A = Not Applicable; A recovery could not be calculated as ttie detected value viras below the limit of quantitation. 

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

Page 17 of 67 
GLP10-01-02, Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 11/23/10 

Lab ID 

LCS-101115-10 

LCS-101115-11 

LCS-101115-12 

Average ±%RSD 

LCS-101115-13 

LCS-101115-14 

LCS-101115-15 

Average ± %RSD 

LCS-101115-16 

LCS-101115-17 

LCS-101115-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.196 

0.196 

0.196 

Calculated 

Concentration 

(ng/mL) 

<0.250 

<0.250 

<0.250 

%Recovery 

N/A 

N/A 

N/A 

N/A"" 

1.97 

1.97 

1.97 

2.63 

2.63 

2.73 

134 

134 

139 

136% ±2.1%' ' 

9.90 

9.90 

9.90 

12.9 

13.3 

13.4 

130 

134 

135 

133% ±2.2% "^ 

Lab ID 

LCS-101120-1 

LCS-101120-2 

LCS-101120-3 

Average ±%RSD 

LCS-101120-4 

LCS-101120-5 

LCS-101120-6 

Average ±%RSD 

LCS-101120-7 

LCS-101120-8 

LCS-101120-9 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.196 

0.196 

0.196 

Calculated 

Concentration 

(ng/mL) 

0.298 

<0.250 

<0.250 

%Recovery 

152 

N/A 

N/A 

N/A"' 

1.97 

1.97 

1.97 

2.03 

2.34 

2.29 

103 

119 

116 

113% ±7.5% 

9.90 

9.90 

9.90 

10.3 

11.7 

11.7 

105 

118 

118 

114% ±6.6% 

(1) N/A = Not Applicable; A recovery could not be calculated as the detected value was below the limit of quantitation. 

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

Page 18 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 6 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 12/15/10 

Lab ID 

LCS-101215-1 

LCS-101215-2 

LCS-101215-3 

Average ±%RSD 

LCS-101215-4 

LCS-101215-5 

LCS-101215-6 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.139 

0.172 

0.162 

%Recovery 

70.3 

86.8 

81.9 

79.7% ±11% 

1.98 

1.98 

1.98 

1.63 

1.94 

1.92 

82.5 

97.9 

96.7 

92.4% ±9.3% 

Lab ID 

LCS-101215-7 

LCS-101215-8 

LCS-101215-9 

Average ±%RSD 

LCS-101215-10 

LCS-101215-11 

LCS-101215-12 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.196 

0.196 

0.196 

Calculated 

Concentration 

(ng/mL) 

0.207 

0.214 

0.200 

VoRecovery 

106 

109 

102 

106% ±3.3% 

1.97 

1.97 

1.97 

2.20 

2.18 

2.17 

112 

111 

110 

111% ±0.90% 

(1) N/A = Not Applicable; A recovery could not be calculated as ttie detected value was below the limit of quantitation. 

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

Page 19 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

8.7 Analytical Method Uncertainty 

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

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

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

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

con-esponds to a confidence level of 95%. 

Table 7. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

8.02 

6.27 

15.2 

Method 

Uncertainty 

±16% 

±13% 

± 30% 

8.8 Field Matrix Spikes (FMS) 

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

applicable to the 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. 

Table 8. Field Matrix Spilte Levels. 

Sampling Location 

All sampling locations - Low Spike 

All sampling locations - High Spike 

PFBS, ng/mL 

0.970 

9.72 

PFHS, ng/mL 

0.960 

9.61 

PFOS, ng/mL 

0.980 

9.78 

FMS Recovery: 

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

Spilce Concentraton 

100% 

9 Data Summary and Discussion' 

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

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

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

from those listed in the raw data. 

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

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

DAL GW MCL MW 2B 101110 - The HS recovery for PFOS was 135%. This was the only 

appropriate spike level for this sampling location. The analytical uncertainty has been adjusted for 

the sampling location for PFOS to ± 35%. 

Page 20 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Tables. DAL GWMCLMW IB 101110 

3M LIMS ID 

GLP10-01-02-13-001 

GLP10-01-02-13-002 

GLP10-01-02-13-003 

GLP10-01-02-13-004 

Description 

DAL GW MCL MW 1B 0 101110 

DALGWMCLMW1BDB 101110 

DAL GW MCL MW IB LS 101110 

DAL GWMCL MW IB HS 101110 

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

PFBS 

Concentration 

(ng/mL) 

1.98 

2.54 

3.17 

12.8 

YoRecovery 

NA 

NA 

NC 

108 

2.26 ng/mL ±25%'^' 

PFHS 

Concentration 

(ng/mL) 

2.92 

3.63 

4.09 

13.9 

YoRecovery 

NA 

NA 

NC 

111 

3.28 ng/mL ± 22% <^' 

PFOS 

Concentration 

(ng/mL) 

6.29 

8.50 

7.49 

17.6 

YoRecovery 

NA 

NA 

NC 

104 

7M) ng/mL ±30Yo 

13C4-PFOS 

XRecovery 

98.2 

90.2 

99.9 

94.7 

95.7% ±4.5% 

NA = Not Applicable 

(1) The sample/sample duplicate RPD was ^0% . 

Table 10. DAL GWMCLMW 11101110 

3MUIVISID 

GLP10-01-02-13-005 

GLP10-01-02-13-006 

GLP10-01-02-13-007 

GLP10-01-02-13-008 

Description 

DAL GWMCLMW 11 0 101110 

DALGWMCLMW1IDB 101110 

DAL GW MCL MW 11 LS 101110 

DAL GW MCL MW 11 HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.520 

0.466 

1.72 

11.5 

YoRecovery 

NA 

NA 

126 

113 

0.493 ng/mL ±11Yo 

PFHS 

Concentration 

(ng/mL) 

1.01 

0.922 

2.16 

12.3 

YoRecovery 

NA 

NA 

124 

118 

0.966 ng/mL ±9.1Yo 

PFOS 

Concentration 

(ng/mL) 

1.56 

1.37 

2.61 

12.9 

YoRecovery 

NA 

NA 

117 

117 

1.47 ng/mL ±13Yo 

13C4-PFOS 

YoRecovery 

95.6 

96.0 

95.6 

101 

97.1Yo±Z8Yo 

NA = Not Applicable 

Page 21 of 67 
Table 11. DAL GWMCLMW IS 101110 

GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

3M LIMS ID 

GLP 10-01-02-13-009 

GLP10-01-02-13-010 

GLP10-01-02-13-011 

GLP10-01-02-13-012 

Description 

DAL GWMCLMW IS 0 101110 

DAL GWMCLMW IS DB 101110 

DAL GW MCL MW IS LS 101110 

DAL GWMCLMW IS HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

rgA = Not Applicable 

PFBS 

Concentration 

(ng/mL) 

1.93 

1.60 

2.84 

12.8 

YoRecovery 

NA 

NA 

111 

114 

1.77 ng/mL ±19Yo 

PFHS 

Concentration 

(ng/mL) 

2.45 

2.00 

3.32 

13.7 

YoRecovery 

NA 

NA 

NC 

119 

2.23 ng/mL ±20Yo 

PFOS 

Concentration 

(ng/mL) 

7.05 

5.78 

7.21 

17.7 

%Recovery 

NA 

NA 

NC 

115 

6.42 ng/mL ±20Yo 

13C4-PFOS 

%Recovery 

87.7 

98.0 

99.1 

97.9 

95.6% ±5.6% 

Table 12. DAL GW MCL MW2B 101110 

-

3M LIMS ID 

GLP10-01-02-13-013 

GLP10-01-02-13-014 

GLP10-01-02-13-015 

GLP10-01-02-13-016 

Description 

DAL GW MCL MW 2B 0 101110 

DAL GW MCL MW 2B DB 101110 

DAL GWMCLMW 28 LS 101110 

DAL GWMCLMW 28 HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

1.25 

1.23 

2.42 

12.1 

%Recovery 

NA 

NA 

122 

112 

1.24 ng/mL ± I.6Y0 

PFHS 

Concentration 

(ng/mL) 

1.36 

1.39 

2.61 

12.7 

YoRecovery 

NA 

NA 

129 

118 

1.38 ng/mL ±2.2Yo 

PFOS 

Concentration 

(ng/mL) 

14.6 

14.9 

16.2 

28.0 

YoRecovery 

NA 

NA 

NC 

135 <^' 

14.8 ng/mL ±2.0Yo'^ 

13C4-PFOS 

YoRecovery 

102 

97.1 

100 

99.9 

99.7Yo ± f.9% 

NA= Not Applicable 

(1) Field matrix spike recovery did not meet mettiod acceptance criteria of 100% ± 30%. 

(2) The analytical uncertainty tias been adjusted for FMS recovery to 100% ± 35%. 

Page 22 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 13. DAL GWMCLMW 21101110 

3M LIMS ID 

GLP10-01-02-13-017 

GLP10-01-02-13-018 

GLP10-01-02-13-019 

GLP10-01-02-13-020 

Description 

DAL GWMCL MW2I 0 101110 

DAL GWMCL MW2I DB 101110 

DAL GWMCL MW2I LS 101110 

DAL GW MCL MW 21 HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

2.09 

2.02 

3.16 

12.8 

YoRecovery 

NA 

NA 

NC 

111 

2.06 ng/mL ±3.4Yo 

PFHS 

Concentration 

(ng/mL) 

1.39 

1.36 

2.54 

12.2 

YoRecovery 

NA 

NA 

121 

113 

1.38ng/mL±2.2% ' 

PFOS^^ 

Concentration 

(ng/mL) 

5.61 

4.78 

6.17 

17.0 

%Recovery 

NA 

NA 

NC 

121 

5.20 ng/mL ±16Yo 

13C4-PFOS 

YoRecovery 

96.3 

96.0 

97.7 

103 

98.3% ±3.5% 

NA= Not Applicable 

(1) Samples were bracketed by a CCV that outside method acceptance criteria with a recovery of 149%. 

Table 14. DAL GW MCL MW3B 101110 

3M LIMS ID 

GLP10-01-02-13-021 

GLP10-01-02-13-022 

GLP10-01-02-13-023 

GLP10-01-02-13-024 

Description 

DAL GW MCL MW 38 0 101110 

DAL GWMCL MW3BDB 101110 

DAL GW MCL MW 38 LS 101110 

DAL GWMCL MW38HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0403 

0.0359 

1.22 

11.4 

YoRecovery 

NA 

NA 

122 

117 

0.0381 ng/mL ± 12% 

PFHS 

Concentration 

(ng/mL) 

0.0332 

0.0320 

1.21 

11.4 

YoRecovery 

NA 

NA 

123 

118 

0.0326 ng/mL ±3.7Yo 

PFOS 

Concentration 

(ng/mL) 

0.293 

0.272 

1.22 

NA<^' 

YoRecovery 

NA 

NA 

95.7 

NA<^' 

0.283 ng/mL ±7.4Yo 

13C4-PFOS 

%Recovery 

101 

98.3 

98.2 

99.6 

99.4Yo ± I.6Y0 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample v*as not analyzed in this mn. 

Page 23 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 15. DAL GW MCL MW 31101110 

3M LIMS ID 

GLP10-01-02-13-025 

GLP10-01-02-13-026 

GLP10-01-02-13-027 

GLP10-01-02-13-028 

Description 

DAL GWMCL MW3I 0 101110 

DAL GWMCL MW3I DB 101110 

DALGWMCLMW3ILS 101110 

DAL GWMCL MW3I HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0278 

0.0280 

1.19 

11.2 

YoRecovery 

NA 

NA 

120 

115 

0.0279 ng/mL ±0.72% 

PFHS 

Concentration 

(ng/mL) 

0.0311 

0.0337 

1.26 

11.1 

YoRecovery 

NA 

NA 

128 

115 

0.0324 ng/mL ±8.0Yo 

PFOS 

Concentration 

(ng/mL) 

0.261 

0.262 

1.24 

NA'^' 

YoRecovery 

NA 

NA 

99.8 

NA'^> 

0.262 ng/mL ±0.38Yo 

13C4-PFOS 

%Recovery 

96.5 

98.0 

101 

103 

99.5% ± 2.9Yo 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this mn. 

