GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

GLP10-01-02: Interim Report 22 - Analysis of PFBS. PFHS. and PFOS in 

Groundwater Samples Collected from Decatur. AL. 3*^" Quarter 2011 

Study Title 

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

(PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone: 610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

St Paul, MN 55144 

Project Identification 

GLP10-01-02-22 

Total Number of Pages 

99 

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

Requirements for the Competence of Testing and Calibration laboratories", in 

accordance with the A2LA Testing Certificate # 2052.01. Testing that complies with this 

1 1 International Standard also meets principles of ISO 9001:2000. 

ACCREDITED 

Testing Cert #2052.01 

Page 1 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

This page has been reserved for specific country requirements. 

Page 2 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 22 - Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected from Decatur, AL, 3"^ Quarter 2011 

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

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

Site-Related Monitoring Program. 

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

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

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

system and no dosing of a test system. 

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

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

3, 

Gary Hopenstein,|Sponsor Representative Date 

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

Page 3 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 22 - Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected from Decatur, AL, 3"^ Quarter 2011 • : 

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

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

Site-Related Monitoring Program. 

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

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

laboratory management and study director. 

Inspection Dates Phase 

Date Re ported to 

Inspection Dates Phase Testing Facility 

lUlanagement 

Study Director 

11/10/11-11/11/11 Data / Interim Report 11/30/11 11/30/11 

QAU Representative Date 

Page 4 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

TABLE OF CONTENTS 

GLP Compliance Statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Information 8 

2 Summary... 9 

3 Introduction 11 

4 Test & Control Substances 11 

5 Reference Substances 12 

6 Test System 13 

7 Method Summary 14 

' 7.1 Methods 14 

7.2 Sample Collection 14 

7.3 Sample Preparation 14 

7.4 Analysis 14 

8 Analytical Results 16 

8.1 Calibration 16 

8.2 System Suitability 17 

8.3 Limitof Quantitation (LOQ) 17 

8.4 Continuing Calibration 17 

8.5 Blanks 18 

8.6 Lab Control Spikes (LCSs) 18 

8.7 Analytical Method Uncertainty 21 

8.8 Field Matrix Spikes (FMS) 21 

Page 5 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

9 Data Summary and Discussion 22 

10 Conclusion 34 

11 Data/Sample Retention 34 

12 Attachments 34 

13 Signatures 35 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (DecaturGroundwater-Q3 2011)...10 

Table 2. Sample Description Key Code 13 

Table 3. Instrument Parameters 15 

Table 4. Liquid Chromatography Conditions 15 

Table 5. Mass Transitions 16 

Table 6. Limit of Quantitation (LOQ) 17 

Table 7. Laboratory Control Spike Recovery 18 

Table 8. Analytical Uncertainty 21 

Table 9. Field Matrix Spikes 21 

Table 10. DAL GW 203L 110930 23 

Table 11. DAL GW220R110930 23 

Table 12. DAL GW220L110930 24 

Table 13. DAL GW222R 110930 .....24 

Table 14. DAL GW227R 110922... 25 

Table 15 DAL GW227L 110922 25 

Table 16. DAL GW 31 OR 110928 26 

Table 17. DAL GW 312R 110929 26 

Table 18. DAL GW 317L110928 .27 

Table 19. DAL GW 324L 110923 27 

Table 20. DAL GW 327R 110928 28 

Page 6 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Table 21. DAL GW 328R 110927 28 

Table 22. DAL GW 328L110928 29 

Table 23. DAL GW 330R 110928 29 

Table 24. DAL GW 330L110928 30 

Table 25. DAL GW 331S 110929 30 

Table 26. DAL GW 335R110927 31 

Table 27. DAL GW GRS04 110930 32 

Table 28. Trip Blank 1 :....32 

Table 29. Trip Blank 2 33 

Table 30. Equipment Rinseate Blanks 33 

Page 7 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

St. Paul, MN 55144 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Chelsie Grochow; analyst 

Kelly Ukes; analyst 

Jonathan Steege; analyst 

Study Dates 

Study Initiation: March 8,2010 

Interim 22 Experimental Termination: October 25, 2011 

Interim Report Completion: Date of Interim Report Signing 

Location of Archives 

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

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

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

Page 8 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

2 Summary 

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

representing eighteen (18) different sampling locations collected September 22 - 30, 2011. A total of 

eighty-two sample bottles were received at the 3M Environmental Laboratory for perfluorooctane 

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

For each sampling location, four sample bottles were collected; sample, sample duplicate, low field 

matrix spike, and high field matrix spike. Two trip blanks containing Milli-QTM water and appropriate trip 

blank spikes were analyzed with the groundwater samples. In addition, two equipment rinseate blank 

samples were collected. The equipment rinseate blanks did not have FMS samples prepared for 

determination of PFBS, PFHS, or PFOS recovery. All groundwater samples for this project were 

logged under GLP10-01-02-22. 

The groundwater samples, trip and equipment rinseate blanks for GLP10-01-02-22 were received from 

Weston personnel on October 6, 2011. All of the samples were prepared and analyzed for PFBS, 

PFHS, and PFOS following 3M Environmental Laboratory Method ETS-8-044.0. Many of the 

groundwater samples required dilution to obtain PFBS, PFHS, and/or PFOS concentrations within the 

range of the cun/e, in some instances up to a 500-fold dilution were required. The average measured 

PFBS, PFHS, and PFOS concentrations are summarized in Table 1. Equipment rinseate and the trip 

blanks 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 

groundwater locations ranged from <0.0400 ng/mL to 3070 ng/mL. The PFHS concentration results for 

all groundwater locations ranged from 0.0984 ng/mL to 6060 ng/mL. The PFOS concentration results 

for the reported groundwater locations ranged from 0.205 ng/mL to 3350 ng/mL. The analytical 

uncertainties associated with the reported results are as follows: PFBS 100% ± 14%, PFHS 100% ± 

18%, and PFOS 100% ± 26%. 

Page 9 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Table 1. Summarized PFBS, PFHS, and PFOS Results (Decatur Groundwater - 03 2011). 

PFBS PFHS PFOS 

Sampling Location 

Avg. Cone. (ng/mL) 

± %RPD 

Avg. Cone. (ng/mL) 

± %RPD 

Avg. Cone. (ng/mL) 

± %RPD 

DAL GW203L 110930 23.2 ±9.9% 142 ±9.2% 478 ±3.1% 

DALGW220R110930 4.76 ±2.9% 17.9 ±2.2% 27.4 ±7.3%'^' 

DALGW220L110930 7.87 ±1.0% 37.6 ±1.1% 49.2 ± 10% 

DAL GW222R 110930 62.5 ±0.16% 429 ± 0.93% 511 ± 0.39% 

DAL GW227R 110922 13.4 ±4.5% • 61.7 ±4.5% 578 ±2.1% 

DAL GW227L 110922 256 ±1.6% 68.5 ± 0.58% 474 ± 3.6% 

DAL GW 31 OR 110928 730 ± 3.7% 320 ±1.3% 611 ±3.4% 

DALGW312R 110929 1140 ±1.8% 831 ±0.48% 1440 ±8.3% 

DAL GW317L 110928 <0.0400 0.0984 ±9.3% 0.205 ± 8.8% 

DALGW324L110923 70.0 ± 0.0% 82.5 ±0.97% 211 ±0.95% 

DAL GW327R 110928 51.6 ±0.58% 126 ±1.6% 397 ±1.3% 

DAL GW328R 110927 27.9 ±1.4% 57.9 ± 2.2% 178 ±0.28% 

DAL GW328L 110928 40.3 ± 0.0% 18.4 ±1.1% 1.29 ±3.9% 

DAL GW330R 110928 3070 ± 0.48% 196 ±1.5% 593 ± 2.4% 

DAL GW330L 110928 530 ± 5.5% 434 ±1.4% 169 ±1.4% 

DAL GW331S 110929 525 ± 3.8% 331 ± 3.0% 506 ±4.5% 

DAL GW335R 110927 1080 ± 3.7% 1420 ±2.1% 3350 ± 3.3% 

DAL GWGRS04 110930 1690 ± 3.6% 6060 ± 5.5% 1330 ± 1.5% 

Trip Blank (Milli-QTM Water) - 2 sets <0.0400 <0.0250 <0.183 

Equipment Blank s - 2 rinseate blanks <0.0400 <0.0250 <0.232 

The analytical method uncertainties associated with the reported results are as follows: PFBS 100% ± 14%, PFHS 100% ± 18%, 

and PFOS 100% ±26%. 

(1) The analytical uncertainty has been expanded for the following samples based on FMS recovery: DAL GW 220R (PFOS ± 

38%), DAL GW 220L (PFOS ± S8%), DAL GW 222R (PFOS ± 43%; PFHS ± 35%), DAL GW 330L (PFBS ± 34%), DAL GW 

331S (PFBS ± 32%), DAL GW SS5R (PFBS ± 31%), and DAL GW GRS04 (PFOS ± S7%). 

(2) Sampling location did not contain an appropriate spil<e level to assess PFOS recovery. 

Page 10 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

3 Inlj^oduction 

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

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

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

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

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

conducted to analyze ground water samples collected from various 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 containers (250 mL high-density polyethylene 

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

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

samples. Each empty container was marked with a "fill to here" line to produce a final sample volume 

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

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

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

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

Laboratory method ETS-8-044.0 "Method of Analysis for the Determination of Perfluorinated 

Compounds in Water by LC/MS/MS; Direct Injection Analysis". 

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

collected, trip blanks and equipment rinseate samples. Tables 10-30 summarize the individual sample 

results and the associated FMS recoveries. All results for the quality control samples prepared and 

analyzed with the samples are reported and discussed elsewhere in this report 

4 Test&Control Substances 

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

was purely analytical in nature. 

Page 11 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

5 Reference Substances 

Reference Substance 

PFBS 

(predominantly linear) 

PFHS 

(linear) 

Chemical Name Perfluorobutane sulfonate Perfluorohexane sulfonate 

Chemical Formula C4F9SO3" CgFisSOa 

Identifier Potassium Salt Sodium Salt 

Source 3M Wellington 

Expiration Date 1/10/2017 3/25/2018 

Storage Conditions Frozen Frozen 

Chemical Lot Number 101 LPFHxSAMOS 

TCR Number TCR-121 TCR08-0018 

Physical Description White Powder Crystalline 

Purity 96.7% 98% 

Use 

Target Analyte Reference 

Standard 

Target Analyte Reference 

Standard 

Reference Substance 

PFOS 

(linear) 

PFOS 

(linear + branched) 

Chemical Name Perfluorooctane sulfonate Perfluorooctane sulfonate 

Chemical Fomnula CsF-iySOa CsF-iySOs 

Identifier 

Potassium Salt 

CAS #2795-39-3 

Potassium Salt 

CAS #2795-39-3 

Source Wellington Wellington 

Expiration Date 10/18/2018 03/17/2014 

Storage Conditions Frozen Frozen 

Chemical Lot Number LPFOSKBM06 brPFOSK0708 

TCR Number TCR08-0001 TCR11-0010 

Physical Description Crystalline Liquid 

Purity 98% 99.9% 

Use 

Field Matrix Spike Reference 

Standard 

Target Analyte Reference 

Standard 

Page 12 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Reference Substance 

"Cg-PFOS 

(linear) 

Chemical Name 

Sodium 

Perfluorooctanesulfonate 

Chemical Formula "CsFuSOa'Na" 

Identifier CAS#MPFC-C-0511 

Source Wellington 

Expiration Date 05/25/2014 

Storage Conditions Frozen 

Chemical Lot Number 092310 

TCR Number TCR11-0016 

Physical Description Liquid 

Purity 5|jg/mL<^> 

Use Internal Standard 

(1) Custom mixture of seven mass-labeled ( C) pertluoroalkylcarboxylic acids, two 

mass-labeled ("C) perfluoroalkylsulfbnates and one mass-labeled ("C) 

perfluoro-1 -octanesulfonamide. 