Table 16. DAL GW MCL MW3S 101110 

3M LIMS ID 

GLP10-01-02-13-029 

GLP10-01-02-13-030 

GLP10-01-02-13-031 

GLP10-01-02-13-032 

Description 

DAL GW MCL MW 3S 0 101110 

DAL GW MCL MW 3S DB 101110 

DAL GW MCL MW 3S LS 101110 

DAL GW MCL MW 3S HS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.22 

11.3 

XRecovery 

NA 

NA 

126 

116 

<0.0250 ng/mL 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.23 

11.2 

YoRecovery 

NA 

NA 

128 

117 

<0.0250 ng/mL 

PFOS 

Concentration 

(ng/mL) 

0.0331 

0.0281 

0.980 

NA<^) 

YoRecovery 

NA 

NA 

96.9 

NA'^> 

0.0306 ng/mL ±16Yo 

13C4-PFOS 

YoRecovery 

94.7 

101 

104 

101 

100Yo±4.0Yo 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this run. 

Page 24 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 17. DAL GW MCL MW4B 101110 

3M LIMS ID 

GLP10-01-02-13-033 

GLP10-01-02-13-034 

GLP10-01-02-13-035 

GLP10-01-02-13-036 

Description 

DAL GW MCL MW 4B 0 101110 

DAL GWMCL MW4BD8 101110 

DAL GW MCL MW 4B LS 101110 

DAL GWMCL MW4BHS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.19 

11.1 

YoRecovery 

NA 

NA 

123 

114 

<0.0250 ng/mL 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.23 

11.4 

YoRecovery 

NA 

NA 

128 

119 

<0.0250 ng/mL 

PFOS 

Concentration 

(ng/mL) 

0.0511 

0.0439 

0.991 

NA<^' 

YoRecovery 

NA 

NA 

96.3 

NA'^' 

0.0475 ng/mL ±15Yo 

13C4-PFOS 

YoRecovery 

101 

102 

102 

106 

10r/o±2.2Yo 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample wras not analyzed in this ain. 

Table 18. DAL GW MCL MW 41101110 

3M LIMS ID 

GLP10-01-02-13-037 

GLP10-01-02-13-038 

GLP10-01-02-13-039 

GLP10-01-02-13-040 

Description 

DAL GWMCL MW4I 0 101110 

DAL GW MCL MW 41 DB 101110 

DAL GWMCL MW4ILS 101110 

DAL GWMCL MW4IHS 101110 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.18 

11.7 

YoRecovery 

NA 

NA 

122 

120 

<0.0250 ng/mL 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.20 

11.7 

YoRecovery 

NA 

NA 

125 

122 

<0.02SO ng/mL 

PFOS 

Concentration 

(ng/mL) 

0.147 

0.140 

1.11 

NA<^' 

YoRecovery 

NA 

NA 

98.6 

NA<^' 

0.144 ng/mL ±4.9Yo 

13C4'PFOS 

YoRecovery 

99.9 

98.0 

98.1 

102 

99.5% ± 19% 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this run. 

Page 25 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 19. DAL GW MCL MW4S 101110 

3M LIMS ID 

GLP10-01-02-13-041 

GLP10-01-02-13-042 

GLP10-01-02-13-043 

GLP10-01-02-13-044 

Description 

DAL GW MCL MW4S 0 101110 

DALGWMCLMW4SDB 101110 

DALGWMCLMW4SLS 101110 

DAL GW MCL MW4S HS 101110 

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

PFBS 

Concerrtration 

(ng/mL) 

<0.0250 

<0.0250 

1.21 

11.7 

YoRecovery^ 

NA 

NA 

125 

120 

<0.0250 ng/mL 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

1.23 

11.7 

YoRecovery 

NA 

NA 

128 

122 

<0.0250 ng/mL 

PFOS 

Concentration 

(ng/mLj^ 

0.263 

0.248 

1.11 

NA<^' 

YoRecovery 

NA 

NA 

87.2 

NA<^> 

0.256 ng/mL ±5.9Yo 

13C4-PFOS 

XRecovery 

102 

99.3 

106 

104 

103Yo ± 2.8% 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this mn. 

Table 20. DAL GW MCL MW 13B 101111 

3M LIMS ID 

GLP10-01-02-13-045 

GLP10-01-02-13-046 

GLP10-01-02-13-047 

GLP10-01-02-13-048 

Description 

DAL GW MCL MW 138 0 101111 

DAL GWMCLMW 138 D8 101111 

DAL GWMCLMW 138 LS 101111 

DAL GWMCLMW 138 HS 101111 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0964 

0.101 

1.31 

10.9 

XRecovery 

NA 

NA 

125 

111 

0.0987 ng/mL ±4.7% 

PFHS 

Concentration 

(ng/mL) 

0.0711 

0.0722 

1.31 

11.2 

YoRecovery 

NA 

NA 

129 

116 

0.0717 ng/mL ±1.5% 

PFOS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

0.987 

NA<^> 

YoRecovery 

NA 

NA 

101 

NA<^' 

<0.0250 ng/mL 

13C4-PFOS 

YoRecovery 

104 

99.2 

98.9 

99.8 

101% ±2.6% 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this mn. 

Page 26 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 21. DAL GW MCL MW 131101111 

3M LIMS ID 

GLP10-01-02-13-049 

GLP10-01-02-13-050 

GLP10-01-02-13-051 

GLP10-01-02-13-052 

Description 

DAL GWMCLMW 131 0 101111 

DAL GWMCL MW 131 DB 101111 

DALGWMCLMW13ILS 101111 

DAL GW MCL MW 131 HS 101111 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0875 

0.0811 

1.29 

11.3 

YoRecovery 

NA 

NA 

124 

115 

0.0843 ng/mL ±7.6% 

PFHS 

Concentration 

(ng/mL) 

0.0537 

0.0514 

1.29 

11.7 

YoRecovery 

NA 

NA 

129 

121 

0.0526 ng/mL ±4.4% 

PFOS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

0.955 

NA'^> 

XRecovery 

NA 

NA 

97.4 

NA<^> 

<0.0250 ng/mL 

13C4-PFOS 

YoRecovery 

99.1 

99.9 

100 

100 

99.9Yo±0.59X 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this mn. 

Table 22. DAL GW MCL MW 13S 101111 

3M LIMS ID 

GLP10-01-02-13-053 

GLP10-01-02-13-054 

GLP10-01-02-13-055 

GLP10-01-02-13-056 

Description 

DAL GWMCL MW13S 0 101111 

DAL GWMCL MW13SDB 101111 

DAL GWMCL MW13SLS 101111 

DAL GW MCL MW 13S HS 101111 

Average Concentration (ng/mL) ± YoRPD/RSD 

PFBS 

Concentration 

(ng/mL) 

0.0977 

0.0937 

1.27 

11.6 

YoRecovery 

NA 

NA 

121 

118 

0.0957 ng/mL ±4.2X 

PFHS 

Concentration 

(ng/mL) 

0.0582 

0.0535 

1.25 

11.5 

YoRecovery 

NA 

NA 

124 

119 

0.0559 ng/mL ±8.4X 

PFOS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

0.943 

NA'^> 

YoRecovery 

NA 

NA 

96.2 

NA*^' 

<0.0250 ng/mL 

13C4-PFOS 

YoRecovery 

104 

105 

98.7 

103 

103X±2.r/o 

NA = Not Applicable 

(1) Sample set was analyzed for PFOS on 12/15/10. The high field matrix spike sample was not analyzed in this mn. 

Page 27 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Table 23. Trip Blank 

3M LIMS ID 

GLP10-01-01-13-058 

GLP10-01-01-13-059 

GLP10-01-01-13-059 

GLP10-01-01-13-060 

Description 

Trip Blank Sample 

Trip Blank Low Spike 

Trip Blank Low Spike 

Trip Blank High Spike 

PFBS 

Concentration 

(ng/mL) 

<0.0250 "' 

1.18 <^> 

NA 

11.5 <^> 

YoRecovery 

NA 

122 

NA 

118 

PFHS 

Concentration 

(ng/mL) 

<0.0250 *'> 

1.23 <^' 

NA 

11.6'^' 

YoRecovery 

NA 

128 

NA 

121 

PFOS 

Concentration 

(ng/mL) 

<0.0250 '^> 

0.936 <^' 

1.12'^' 

10.9 <^' 

YoRecovery 

NA 

95.5 

114 

111 

NA = Not Applicable 

(1) Results reported from analytical mn 11/23/10. 

(2) Results reported ft-om analytical mn for PFOS on 12/15/10. 

Table 24. DAL GW 602S RB 101029 

3M LIMS ID 

GLP10-01-01-13-057 

Description 

DAL GWMCLMW 21 RB 101110 

PFBS 

Concentration 

(ng/mL) 

<0.0250 '^' 

PFHS 

Concentration 

(ng/mL) 

<0.0250''' 

PFOS 

Concentration 

(ng/mL) 

<0.0250 <^' 

NA= Not Applicable 

(1) Results reported from analytical mn 11/23/10. 

(2) Results reported fi-om analytical mn for PFOS on 12/15/10. 

Page 28 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

10 Conclusion 

Laboratory control spikes and field matrix spikes were used to determine the analytic^al method 

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

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

11 Data/Sample Retention 

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

to 3M Environmental Laboratory standard operating procedures. 

12 Attachment s 

Attachment A: Protocol Amendment 13 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 29 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

13 Signatures 

Date 

^-^Iz^i] 

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

3/ x^c^// 

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

:7-. 

i{ 

Gary Hohemstein/yJM Sponsor Representative 

(MA/ 

Date 

M 

Jaisimha Kesari, study Director Date 

Page 30 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment A Morgan County ^^%%^,f^ff^^fa'cW'^M°01-02 

Amendment 13 

Study Title 

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

Perfluorobutane sulfonate (PFBS) In Groundwater, Sol! and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 13 

Amendment Date: 

November 9, 2010 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02-13 

Sampling Event 

Morgan County Landfill - Groundwater Sampling 

Exad Copy of Original 

Inltiai DM© 

Page 1 of 6 

Page 31 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment A Morgan County ^^')^j\»^i^%ff^^tO%f'&^Mh-02 

Amendment 13 

This amendment modifies tlie 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. 

AMBNDTOREAD: 

No changes to the wording of the protocol are required. This amendment orlly 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 tirheframe of November 10-11, 

2010. The groundwater samples for this sampling event will be entered into the 3M Environmental 

Laboratory LIMS as project GLP10-01-02-13 and reported as interim report GLP10-01-02-13, (reflecting 

study GLP10-01-02 and amendment-13). 

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 three pages in length and included as attached to this amendment fomn. 

Page 2 of 6 

Page 32 of 67 
Attactiment A 

GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County ^^mim^Ymtb'^Wm^-h-0 2 

Amendment 13 

Amendment Approval 

Uu WPnmnii iO 

t J 

Gary HoheiTistein, Sponsor Representative Date 

yf/2^/^ 

Cleston C. Lange, Principal Analytical Investigator Date 

///fA^ / 

VWIIiam Reagen, EHS Opns Environmental Lab Management 

MX(. 

Date 

i//i<hm 

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

Page 3 of 6 

Page 33 of 67 
Attachment A 

GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County ^^mim'f'F^^(oW^f=m}1-0 2 

Amendment 13 

Environmental Health & Safety Operations, Environmental Laboratory 

Genera! Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

cc: WiMm Reagen, 3M EHS&Opns; Environmentel Lab 

Cliffton Jacoby, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charles Young, Weston Solutions 

Tim Frinak, Weston Solutions 

Date: Novembers, 2010 

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

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

Phase 3 Site-Related Monitoring Program; GLP Interim Report 13-Morgan County Landfill 

Groundwater 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Numljer 

Project Schedufe/Test Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

flahotiensteIn@miT!m,,:«>'r! 

3M Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wk reaaen<S)mmm. com 

Principal Analytical Investigator 

Cleston Lange 

3IW1 EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

(Jdange^mmrp.com, 

Sampling Coordinator 

Timothy Frinal< 

Weston Solutions 

Timothv.frinakSjwestonsolutlons.com 

Phone; (334).332-9123 

GLP10-01^2-13 

Dept #530711. Project #0022674449 

Sampling scheduled for November 10-11, 2010 

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

Page 4 of 6 

Page 34 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment A Morgan County Larj^fil^/Dgc|tyr^L^^No,^e^e^0J_0^^_^2 

Amendment 13 

2 Background Information and Project Objective(s) 

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

samples collected from five monitoring stations. Each monitoring station at the facility is constructed with 

two to three wells, monitoring the residuum, the intermediate zone (epikarst) and bedrock. Based on 

review of the well locations and groundwater flow patterns for the site, the following wells have been 

selected for sampling and the rationale is provided for each selected location: MW-1 (S, I, B); MW-2 (I, B); 

MW-3 (S, I, B); and MW-4 (S, I, B) - These eleven wells represent downgradient compliance wells for the 

facility which, based on groundwater contours, monitor flow from most of the active landfill area. Well 

designations are: S-shallow well, I - Interface well, and B ~ Bedrock well. MW-13 (S, I, B) - This well 

cluster represents an upgradient monitoring point to the landfill and serves as a background monitoring 

point. Sampling locations will be analyzed for Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate 

(PFHS), and Perfiuorooctanesulfonate (PFOS) as part of the Morgan County Landfill groundwater 

sampling. 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 November 10-11, 

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

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

submitted to Gary Hohenstein and Jai Kesari upon completion under interim report GLP10-01-02-13. 

3 Project Schedule 

Sample collection bottles vwl! be prepared by 3M Envinanmental Laboratory for sampling November 10-11, 

2010. Sample bottles will be shipped in coolers overnight to 3M Decatur for anrival on Wednesday, November 

10, 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 fourteen sampling locations have been specified. For each sampling location, a total of four sample 

bottles will be collected (sample, sample duplicate, low-level field matrix spike, and high-level field matrix 

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

reagent-grade water, a low-level trip blank 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 twttles. The low field matrix spike 

will fcie prepared at 1 ng/mL and the high field matrix spike at 10 ng/mL. Two additional bottles will be prepared 

to be used for the preparation of the equipment rinseate blanks. In addition to frie sample bottles, a 1-L 

container of Milli Q water will be included to be used for the preparation of the rinseate blanks. 

All sample bottles will include frie addition of '®Oz-PFBS, ^^Oz-PFHS, and ^^Cn-PFOS. 1802-PFBS (internal 

standards) at a nominal concenfi^tion of 1 ng/mL. All sample bottles will also include the addition of "C4-PFOS 

(surrogate spike) at a nominal concentration of 0.1 ng/mL. A total of 61 sample bottles will be prepared. 

Page 5 of 6 

Page 35 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment A Morgan County ^^M^i^m)^l^o^ll^tPfd^dl-02 

Amendment 13 

5 Test Methods 

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

Compounds In Water by High Perfbmiance Liquid Chromatography/Mass Spectromefry Direct Injection 

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

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

Chromatography/Mass Spectrometry. 

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

contain isotopically-labeled PFBS, PFHS. and PFOS at a nominal ojncentration of 1 ng/mL. The calibration 

curve will be generated by taking ttie ratio of the standard peak area counts over the internal standard peak 

area counts to fit the data for each analyte. 

Laboratory control samples prepared with the samples must have an average recovery within 100±20% and a 

RSD 520%. The data quality objective for this study is quantitative results for the target analytes with an 

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

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

6 Reporting Requirements 

For each sampling location, the report will contain the results for the sample, sample duplicate, and the two 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 ttie time 

of sample extracfibn will also be reported and used to evaluate the overall method acxnjracy and precision. 

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

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

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

the final report:. 

Page 6 of 6 

Page 36 of 67 
•ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^is^SiPf ^i.? f nS9??f359?diP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

• 

(0 

< 

ro 

< 

B 

">. 

as 

m101123a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -0.00808 x''2 + 1.29 x + 0.0173 (r = 0.9993) 

46-

44-

42-

40-

38-

36-

34-

32-

30-

28-

26-

24-

22-

20-

18-

16-

14-

12-

10-

8-

6-

4-

2 

0-

y 

y 

y ^ 

^ y 

^ y ' 

y ' 

y'' m 

y 

y 

y 

y 

y 

y 

/ / 

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 

Analyte Cone. / IS Cone. 

^ • ^ 

/-""' " 

32 34 36 38 

/-"" ' 

40 

--'" 

42 

'"' " 

44 

^,,-'''' 

46 

• ^ 

48 

f. 

50 

Data worked up by STW 

Printing Time: 11:10:20 AM 

Printing Date: Wednesday, January 26, 2011 

Page 1 of 1 

Page 37 of 67 
••ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^^^g^ff ^^^FHJSgP^falJPPdiP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

• 

ra 

(D 

< 

<D 

a> 

< 

B 

*>0! * 

C 

< 

mIOl 123a.rdb (PFHS): "Quadratic" Regression ("1 /x " weighting); y = 

48-1 

46-

44-

42 

40-

38-

36-

34-

32-

30-

28-

26-

24-

22-

20-

18-

16-

14-

12-

10-

8-

6-

4-

2 

0-

y 

y 

y 

y ' 

y 

y 

y 

y' 

y 0 5 10 15 

-0.00591 x'^2 -H.19 x -H 0.0152 (r = 0.9996) 

"^ 

. 

y 

,^ y " 

,/-"• 

y ' X 

y 

y 

y 

y 

y 

20 25 30 

Analyte Cone. / IS Cone. 

,^' 

y ' 

^ 

35 

^ 

^ ,^-"' 

^ ^ 

40 

,,-^' ' 

,,-•-

• ^ 

45 

.^-'"' 

.---' 

50 

J^ 

Data worked up by STW 

Printing Time: 11:10:34 AM 

Printing Date: Wednesday, January 26, 2011 

Page 1 of 1 

Page 38 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^elf f ^^? f HlSe^^lfs^PaiP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

• 

TO 

0) 

< 

CO 

2 

< 

OJ 

>* TO 

c 

< 

mIOl 123a.rdb (PFOS); "Quadratic" Regression ("1 / x" weighting): y = -0.00973 x''2 + 1.5 x -H 0.251 (r = 0.9992) 

54 

52 

50-

48-

46-

44-

42-

40-

38-

36-

34-

32-

30-

28-

26-

24-

22-

20-

18-

16-

14-

12-

10-

8-

6-

4-

2 

0-

^''' 

X ' 

y ^ 

y'k 

X ' 

y ' ^ 

X 

X y ^ 

y ^ 

y y ' 

y ' 

y ' 

y' 

y 

y 

y 

y 

y 

/ 

0 5 10 15 20 25 30 

Analyte Cone. / IS Cone. 

.--^ 

X^^^ 

'" 

35 

^ 

^--'"" " 

•^' ^ 

40 

^ . " ' 

-"" " 

45 

, ^ 

, — 

50 

Data worked up by STW 

Printing Time: 11:10:50 AM 

Printing Date: Wednesday, January 26, 2011 

Page 1 of 1 

Page 39 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy§iS3g^ff ^^5F^^g55lf3|9g^^5, Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

mIOl 123a.rdb (13C4-PFOS): "Quadratic" Regression ("1 / x" weighting): y = -0.02 x*2 + 0.992 x + 0.0261 (r = 0.9998) 

8.0-

7.5-

7.0-

6.5-

6.0-

5.5-

5.0-

4.5-

4.0-

3.5-

3.0-

2.5-

2.0-

1.5-

1.0^ 

0.5-

0.0: 

• 

^ 

/ • ' 

/ 

/ 

/ 

/ ' 

y 

y 

y 

y 

/ ' 

^ / 

y 

, y 

y 

y 

y 

y 

X j ^ 

/ 

,/ 

y ^ 

y 

^ y y 

y ' 

y ^ 

.' 

y ' ^ 

y " ^ 

,-^'' 

y ' 

^'' 

,..-•' 

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

Analyte Cone. / IS Cone. 

6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 

Data worked up by STW 

Printing Time: 11:11:12 AM 

Printing Date; Wednesday, January 26, 2011 

Page 1 of 1 

Page 40 of 67 
"ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^is^glf f ^^PF^1S95t^f350g^i5l Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

SampteName;-m101123a019- SarT^te rO: "10007-6-8-

PeakName:-13C4-PF0S- Pttess^es):-503.0/80.0 amu" 

I Cor>wnent-1.0n9AnLFC«tdin95%Synth.V*ter/5%ACNFte;-m101123a.wir Annotation;"" 

Concentration : 

C»Unl3i:« d Cone : 

Acq. VAZb-. 

Acq. Ti.T.e: 

H=Ji£ied : 

Proc . Alqorichn : 

Mil.. Pta k Hfiioht 

Hin - Peak Vlidth : 

?noot!iin q Width : 

ST WinJ^jw: 

Expecte d KT: 

O.sS i ng 

ii.SOO nq 

11/2J/201 0 

•:<6:? 3 PH 

Ko 

Int^lliCua n -

: 0.0 0 cf.-E 

0.0 0 sa c 

0 pui n 

30. 0 .•^ec 

15. ? mil, 

OL 

n.l. 

I'.' 

3 

2.105 

2.0.5 

1.9e5 

,.8. 5 

,.7. 5 

1.6e5 

1.5e5 

1.4 ^ 

1.3e5 

1.2o5 

l.leS 

1.0-5 

9.064 

8.0 ^ 

7.0»4 

6.0e4 

5.0e4 

4.0mA 

3.0a4 

2.064 

1.0e4 

15 27 

1 L 

I Sample Name:'m101l233034' Sampto 10; 

PeakNama;-13C4-PFOS' Mass(«s):-S03.' 

I Comnwnt'2ppbLCS/1ppbsun'ogatBLCS" 

•LCS-101115-4- File;"m101123a.wir 

.0/80.0 amu" 

Annotation: " 

Sampl* Type: 

<:*lcuUt« d <. 

0,94 0 nq/nL 

0.9S 0 nq/mL 

11/23/201 0 

9:00:1 8 PM 

PH«>; H^igtit : 

Peak Width : 

.ihini j Width : 

it-lliQu ; 

O.DO 

0.00 

BT Ki ; 

Expflf.pri RT 

Use R«lativ . 

Int . Typfl: 

nr.io 

H«iqlv 

Vslle y 

15. : 

e:7&e i =< 

212000 . < 

15. 1 

lb. 7 

2.1 eS 

ZOftS 

1.9e5 

1.8.5 

1.7«5 

1.665 

1.Se5 

1.4«5 

1.3e5 

1.2B5 

1.le5 

1.065 

9.0e4 

e.0«4 

7.064 

6.0e4 

5.064 

4.064 

3.0*4 

2.064 

1.0*4 

15.24 

L 

14 16 18 

I

Sample Name: "ml01123a048- Sample ID; "LCS-101115-15" FBe;-fn101123a.wir 

Peak Name: -13C4-PF0S- Mass(e5): -503.0^0.0 amu" 

Comment '2ppb LCS ECP Annotalion;"" I

Sample Name: "m10ll23a060- Sample ID; 

Peak Name: -13C4-PF0S' Mass(as): "503.' 