6 Test System 

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

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

specific lot of test substance. 

Table 2. Sample Description Key Code. 

Example DAL GW 203L DB 110930 

string Number string Descriptor Example 

1 Sampling Location DAL = Decatur, Alabama 

2 Sample Type GW= Ground water 

3 Well Identifier Example: 203 

4 Well Level R = Residuum shallow water-bearing zone 

L = Bedrock water-bearing zone 

S = Epikarst middle water-bearing zone 

5 Sample Type 0=primary sample 

DB=duplicate sample 

LS = low spike 

MS = mid spike 

HS = iiigh spike 

6 Sampling Date 110930 = September30,2011 

Page 13 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

7 Method Summary 

7.1 Methods 

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

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

Direct Injection Analysis". 

7.2 Sample Collection 

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

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

October 6, 2011. Samples were stored refrigerated at the laboratory after receipt. A set of laboratory 

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

7.3 Sample Preparation 

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

analysis. 

Samples that required dilution were prepared as follows: 

1:5 dilutions were prepared by diluting 2mL sample with 8 mL of Milli 0 water, 

1:10 dilutions were prepared by diluting ImL sample with 9 mL of Milli Q water, 

1:20 dilutions were prepared by diluting 0.5mL sample with 9.5mL of Milli Q water, 

1:50 dilutions were prepared by diluting 0.2mL sample with 9.8mL of Milli Q, and 

1:100 dilutions were prepared by dilufing O.lmL sample with 9.9mL of Milli Q water. 

Samples may also have been diluted further by varying the injection volume during analysis. 

Sampling locations DAL GW 317L and DAL GW 328L were prepared for PFOS by removing a 5 mL 

aliquot and adding an aliquot of a separate intemal standard spiking solution (nominal concentration of 1 

ng/mL). This same procedure was followed for the laboratory control samples. 

7.4 Analysis 

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

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

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

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

Page 14 of 99 
Table 3. Instrument Parameters. 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Instrument Name ETS Buster ETSKiri< 

Analytical Method Followed ETS-8-044.0 ETS-8-044.0 

Analysis Date 10/12/11 10/20/11, 10/24/11 

Liquid Chromatograph Agilent 1100 Agilent 1200 

Guard column Prism RP (2.1 mm X 50 mm), 5 n Betasil 018 (4.6 mm X 100 mm), 5u 

Analytical column Betasil 018 (2.1 mm X 100 mm), 5n Betasil 018 (4.6 mm X 100 mm), 5n 

Injection Volume 2or10uL 10 or 50 uL 

IVIass Spectrometer Applied Biosystems fiP\ 4000 Applied Biosystems API 5500 

Ion Source Turbo Spray Turbo Spray 

Electrode Turbo ion electrode Turbo ion electrode 

Polarity Negative Negative 

Software Analyst 1.4.2 Analyst 1.5.2 

Table 4. Liquid Chromatography Conditions. 

step 7ota/ 77ine Flow Rate Percent A PercentB 

Number (min) (fJJmln) (2 mM ammonium acetate) (Methanol) 

ETS-8-044.0 Analysis 10112111 

0 0 300 97.0 3.0 

1 2.0 300 97.0 3.0 

2 14.5 • 300 5.0 95.0 

3 15.5 300 5.0 95.0 

4 16.5 300 97.0 3.0 

5 20.0 300 97.0 3.0 

ETS-8-044.0 Analysis 10/20111 and 10/2A/11 

0 0 750 97.0 3.0 

1 2.0 750 97.0 S.O 

2 14.5 750 5.0 95.0 

3 15.5 750 5.0 95.0 

4 16.5 750 97.0 3.0 

5 20.0 750 97.0 3.0 

Page 15 of 99 
Table 5. IVIass Transitions. 

, GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Analyte 

Reference Material 

Structure 

Mass Transition 

Q1IQ3 

Intemal Standard Mass Transition 

Q1/Q3 

PFBS Linear 

299/80 

NA NA 

299199 

PFHS Linear 

399180 

NA NA 

399/99 

PFOS Linear+Branched 

499/80 

499/99 ["CJPFOS'" 507/80 

499/130 

Dwell time was 75 msec (10/12/11 analysis) or 30 msec (10/20/11 and 10/24/11 analysis) for eacti transition. The 

individual transitions were summed to produce a 'total ion chromatogram" (TIC), which was used for quantitation. 

NA = Not Applicable 

(1) Intemal standard was only used for the analysis of locations DAL GW 317L and DAL GW S28L for PFOS. 

8 Analytical Results 

8.1 Calibration 

8.1.1 Extemal Standard Calibration -10/12/11 and 10/20/11 analysis: 

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

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

water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL were prepared, 

however, not all analytical runs included all fifteen standards. Low curve points may have been 

disabled to meet accuracy or method blank criteria. A quadratic, 1/x weighted, calibration curve of the 

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

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

accuracy of each curve point. 

The PFOS reference standard used for the preparation of the calibration standards contained both linear 

and branched isomers. The samples conained both linear and branched isomers, many with 

concentrations >100 ng/mL, however, the field matrix spikes were prepared using predominantly linear 

PFOS. To help minimize any potenfial analytical bias in the quantitation of linear isomers of PFOS 

against mixed linear and branched PFOS, the linear PFOS peaks and the branched PFOS peaks were 

integrated separately. For the linear calibration, only the linear peaks of all samples were integrated, 

including the calibration curve. The branched calibration was done in the same manner, integrating only 

the branched isomers. The concentrations of the calibration curve points were based on the percent 

linear and branched isomers in the standard, 21.1% branched and 78.8% linear. The final calculated 

concentrations were detemnined using the summed calculated concentrations of the linear and branched 

peaks. 

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 ali 

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

8.1.2 Intemal Standard Calibration -10/24/11 analysis: 

Sampling locations DAL GW 317L and DAL GW 328L for PFOS were analyzed against a matrixmatched stable isotope internal standard calibration curve. Calibration standards were prepared by 

Page 16 of 99 
GLP10-01-02; Interim Repori 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

spiking known amounts of the stock solution containing the target analytes into a laboratory-prepared 

synthetic groundwater containing calcium and magnesium. The calibration standards contained an 

intemal standard mix containing "Cs-PFOS at a nominal concentration of 1 ng/mL. A total of thirteen 

spiked standards ranging from 0.025 ng/mL to 25 ng/mL were analyzed for PFOS. The PFOS 

reference standard used for the preparation of the calibration standards contained both linear and 

branched isomers. A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area 

counts over the intemal standard peak area counts was used to fit the data for each analyte. The data 

were not forced through zero during the fitting process. 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 correlation coefficient (r) 

was greater than 0.995 for PFOS. The PFOS linear and branched isomers were integrated together as 

one analyte peak and not separately as done for the 10/12/11 and 10/20/11 analyses. These samples 

did not require the linear and branched isomers to be integrated separately since the samples had low 

amounts of PFOS and were aided with the addition of intemal standard "Cs-PFOS. 

8.2 System Suitability 

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

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

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

met for PFBS, PFHS, and PFOS for each analytical batch with the exception of the 10/12/11 and 

10/20/11 analyses, in which PFOS (linear and branched summed) had an area count RSD of 7.5% in 

the 10/12/11 analysis and 9.1% in the 10/20/11 analysis. A method deviation is included in Attachment 

D. 

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 LOQs associated with the sample analysis are listed in the table below. 

Table 6. Limit of Quantitation (LOQ). 

Analysis Date Dilution 

PFBS 

LOQ, nglmL 

PFHS 

LOQ, nglmL 

PFOS 

LOQ, nglmL 

10/12/11 

1 0.0400 0.0250 0.232 

10/12/11 

5 0.200 0.125 1.16 

10/12/11 

10 0.400 0.250 2.32 

10/12/1 10/12/11 20 0.800 0.500 4.64 

50 2.00 1.25 11.6 

10/12/11 

100 4.00 2.50 23.2 

10/12/11 

500 20.0 12.5 116 

10/20/1 10/20/11 1 NA 0.0250 0.0232 

500 NA 12.5 11.6 

10/24/11 1 NA NA 0.0232 

NA = Not Applicable; analytical results for were not reported from the njn. 

8.4 Continuing Calibration 

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

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

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

of several CCVs analyzed for PFOS on 10/12/11 which had recoveries greater than 125% (127% -

135%). Sample sets bracketed by the non-compliant CCVs include: DAL GW 317L, DAL GW 324L, 

Page 17 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

DAL GW 327R, DAL GW 328R, DAL GW 328L, DAL GW 330R, DAL GW 330L, DA; GW 331S, DAL 

GW 335R, and DAL GW GRS04. A method deviation is included with the raw data. 

8.5 Blanks 

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

field/trip blanks, and equipment blanks. Method procedural blank results were reviewed and used to 

evaluate method performance and to determine the LOQ for each analyte. 

8.6 Lab Control Spikes (LCSs) 

Three lab control spike levels were prepared and analyzed in triplicate with each preparation set. LCSs 

were prepared by spiking known amounts of the analyte into 10 mL of Milli Q water or synthetic 

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

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

should be within 100% ± 20% with an RSD <20%. 

For the 10/12/11 and 10/20/11 analyses, the PFOS LCS recovery was based on the sum of the 

calculated concentrations of the linear and branched isomers integrated separately. 

All LCSs met acceptance criteria for each analyte except for the 0.2ppb and 2ppb LCSs for PFOS in the 

10/20/11 analysis, which had average recoveries of 74.1% and 78.1% respectively. A method deviation 

is included with the raw data. 

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

LCS Percent Recovery = 

Calculated Concentration, 

Spike Concentration 

100% 

LCS% RSD = 

standard deviation LCS replicates , 

average LCS recovery 

100% 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 10/12/11 

Extemal Calibration PFBS PFHS 

Spiked 

Concentration 

Calculated 

Concentration 

Spiked 

Concentration 

Calculated 

Concentration 

LabID (nglmL) (nglmL) VoRecovery (nglmL) (nglmL) %Recovery 

LCS-111007-1 2.00 2.07 103 2.00 2.10 105 

LCS-111007-2 2.00 2.04 102 2.00 2.03 101 

LCS-111007-3 2.00 2.10 105 2.00 2.09 104 

Average ±%RSD 103% ±1.5% 103% ±2.0% 

LCS-111007-4 20.0 18.4 92.0 20.0 18.3 91.6 

LCS-111007-5 20.0 19.0 95.2 20.0 19.1 95.6 

LCS-111007-6 20.0 19.3 96.5 20.0 18.8 93.9 

Average ±%RSD 94.6% ±2.4% 93.7% ±2.1% 

LCS-111007-7 49.8 50.8 102 49.8 54.7 110 

LCS-111007-8 49.8 49.6 99.6 49.8 50.4 101 

LCS-111007-9 49.8 50.5 101 49.8 51.0 102 

Average ±%RSD 101% ±1.2% 104% ±4.7% 

Page 18 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 10/12/11 

Extemal Calibration PFOS (Linear+Branched summed) 

Spiked Calculated Calculated 

LabID 

Concentration 

(nglmL) 

Cone (Linear) 

(nglmL) 

Cone (Branched) 