Comment 'OAL GWMCL MW IB 0 101110" 

ampl e Index : £1 

ampl e Type : Vnfcnown 

oiicon t ration : H/A 

alculatf d Cone : 0.097 4 nq/mL 

11/24/201 0 

AC4. • 6:04:i 5 AM 

Mod1i, [lo 

•GLP 10-01-01-13001" Fito;"m101123a.*Mfr 

.0/80.0 amu' 

Annotation; ~ 

Z564 

2.464-

Z364 

2.264 

Min . r«ak Width 

Sn.oothiny Width 

RT Kiiidov : 

E.-.pact«d RT: 

Base T3 Base 

15. ^ min 

95171 counts 

253O0. cp s 

15. 1 min 

15. 5 min 

2.1 e4 

2.064 

1.964 

1.864 

1.7e4 

1.664 

l.Se4 

1.464 

1.3e4 

1.264-

1.1e4 

1.0*4 

9000.0 

BOOa.D 

7O0O.0-

6000.0 

5000.0 

4000.0 

3000.0-

2000.0 

1000,0 

0.0 

16.64 

12 14 16 

Data worked up by STW 

Printing Time: 11:13:20 AM 

Printing Date: Wednesday, January 2 6, 

Page 1 of 9 

Page 41 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^is^g^ff ^^^Fh^g5i5!f3^0g,p Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

• Sample Name: •'ml01123a083" San ^ ID: "Method Blank" Fde:'ml01123a.<Mr 

I Peak Name:-13C4-PF0S- Ma»s<es):-503.0/80.0 amu* 

I Comment: "10 005-229" Annotation;"" 

.^anplt Index : 94 

Simpl f Typo: "nkno-vn 

Concentration : N/A 

Calculate d Cone: 

flr^. D*t« : 

Acq. Time: 

M^Jiri«J: 

Proc. Algorithm : 

Min . P«afc H.;ight 

Min . Faak Hidth : 

Smoothing Width : 

RT VJinduw: 

Expected f<T: 

Use Relativ e RT: 

Inc . Type: 

Retentio n Tin.e: 

Area : 

Haiqht : 

Star t Tirae: 

End Time: 

•; 0 

11/2J/2 

2:06:24 

No 

Incoll i 

1 0.00 

0.00 

0 

.iO.O 

No 

basp To 

15.2 

iI15 5 

soil). 

15.1 

15.4 

1 0 

PM 

\ i a 

B a 

- P 

0.95 0 ng/mL 

ti/A 

11/23/2L'1 C 

J:46:2 J PM 

2.3*51 

2.2*5 

2.165 

2.0*5 

1.9*5 

1.8*5 

1.7*5 

1.6*5 

1.5*5 

1.4e5 

1.3*5 

1.2*5 

1.1*5 

1.0*5 

9.0*4 

8.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4 

3.0*4 

2.0*4-

1.0*4 

15.27 

i T 

I

SampI* Name: -m101123a034- Sample ID; "LCS-IOI115-4' Fll*: -m101123a.w(r 

Peak Name: "MBPFOSflS)- Mass{e»); "507.0/80.0 amu" 

Comment •2ppb LCS/1 ppb sunngat* LCS- Annotation;' 

Sampl e Index : i ^ 

Sample Nam*;-mIOl 1238048- San^ID : •LCS-101115-15- Fi«e:"m101123a.iMr 

Paak Nam*: -M8PF0S(ISr Mass(es): -507.0ffi0.0 amu" 

Comment •'2ppb LCS ECF" Annotation;"" 

tion : 0.54 4 

Calculate d Cone : N/A 

Arq . Ddt« : \l/2:/2i . 

Ac'.j. Tine : S:CO:l a 

M-'difit-d: ¥e j 

Proc . Algorithm : Intelli t 

Hin . Peak: Height : 0.0 0 

Min. real : Hi^tii : 0.0 0 

.'!^rt>othi.^g Vlidth : 0 

RT Wi:idrji.-: 30. 0 

Etf.act5 d RT: 15. 3 

I'se Relativ e BT: No 

ny/r 

6e-00 5 cp s 

15. 1 mill 

15. 0 n,in 

Sample Type: 

Calculatn d Cone: 

Acq. [Mte : 

AC'j. Tima: 

M.jdlfibd : 

Proc . Alocrithr.. : 

Hin . Peak Heigfit 

Hin . Peak Widtli : 

Sn.oC'thina Width : 

RT Kindu-v: 

E-nactaU RT: 

Use Relativ e RT: 

Int . Type: 

R.ttntio n Tir,*: 

Area : 7 

H«iqhr: 

oc 

0.955 

H / A 

n/24/21M 0 

1:53:27 AM 

Y « S 

lnt«!!iQ'J a 

0.00 

0.0 0 

0 P 

1-0. n 

15.3 

N o 

Valle \ 

15.2 

75S2 cou 

.S43'005 

1.9*5 

1.8*5 

1.7*5 

1.6*5 

1.5*5 

1.4*5 

1.3*5 

1.2*5 

1.1*5 

1.0*5 

9.0*4 

6.0*4 

7.0*4 

6.0*4 

5.0*4 

4.0*4 

3.0*4 

2.0*4 

1.0*4 

15.23 

L 1 

Data worked up by STW 

Printin g Time: 11:13:2 0 AM 

Printin g Date : Wednesday, Januar y 26, 2011 

Page 2 of 

Page 42 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^|?38iff ^^P f K|ag5,5lf3l|Op^ip Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Proc . 

Min . 

Kmu^jt 

RT VI i 

Expa^ 

Algorithm : 

^eal: Hpi(3ht: 

l-saK Hidth : 

•.iiig Width : 

ted RT: 

Inte l lit ' 

0.00 

O.QO 

0 

.^O.C 

15.3 

.in -

c p = 

m m 

I

Sample Nam*; "011011233060- Sample )0: "GLP10-01-01-13-001' File; "m101123o.mifr 

Peak Name: -M8PF0S(!S)" Mass(es): "507.0/80.0 amu" 

Comment "DAL GW MCL MW 1B 0 101110' Annotation: "" 

£in[>le Typp: Mnkno'^n 

,1.560 ng/ri,L - _ 

N/A ^-^ ^ 

11/24/2010 

6:04:i 5 AM 1 •8«5 

YG3 1.7e5 

1.6*5 

1.5*5 

1.4*5 

1.3*5 

1.2*5 

1.1*5 

^ l.OeS 

a 

I 9.0*4 

8.0*4 

7.0*4 

6.0*4 

5.0e4 

4.0*4 

3.0»4 

2.0*4 

1.0e4 

Hfii.jht : 

St^c t Tit 

End Time: 

0.0 

12 14 16 

I

SamplB Name; "mlOl 123a083" Sample ID; "Method Blantc" Fite; -m101123a.wir 

Peak Name: "M8PF0S<IS)" Mas5(*s); "507.0/80.0 amu" 

Comment "10.005-229" Annotation;"" 

iarafjl*^ Index : 84 

iample Type: Unkncvn 

:oncenrtitiori : 0. 950 ng/mL 

;alculat6 d Cone: H/A 

•«3i: Hiiqh t 

'ea k Widrh : 

dn<j Width : 

• eri RT: 

3.0*5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0e5 

1.8*5 

1.6*5 

1.4*5-

1.2*5 

1.0*5-

8.0*4 

6.0*4 

4.0*4 

Z0e4 

1523 

» 

12 14 16 

I

Sample N3me:-m101123a019" Sanpl* 10: "10007-6-8" 

Peak Name; "MPFBS{IS)- Mas&(es): "303.0/84.0 amu" 

Comment "1.0 ng/mL FC sld in 95% Synth. Wat*r/S%ACN" 

Cilcrjlateri 

Acq. D,,t«; 

Acq. Tims : 

FBe:-m101123a.» 

Annotatiofi:"" I

Sample Name; "ml01123a034- Sampte ID: •LCS-101115-4" File; "m101l23a.wi«fr' 

Peak Name; "MPFBS{[S)" Mass(*s); -303.a«4.0 amu" 

Comnwnt "2ppb LCS/lppb tuffogate LCS" Annotation:"" 

0 . 7 5 

N / A 

11/ 2 

3:4 6 

/ 2 

' ¥« s 

Int e 

0 

10 

PH 

UOua n 

0 0 c 

?n,oothinq HiRT Window: 

Exp^ctsd RT: 

4.0*5 

3.6*5 

3.6*5 

3.4*5 

3.2*5 

3.0*5-

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0*5 

1.8*5 

1.6*5-

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4-

4.0*4 

2.0*4 

12.61 

L^ 

p i e Type : 

culate d C 

. Date : 

. Tirae : 

ified : 

c . Al^cr i 

. Pe.3k He 

. Peak Wi 

orhin y Wi 

Window: 

«CtsJ BT: 

Relativ e 

. Type : 

entio n Ti 

J : 

Qhr: 

r t Tim«: 

Time : 

n c 

hra 

gh 

til 

T h 

RT 

., 

Q C 

0.95 5 

H/A 

n g ,. 

11/23/201 0 

S:0O:i e PH 

Y s 3 

IntelliQ i 

: 0.0 0 

I'O.O 

12. 6 

N o 

Valle y 

12. 6 

1712574 CO 

3.S4.3-005 

12. 4 

13. 3 

an -

c p s 

pcjint 

m i n 

. . n 

lints 

c p s 

rain 

rain 

raL 

l O A 

^ 

t 

3.6*5 

3.4*5-

3.2*5 

3.0*5-

Z8e5 

2.6*5-

2.4e5 

2.2*5 

2.0*5 

1.4eS 

1.2*5-

1.0*5 

8.0*4 

6.0*4 

4.0e4 

2.0*4 

16 18 

0.0-

12 14 

Data worked up by STW 

Printing Time: 11:13:21 AM 

Printing Date; Wednesday, January 26, 2011 

Page 3 of 9 

Page 43 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analym8l?f ^Ya?f nag^'JfslOaff Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Pro= . Algorithm : 

Miti- pMak Height : 

Min . PaaV WiJtti : 

Smoothin g Wirtth: 

RT VJinduw; 

Expecte d RT: 

Vsa Relativ e BT: 

Int . Tipe : 

Retantio n Tlrae: 

Atoa : 1S7 

H«i^tit : i 

IntflliQua n 

0.0 0 c 

0.0 0 s 

0 y.a 

30. 0 3 

1?. S m 

No 

Valle y 

1 i . S n. 

717a cou n 

.S6«-00 5 CF 

• Sample Name; •m101123a048" Sample ID:'LCS-101115-15" FH*;-m101123a.wir 

I Peak Name; -MPFBS(IS)- Mass(*s}: -303.0«4.0 amu' 

I Comnn*nt: "2ppb LCS EOF" Annotation:"-

.-amplt Indar : 45 

aispl f Typn; vc 

C-~n'-entracion: O.STO ng/r.L 

Caic.i!ar« d Cone: N/A ^•^' ' 

Af^. D-tt^: 11/24/2010 

Acq. Time: 1:53:: ' AM 3.4*5 

3.2*5 

3.0*5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

&. 2.0*5 

» 1.8*5 

- 1.6*5 

1.4*5 

1.2*5 

1.0*5 

6.0*4 

4.0*4 

2.0*4 

0.0 

I

Sample Nam*; 'mIOl 123a060- Sampte ID: -GLP10^1-01-13-001- FOa; "mlOl 123a.wir 

P*ak Nam*: 'MPFBSdS)- M3Ss{*s}; "303.0/84,0 amuComm*nt "DAL GWMCL MW IB 0 lOIHO' Annototkin: -

SatTf-le lr,de}i: Gl 

Concentration : 0.97 5 n'j/ni 

x-Lj. LMte: 

jmoothinq Width 

KT Window: 

Eipec-ed ftT: 

it^Uiptjai i - IQA 

0.00 cps 

0.0 0 s«c 

3.2*5 

3.0*5 

2.8*5 

^6* 5 

2.4*5 

2.2*5 

2.0*5 

1.6*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4-

4.0*4 

Z0*4 

0.0 

16 18 

I

Sample Name: 'm1011233083' Ssm; ^ ID: 'Method Blank" Fie: "m101123a.wir 

Peak Name; -MPFBS(IS)- Masses): '303.0/84.0 amu' 

Comnwnt: "10 005-229" Annotalion;"" 

Cili:ul.--tnd Cone: N/A 

flc^. D-.t«: 11/24/2010 

AC-J. Ti!l,s: 2:06:: 4 PH 

Proc. Algorithm : Intelliiua n - I^A 

Min . peak Height : 0.00 cps 

Hin . Tdak. Hidth : 0.00 sec 

."imoothinq Width : 0 point s 

RT Kiiid.ju: 20.0 E«C 

V'5e R-iativ e FIT: No 

Int . Tipe : Valle y 

Retentio n Time: 12.8 mil. 

Area : 1545643 count s 

Hoiqht : i.70n'00 5 cps 

End Tiae : 13.2 n,in 

& £• 

3.6*5 

3.4*5 

3.0*5 

2.8*5 

Z6*5 

2.4*5 

2.2*5 

2.0*5 

1.8*5 

1.6*5 

1.4*5-

1 A 5 

1.0o5-

8.0*4 

6.0*4 

I

SampI* Nam*;-m10n23a019' Sampto ID; "10007-6-8" 

Paak Name: "MPFHSdSr Mas*(*»); '403.0B4.0 amu" 

Comm*nt "1.0 ngftnL FC std in 95% Synth. V\bter/5%ACN" 

sample Type: Standard 

0.94 5 ri'j/raL 

ite d ; N/A 

Acq. Dac^: 

Acq. Time: 

tloditied : 

Proc . Alv^t-cithm: 

Min . Peak Height : 

Min . Pfcat Widrh : 

Sraoothinq Width : 

RT Kindo-*: 

E-p£Ct5d RT: 

L'se Relativ e RT: 

Int . Type: 

R-tentio n Time: 

H3ig.-,t: 1 

End Time: 

1/23/2010 

: 46:23 PM 

N o 

ntelli'J.ia n -

0.00 cps 

0.00 sec 

0 poin t 

:-0.0 s«c 

14.3 min 

Ho 

Valle y 

14.3 rain 

442 count s 

57.S.005 cps 

15.0 min 

I D A 

' 

& 

f 

3.4*5 

3.2*5 

3.0*5 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0*5 

1.8*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

16 16 

Data worke d up by STW 

Printing Time: 11:13:21 AM 

Printing Date: Wednesday, January 26, 2011 

Page 4 o f 9 

Page 44 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^^s^g^ff ^^^Fh^g5i^f3|9P^i5, Groundwater Samples 

Morgan County Landfill. Decatur. AL - November 2010 

r

Sampla Name; "ml01123aO34' SampI* ID; "LCS-101115-4" File; "m101123a.wifr 

Peak Name; -MPFHS<IS)" Ma»s<*s); '403.0/84.0 ami/ 

Comment '2ppb LCS/1 ppb eurrogala LCS" /Annotation: 

Sample Indoy : 35 

S^!T.f>le Type: yc^ 

Concenitition : .1.925 nq/oiL 

Cal-;'i;at.ed Cone: N/A 

Af4 . DrfC«: l]/2;-/201 0 

Acq. Time: 9:00:l e PM 

Proc . Algoritli:r.: IntPlli'Ju . 

Min. Pwak H.>iij|-]t: 0.0 0 

Min. Peal: Ui-ith : 0.0 0 

Smuijthinq Width ; 0 [ 

RT Wind.)v: iO.C 

Expecte d RT: 14. i 

Use Relativ e RT: Ho 

Int . T\pe ; Valle y 

Betentio.-i Time : 14 . i 

Area : 137 i97 5 coi 

Height : J.27«.&C5 

Jtsr t Tine ; 14. 1 

End Tim3 : 14. 9 

Sample Nam*; "ml01123a048" Sample ID:'LCS-IOIIIS-IS' File:'m101123a.wjfr 

Paak Nam*: *MPFHS{ISr MaM(*»): "403.0ffl4.0 amu" 

Comment "2ppb LCS ECF" Annotation; ~ 

Sample Typo: C.KT 

calculate d Cone : Il/A 3.3,5 

Acq. L'-ta: 11/24/2010 

Acj. TimB: 1:52:27 AM 

3.0*5 

"^ 2.6*5. 

2.6*5-

Z4*5 

2.2*5 

Z0*5 

a. 1.8*5 

I 1.6*5-

I 

1.4*5 

1,2*5 

1.0*5 

8.0*4 

6.0*4' 

4.0*4 

2.0*4 

Pcou . Alqcrith m 

Hin . P«3k Heigli 

Hin . P«ak Widrn 

Smootninrj wijc h 

RT Kjnd!;-J: 

Expecte d RT: 

Use Relativ e ST 

Int . Tvpo : 

Ratsntior , Time : 

Acaa : 1 

H-.iqt,t: 

Star t Tin,*: 

iritelU Q 

: 0.0 0 

0.0 0 

C 

;-o.o 

IJ .3 

Ho 

7a[le i 

14. 3 

60633 =C 

3..'l.i»0C5 

11. l 

0.0 

I

Sampte Name; "m101123a060' Sampta ID;'GLP10-01-01-13<»1" Fil*; •m101123a.vi(ir 

Peak Name; -MPFHS(IS)- Mass(*s); "403.0/84.0 amuCommenL"D/y.GWMCLMW1B 0101110" Annotation: ~ 

Sampl e Index : 61 

Concen t ra t i-in: 0.S4 5 ny/n-.L 

Calculater i Cone : N/A 

Ac-q. Dat.:: 11/24/201 0 

Ac^ . Tir^£: 6:04:3 5 AH 

Area : 1225S52 counts 

Height : 2.95e»00 5 cp s 

Star t Tima : 14. 1 min 

EnJ Time : 14. 9 n.in 

s 

2.8*5 

2.6*5 

2.4*5 

2.2*5 

2.0*5 

1.8*5 

1.8*5 

1.4*5 

1,2*5 

l.OeS 

8.0*4 

6.0*4 

4.0*4 

2.0*4 

14 25 

L 

I

SampI* Name; -m101123a083- SampI* ID; "M*thod BlanK" Fil*; 'm101123a.wifr 

P*sk Name: "MPFHSflSr Mas«(*a); •403.0fi4.0 amu" 

Comm*nt "10 005-229" Annotation; "" 

Sample Inrtex: 94 

Sample Type; Vnknowti 

Concentrar ion : 0.94S n^/mL 

Calculate d Cone: rl/A 

Acq. Vit-. : ll/24/2in O 3.8*5 

Acq. Time : 2:06:2 4 PH 

3.6*5 

I1-.3dilie.l: Ho 

Proc . AlocritMiT,: intelliOJ^ n - IQA 34^5 . 

Mill, peak Height : 0.0 0 t-ps 

Min. P*. k Widr.^: 0.0 0 ,e c ^^^^ ^ 

Stficjothino Hidrn : 0 point s 

RT Kitidu-v: :T.. 0 S^C 

E.-f.«cted BT: 14. 3 min 3.0*&-i 

li*e Relaci-/s RT: Mo 

2.8*5 

Int . Type : /alU i 

R-tontio n Ti=e : 14. 3 min Z6* 5 

2.4*5 

I 2.2*5-

'\ ZOeS-

; 1.8*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5-

8.0*4 

6.0*4 

4.0*4-

2.0*4 

IS52745 co(ints 

3.ESe-O0 5 cp s 

14. 1 min 

0.0 

12 14 

Data worke d up by STW 

Printing Time: 11:13:22 AM 

Printing Date: Wednesday, January 26, 2011 

Page 5 o f 9 

Page 45 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Anafy^^^g^ff ^^|FHtag?<ilf350p^i5i Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

(

Sample Name: •m101123a019" Sarrvle ID; -10007-6-8" File: "mlOl 123a.wir 

Peak Hume: "PFBS" Ma5«(*s); "299.0ffi0.0 amu,299.Qf99.0 amu' 

Comment; "1.0 ng/mL FC std in 95% Synth. \ftfat*r/5%ACN' Annotation; "" 

FampLe Indt./.: 20 

Sampl e Typ» : itandar d 

Concentration : ?.S9 5 ng/mL 

Cal'jiilate d Cone : 1.07 ncj/ml 5: 

Ar-ij. Dat*,: ll/2;"/201 0 

Rela--iv e RT 

Tlpe : 

ntio n Time : 

: 2.. 

lir: 

4. 

55 

No 

lanua l 

12. 6 

2«1 

4000 . 

8- 3.0*5 

I

Sample Nanfie:"ml01123a034" SampI* ID: "LCS-101115^1" Fito; "m101123a.iMr 

Peak Name; "PFBS" Mass(es): "239.0/80.0 amu,299.0/99.0 amu" 

Comn^nt "2ppb LCS/lppb sun-ogate LCS* Annotalion; 

1.5G nq/raL 

1.B5 ng/mL 

1/23/201 0 

•: 00:1 8 PM 

I

Sample Name: "m10n23aO48" Samph ID:'LCS-IOI 115-15' FBe:'m101123a.wir 

Peak Nam*: "PFBS* Ma5s{*s); "299.0/80.0 amu,299.0/99.0 amu" 

Comment "2ppb LCS ECP Annotation;'" 

S.'imple Type : QC 

Concentration : 0.0 0 ng/mL 

Calculate d Cone:: 0.016 0 ng/mL 

Ac-,?. Date : 11/24/201 0 1,5*4 

Ac-j. Ti=is: 1:53:27 AM 

No 

Intellig i 

: 0.0 0 

0.0 0 

12. S 

6J4S2 cc 

1S200 . ; 

12. 5 

12.B 

1.3*4 

1.2*4 

^ 8000.0-

- 7000.0 

6000.0-

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 L 

[

Sample Name: -m101123aD60' Sample ID: 'GLP10-01-01-13-001' File; 'm101123a.vKfr 

Paak Name: "PFBS" Mass(*s): "299.0/80.0 amu.299.0/99.0 

Comment 'DM . GWMCL MW IB 0 101110" Annotation; 

Cancentratlon : N/A 

Calculate d Cone : 1.SB i 

Acq. L-ato: ll/24/2i^l O 

ACfj. Time : 6:04 : i h AH 

H-:;dified: Yes 

RT Windo-J: 30. 0 si 

Expecte d RT: 12. 6 m 

Use Relativ a BT: No 

Data worked up by STW 

Printing Time: 11:13:22 AM 

Printing Date: Wednesday, January 26, 2011 

Page 6 of 9 

Page 46 of 67 
••ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analyas38i§f ^^^ f H|a955'f3l??diP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

•

Sample Name; •m101123a083" SarT^I* ID; •M*thod Blank" File; 'm101123a.wir 

Peak Name; "PFBS" Massjes); -299.0/80.0 ami 

Comment: '10 005-229" Annotation: •" 

-''araplo lndu>:: 34 

Sample Type: Unkno-wn 

Con'-entration : N/A 

Calculate d Cone: •; 0 

Ar-.]. Dat« : 

Acq. Time : 

HcJitiud : 

Proc . Algorithm : 

Hin . P«al; Heigh t 

Min . Peak Hidth : 

Smoothin g Hidth : 

RT Window-; 

Expecte d RT: 

U3B R«lativ e RT: 

Int . Type : 

Retentio n Time : 

Area : 

H«ight : 

Ctar t Time : 

End Time : 

11/24/ 2 

2:06:2 4 

No 

Intell i 

: 0.1)( 

O.O i 

30. 0 

12. i 

No 

Valle \ 

12.1 

LOSl! 