(nglmL) %Recoveiy 

LCS-111007-1 1.85 1.44 0.382 98.5 

LCS-111007-2 1.85 1.32 0.354 90.5 

LCS-111007-3 1.85 1.44 0.383 98.5 

Average ±%RSD 95.8% ±4.8% 

LCS-111007-4 18.5 14.4 3.76 98.2 

LCS-111007-5 18.5 15.2 3.95 104 

LCS-111007-6 18.5 14.4 3.78 98.3 

Average ±%RSD 100% ±3.1% 

LCS-111007-7 46.2 35.1 9.70 97.0 

LCS-111007-8 46.2 35.1 9.56 96.7 

LCS-111007-9 46.2 36.1 9.69 99.1 

Average ±%RSD 97.6% ±1.4% 

ETS-8-044.0 

Analyzed 10/20/11 

Extemal Calibration PFHS 

Spiked 

Concentration 

Calculated 

Concentration 

LabID (nglmL) (nglmL) VoRecovery 

LCS-111020-1 2.00 0.174 86.8 

LCS-111020-2 2.00 0.172 86.1 

LCS-111020-S 2.00 0.170 85.1 

Average ±%RSD 86.0% ±0.99% 

LCS-111020-4 2.00 1.76 87.8 

LCS-111020-5 2.00 1.65 82.6 

LCS-111020-6 2.00 1.70 84.8 

Average ±%RSD 85.1% ±3.1% 

LCS-111020-7 20.0 17.8 89.0 

LCS-111020-8 20.0 16.8 84.2 

LCS-111020-9 20.0 17.4 87.1 

Average ±%RSD 86.8% ± 2.8% 

Page 19 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 10/20/11 

Extemal Calibration PFOS (Linear+Branched summed) 

LabID 

Spiked 

Concentration 

(nglmL) 

Calculated 

Cone (Uneai) 

(nglmL) 

Calculated 

Cone (Branched) 

(nglmL) VoRecovery 

LCS-111020-1 0.185 0.113 0.0320 78.4 

LCS-111020-2 0.185 0.112 0.0299 76.7 

LCS-111020-S 0.185 0.0989 0.0255 67.2 

Average ±%RSD 74.1% ±8.1%TM 

LGS-111020-4 1.85 1.16 0.316 79.8 

LCS-111020-5 1.85 1.07 0.305 74.3 

LCS-111020-6 1.85 1.17 0.312 80.1 

Average ±%RSD 78.1% ±4.2%'" 

LCS-111020-7 18.5 13.7 3.52 93.1 

LCS-111020-8 18.5 13.0 3.40 88.6 

LCS-111020-9 18.5 13.2 3.28 89.1 

Average ±%RSD 90.3% ±2.7% 

ETS-8-044.0 

Analyzed 10/24/11 

Intemal Standard Calibration PFOS (Linear + Branched) 

Spiked 

Concentration 

Calculated 

Concentration 

LabID (nglmL) (nglmL) VoRecovery 

LCS-111024-1 0.184 0.166 90.0 

LCS-111024-2 0.184 0.166 90.1 

LCS-111024-3 0.184 0.167 90.9 

Average ±%RSD 90.3% ±0.55% 

LCS-1110244 1.84 1.72 93.7 

LCS-111024-5 1.84 1.72 93.5 

LCS-111024-6 1.84 1.65 89.7 

Average ±%RSD 92.3% ± 2.4% 

LCS-111024-7 9.22 8.89 96.4 

LCS-111024-8 9.22 8.01 86.9 

LCS-111024-9 9.22 8.91 96.7 

Average ±%RSD 93.3% ±6.0% 

(1) LCS average did not meet acceptance criteria of 100 ± 20%. 

Page 20 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

8.7 Analytical Method Uncertainty 

Analytical uncertainty is based on historical LCS 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 LCS samples. 

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

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

method uncertainty values. The analytical method uncertainty for PFOS when determined by ETS-12-

012.2 was ± 18%, however, since the average recovery of the low set of LCS samples analyzed on 

10/12/11 had an average recovery of 74.1 %, the analytical uncertainty for this analysis will be 

expanded for PFOS to ± 26%. 

Table 8. Analytical Uncertainty. 

Analyte Standard Deviation Method Uncertainty 

PFBS 6.93 ±14% 

PFHS 9.05 ±18% . 

PFOS NA ±26% 

(1) NA= Not Applicable 

8.8 Field Matrix Spikes (FMS) 

Field matrix spikes were collected at each sampling point to verify that the analytical method is 

applicable to the collected matrix. Field matrix spikes were generated by adding a measured volume of 

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

prior to shipping sample containers for sample collection. Field matrix spike recoveries within method 

acceptance criteria of 100±30% confirm that "unknown" components in the sample matrix do not 

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

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

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

Table 9. Field IVIatrix Spikes. 

Sampling Location Spike Level 

PFBS 

(ng/mL) 

PFHS 

(ng/mL) 

PFOS 

(ng/mL) 

317L 

Low FMS 

High FMS 

1.00 

10.0 

1.00 

10.0 

1.00 

10.0 

220R, 220L, 328L 

Low FMS 

High FMS 

10.0 

100 

10.0 

100 

10.0 

100 

203L, 222R, 227L, 227R, 31 OR, 324L, 

327R, 330L, 331S, 335R 

Low FMS 

High FMS 

100 

1000 

100 

1000 

100 

1000 

GRS04, 312R, 330R 

Low FMS 

High FMS 

1000 

5000 

1000 

5000 

1000 

5000 

328R 

Low FMS 

High FMS 

100 

500 

100 

500 

100 

500 

Low FMS 10.0 10.0 10.0 

Trip Blank Sets 1 and 2 Mid FMS 100 100 100 

High FMS 1000 1000 1000 

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

FMS Recovery = * 100% 

Spike Concentraton 

Page 21 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

d Bata 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 blank. 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 220R (Table 11) - The recovery of the HS for PFOS was 61.9%. Since this was the only 

appropriate spike level, the analytical uncertainty has been adjusted for PFOS to ± 38%. 

DAL GW 220L (Table 12) - The recovery of the HS for PFOS was 61.9%. Since this was the only 

appropriate spike level, the analytical uncertainty has been adjusted for PFOS to ± 38%. 

DAL GW 222R (Table 13) - The recovery of the HS for PFBS, PFHS, and PFOS was 66.8%, 65.1 %, 

and 56.9%, respectively. Since the LS for PFBS met acceptance criteria, the method uncertainty will 

not be adjusted for PFBS. Since the HS was the only appropriate spike level for PFHS and PFOS, the 

analytical uncertainty has been adjusted for PFHS to ± 35% and for PFOS to ± 43%. 

DAL GW 327R (Table 20) - The recovery of the HS for PFBS and PFHS was 65.4% and 69.1 %, 

respectively. Since the LS for PFBS and PFHS met acceptance criteria, the method uncertainty will not 

be adjusted. 

DAL GW 330L (Table 24) - The recovery of the HS for PFBS was 66.1%. Since this was the only 

appropriate spike level, the analytical uncertainty has been adjusted for PFBS to ± 34%. 

DAL GW 331S (Table 25) - The recovery of the HS for PFBS was 68.5%. Since this was the only 

appropriate spike level, the analytical uncertainty has been adjusted for PFBS to ± 32%. 

DAL GW 335R (Table 26) - The recovery of the HS for PFBS was 69.1%. Since this was the only 

appropriate spike level, the analytical uncertainty has been adjusted for PFBS to ± 31 %. 

DAL GW GRS04 (Table 27) - The recovery of the LS for PFOS was 63.0%. Since this was the most 

appropriate spike level, the analytical uncertainty has been adjusted for PFOS to ± 37%. 

Trip Blank 1 (Table 28) - The recovery of the MS for PFOS was 68.0%. 

Trip Blank 2 (Table 29) - The recovery of the MS and HS for PFOS was 65.9% and 68.9%, 

respectively. 

Page 22 of 99 
Table 10. DAL GW 203L 110930 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) %Recovery (ng/mL) %Recovery 

GLP1(K)1-02-22-001 DAL GW203L 0110930 24.3 NA 148 NA 485 NA 

GLP10-01-02-22-O02 DALGW203L DB 110930 22.0 NA 135 NA 470 NA 

GLP10-01-02-22-003 DALGW203L LS 110930 106 82.9 230 88.5 668 NC 

GLP10-01-02-22-004 DALGW203L HS 110930 819 79.6 952 81.1 1190 71.2 

Average Concentralion (ng/mL) ± %RPD 23.2 ng/mL ±9.9% 142 ng/mL ±9.2% 478 ng/mL ±3.1% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 10/12/11. 

Table 11. DAL GW 220R110930 

PPBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-005 DAL GW220R 0110930 4.69 NA 177 NA 26.4 NA 

GLP10-01-02-22-006 DALGW220R DB 110930 483 NA 18.1 NA 28.4 NA 

GLP10-01-02-22-007 DALGW220R LS 110930 12.7 79.4 25.3 74.0 33.4 NC 

GLP10-01-02-22-008 DALGW220RHS 110930 84.4 79.6 99.0 81.1 89.3 61.9TM 

Average Concentration (ng/mL) ± %RPD 4.76 ng/mL ±2.9% 17.9 ng/mL ±2.2% 27.4 ng/mL ± 7.3% ^ 

NA = Not /\pplicable 

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

Samples diluted 5x and analyzed 10/12/11. 

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

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

Page 23 of 99 
Table 12. DAL GW 220L 110930 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3MUMSID Description (ng/mL) %Recovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-009 DAL GW220L 0110930 7.91 NA 37.8 NA 46.6 NA 

GLP10-01-02-22-010 DALGW220LDB 110930 7.83 NA 37.4 NA 51.7 NA 

GLP10-01-02-22-011 DAL GW220LLS 110930 157 78.3 45.1 NC 53.3 NC 

GLP10-01-O2-22-012 DALGW220L HS 110930 86.3 78.4 119 81.4 111 .61.9TM 

Average Concentration (ng/mL) ± VoRPD 7.87 ng/mL ±1.0% 37.6 ng/mL ±1.1% 49.2ng/mL ±10%'^ 

NA = Not Applicable 

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

Samples diluted 5x and analyzed 10/12/11. 

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

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

Table 13. DAL GW 222R 110930 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-013 DAL GW222R 0110930 62.4 NA 427 NA 510 NA 

GLP10-01-02-22-014 DAL GW222RDB 110930 62.5 NA 431 NA 512 NA 

GLP10-01-02-22-015 DALGW222R LS 110930 149 86.6 532 NC 625 NC 

GLP10-01-02-22-016 DALGW222R HS 110930 730 66.8TM 1080 65.1 TM 1080 56.9TM 

Average Concentration (ng/mL) ± VoRPD 62.5 ng/mL ±0.16% 429 ng/mL ± 0.93% 511 ng/mL ±0.39%'^ 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 10/12/11. 

(1) Field matrix spike did not meet method acceptance criteria of 100% ± 30%. TTie analytical uncertainty will be adjusted based on the recovery of the most appropriate spiking level. 

(2) TTie analytical uncertainty has been adjusted for PFHS to ± 35% and for PFOS to ± 43%. 

Page 24 of 99 
Table 14. DAL GW 227R110922 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) %Recovery 

GLP10-01-02-22-017 DAL GW227R 0110922 13.1 NA 60.3 NA 584 NA 

GLP10-01-02-22-018 DALGW227R DB 110922 137 NA 63.1 NA 572 NA 

GLP10-01-02-22-019 DALGW227RLS 110922. 95.7 82.3 147 85.3 637 NC 

GLP10-01-02-22-020 DALGW227R HS 110922 832 81.9 955 89.3 1380 80.2 

Average Concentration (ng/mL) ± %RPD 13.4 ng/mL ±4.5% 61.7 ng/mL ±4.5% 578 ng/mL ±2.1% 

NA = Not Applicable 

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

Samples diluted 20x and analyzed 10/12/11. 