250D. 

12. 5 

12. 7 

Oil) 

PM 

poin t 

min 

coiint.f 

t p s 

min 

:oA 

I

SampI* Nam*; "mlOl 1233019" Samf ^ ID; "10007-6-8" File: "m101123a.w4ir 

Peak Name; 'PFHS' Mass(es): '399.0/80.0 amu.399.0/99.0 amu" 

Comm*nt '1.0 ng/mL FC std in 95% Synth, Water/SWACN" Annotation; " 

S.imple Typ-: 

calculate d Cone 

Ac;j. Catu : 

Acq. Time : 

H-jdi fifed: 

Proc . Algcrith n 

Koia e Percentag e 

Ba?e . Sob . Mindo 

Standar d 

1.00 

1.07 

11/23/201 0 

3:46:2 3 PM 

No 

Intellipua n 

: SO 

w: l.O I 

P-ijV.-Spllt . Factor : i 

Repor t Litr:)« = t 1 

I'^in. Peak Heigh : 

Min . P«ak Widt h 

Sniootliinvi Widt h 

RT Window: 

E.".pect«d RT: 

Use Relativ e RT 

int . Typ* : 

Retentio n Time : 

eak : Wo 

: 0.0 0 

0.0 0 

0 

30. 0 E 

14. 3 n 

No 

Bas e T3 Bas 

14. 3 m 

Ataa : 2024754 -c^-m 

Height : 454000 . cp s 

nq/mL 

ng/mL 

- My 

min 

c p j 

s u e 

p c 

n 

n 

3 

I

Sample Nam*; "m101123a034' San^jl* ID; •LCS-101115-4- File; "m101123a.wifr 

P*ak Name: "PFHS' Mass(*s); "399. 

Comm*nt; "2ppb LCS/1 ppb surrogate LCS" Annotation: 

Calculate d ! 

Acq. Date : 

I

SampI* Nam*; "ml01123a04r Samfrf* ID; 'LCS.101115-15" F8e; "m101123a.wifr 

P*ak Nam*: 'PFHS" Mass(es); '399.0/80.0 amu,399.0/99.0 amu" 

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

Sampl e Index : 49 

QC 

n-j/mL 

Sample Type: 

C(jncontration : 

Calculate d Cone 

Acq. Date: 

AC). Time: 

M-iditied : 

RT Windo-j: 

Expected RT: 

QC 

0.00 

0.124 

11/24/2010 

1:53:27 AH 

Yss 

•0.0 

14.3 

Data worked up by STW 

Printin g Time: 11:13:2 2 AM 

Printin g Date : Wednesday, Januar y 26, 2011 

Page 7 of 9 

Page 47 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy§is^8lff ^^^lf^iS9?^f3l9?di5' Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

I

SampI* Name;-ml01123aO60" Sample ID; "GLP10O1-01-13-001" File:"m101123a.wrfr 

Peak Name: 'PFHS" Mass(e6): "399.0/80.0 amu.399.0/99.0 amu" 

Comment; "DAL GWMCL MW1B 0 101110" Annotation; "" 

ampl« In. 

Concen t ra t ion : N/A 

CaKiilate d 

Ac:). Date : 11/24/20 ! 

Acq. Tin,6: £:04:.' S ; 

MjJified : Yes 

RT Window: 30. 0 

Expjict^d RTi 14. ? 

Use Relativ e RT: Ho 

I:jt . Type : Manual 

!ketentio n Time : 14. 3 

Area : 4(4393 2 ct 

Hfei-jht: B59000. . 

Star t Time : I'-. t 

8.5e5 

8.0*5 

7.5*5 

7.0*5 

6.5*5 

e.OeS 

5.5*5 

S.OeS 

4.5*5 

4.0*5 

3.5*5 

3.0e5 

Z5e5 

2.0e5 

1.5*5 

1.0*5 

5.0*4 

14.25 

1 

14.11 

1 , 1 , , 1 1 1 • 1 • • ^ ^ 

14 16 18 

SampI* Nam*: "m101123a083' SampI* ID; "Method Blank" 

I

Paak Nam*: 'PFHS' Mass(*s): "399.0/80.0 amu.399.0/99.0 

Commant'10 005-229" Annotation;TM 

Sampl e Indo;<: Bi 

Sampl e Type : I'nknown 

Concentration : H/A 

Calculate d Cone : ^ 0 

Ac;]. [.Mtu: 11/24/201 0 

Acq. Tima : 2:06:2 4 PM 

6000 

H-jdi 

Proc 

Ba^e 

P..aK 

R'fpc; 

Mi.-i. 

Hin . 

SltiOO 

KT K 

liod : 

Alge r 

EutJ 

-iJpl i 

r t La 

Pea k 

Peak 

rhin o 

ndo-v 

tlim: 

taqe : 

Factu 

g«=t Pe 

Height : 

W 

14 

dth : 

dUi : 

5500 

14759 jaunr : 

4 900 . CP5 

IJ. 2 mir 

16 18 

I

Sample Name; "ml01123a019" Sanple ID: "10007-6-6' File: 'ml01123a.wifr 

Peak Name: "PFOS' Mac£(es}: "499.0/99.0 amu.499.0/80.0 amu,499.0/130.0 amu" 

Comment; '1.0 ng/mL FC std in 95% Synth. VUatmy5%ACN' Annotation: 

Sample Index : 20 

Sanple T-.-pe: Standard 

Concentration : 0.395 ng/mL 

Calculate d Cone: 1.05 ng/mL 

Acq. D;.t.): Il/2;/2;31C 

Expecte d RT: 

Use Relativ e RT: 

Int . T^p« : 

Retentio n Time : 

Area : 1645 

Hfeight: 3= 

15 

No 

Va!l 

i ; 

457 

Jcoo 

I

SampI* Nam*; •ml0n23a034- SampJelD: •LCS-101115-4" Fil*; 'ml01123a.wir 

Peak Nam*; "PFOS" Mas*<*6): •499.0ffi9.0 emu,499.QreO.O amu.499.0n 30.0 amu" 

Comment '2ppb LCS/lppb sutTogato LCS" Annotation:" 

Sampl e Inden : 35 

Sample Type: 

Concentration : 1.56 irj/mL 

i.c-e nq/mL 

Acq. Dat» : 

Acc). Tima : 

14,>di£ied: 

RT Kindo-v: 

Expecte d RT: 

Use Relativ a 

Int . Typ^ : 

Retentio n TJ 

Area : 

Height : 

RT 

ll/?5/2l?1 0 

5:00:i e PH 

Yea 

30. 0 

15. 3 

tio 

Manua l 

IS. 2 

263125 5 -ou 

613000 . r.p 

& 

i 

1 

6.0*5 

5.5*5 

5.0*5 

4.5*5 

4.0e5 

3.5*5 

3.0*5 

2.5*5 

Z0*5 

1.5*5 

1.0*5 

5.0*4 

15 25 

i y \ ^ . . 

14 16 IB 

Data worked up by STW 

Printing Time: 11:13:23 AM 

Printing Date: Wednesday, January 26, 2011 

Page 8 of 9 

Page 48 of 67 
*ETS-Mary Ann 

Attachment B 

GLP10-01-02; Interim Report 13 

AnalymSief ^..^ f ha9?5'f3|OaiP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

r

San^eName:"m101123aO48* Sample ID:" 

Peak Name: "PFOS' Mas*(ee): '499.0/99.0 ai 

Comment "2ppb LCS ECF" Annotation:" 

1.9T 

RT Window: 

Exp^cf d RT: 

U.ve Relativ e fiT: 

nq/r 

5.0*5 

4.6*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 

3.0a5 

2.8*5 

2.6*5 

2.4*5 

2.2*5-

2.0*5 

1.8*5 

1.6*5 

1.4*5 

1.2*5 

1.0*5 

8.0*4 

6.0e4 

4.0e4 

2.0*4 

0.0 1 -£t_ 

I

SampI* Name: "mlOl 123a083" Sample ID:" 

Peak Name: "PFOS' M*s«(*«): "499.0/99.0 ai 

Comment "10 005-22?" Annotation: ~ 

Sampl e I n 

I

Sample Name: "ml011233060- Sample ID: "GLPIOOl-OI-lS-OOr File:-m101123a.v«fr 

Peak Nam*: "PFOS" Mass(*s): "499.0/99.0 amu.499.0ffi0.0 amu,499.0/130.0 amu" 

Comment "DAL GW MCL MW 1B 0101110" Anrwtatkin;"" 

imple Type; 

oncGiT. id t i( 

alculate d ' 

L'nkncwn 

N/A 

6.2 9 t 

11/24/201 0 

Kelative BT: 

. Type: 

a: 12 

qht: 

rt Time: 

Time: 

Ho 

Hrfnual 

15.: 

47047 

05^-00 0. 

14.7 

15.e 

9.5*5 •) 

9.0*5 

8.5*5 

8.0*5 

7.5*5-

7.0*5 

6.5*5 

6.0*5 

5.5*5 

S.OeS 

4.5*5 

4.0*5 

3.5*5 

3.0*5-

2.5*5 

2.0*5 

1.5*5 

1.0*5 

5.0*4 

0.0 

T-.-pe: 

,tn d COI 

H.-.Ji£ied : 

RT Windfjw: 

Expecte d RUse Relati ' 

N/A 

0.13 1 ng/mL 

11/24/701 0 

15. 2 

nooo. I 

1.10*5 

1.05*5-

1.00e5 

9.50*4 

9.00*4 

8.S0e4 

8.00e4-

7.50e4 

7.00e4 

6.50*4 

J 6.00*4 

=• 

^ 5.50*4 

S 

= 5.00*4 

4.50*4: 

4.00*4 

3.50*4 

3.00*4 

2.50*4 

Z00e4 

1.50*4 

1.00*4 

5000.00 

• 0.00 10 12 1Jj 4 16 1 L 8 

Data worked up by STW 

Printing Time: 11:13:23 AM 

Printing Date: Wednesday, January 26, 

Page 9 of 9 

2011 Page 49 of 67 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 13 

AnalymSlff ^*? f H^S^^illPPdiP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

g101215a.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting); y = -0.0512 x'^2 + 1.74 x -^ 0.019 (r = 0.9995) 

/.a 

7.5-

7.0-

6.5-

6.0-

5.5-

5.0-

4.5-

4.0-

3.5-

3.0-

2.5-

2.0-

1.5-

1.0-

0.5-

0.0-

^ * ' 

0 

. > 

X^ 

y' ' 

, • " 

y 

y 

,^' 

./' 

,.. / 

/ ' 

^ 

y 

y 

y X 

y 

y 

y 

y ' 

X' 

X 

^/-""' 

,-

y ^ y 

X ' ' 

'-'^ 

^ X 

, y 

^^.-•4 

-^'"^ 

0.0 0.5 1.0 1.5 2.0 2.5 3.0 

Analyte Cone. / IS Cone. 