Table 15. DAL GW 227L 110922 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) %Recovery (ng/mL) VoRecovery 

GLP10-01-02-22-021 DAL GW227L 0110922 258 NA 68.7 NA 482 NA 

GLP10-01-02-22-022 DALGW227L DB 110922 254 NA 68.3 NA 465 NA 

GLP10-01-02-22-023 DALGW227L LS 110922 329 NC 147 78.5 542 NC 

GLP10-01-02-22-024 DALGW227LHS 110922 966 71.0 989 92.1 1300 82.7 

Average Concentration (ng/mL) ± VoRPD 256 ng/mL ±1.6% 68.5 ng/mL ±0.58% 474 ng/mL ±3.6% 

NA = Not Applicable 

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

Samples diluted 20x and analyzed 10/12/11. For PFBS, the HS was further diluted to 40x. 

Page 25 of 99 
Table 16. DAL GW 31 OR 110928 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-025 DAL GW310RO 110928 716 NA 318 NA 600 NA 

GLP10-01-02-22-026 DAL GW 31 OR DB 110928 743 NA 322 NA 621 NA 

GLP10-01-02-22-027 DAL GW 31 OR LS 110928 782 NC 395 NC 692 NC 

GLP10-01-02-22-028 DAL GW 31 OR HS 110928 1450 72.1 .1080 76.0 1360 75.0 

Average Concentration (ng/mL) ± VoRPD 730ng/mL ±3.7% 320 ng/mL ±1.3% 611 ng/mL ±3.4% 

NA = Not Applicable 

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

Samples diluted lOOx and analyzed on 10/12/11. 

Table 17. DAL GW 312R 110929 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) %Recovery 

GLP10-O1-02-22-029 DAL GW312R 0110929 1130 NA 829 NA 1380 NA 

GLP10-01-02-22-030 DALGW312R DB 110929 1150 NA 833 NA 1500 NA 

GLP10-01-02-22-031 DALGW312R LS 110929 1910 77.0 1620 78.9 2190 75.0 

GLP10-01-02-22-032 DALGW312R HS 110929 5260 82.4 5150 86.4 5990 91.0 

Average Concentration (ng/mL) ± %RPD 1140 ng/mL ±1.8% 831 ng/mL ±0.48% 1440 ng/mL ±8.3% 

NA = Not Applicable 

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

Samples diluted 10Ox except HS was diluted 500x. Samples analyzed 10/12/11. 

Page 26 of 99 
Table 18. DAL GW 317L 110928 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-033 DAL GW 317L Oi l 0928 <0.0400 NA 0103 NA 0214 NA 

GLP10-01-02-22-034 DALGW317L DB 110928 <0.0400 NA 0.0938 NA 0196 NA 

GLP10-01-02-22-035 DALGW317L LS 110928 0813 81.3 0.907 80.9 0.923 71.8 

GLP10-01-02-22-036 DALGW317L HS 110928 8.37 83.7 8.65 85.5 NA<^> NA*^' 

Average Concentration (ng/mL) ± VoRPD <0.0400 ng/mL 0.0984 ng/mL ±9.3% 0.205 ng/mL ±8.8% 

NA= Not Applicable 

Results for PFBS and PFHS reported from 10/12/11 analysis. Results for PFOS reported firom 10/24/11 intemal standard analysis. 

(1) Sample was not analyzed since the spike level was not expected to be appropriate as compared to the sample concentration. 

Table 19. DAL GW 324L 110923 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) %Recovery (ng/mL) VoRecovery (rtg/mL) %Recovery 

GLP10-01-02-22-037 DAL GW324L 0110923 70.0 NA 82.9 NA 212 NA 

GLP10-01-02-22-O38 DALGW324L DB 110923 70.0 NA 82.1 NA 210 NA 

GLP10-01-02-22-039 DAL GW324L LS110923 146 76.0 163 80.5 274 NC 

GLP10-01-02-22-040 DALGW324L HS 110923 800 73.0 846 76.4 999 78.9 

Average Concentration (ng/mL) ± VoRPD 70.0 ng/mL ±0.0% 82.5 ng/mL ±0.97% 211 ng/mL ±0.95% 

NA= Not Applicable 

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

Samples diluted 50x and analyzed 10/12/11. 

Page 27 of 99 
Table 20. DAL GW 327R 110928 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-041 DAL GW327R 0110928 51.4 NA 125 NA 394 NA 

GLP10-01-02-22-042 DALGW327R DB 110928 51.7 NA 127 NA 399 NA 

GLP10-01-02-22-043 DAL GW327R LS110928 135 83.5 214 88.0 485 NC 

GLP10-01-02-22-044 DALGW327R HS 110928 706 65.4TM 817 69.1 TM 1140 74.4 

Average Concentration (ng/mL) ± VoRPD 51.6 ng/mL ±0.58% 126 ng/mL ±1.6% 397 ng/mL ±1.3% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 10/12/11. 

(1) Field matrix spike did not meet method acceptance criteria of 100% ± 30%. The analytical uncertainty will be adjusted based on the recovery of the most appropriate spiking level. 

Table 21. DAL GW 328R 110927 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-O2-22-O45 DAL GW328R 0110927 27.7 NA 57.2 NA 178 NA 

GLP10-01-02-22-046 DALGW328R DB 110927 28.1 NA 58.5 NA 178 NA 

GLP10-01-02-22-047 DALGW328RLS 110927 106 78.1 137 79.2 249 71.5 

GLP10-01-02-22-048 DALGW328R HS 110927 380 70.4 426 73.6 545 73.5 

Average Concentration (ng/mL) ± VoRPD 27.9 ng/mL ±14% 57.9 ng/mL ±2.2% 178 ng/mL ±0.28% 

NA = Not Applicable 

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

Samples diluted 20x and analyzed 10/12/11. 

Page 28 of 99 
Table 22. DAL GW 328L 110928 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-049 DAL GW328L 0110928 40.3 NA 18.3 NA 1.31 NA 

GLP10-01-02-22-050 DALGW328L DB 110928 40.3 NA 18.5 NA 1.26 NA 

GLP10-01-02-22-051 DAL GW328LLS 110928 47.9 76.0 267 83.0 8.64 73.6 

GLP10-01-02-22-052 DALGW328L HS 110928 115 74.7 98.2 79.8 NA'^' NA'^' 

Average Concentration (ng/mL) ± VoRPD 40.3 ng/mL ±0.0% 18.4ng/mL±1.1Vo 1.29 ng/mL ±3.9% 

NA = Not Applicable 

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

Samples diluted lOx and analyzed for PFBS and PFHS on 10/12/11. Results for PFOS reported on undiluted samples analyzed 10/24/11 by intemal standard calibration. 

(1) Sample was not analyzed since the spike level was not expected to be appropriate as compared to the sample concentration. 

Table 23. DAL GW 330R 110928 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-053 DAL GW330R 0110928 2070 NA 197 NA 600 NA 

GLP10-01-02-22-054 DALGW330R DB 110928 2060 NA 194 NA 586 NA 

GLP10-01-02-22-055 DALGW330RLS 110928 2780 NC 958 76.3 1430 83.7 

GLP10-01-02-22-056 DALGW330R HS 110928 5980 78.3 4360 83.3 5290 93.9 

Average Concentration (ng/mL) ± VoRPD 3070 ng/mL ±OMVo 196 ng/mL ±1.5% 593 ng/mL ±2.4% 

NA = Not Applicable 

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

Samples diluted lOOx except HS was diluted 500x. Samples analyzed 10/12/11. 

Page 29 of 99 
Table 24. DAL GW 330L 110928 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-057 DAL GW330L 0110928 544 NA 431 NA 168 NA 

GLP10-01-02-22-058 DALGW330L DB 110928 515 NA 437 NA 170 NA 

GLP10-01-02-22-059 DAL GW330L LS110928 504 NC 526 NC 254 85.0 

GLP10-01-02-22-060 DALGW330L HS 110928 1190 66.1 TM 1280 84.6 1070 901 

Average Concentration (ng/mL) ± VoRPD 530 ng/mL ±5.5%*^ 434 ng/mL ± 1.4% 169 ng/mL ±1.4% 

NA = Not Applicable 

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

Samples diluted 50x and analyzed 10/12/11. 

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

(2) The analytical uncertainty has been adjusted for PFBS to ± 34%. 

Table 25. DAL GW 331S 110929 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3MUMSID Description (ng/mL) %Recovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-061 DAL GW331S0 110929 535 NA 336 NA 517 NA 

GLP10-01-02-22-062 DALGW331SDB 110929 515 NA 326 NA 494 NA 

GLP10-01-02-22-063 DALGW331SLS 110929 596 NC 403 NC 598 92.5 

GLP10-01-02-22-064 DALGW331SHS110929 1210 68.5TM 1090 75.9 1310 80.4 

Average Concentration (ng/mL) ± VoRPD 525 ng/mL ±3.8%'^ 331 ng/mL ±3.0% 506 ng/mL ±4.5% 

NA= Not Applicable 

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

Samples diluted 50x and analyzed on 10/12/11. 

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

(2) The analytical uncertainty has been adjusted for PFBS to ± 32%. 

Page 30 of 99 
Table 26. DAL GW 335R 110927 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-065 DAL GW335R 0110927 735 NA 1430 NA - 3400 NA 

GLP10-01-02-22-066 DALGW335R DB 110927 744 NA 1400 NA 3290 NA 

GLP10-01-02-22-067 DAL GW335RLS 110927 748 NC NA<^' NA<^> NA<^' NA(^' 

GLP10-01-02-22-068 DALGW335R HS 110927 1430 69.1 TM 2180 76.5 4170 NC 

Average Concentration (ng/mL) ± VoRPD 1080ng/mL±3.7%^ 1420ng/mL ±2.1% 3350 ng/mL ±3.3%*'" 

NA = Not Applicable 

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

Samples diluted 50x for PFBS and analyzed on 10/12/11. Samples were diluted 500x for PFHS and PFOS and analyzed on 10/20/11. 

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

(2) The analytical uncertainty has been adjusted for PFBS to ±31%. 

(3) Sample vras not analyzed since the spike level was not expected to be appropriate as compared to the sample concentration. 

(4) No appropriate spike level was available to assess sample recovery for PFOS. 

Page 31 of 99 
Table 27. DAL GW GRS04 110930 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-069 DAL GWGRS04 0110930 1720 NA 6220 NA 1320 NA 

GLP10-01-02-22-070 DAL GW GRS04 DB 110930 1660 NA 5890 NA 1340 NA 

GLP10-01-02-22-071 DAL GWGRS04 LS110930 2460 77.0 NA<^' NA'^' 1960 63.0 

GLP10-01-02-22-072 DAL GW GRS04 HS 110930 5530 76.8 11800 115 5330 80.0 

Average Concentration (ng/mL) ± VoRPD 1690 ng/mL ±3.6% 6060 ng/mL ±5.5% 1330 ng/mL ±1.5%'^ 

NA = Not Applicable 

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

Samples diluted lOOx for PFBS and PFOS, except HS was diluted 500x, and analyzed on 10/12/11. Samples diluted 500x for PFHS and analyzed on 10/20/11. 

(1) Sample vras not analyzed since the spike level was not expected to be appropriate as compared to the sample concentration. 

(2) Field matrix spike did not meet method acceptance criteria of 100% ± 30%. TTie analytical uncertainty will be adjusted based on the recovery of the most appropriate spiking level. 

(3) The analytical uncertainty has been adjusted for PFOS to ± 37%. 

Table 28. Trip Blank 1 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3M LIMS ID Descrfpt/on (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-074 DALGWTRIP01 0 <0.0400 NA <0.0250 NA <0.183 NA 

GLP10-01-02-22-075 DALGWTRIP01 LS 8.18 81.8 8.35 83.5 7.98 79.8 

GLP10-01-02-22-076 DALGWTRIP01 MS 81.1 81.1 82.3 82.3 68.0 68.0 

GLP10-01-02-22-077 DALGWTRIP01 HS 867 86.7 869 86.9 727 72.7 

NA= Not Applicable 

FMS Mid diluted 10x, FMS High diluted lOOx, and analyzed on 10/12/11. 

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

Page 32 of 99 
Table 29. Trip Blank 2 

GLP10-01-02; Interim Report 22 

/^alysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

PFBS PFHS PFOS 

Concentration Concentration Concentration 

3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery 

GLP10-01-02-22-078 DALGWTRIP02 0 <0.0400 NA <0.0250 NA <0183 NA 

GLP10-01-02-22-079 DALGWTRIP02LS 8.09 80.9 8.27 82.7 7.94 79.4 

GLP10-01-02-22-080 DALGWTRIP02MS 79.1 79.1 80.1 80.1 65.9 65.9TM 

GLP10-01-02-22-081 DALGWTRIP02HS 838 83.8 842 84.2 689 68.9 

NA = Not/Vpplicable 

FMS Mid diluted lOx, FMS High diluted lOOx, and analyzed on 10/12/11. 

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

Table 30. Equipment Rinseate Blanks 

PFBS PFHS PFOS 

3M LIMS ID Description 

Concentration 

(ng/mL) 

Concentration 

(ng/mL) 

Concentration 

(ng/mL) 

GLP10-01-02-22-082 

GLP10-01-02-22-083 

DALGW203L RB 110930 

DALGW220L RB 110930 

<0.0400 

<0.0400 

<0.0250 

<0.0250 

<0.232 

<0.232 

Sample was analyzed on 10/12/11. 

Page 33 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

10 Conclusion 

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

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

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

11 '^niafa/Sample Retention 

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

to 3M Environmental Laboratory standard operating procedures. 

12 Attachments 

Attachment A: Protocol Amendment 22 (General Project Outiine) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 34 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

13 Signatures 

/ 2 

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

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

Gary Hohenstein/Sponsor Representative 'A Date 

Jaisimha Kesari, Study Director / / Date 

Page 35 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 36 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-01 

Amendment 22 

Study Title 

Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 

3M Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 22 

Amendment Date: 

September 14, 2011 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-01 

Sampling Event 

Decatur 3'^^ Quarter Groundwater Sampling 

Page 1 of 7 

Page 37 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-01 

Amendment 22 

This amendment modifies the following portion of protocol: 

"Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 

3M Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording of the protocol are required. 

AMEND TO READ: 

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

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

at Decatur, AL, and conducted as part of the 3M Decatur Phase 3 Program for PFOA (GLP10-01-01). 

The anticipated sample collection will occur around the timeframe of the week of September 19. The 

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

as project GLP10-01-01-22 and reported as interim report GLP10-01-01-122, (reflecting study GLP10-01-

01 and amendment -22). 

Reason: 

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

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

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

Page 2 of 7 

Page 38 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-01 

Amendment 22 

Amendment Approval 

Vy 

Gary Hohens tein. Sponsor Representative Date 

ikJi 

Date Cleston C. Lange, Principal Analytical Investigator 

William Reagen, EH6 Opns Environmental Lab Management Date 

Jaisimha Kes: Study Director 

Page 3 of 7 

Page 39 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-0f 

Amendment 22 

3M Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cleston Lange, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charies Young, Weston Solutions 

Date: September 14, 2011 

Subject: Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program; GLP Interim Report 22 - Decatur 3'" 

Quarter 2011 Groundwater Sampling 

1 General Project Information 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, IVIN 55144-1000 

Phone:(651)737-3570 

Qahohenstein(@mmm.com 

3NI Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

Contacts wkreaQen©mmm.com 

Principal Analytical Investigator 

Cleston Lange 

SWl EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

ccia naetffimmm .com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinak(a>westonsolutions.com 

Phone: (334)-332-9123 

Lab Request Number GLP10-01-01-22 

•Six Digit Department Number Dept #530711, Project #0022674449 

Project Schedule/Test Dates Sampling scheduled for the week of September 19, 2011 

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

Page 4 of 7 

Page 40 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-01 

Amendment 22 

2 Background Information and Project Objective(s) 

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

samples collected from seventeen groundwater wells for Perfluorooctanoic Acid (PFOA). Analyses will be 

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

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

September 19, 2011. The 3M Environmental Laboratory will prepare the sample bottles with all required . 

spikes to ensure that results for PFOA are of a known precision and accuracy. The final report will be 

submitted to Gary Hohenstein and Jai Kesari upon completion under interim report GLP10-01-01-22. 

3 Project Schedule 

Sample collection bottles will be prepared by the 3M Environmental Laboratory. Sample bottles will be shipped 

in coolers overnight to 3M Decatur for arrival by Friday, September 16, 2011. 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 PFOA. 

A total of eighteen sampling locations have been specified. For each sampling location, four sample bottles will 

be collected (sample, sample duplicate, low field matrix spike, and high field matrix spike). The "fill to here" line 

on each 250 mL Nalgene bottle will be 200 mL. Two sets of trip blank spikes consisting of reagent-grade water, 

as well as WJO additional bottles to be used for the preparation of equipment rinseate blanks, will be prepared at 

the 3M Environmental Laboratory and sent to the sampling location wiUi the other bottles. Results from 

GLP10-01-01-02, GLP10-01-01-09, and GLP10-01-01-17 were used to detennine the field matrix spike levels 

for GLP10-01-01-22 listed in Table 1. 

Table 1. Sampling Locations and Field Matrix Spike levels. 

Well No. Sample Level Spike Cone. (ng/mL) 

317L Low 1 

High 10 

220R, 220L, 328L Low 10 

High 100 

203L, 222R, 227R, 227L, 310R, 

324L, 327R, 330L, and 331S 

203L, 222R, 227R, 227L, 310R, Low 100 

324L, 327R, 330L, and 331S High 1000 

GRS04, 312R. 330R, and 335S Low 1000 

High 5000 

328R Low 100 

High 500 

Trip Blank Sets 

1 and 2 

Trip Blank Sets Low 10 

1 and 2 Mid 100 

Trip Blank Sets 

1 and 2 

High 1000 

Page 5 of 7 

Page 41 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-01 

Amendment 22 

5 Test Methods 

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

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

Analysis". Due to previous data for these sampling locations (GLP10-01-01-02, GLP10-01-01-09, and GLP10-

01-01-17), samples GLP10-01-01-22 will most likely require dilution. Samples requiring dilution will be 

prepared in Milli-Q water prior to analysis by ETS-8-044.0. The data quality objectives for these studies are 

quantitative results for tiie target analytes with an analytical accuracy of 100+30%. Field matrix spikes not 

yielding recoveries within 100±30% will be addressed in the report and the filial accuracy statement may be 

adjusted accordingly. 

Alternately, samples may be analyzed by ETS 8-110.1 "Analysis of Fluorochemicals in Exti-acts Using HPLCElectrospray-Mass Spectrometry-Mass Spectrometry as an analytical reference for the sample locations 

analyzed by direct on-column injection analysis of samples diluted with methanol as opposed to Milli-Q water. 

Calibration curves used for both ETS-8-044.0 and ETS-8-110.1 will be constructed using a reference material 

containing both linear and branched isomers of PFOA. Field matiix spikes will be prepared with a solution 

prepared with a reference material containing predominantly linear PFOA. Laboratory control samples (LCS) of 

linear and branched PFOA will be prepared at three concentration levels. 

6 Reporting Requirements . 

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

mati-ix spikes. Trip blank sets will be reported for the sampling event as will any equipment blanks prepared in 

the field. Laboratory control spikes of reagent water prepared at the time of sample extraction will also be 

reported and used to evaluate Uie overall method accuracy and precision. Method blanks of reagent vrater 

prepared at the time of sample exti-action will be used to determine the method detection limit. Any laboratory 

mati-ix spikes that may be prepared will also be included in the final report. 

7 Email Correspondence • 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 42 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Analytical Protocol: GLP10-01-01 

Amendment 22 

From: Frinak, Timothy R. . 

Sent: Monday, September 12, 2011 10:48 AM 

To: Young, Charles T. 

Cc: Smith, Mart:in; Johnson, Kevin A.; Missildine, Bret C. 

Subject: Bottles - GW sampling Decatur, AL 

Charlie, 

The 3"* quarter GW sampling will begin next Monday at Decatur. The sampling for FCs will be inside this 

time and include the following: 

203L 

220R ' 

220L 

222R 

227R 

227L 

310R 

317L 

324L 

328R 

328L 

,330R 

330L 

335R 

GRS04 

RW312R 

RW327R 

RW331S 

We will also need Milli-Q water and bottles for two (2) rinseate blank samples. 

Page 7 of 7 

Page 43 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

ATTACHMENT B: REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S) 

Page 44 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

bl 11012a linear.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = -1.81e+003 x'^2 + S.55e+005 x + 1.68e+004 (r = 0.9997) 

1.7e7 

1.6e7-

1.5e7-

1.4e7-

30 35 40 

Concentration, ng/mL 

Data printe d by STW 

Printin g Time: 11:10:29 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 1 o£ 1 

Page 45 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

• bl l 1012a branched.rdb (PFOS): "Quadratic" Regression ("1 /x" weighting): y =-2.44e+003 x'^2 + 4.45e+005 x + 1.66e+00S (r = 0.9999) 

8.0e6 . 

7.5e6; 

7.0e6^ 

6.5e6^ 

6.0e6^ 

5.5e6^ 

5.0e6^ 

4.5e6^ 

c 

8 4.0e6^ 

ro" 

< 3.5e6^ 

3.0e6^ 

2.5e6-

2.0e6 

1.5e6 

1.0e6-

5.0e5 

9 10 11 

Concentration, ng/mL 

12 13 14 15 16 17 18 19 

Data printe d by STW 

Printin g Time: 11:05:28 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 1 o f 1 

Page 46 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

*** Buster J2930203 Batch Name: blll012a.dab 

bl 11012a.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -5.75e+003 x'^2 + 6.98e+005 x + 9.76e+003 (r = 0.9998) 

S.1e7 

S.0e7 

45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Data printe d by STW 

Printin g Time: 10:54:50 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 1 o£ 1 

Page 47 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

**• Buste r J2930203 Batch Name: blll012a.da b 

bl 11012a.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -7.04e+00S x'^2 + 8.84e+005 x + 2.05e+004 (r = 0.9999) 

45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Data printe d by STW 

Printin g Time: 10:53:44 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 1 o f 1 

Page 48 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I

Sampto Nome: til11012a017' Sarripte ID: •10007.27-8- Rte: •b111012B. 

PeaK Namo: 'PFOS- Mass{M): '499.0/99.0 armJ,499.0/B0.0 amu,499.0/130.0 

Commani: '1.0 ng'mL FC std In MiDI Q Watw* Annoialion:' 

Sample Index: 17 

Sampla Type; Standard 

Concentration: 0.732 ng/mL 

Calculated Cone: 0.767 ng/mL 

Acq. Date: 10/12/20 

Modified : 

Proc. Algorilli i 

Noise Percental 

Base. Sub. Win< 

Peak-Split. Fai 

Report Largest 

Min. Peak Height: 

Smoothing Width; 

RT Window: 

Height: 

Start Tin 

':49 PM 

Peat 

r

SarapteName:-b111012B02e- Sampte ID:-Solvent BJank' FOe: •bl11012a.wtfr 

Peak Name: "PFOS* Mass{es): •499.IV99.0 amu .499.0/80.0 amu ,499.0/130.0 amu" 

Comment "Mii O Wat«r TN11-0334" Annolatkm: ~ 

Sample 

iraple Type: 

.ration : 

Peak Height: 

! Relative RT; 

Height; 

Start Time 

End Time; 

13.0 

I

SampleName:-b111012a030- SamptelD:-LCS-111007-r 

Peak Name: "PFOS" Mas»{es): -499.0«9.0 amu,499.0/80.0 

Comment: "2pp*) LCS" Annotation: ~ 

Sanple Index; 30 

Saraple Type: OC 

Calci 

Acq. Time; 

Modified ; 

Proc. AJgorittio: 

Noise Percentage 

Base. Sub. Hindo: 

Peak-Split. Facti 

0/12, 

Min. 