3.5 4.0 4.5 5.0 

Data worked up by STW 

Printing Time: 11:14:33 AM 

Printing Date: Wednesday, January 26, 2011 

Page 1 of 1 

Page 50 of 67 
Ginger AG01330509 

Attachment B 

GLP10-01-02; Interim Report 13 

AnalyiEStff ^^PlfH^gp^fs^Op^iji Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

Data worked up by STW 

Printing Time: 11:14:56 AM 

Printing Date: Wednesday, January 26, 2011 

Page 1 of 1 

Page 51 of 67 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^iA^g^ff ^^^FH^gy^fj^pgjjp Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

• Sample Name; "gl0l2l53019- Sample ID; ' 

I PeakName;"l3C4-PFOS- M3ss(es): 

10007* ^ Fil.:-s101215>.»r 

•503.0/80.0 amu" 

• Comment "1.0 ng/mL FC std in Synlti. Watet" 

?air.ple Inde/ : 19 

Sample Typ-: standar d 

Cancantration : 0.00 ny 

Calculate d Cone: < 0 

Acq. Uatij: 12/15/20U> 

Acq. Time: 1:12:30 PM 

rr.JC. Algr,irlthm; Inte l !:'^i:an -

Min . pHak H«i(jht: O.&O cp= 

Min . Peak kiidth : 0.00 sac 

FmtJ'jtluncj (lidth : 0 pui n 

RT Window: JO.O sec 

Us* Relativ e RT: No 

Int . Typ*.: Valle y 

Retentio n Time: 12. J min 

Area : 5B60 count s 

Star t Time: 12.2 min 

End Tim-.: 12.5 min 

mL 

ICJA 

3 

A/fnotat»n:"" 

& 

-^ 

1400 

1200 

1000 

900 

iiiL.iiLl. ,1^. m i|..i,u.4t.tJi 

12 13 14 15 16 17 

•

Sample Name; 'glOIZlSaOSr Sarr ^ ID; 'LCS-101215-2' File: -g10121Sa.wir 

Peak Name: -13C4-PFOS" Masstles): '503.0/80.0 amu~ 

Comm*nt '0.2ppb LCS' Anrwtation;"" 

Samfile Indiit : 64 

Sajipl- Typ- : 

V 0 

nq/7iiL 

1.49e-00 i 

12. -

i;. 5 

I

SampI* Name; 'gl01215a0e6' Sample ID; 'LCS-101215-6" File; "g101215a.wff' 

P*ak Nam*; '13C4-PFOS" Mass(**): '503.0/80.0 amu* 

Comment'"0.2ppb LCS ECP Annotation: " 

0.0 0 ny/niL 

12/lf/201 C 

1350 

1300 

1250 

1200 

1150-

1100 

1050 

1000 

600 

550-

350; 

300 

jJUJiiJii k i 

6.50 7 

I

SampI* Nam*; "g101215a02r Sample ID:"GLP1(W)l-02-

P*ak Name: •13C4-PFOS" Mass{*s); "503.0/80.0 

Comm*nt-D/U.GWMCLMW3B0101110- Annotation: 

ample Index : 26 

Acq. Pate 

Ac^ . Tima: 

It/A 

0.004 6 

12/lb/ Z 

J:^4 : 23 

IIo 

10 

PM 

IntclliOu a 

0.0 0 

Saoo t 

RT Wi 

E-pe c 

I'se P 

Int . 

R?te i 

Heigh 

End T 

hin u 

,tia:. 

t a d 

Type 

tio n 

Tinine : 

W 

;T 

I V 

1 

'illiiiliiiii ilAitiihiiirii 

Data worked up by STW 

Printing Time: 11:16:51 AM 

Printin g Date : Wednesday, Januar y 26, 2011 

Page 1 of 4 

Page 52 of 67 
*** Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 13 

Analyf^giff §^^^f H|^95.gf5|Og^i5. Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

I

Sample Name: "g10121SaO39- Samfrfe ID: "10 01O-39' Fite; •g101215a.wir 

Peak Name -13C4-PFOS" Mass{es): "503.0/80.0 amu' 

Comment: "Mettwd blank" Annotation: "" 

."^arnpla Index : "3 9 

C:^ncenrtJriQn : U/A 

c:alculat* d cone : -; 0 ^ ^ 

Ac;). Djtn : 12/15/201 0 

Acq. Time : 7:12:3 J PM 

1500 

Proc . Algorithm : InteiliCua n - K]A 

Min . Ppak Height : 0.00 cps 1400-

Min . PeaK Width : O.OO st c 

Smcothiii q Width : 0 f-'ii-ts ^-^QQ. 

Ejjpacte n RT: 12.-- rain 

Use Relativ e RT: tio 1200 

1000 

57&5 c 

1. s;.a+&0.' 

12. 3 

900 

I

Sampte Name; •gl01215a019" Sample ID: "10007-6-8' File: "gl01215a.vwr 

Peak Name; "MSPFOSflS)' Mass(es): '507.0/80.0 amu" 

Comment "1.0 ng/mL FC std in Synth. Water Annotation: "" 

9.0e4 

8.5*4 

8.0*4: 

7.5*4 

7.0*4-

6.5*4 

6.0*4-

5.5*4 

5.0*4 

4.5*4 

4.0*4 

3.5*4-

3.0e4 

2.5e4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

H.<Lght: 

Stat t 1 

End Tir 

0.0 -.^^^ ^ '•]3-7A 

10 11 12 13 14 15 16 17 

(

Sample Name; "g101215aD83" Sampte lD;"LCS-101215-r File; "g101215a.wir 

Peak Name: "M8PF0S(IS)" Mass(«s); "507.0«0.0 amu" 

Comment "0.2ppb LCS" Annotation: ~ 

SampI e Type : yC 

Cfncantra t 

Cal.tulate d 

AcL]. Dat«: 

Acq. Time: 

Mr.Jified : 

RT Window: 

Exoectcrj Ik 

cCn. 

0. 95.' 

N/A 

12/lf/201 C 

5:57:0 5 PL' 

30.0 

13.1' 

ny 

, . c 

ml 

7.5*4 

7.0*4 

6.5e4 

I

Sampte Name: "g101215a086" Sampte ID; 'LCS-1D1215-e" Fite: 'gl01215a.iMr 

Peak Nam*; "M8PFOS(ISr Mass(*s): '507.0/80.0 amu* 

Comment "0.2ppb LCS ECP Annotation: "* 

Sampl e Inoex : 97 

Sampl e Type : 

Height : 

5t.st t Tir 

EnH Time: 

0.95 3 

N/A 

12/15/201C 

S:51:1 2 PM 

Manua l 

•: i:. e 

3T2e07 -• 

12. 7 

ng/ i 

7.5*4 

7.0*4 

6.5*4 

8.0*4 

5.5*4 

5.0*4 

4.5*4 

4.0*4 

3.5*4 

3.0*4 

2.5*4 

Z0* 4 

1.5*4 

1.0*4 

5000.0 

0,0-

Data worked up by STW 

Printing Time: 11:16:52 AM 

Printing Date: Wednesday, January 2 6, 2011 

Page 2 of 4 

Page 53 of 67 
Ginge r AG01330509 

Attachment B 

GLP10-01-02; Interim Report 13 

Analy^i^SiPf ^ta^lfH^gP^iPslOai? Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

• Sample Nam*;'g101215a02e- Sample ID; •GLP1&O1-02-13O21" Fite;'g101215a.wir 

I Peak Nam*: "M8PF0S(IS)- Mass(es):'SOT.OffiO.O amu" 

• Comm*nt;'DALGWMCLMW3B0101110" Annotation;"" 

."lample Indez : 29 

Sanple Type: Unlctiown 

Concentration : 0.560 nq/n.L 8.5*4 

Calculate d Cont:: N'/A 

Acq. Dat«: 12/15/2CU' 

Acq. TiEia: 3:54:: ' PH "-" ^ 

Mcdilied : Hi. 7.Se4 

Proc . Algorichw : Intellifus n - lOA 

Hin . P«ak H-iqtit ; 0.00 cps 

Hin . Peat: Width : 0.00 s^c '•°* * 

Smoothing Width : o point s 

RT Wind.jw: .10.C s^<- 65e4 

Expected RT: 12. i itiin 

Use Relativ e BT: Nu 

6.0e4 

Int . Type: Valle y 

fistention Tin.e: li. J n,in 55 ^ 

Area : 300115 count s 

Star t Time: 12.2 r.in 5,De4 

End Time: 12.5 min . 

". 4.5*4 

1 4.0*4 

3.5*4 

3.0*4 

2.5*4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

1 2 3 4 5 

• SampI* Nam*: "g101215a0ir Sampte ID;'10007-6-8" Fite; "gl01215a.wir 

1 P*ak Name;'PFOS- Mass(es):'499.0/S9.0amu.49g.ara0.0amu,439.0/130.0 ami/ 

• Comment;'1.0 ng/mL FC std in Synth. Water- Annotation: " 

Sample In-iex : 1 " 

Sample Type: atanrtard" 

Cot,cantration : 0.590 ng/:T,L 

Calculit«r f cone : O.^'? ng/nL 

Acq. D.,ta: 12/1?/20U ' ,.5^5. 

Acq. Time: 1:12:30 Pi« 

Hc,di£jo(3: No 1.4e5-

RT Window: 30.0 sec 

EKpecced FiT: 12.3 mi:i 

Use Relativ e RT: Nn 1-3*5-

Je^enll^rTi^e : ""'iT ] .i n 

Area : 563437 count . 

Star t Tine : 12.2 min 

End Tim- : 12.5 min 

l.OeS 

« 9-0«4 

& ^ 8.0e4-

S 

- 7.0e4-

6.0e4-

S.0e4-

4.0e4-

3.0e4-

2.0*4 

1.0*4 

0.0 •;•••••-••••• , 

6 7 8 9 1C 

Tim*, min 

7 8 9 10 

12 31 

L 11 12 13 14 15 16 17 

1231 

11 12 13 14 15 16 17 

• Sample Nam*:-g10121SaO39" Sanpte ID; "10010-39" FH*; "g101215a.<Mr 

1 P*ak Nam*:-M8PFOS(tS}' ' Masses);'507.0/80.0 amu' 

1 Comment 'Method blanlT /^notation; ~ 

.Sample Indes : 35 

Sample Type: (•nki-.cwn 

Concent ta t ion : 0.9-JO n-j/mL 

Calculate d 'Jonc: H/A 

Acq. DJt^ : 12/15/201.1 g_o*4 

Acq. Tima: 7:12:J 3 PM 

85* 4 

H-idified : No ""^ ^ 

Ptoc . Algcritnrs : Inteilipua n - lOA 

Min - Peak H-iiht : 0.00 cps ^-O** 

Min . Peak Mid-.T: 0.00 sec 

Jmoothin-j Width : 0 point s 7.5*4 

RT Kindu-.v: -O.O =sr 

Expecte.-i hT: i:. i min 70 ^ 

Use Relativ e RT: Nc 

Int . Type: Valle y ^-^ ^ 

Retentio n Tin-e: la. i min 

Area : iiilS' b co-ints 6.0*4 

H-iiaht: 0.45d-C04 '•f..a 

Stat t Time: 12.2 min 5.5*4 

End Time: i:. 5 min » 

^ 5.0*4 

t 1 4.5*4 

4.0*4 

3.5*4 

3.0*4 

2.5*4 

2.0*4 

1.5*4 

1.0*4 

5000.0 

1 

1 2 3 4 5 

• SamfrieName:-g101215aO83" Sampte ID; "LCS-101215-r Fde: "gl01215a.»vtr 

1 Peak Name; "PFOS" Mas*(es);"499.Qre9.0amu.499.oraO.Oamu,499.0/130.0amu-

• Comment "0.2ppb LCS" Annotation; " 

Sample Index ; 54 

Sample Type: QC 

Concentration : 0.1S8 ng/mL 

Calculat-. d Cone: 0.172 ng/mL 27e4-

Acq. l:at*!: 12/1S/2P1C 

Acq. Tims : 5:^7:0 9 PM 2.6*4-

„„di»., , ,. , ^ ^ 

RT Kindo-j; 30.0 sec 2.4*4-

Expected RT; 12.? r.in 

Use Relativ e RT: Ho ^•*" ' 

Z2*4 

j".jr^r„„: ""in .i„ 

^rea : seSlO counts 2.0*4-

Haight : 2.7£e-00.) cpa 

Star t Time: i:. 9 min '-S^ ' 

Enn Time: 13.0 min 18*4-

1.7*4 

1.6*4 

1 1.5*4 

^ 1.4*4 

1 1.3*4 

~ 1.2*4 

1.1*4 

1.0*4 

gooo.o8000.0 

7000.0-

6000.0 

5000,0-

4000.0-

3000,0 

2000.0-

1000.0 

0 0 J- •.• ^ ~t— ^ -„—^. , .—y—,— ,-,..^ 

1 2 3 4 5 

—= 

1231 

L_^_ 6 7 8 9 10 11 12 13 14 15 16 17[ 

Tim*, min 

1. i . 1 , . .,. . 

6 7 6 9 10 

1285 

1, „ ^ 

1 L- •*<*V 

11 12 13 14 IS 16 171 

1 

Data worked up by STW 

Printin g Time: 11:16:5 3 AM 

Printin g Date : Wednesday, Januar y 26, 2011 

Page 3 of 4 

Page 54 of 67 
Ginger AG01330509 

Attachment B 

GLP10-01-02; Interim Report 13 

Analyfi?s8iff ^Y»?f H^S?^f5l9?diP Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

[ Sample Name; -g101215a088" Sample ID:"LCS-101215*" Fil*; 'gl01215a,wir 

I Peak Name: "PFOS" Mas$(es}: '499.0J99.0 a. 

I Comment; "0.2ppb LCS ECF" /\nnotabon; " 

Sample Indaz : 87 

Simple Type: yC 

Concentration : 0. 195 nq/mL 

Calciilata d Cone: 0.21fl nq/mL 

Ar-.). Date : 12/lf/20U ' 

u,499.0/130.0 amu' 

1.9e4 

1.8*4 

1.7*4 

1.6*4-

1.5*4 

1.4*4 

l,3e4 

1,2*4 

1.1*4 

l,0e4-

9000.0 

8000.0 

7000.0-

6000.0 

5000.0 

4000.0 

3000.0 

2000.0-

1000.0-

0.0 i - ^ 

10 I I 12 13 14 15 16 17 

I Sample Name: "91012153028" Sample ID:"GLP1(M31-02-13<J21" Fil*; "gl01215a.V( 

Peak Name: "PFOS" Masses): "499,0«9.0 amu,499.0ffiO.D amu.499.0/130.0 amu" 

I Comnwn f OALGWMCLMW3B0101110- Annotation; " 

Sample Index : 25 

Sample Type: Unknown 

Acq. fatn ; 

Acq. Time: 

Hodilibd ; 

RT Kindo-j: 

Expecl 

riv e RT 

Int . Type: 

Height: 

Start Ti 

End Time 

Manu: 

163716 

26*4-1 

25*4 -

24*4 -

23*4-

22*4 -

2.1*4-

20*4 -

1.9e4-

1.8e4 

1.7*4-

1.6*4-

1.5*4-

1.4*4-

1.3*4-

1.2*4-

1.1*4-

1.0*4-

9000.0-

8000.0-

7000.0-

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

0.0 -MW*V , 

• .IfiL. , -i.. ^ , I,,I., l,*.„t..f.M 

7 8 9 10 11 12 13 14 15 16 17 

I

SampI* Name; "gl01215a039' Sampte ID; '1001&<39' File: 's10l215a.wir 

P*ak Nam*: "PFOS* Msss(es); '498.0/99.0 amu.439.0/80.0 amu.493.0^30.0 amu" 

Comment *M*ttK>d blank* Annotation: ~ 

Sampl e Index : J9 

Sampl e Type : Unkno-vn 

IJ/A 

Calculate d 

Acq. D.iti ; 

Acq. Tima: 

M.->Jl(iad: 

Proc. Aiqo 

fJjiae P^rc 

Ea.-e. Sue. 

Cone: 

i 

W 

hra: 

ige 

0.00203 nq/mL 

12/15/2011' 

7:12:I 3 PI1 

Mt, 

Intelliyua n - MOIl 

10 

ndow: l.,-^0 ::an 

8500 

8000 

7000 

5500 

5000 

4500 

4000 

3500 

3000 

2500-

2000-

1500 

|l.itljfkU.j.t|tlp.i|ill|ti,»i^ll 

12.90 

10 11 12 13 14 15 16 17 

Data worked up by STW 

Printing Time: 11:16:53 AM 

Printing Date: Wednesday, January 26, 

Page 4 of 4 

2011 Page 55 of 67 
Document ntafifeei«ft6T^ri}viB,e|ji5reT*, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS In Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

3M Environmental Laborafmy 

Method 

Method of Analysis for the Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8'044.0 

Adoption Date: Upon Signing 

Effective Date: Q ^ 1(1 [ o "1 

Approved By: 

^y •g- > 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11. 

Mettiod of Analysis forttie Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct 

Injection Analysis Page 56 of 67 
Document nmnfmrnmifit^kr^swcimt, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PROS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

1 Scope and Application 

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

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

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

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

and Perfiuorooctanesulfonate (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 Method 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 Working Standard (WS) into a predetermined 

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

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

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

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 57 of 67 
Document ns:».filK-ai«g^arij!erilli36pr8f;S, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

3.4 Field Duplicate Sample (FDS, Field Dup) 

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

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

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

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

3.5 Field Matrix Spike (FMS) 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

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

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

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

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

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

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

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

ETS-8-044.0 Page 3 of 11 

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

Injection Analysis 

Page 58 of 67 
Document ntayiban^SieriferiifiSijjrorert, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

3.11 Method Blank 

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

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

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

environment, the reagents, or the apparatus. 

3.12 Sample 

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

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

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

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

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

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

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

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

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

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

4.2 Cautions 

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

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

appropriate equipment procedure or operator manual for additional 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 59 of 67 
Attachment C 

Document n©,aiyii>8i«i9rtkiifiS6pr8f3t, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

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

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

caps, autovial caps, HPLC parts, etc. 

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

calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Equipment 

6.1 Instrumentation and Equipment 

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

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25pL, 50pL, 100pL, 250^JL, 500pL, lOOOpL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographic System 

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

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

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 pL. 

Quantitation: Peak Area-quadratic curve 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 60 of 67 
Attachment C 

Document niaf'ib>ai«s;QrftWiffie:!3preT3t, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

6.3 MS/MS System 

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

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213-^169 

263^219 

313-^269 and 313-^119 

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

413-» 369, 413 ^ 219 and 413 ^ 169 

463 ^ 419, 463 ^ 169 and 463 ^219 

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

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

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

299 -> 80 and 299 ^ 99 

399 -^ 80 and 399 ^ 99 

499 -^ 80, 499 -» 99 and 499 ^ 130 

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

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

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

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

The previous information is intended as a guide, alternate instalments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate - A.C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfluorooctanoic Acid (PF0A-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-C12 acid); Oakwood Products, Inc 

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfiuorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 61 of 67 
Document mm}^b•m^2>^^ikr^BmrG^, for 14 days from 01/26/201' 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

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

used. 

7.3 Reagent Preparation 

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

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

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

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

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

„ X- r X molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

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

538 

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

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

flask and bring up to volume with solvent. 

250 ng/mL mixed worl<ing standard—Add 1.25mL of the 5 pg/mL -mixed working 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 working standard solution to a 25mL volumetric 

flask and bring up to volume with solvent. 

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

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

ETS-8-044.0 Page 7 of 11 

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

Analysis 

Page 62 of 67 
Attachment C 

Document ncRfift-aiffls^iBfcrimB&i^meTrt, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Morgan County Landfill, Decatur, AL - November 2010 

7.5 Calibration Standards 

Using the working 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 working 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, /jL 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

ofASTIVI Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTIVI Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

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

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

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

Prepare at least five method blanks. 

9 Sample Analysis - LC/MS/MS 

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

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

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

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

thoroughly documented in the raw data. 

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

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

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

The coefficient of determination (r^) value for the calibration curve must be greater than or equal to 0.990. Each 

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

ETS-8-044.0 Page 8 of 11 

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

Analysis 

Page 63 of 67 
Document maijiMi-meh'tWim B&jireTst, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

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

points will be used to constmct the calibration curve. 

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

curve (if necessary) and reanalyze. 

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

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

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

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

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 

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

10.5 Lab Control Sample 

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

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

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

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

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

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

ETS-8-044.0 Page 9 of 11 

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

Analysis 

Page 64 of 67 
Document n(S:ftfil)>ei««;6rJierimge^c«r8T:*, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

10.6 Field Matrix Spikes / Lab Matrix Spikes 

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

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

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

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

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

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

11 Data Analysis and Calculations 

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

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

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

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

Slope 

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

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

percent recovery. 

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

Analyte added (ng/mL) 

12 Method Performance 

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

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

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

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

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

discussed in the text of the report. 

12.1 System Suitability 

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

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

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

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

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

12.2 Quantitation 

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

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

the LLOQ, which may be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

ETS-8-044.0 Page 10 of 11 

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

Analysis 

Page 65 of 67 
Document nmj^tbmismt^rmsm^eTA, for 14 days from 01/26/2011 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

Attachment C Morgan County Landfill, Decatur, AL - November 2010 

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

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

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

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

to Section 10 for addifional details. 

12.4 Accurac y 

This method and required quality control samples are designed to generate data that are accurate to +1-30%. 

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

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

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

14 Records 

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

Infonnation 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, instrument acquisition 

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

ETS-8-044.0 Page 11 of 11 

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

Analysis 

Page 66 of 67 
GLP10-01-02; Interim Report 13 

Analysis of PFBS, PFHS and PFOS in Groundwater Samples 

AMcWfl&^l^"^'^' Morgan County Landfill, Decatur, AL - November 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

Study / Project No. 

GLP10-01-02-13 

Date(s) of Occurrence: 

m101123aandg101215a 

Document Number: 

ETS-8-044.0 

Deviation type D SOP D Equipment Procedure IZI Method 

(Check one) D Protocol El GPO D Other: 

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

Method Requirements: 

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

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

(3) Field matrix spike recovery of 100% ± 30%. 

Actual procedure/process: 

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

criteria with average recoveries of 136% and 133%. 

(2) The RPD values for PFBS, PFHS, and PFOS for one sampling location were >20%. 

(3) The recovery of the high FMS sample for DAL GW MCL MW2B 101110 was 135%. 

///. Actions Taken 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

(1) It was suspected that the ECF stock standard used to prepare the linear+branched LCs may have 

become contaminated. A new linear and branched stock standard was prepared, with new LCS 

prepared at the same three concentration levels. Two of the low level linear and branched LCS could 

not be calculated as the detected concentration was below the limit of quantitation. One replicate at the 

low level had a recovery of 152%, while both the new mid and high level linear and branched LCS met 

method acceptance criteria with average recoveries of 114%. The mid and high level LCS 

concentrations were more appropriate as compared to the sample concentrations reported from this run. 

All LCS were used in the determination of method uncertainty. 

(2) Sampling location DAL GWMCL ME IB 101110 had RPD values >20% for all three analytes. The 

results will be footnoted in the data tables. 

(3) The high FMS sample was the only appropriate spike level for PFOS for this sampling location. The 

analytical uncertainty will be adjusted to ± 35%. 

IZI Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: Sijsan Wolf <-_5i,^fV^>H_ 

study Director (if GLP): 

Sponsor Approval (for GLP protocol deviations): NA 

Technical Reviewer (optional): NA 

Laboratory Department Manager Approval: 

Date: NA 

Date: 

IV. Authorization to Resume Work 

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

Laboratory Department Manager Approval: NA I Date: NA 

Deviation No. 

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

Attachment A ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing ^^^^ ^^ °' ^^