Min. Peak W: 

Smoothing M: 

RT Window: 

Expected RT 

Use Belativ t 

Pea) 

1.25e5-

1.20e5-

1.15e5-

LlOeS 

I.OSeSI.OOeS9,S0e4-

9.00e4-

8.50e4-

S.00e4-

7.50*4 • 

7.00e4• 

S.S0e4-

S.00e4' 

5.S0ft4' 

5.00e4' 

4.50e4' 

4.00e4' 

3.50e4' 

3.00»4' 

2.50»4' 

2.00e4 

1.50e4 

1.0064 

5000.00 

0.00 

I

Sample Name: *b111012a033" Sample ID: •LCS-111M7-4- File: 1)1110123,' 

Peak Name: "PFOS" Mass{es): "499.0/99.0 amu,499.0/80.0 antu,499.0'130.0 amu" 

Comment; *20ppb LCS" Annoiatkxi: ~ 

Sample Index; 33 

Sample Type: QC 

Concentration: 18.5 ng/mL 

Calculated Cone: 14.4 ng/nL 

Acq. Date: 10/12/2011 

Acq, Tine; 8:«5:05 PM 

1.00 0 

Type; Valle i 

15.< 

r42915 

16.9517.37-J7.46 

Data printe d by STW 

Printin g Time: 11:12:52 AM 

Printin g Date: Wednesday, December 07, 

Page 1 o f 5 

Page 49 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

*** Buste r J2930203 Batch Name: blll012a.da b 

I

Sample Name: tlllOIZaOSe" Sample ID: 1.CS-111007-7" 

Peak Name: "PFOS" Ma»s{es): "499.0/99.0 amu,499.0/80.0 ai 

Comment: "SOppb LCS" Annotatton;"" 

Sampl e Index : 36 

Sampl e Type : OC 

Concentration : 16. 2 r 

Calculate d Cone : 35. 1 r 

Acq . Date : 10/12/201 1 

Acq , Tine ; 9:4B:2 2 PM 

Modlfi i 

. Algo l 

ntage : 

fiaae. Sub . Window: 

Peak-Split . Factor ; 

Repor t Larges t Pea k 

Min . Pea k Height : 

Pea k Width : 

Smoc ) Widt 

2.1fl6 

Z0e6 

1.9o6-

1.SeE' 

1.7e6 

1.e«B' 

1.5ft6-

1.4e6' 

1.3e6 

1.2eel.leS1.0e6-

9.0eS 

8.0*5 

7.0e5-

6.0e5 

5.0e5 

4.0e5 

3.0e5 

2.0e5 

I SamriBName:T>in012a057" Sample ID; "GLP10^H-02-22-001* File: "b111012a.wir 

Peak Name: 'PFOS' M3ss(es): "439.0/99.0 ai 

• Comment "DAL GW203L0" Annoialioo:-

Sampl e Index : 57 

Sanpl e Type ; Unknown 

Calculate d Cone : 

Acq . Date : lOi 

Acq . Time : 5: ! 

Modified : 

Proc. Algorithm : In l 

Noise Percentage: 

Base. Sub. Uindow: 

u,499.a>'130.0 amu" 

liQua n - MQII 

5,0e5' 

4.ae5 

4.6e5' 

4.4e5' 

4265 

4.0e5' 

3.8e5' 

3.6eS' 

3,4e5-

3.Ze5 

3.0e5' 

2.8e5' 

2.6a5' 

2.4e5-

2.2e5' 

2.0e5' 

1.ee5 

1.6e5-

1.4e5' 

Jl 

I

Sample Namo: "b111012a061' Sample ID: "GLPHW)1-02-22-005" File: "b111012a.wrr 

Peak Name: "PFOS" Ma*»(es): "499.0/99.0 amu.499.0/80,0 amu,499.0/130.0 

Comment:-DAL GW 220ft 0" Annotatksn:-

Modified : 

Proc . Algorithm : 

Nois e Percentage : 

Hin . Pea k Height : 

Min . Pea k Hidth : 

Smoothin g Width : 

:elliQua n - MQI 

Valle y 

l e : 15. 3 

104726 0 c< 

Height ; 

Star t Ti r 

E n d Tim e 

I SainpleName:"b111012aD69" Sample ID: •GLP10-01-02-22-009" File: •b11l012a.wi(r 

Peak Name: "PFOS" M3ss(es):' 

• Comment'DAL GW 220L 0" Annotation:' 

Sampl e Index : 69 

sarapl e Type : Unknown 

Modified ; Yt 

Proc . Algorithm ; Inte l 

Base . Sub . window : 

Peak-Split . Factor : 

Larges t Pe a 

e a k Height : 

e a k Width : 

i n g Width ; 

15. 3 

64772 5 COI 

3.76et00 5 

Data printe d by STW 

Printin g Time: 11:12:52 AM 

Printin g Date: Wednesday, December 07, 2 011 

Page 2 o f 5 

Page 50 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I Sam;i«Nam»:-b111012a073- Sample ID: ^3LP1CKI1^^2.22-013• Flo: •bl110l2a.wiir 

PMk Nam*: "PFOS- Mass<M]:'499.0/99.0 anx],499.(VBD.O amu.499.0/130.0 

I Comn»nt:-DALGW222R0- Annotalkm:-

Data printe d by STW 

Printin g Time: 11:12:52 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 3 o f 5 

Page 51 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

•* Buste r J2930203 Batch Name: blll012a.da b 

Data printe d by STW 

Printin g Time: 11:12:52 AH 

Printin g Date: Wednesday, December 07, 2011 

Page 4 of 5 

Page 52 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

*** Buste r J2930203 Batch Name: blll012a.da b 

Data printe d by STW 

Printin g Time: 11:12:52 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 

Page 53 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buster J2930203 Batch Name: blll012a.da b 

I SamFteN3n«:'b1110l2aOir Sample ID:'10007-27-8" FUe:"b111012a.wlfr 

• Peak Name: 'PFOS* Ma»<es): "499.0/99.0 Bmu,499.0m0.0 amu.499.<V130A ami 

• Comment *1.0 ng'mL FC std m MPK Q Water* Annotation: ~ 

Sample Index: 17 

Sample Type; Standard 

Concentration; 0.196 ng' 

Calculate d Cone; 0.197 ng 

Acq. Dato: 10/12/2011 

Acq. Time; 3;07;49 PM 

7.0e4 

e.5a4 

G,0e4 

5.S»4 

5,0e4 

3.Cle4 

25»4 

I

Sampto Name: "b111012a028" Sample ID: "Solvent Blanit" Fi%: 'b111012a.wir 

Peak Name: 'PFOS' Mass(es): "499.0/99.0 8mu.499.0/8ao amu,499.(V130^ amu" 

Comment: 'Mfli 0 Water TN11-0334* Annotation: 

Sample Index; 2B 

Sanple Type; Unknown 

Concentration: H/A 

Calculated Cone; < 0 

Acq. Date; 10/12/2011 

Acq. Time: 6:59:37 PM 

Modified : Yes 

BT Window: 30.0 sec 

Expected RT: 15.3 min 

Use Relative RT : tia 

Area: 

Height; 

Star t Tin 

End Time: 

3.59e+002 cps 

Modified ; 

BT Window: 

Expected RT: 

I

Sample Name: *b111012aO3O" Sample ID: ^CS-111007-1' 

Peak Name: "PFOS" Massfes): "499.0/99.0 amu.499.0/80.0 

Comment:"2ppbLCS" Annotation:'" 

Sample Index: 30 

Sample Type: OC 

Concentration: 1.85 ng/nL ,^5,5. 

Calculated Cone: 0.3S2 ng/nL 

Acq. Date: 10/12/2011 1.20e5-

Acq. Time: 7:41:46 PM 

1.15«5-

D*0 sec l.lOeS15.3 min 1.05e5-

1.00e5 

11^2 min 9.50e4-

^ 9.00e4-

e4004 cps 

15.0 min 8.50e4 

15,3 min 

8.00e4' 

7.50e4 

g 7.00e4-

^ 6.50e4 

i 6.00e4. 

- 5.50B4 

5.00O4-

4.5004 

4.00o4 

3.50o4 

3.00e4 

2.50»4 

2.00O4 

1.S0»4 

1.00o4 

5000.00 

0.00 

I SamploNamo:"b111012a033" Sample ID: TCS-111007-4' File:"b1110l2a.wi(r 

Peak Nan^: 'PFOS* Mau{es): "499.0/99.0 ar 

• Comment '20ppb LCS" Anrwtatlon:' 

Sanple Index: 33 

ig.O/BO.0 amu,499.0/130.0 at 

Height; 

End Tiro1S.« 17.3707-46 

13.0 13.5 14.0 14.5 15.0 15.5 16.0 16^ 

i.iOee1.05e6 

1.00e6 

9.50eS' 

9.00e5-

8.S0e5 

8.00e5 

7.50e5-

7.00e5 

6.50B5 

§• 6.00e5 

I" 5.50e5 

£ 5.00e5 

4.5ae5 

4.00e5 

3.50e5 

3.00e5 

230e5 

2.00e5 

1.50e5 

1.00e5 

5.00e4 

0.00 

Data printe d by STW 

Printin g Time: 11:08:47 AM 

Printin g Date; Wednesday, December 07, 2011 

Page 1 o f 5 

Page 54 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

Data printe d by STW 

Printin g Time: 11:08:47 AM 

Printin g Date: Wednesday, December 07 

Page 55 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

• Sample Name;'b111012a073' SamplelD:' 

I PeaK Narrte: "PFOS" MaM<es):'499.0/99.0 

1 Comment: "DAL GW 222R 0" Anrwtatlon: "" 

Sanple Index; 73 

•GLPIOKH-02-22-013" Fie: "b111012a.wir 

ainu.499.a/80.0 emu ,499.0/130.0 amu' 

5.4e5 

52e5 

5.0e5' 

43e5' 

4.6e5 

AAe5-

4.2e5 

4.0e5 

3.8e5 

3.6e5 

3,4e5 

3.2e5 

3,0B5 

2^e5 

2.6e5 

2.4e5 

22e5 

2.0eS 

12e5 

1.0eS 

e,0e4 

6.0e4 

4X)e4 

2J)e4 

4,5 15.0 15 J 16.0 16.5 17,0 17.5 

I SanipleNflme:"bl110128081" Sample ID: •6LP10^1-02-22-Oir File: "b111012a.wir 

Peak Name: "PFOS" M8ss{es): •499.(V99.0 amu,499.0/BO.O amu,499.0/130.0 amf 

I CoowenfOALGW227R0* Annotation:-

1.2e6• 

1.2e6' 

1.1e6' 

1.1e6 

1.0e6-

9,5o5 

9.ae5' 

8.5e5-

8.0e5' 

7.5e5-

7.ae5-

6.S«5' 

6.0e5' 

5.5e5 

5.0e5-

4.5e5 

4.0e5-

3.5e5 

3.065-

2.5e5-

2.0o5-

14.5 15.0 17.0 17.5 

I

Sample Name:'b111012aOSS" Sample ID:"' 

Peak Name: "PFOS" Maasfes): '499,0/99.0 at 

Comment: DAL GW 227L 0' Annolation: ~ 

Sample Index: as 

1.20e6-

1.15e6-

I.IOee1.05e6-

1.00ee9.50e5-

9.00e5-

8.50e5-

8.00e5-

7.S0a5-

7.0085-

§• 6.50e5-

i 6.00*5-

s 

t 5.50e5-

5.00e5-

4.50e5-

4.00e5' 

3.50«5' 

3.00e5-

2.50e5-

2.00e5' 

1.50o5 

LOOeS-

' 5.00e4' 

0.00-

I

SanipleName;"b111012a093" Sample ID: •GLP1fr01-02-22-02S" File:"b111012a.WTr 

Peak Name: "PFOS" Mass{es): "499.0/99.0 amu.499.0/80.0 amu,499.0/130.0 amu" 

Comment: 'DAL GW 310R 0" Annotation: ~ 

2.ee5 

2.5c5 

2.4e5 

2.3eS 

2.2e5 

2.1e5 

2.0eS 

EKpected RT: 

Use Relative RT; 

Height: 

Start Ti l 

End Tine 

1.0o5-

g.0e4-

e.0e4-

7.0O4-

6.0e4-

5.0O4-

4.0e4-

3.0o4-

2.0e4-

14,5 15.0 15.5 16,0 16.5 17.0 17.5 13.5 14.0 

Data printe d by STW 

Printin g Time: 11:08:47 AM 

Printin g Date: Wednesday, December 07, 2 011 

Page 3 o f -5 

15.5 16.0 16.5 17.0 

Time, mirt 

Page 56 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I

Sample Name: •blll012a097" Sampto ID: 'GLPKW1-02-22-029" Fie: "b111012a.wifr 

Peak Name: 'PFOS" Mas5(es): "499,0/99.0 Bmu.499.0/B0.0 amu,499.0/130,0 " 

Comn>ent:-DALGW312R0- Annolation:- I

Peak Name: "PFOS" Mass{e»): "499.0/99,0 

Comment "DAL GW 324L 0" Annotation:' 

! Index: 109 

14.5 15.0 15.5 16.0 16.5 

I Sample Name: "b111012a109" Sample ID: "GLP10"01-02-22-03r Fde: "b111012a.wii 

iu,499.0/80,0 amu,499.0/130.0 amu" 

9.De4' 

S.0e4' 

7.064-

6,0»4' 

5.0e4-

4.0e4' 

3.0e4' 

2.0e4' 

1.0e4' 

Sample Nanw: •b111012a117* Sample ID: "GLP1&^1-02-22-041' Fie: •l>111012a.wifr I

Peak Name: "PFOS" Mass(e»}; "499.0/99.0 

Comment:"DALGW327R0" Annotation:" 

Sample Index: 117 

Sanple Type; Unknown 

Concentration: H/A 

iu,499.0/80.0 amu,499.0/130.0 amu" 

I SampleName:T>111012a121" Sampio ID;"GLP1O-O1-02-22-045" Flle:-b11101Za,w«r 

Height; 

Start Titu 

End Time: 

22e5-

2.0*5 

i.4e5-

12e5-

1.0e5-

e.0e4' 

e.0e4' 

4.0e4' 

2.0e4 1 

Peak Name; "PFOS" Mass(e9): "499,0/99.0 ar 

• Comment "DAL GW328R 0" Annotation:' 

Sarnple Index: 121 

Sample Type: Unknown 

Modified ; 

Height; 

Star t T: 

End Tin. 

2,64e40D5 cpa 

j,4S9.0/80.0amu,499,0/130.0 amu' 

3.4eS' 

3.265-

3.0e5-

2.865 

2.ee5-

2.4e5' 

2.2e5-

2.065 

1.eeS 

1.4e5-

13.0 13.5 

Data printe d by STW 

Printin g Time: 11:08:47 AM 

Printin g Date: Wednesday, December 07, 

Page 4 o f 5 

Page 57 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I SamplaNam6:"b111012al33' Sample ID;"GLPIO-01-02-22-053" Fle:"b111012a.w1fr 

Modified; 

RT Hindoi 

Expected 

•

Peak Name: TFOS" Massfes): "499.0«9.0 amu ,499,0/80,0 ar 

Comment; "DAL GWSSORC Annotation:-

Sample Index; 133 

Sanple Type: Unknown 

Concentration; H/A 

Calculated Cone: 225. ng/mL 

Acq- Date; 10/14/2011 ^'^^ 

Acq. Time: 7:56:15 AM 

2.8e5 

Yes 

30.0 sec 

15.3 min 2.665 

Manual 2.4e5 

15.2 min 

52616 counts 

l.Sle-tOOS cps "6 5 

H . 9 min 

^^•^ 2.0e5 

1.2e5 

1,0eS 

8.0e4 

8.064 

4.0e4 

2.064 

J,499.0/130.0amu* 

4.5 15.0 1S.5 16.0 16.5 17.0 17.5 

I SampleN8ine:'bl1101Za141" SampfeID:"GLP10-01-02-22-057" F4e:"bl110128.w 

Peak Name: "PFOS" Mass(es); '499.0/99.0 aniu,499,0/ 

• Comment "DAL GW330LO" Annolation:-

Sanple Index: 141 

Sampl e Type : Unknow n 

Calculate d Cone: 88.5 ng/raL 1,3e5-

Acq. Date: 10/14/2011 

Acq. Time; 10;45;10 AM ^-^^ 

1.2e5 

Kodiried; Yea 

RT Window : 30. 0 se c 1.2e5-

Expecte d RT ; 15. 3 «i n 

Use Relative RT: Uo • " 

1.1e5 

Int . Type ; Manua l 

Retention Time: 15.2 rain 1-0e5 

Area ; 78237 8 count s gj^ . 

Height: 1.14e-tO05 cps 

Start Time: 14.9 nin 9.0a4-

End Time; 15.3 min , 

e.5e4 

B.De4' 

£ 7.5e4. 

7.0e4 

•£ 

« 6.5e4 

M 6.0e4 

5.564 

5.064 

4.5e4 

4.0e4 

3.564 

3.064 

2.5e4 

2.0*4 

1.Se4 

iu,499.CV130.0 amu" 

'.OK H 

i 15.0 15.5 16,0 16.5 17.0 17,5 

I

Sample Name: "b111012al45" Sample ID:'GLP10-01-02-22-O6r File: "b11l012a.wifr 

Peak Name; "PFOS" Mass(es): "499.0/99.0 amu,499.0/80.0 amu,499.0/130.0 

Comment:-DALGW331S0" Annotation: " 

Sample Index: 145 

Saople Type; Unknown 

Concentration: H/A 

Calculate d Cone: 267. ng/nL 

Modified ; 

RT Window: 

Expected RT: 

3.36e+O05 

I Sample Name: "b111012a157' Sample ID;'GLP10-01-02-22-069" File: "blUOIZa.wiT 

Sampl e Type ; 

Calculate d Cone : 75S. r 

10/14/2011 

4:23:15 PM 

Betentii 

Height: 

Manual 

le: 15.2 

3226686 ci 

iu,499.0/80.0 amu,499.0/130.0 amu" 

4.4e5-

4.2e5-

4.065-

3.Be5-

3.6e5-

3.4B5-

3JB5 -

3.0e5-

2.Be5-

2.6e5-

2.4eS2.2e5-

2,0e5-

1J!95-

1.0e5-

e.0e4-

6.0e4-

145 15.0 15.5 16.0 16,5 17.0 17.5 5.0 15.5 16.0 16.5 ^^J3 17,5 

Data printe d by STW 

Printin g Time: 11:08:47 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 5 o f 5 

Page 58 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

• SampleNBine;'b111012a017* Sample ID: "10007-27-6" 

I Peak Name:'PFBS' Mass(«s}:'299.0/99.0 amu,299.a/80. 

I Commenti'l.Ong'mLFCGtdlnMliQWatei' Annotation: 

Sanple Type; Standard 

Concentration; 1.00 ng/mL 

Calculated Cone; 0.999 ng/nL 

Acq. Date; 10/12/2011 

Acq. Time: 3:07:49 PM 

i l f led; 

Smoothing Hidth; 

RT Window: 

Expected RT: 

No 

•: 12. 5 

89620 5 COL 

1.ese+oos 

I

SampleName:"b111012B02B" Sample©:"SolventBlank" File:*b111012a.wHr 

Peak Name: "PFBS" Mas5(es):"299.CV99.0amo,299.0/BO, 

Comment "MB Q Water TN11-0334" Amolatioo:" 

Sample Index: 28 

Sanple Type: Unknown 

Concentration ; H/A 

Calculate d Cone : < 0 

Acq. Date: 10/12/2011 

Acq. Time; 6;59;37 PM 

ModifJ °d; 

itelliQu . 

0.00 

0.00 

I

5ampl6Name;"b111012a030" SamplelD:"LCS-111007-' 

Peak Name: "PFBS" Massfes); "299.0/99.0 amu,299.Q/B0. 

Commeni; '2ppb LCS' Anrwtatlon; ** 

Sanpl e Index : 3 0 

Acq. Time ; 7: 4 1: -le PH 

Modified ; No 

Pcoc. Algorithm; IntelliCua n - IQA 

Min. Peak Height: 0.00 cps 

Min. Peak width ; 0.00 sec 

Smoothing Hidth : 0 points 

RT WindoH: 30.0 sec 

Expected RT; 

Use Beli 

Height: 

Start Til 

End Time 

i RT: 

• Sample Name: "bl11012a033' Sample ID:'LCS-IIIOO/M" 

I Peak Name; "PFBS Massfes): "299.0/99.0 a inu,299.0m0.0 

• Comment; '20ppb LCS" A/inotation: *" 

Sampl e Index : 33 

Sample Type; QC 

Concentration : 20. 0 ng/m L 

Calculate d Cone : IB. 4 ng/m L 2.6eB10/12/201 1 

Acq . Time : 8:45:0 5 PM 2.5e6-

2.4D6-

Modified : Y e s 

2.4D6-

Proc, Algorithm; mtelllQua n - MOI I 2.3e6-

Nois e Percentag e SO 

Base . Sub . Wlnd o I.O O min ' 2.2e6-

Pea)i-Split. Fact r ; 2 2.1e6-

a k : tl o 

Min. Pealt Height 2.0e6-

Min . Pea k Hidth : 0.0 0 se c 1.9e6-

Smoothin g Hidth ; 

1.9e6-

RT Window : 30. 0 se c l.ee6-

12. 6 mi n 

Us e Relativ e RT; 11 o 1.7e6-

1.6e6-

Int . Type ; Valle y 

1.6e6-

12. e mi n 1.5e6 

Area : 13 9766 9 count s 

Height : .egefOoe cps 1.4«6-

Star t Time : 12. t mi n 1.3e6-

E n d Time : 13. 2 ni n 1 1.2ee1.1e6-

1.0e6-

9.065-

8.0e5' 

7.0e5-

6.0e5-

5.0o5-

4.0o5-

3.0e5-

2.0e5-

1.0e5-

0.0-

File: "bil l 012a,w 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 1 of 13 

Page 59 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I

Sample Name; •b111012a036" Sample ID; "LCS-II1007-7' 

Peak Name: "PFBS' Massfes): '299.0/99.0 amu,299,0/80,0 

Comment; "SOppb LCS' Annotation: " 

Sample Index; 36 

Sample Type: QC 

Comment 'DAL GW 203L 0" Annotation;' 

Sample Index: 57 

Sample Type; Unknown 

Modified: 

RT Windov; 

Expected RT: 

Uso Relativ e 

1.70e-(005 cps 

I

SampteNamo:-b111012a069" Sample ID: "GLP1(M)1-02-22-009" File: "b111012a.wir 

Peak Name: "PFBS" Mass{es): -299.0^9.0 amu.299.oraO.O 

Comment "DAL GW 220L 0" Annotation: " 

Height: 

Start Tine : 

11.5 12.0 12,5 13.0 13.5 14,0 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2 011 

Page 2 o f 13 

Page 60 of 99 
GLP10-01-02; Interim Repori 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

•** Buster J2930203 Batch Name: blll012a.dab 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

"Printin g Date: Wednesday, December 07, 2011 

Page 

Page 61 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 62 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I

Sample Name: "t)lll012a12r Sample ID:"i 

Peak Name; 'PFBS' Mass(es): '299.0/99.0 ai 

Comment: "DAL GW 32BR 0" Annolation: ~ 

Sample Type; 

Concentration 

Calculated Coi 

Acq. Date; 

27.7 ng/rsL 

10/14/2011 

3:12:51 AM 

Modified: 

RT Window: 

Expected BT; 

24e5 

2Je5 

2.2B5 

2,1e5 

2.0e5 

1.9e5 

1.Se5 

1.7e5 

l£e 5 

1.5e5 

1,4o5 

1.3e5 

U e 5 

l.leS 

1.0e5 

9,0e4 

6.0*4 • 

7.0«»4 

e.0e4 

5.0e4 

4.0e4 

3.0»4 

1.0e4 

(

Sample Nanw: "blllOUalZg" Sample ID; "GLP10-01-02-22-049' File: "blllOIZa.wir 

Peak Name: "PFBS" Massfes): "299.0/99,0 

Comment "DAL GW 328L 0" Anrwtation: " 

Sample Index: 129 

Expected RT; 

Use Relative RT; Ko 

Start Ti 

End Time 

Hanual 

ie: 12.5 ni n 

3t6B4tO counts 

e.69e'O0S cps 

12.2 oi n 

12.S ni n 

I

Sample Name: "bl 11012a133" Sample ID: '< 

Peak Name: "PFBS" Mass(es): "299.0/99.0 ai 

Comment: "DAL GW330R0" AnnotaSon:-

Sample Index; 133 

Saople Type: Unknown 

Modified; 

RT Window: 

Expected RT: 

I

Sample Name: "b111012a14r Sample ID: "GLP 10^1-02-22-057" File: •b111012a,w«r 

Peak Naff«; "PFBS" Mass(es): "299.0/99.0 amu,299.a'80.0 

Comment "DAL GW 330L 0" Annotation:"" 

Height; 

Start Til 

End Time 

2.75e'006 cps 

2.7e6 

2.6e6 

2.5e6 

2.4e6 

2.3e6 

22ee 

2,1e6 

2,0e6 

1.9e6 

1.6e6 

1.5e6 

1.4o6 

9.0e5 

e.0e5 

7.0e5 

e.0e5 

5,0*5 

4.0e5 

3,0e5 

2,0e5 

12.0 12,5 13.0 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: WednesdayDecember 07, 

Page 5 o f 13 

Page 63 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buster J2930203 Batch Name: blll012a.dab 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 6 of 13 

Page 64 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

T

Sample Name: 'b111012a043" Sample ID; "GLP 1CW)1-02-22-082" Fie: •b111012a.wir 

Peak Name: 'PFBS' Mass(es}: "299.0/99.0 amu,299.0/80,0 amu" 

Commeni: •DAL GW 203L F?B" Annotattoo:-

Sanpl o Index : A3 

Saopl e Type : Unknow n 

Concentration ; M/A 

Calculated Ccnc: 0.00165 ng/nL G 

Acq. Date; 10/13/2011 

Acq. Tine : 12:16:00 AM 

lllied ; Ho 

tthn : IntelliCua n - 1 

sight; 0.00 cps 

tdth; 0.00 sec 

6.07e<003 

-.10.15 -.10.53 11.18 

10.5 11.0 

I

Sampte Name; 'b111012aOir Sample ID: "10007-27-8" File: •b111012a.wtfr 

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

Comment "1.0 ng'mL FC sbl in Ml i Q Watei* Annotation;"" 

Saraple Index; 17 

Saraple Type; Standard 

Concentration; 1.00 ng/mL 

Calculated Cone: 1.04 ng/nL 

Acq. Date: 10/12/2011 

Acq. TlQe: 3:07:19 PM 

Modified : Ho 

Proc. Algorithm: IntelliQua r 

Kin , Peak Height; 0.00 : 

Hin . Peak Width; 0.00 £ 

Smoothing Width: 0 p< 

RT Window: 30.0 ; 

Expected RT: 14.2 n 

Use Relative BT; No 

Typo; 

Heigtit: 

Start TiEie: 

End Tirae: 

Valley 

14.3 min 

17355 counts 

l.69e+0D5 cps 

1.6«5 

1,Se5 

1.4e5 

1.3«5 

1.2o5 

1,1e5 

1.0e5 

9.0e4 

8.0e4 

7.0e4 

6.0e4 

5.0e4 

4.0e4 

3.0e4 

2.0e4 

1.0e4 

12.0 12.5 14.5 15.0 15.5 16.0 16.5 

I

Sample Name: "bll1012a028" Sample ID: 'Solent Slank" Fie: •b111012a.wir 

Peak Nanw: "PFHS" Mass(es): "399.0/99.0 amu,399.0/80.0 amu" 

Comment: "Mli 0 Water TN11-0334' Annotation: ~ 

Sample Index: 23 

Sample Typi 

Conc t 

lalcu l led COI 

Proc. Algi 

N/ft 

Ho 

ithn ; InteliiQua i 

Min. Peak Height: 0.00 ( 

Kin . Peak Hidth : 0.00 : 

SDOothing Width: 0 p< 

RT Window: 30.0 : 

1 RT : 

Use Relativ 

Int . Type; 

Retention 1 

Height: 

! RT: No 

79et002 cps 

I

SampteName:"bll1012a030' Sample ID: "LCS-IIIOO?-!" File: •bll1012a,wifr 

Peak Name: "PFHS" Mass(es): "399.0/99.0 amu,399.0/80.0 

Comment: "2ppb LCS" Annotation: " 

Sample Index: 30 

Sample Type; QC 

Calculated Cone: 2.10 

Acq. Date: 10/12/201 

Acq. Time: 7:11:16 1 

HodiCled; tlo 

Proc. Algorithm; IntelliC i 

Kin . Peak Height: 0.00 

Min. Peak Width: 0.00 

ng/ml 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December- 07, 

Page 7 o f 13 

Page 65 of 99 
GLP10-01-02; Interim Report 22 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

*** Buste r J2930203 Batch Name: blll012a.da b 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2011 

Page 8 o f 13 

Page 66 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

12,0 

I

SampteName:-b111012a073" Sample ID: "GLP1041-02-

Peak Name: "PFHS" Mau(es): "399.0/99.0 amu,399,0/80. 

Comment "DAL GW 222R 0" Annolation:" 

Sample Index; 73 

Sample Type: Unknown 

Calculated Cone; 127. ng/raL 

Proc. Algorithro: 

Hin. Peak Height: 

Hin. Peak width; 

Smoothing Midth: 

Expected RT: 

Use Relative 

Int. Type: 

11.2 

tlo 

Valley 

!; 11.3 

ssieiei cc 

1.00e<006 

13.9 

11,9 

I

Sample Name: "b111012a081" Sampio ID: •GLP1CW)1-02-22-0ir Flle:"t)111012a. 

Peak Nam*: "PFHS" Mass(Bs): "399.0/99.0 an 

Comment; "DAL GW 227R 0" Annotatkxi:" 

Sample Index: Bl 

Sanple Type; Unknown 

Concentration: H/A 

Calculated Cone; €0.3 ng/nL 

Acq. Date: 10/13/2011 

Acq. Tine: 1:37:19 PM 

idl f ic 

Expected Rl 

Use Relativ 

Int. Type; 

Ho 

I

SampleName:"b111012B085" SamplelD: 

Peak Name: "PFHS" MaM(es}: -399.0/99.0 

Comment "DAL GW 227L 0" Anrvrtatton: " 

Sample Index: 85 

Saraple Type; Unknown 

Concent tat ion: 11/A 

Calculated Cone: 68.7 ng/mL 

Acq. Date; 10/13/2011 

Acq. Tine: 3:02:12 PM 

Modified: tlo 

Proc. Algorithm; IntelliCuan - IQA 

Hin, Peak lieight: 0.00 cps 

Hin. Peak Width: 0.00 sec 

Smoothing width; 0 points 

, lee'OOS cps 

13.5 14.0 14.5 15.0 

Data printec i by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2 011 

Page 9 o f 13 

Page 67 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

14.0 14.5 15.0 

I

Sample Name: l)111012a097" Sample ID: 'GLP10-01-02-

Paak Name: •PFHS' Mass(es): "399.0/99.0 

Comment "DAL GW312R0- Annotatton:-

Sample Index; 97 

Sample Type; Unknown 

Concentration: ll/A 

Calculated Cone; 629. ng/nL 

Acq, Date; 10/13/2011 

Acq. line ; 7 

Proc. Algorithm; 1 

Min. Peak Height; 

Hin. Peak Width: 

Smoothing width; 

RT Hindow; 

Expected RI; 

Use Relative RT: 

13.5 14.0 14.5 15.0 15.5 

Comment: "DAL GW 317L 0" 

Sample Type 

I

Sample Name; •b11101Za109" Sample ID: •GLP10-01-02-22-037" File: "bll 1012a.»fir 

Peak Name: "PFHS" Ma£s(es); "399.0/99.0 amu.399.0/80.0 amu" 

Comment "DAL GW 324L 0" Annotation: ~ 

Sample Index; 109 

Sarapl e Type : Unknow n 

Concentration ; (I/ A 

Cone ; 82. 9 ng / 

Acq . Ti n 

Hodlfiec 

Proc. Algori 

10. 

L;29:08 I 

2.1e5-

2.0O5-

1.9eSc Height; 

>eak Width: 

9.0e4 

fl.0o4 

7.0e4 

6.0e4 

5.0«4 

4.0e4 

3.0»4 

2.0»4 

13.5 14,0 14.5 15.0 15.5 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2 011 

Page 10 o f 13 

Page 68 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buster J2930203 Batch Name: blll012a.dab 

Data printe d by STW 

Printin g Time: 11:02:09 AH 

Printin g Date: Wednesday, December 07, 2011 

Page 11 o f 13 

Page 69 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

•* Buste r J2930203 Batc h Name: blll012a.da b 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 

Page 12 of 13 

Page 70 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Buste r J2930203 Batch Name: blll012a.da b 

I Sar 

• Pat 

• Coi 

Sample Name: •b111012aO45" Sample ID: •GLP10-01-02-22-074" Fie: "b111012a.wf 

Poak Name: "PFHS" Ma»»(Bs): "399.0/99.0 amu,399.0/80.0 amu" 

Comment: "DAL GW TRIP01 0" Annotation: "" 

Sample Index: 45 

Sanple Type; Unknown 

Concentration; N/A 

Calculate d Cone: < 0 

Acq. Date; 10/13/2( 

Acq. Tirae; 12:58;lf 

Modified : 

>ak Height; 

^ak Hidtti; 

telliQ i 

0.00 

0.00 

Heigtit; 

Start Ti 

End Timt 

1900 

ISOO 

- IQ l 1700 

cps 1600 

p^int a 

15O0 

1400 

'"tn 1300 

ountE 1200 

min 

min 1100 

1000 

1 900 

700 

500 

400 

300 

200 

100 

I

Sample Name: 1)1110123043" Sample ID; "GLP10-01-02-22-082' File: "bll 1012a. 

Peak Name: "PFHS" Ma£s(es): "399.0/99.0 amu,399.0/SO.O 

Conwnent: "DAL GW 203L FW" Annotation: ~ 

Sample Index; 43 

Sanple Type; Unknown 

Concentration: It/A 

Calculated Cone; < 0 

•13/2( 

Proc. Algorithn : ; 

Hin. Peak Height: 

12:1€:00 AM 

itelliQua n - IQA 

0.00 cps' 

O.OO 

30.0 

2.5 13.0 135 14.0 14,5. 15.0 15.5 16.0 16.5 

Data printe d by STW 

Printin g Time: 11:02:09 AM 

Printin g Date: Wednesday, December 07, 2 011 

Page 13 of 13 

Page 71 of 99 
GLP10-01-02; Interim Report 22 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Results Name: klll020 a linear.rdb 

16 18 20 

Concentration, ng/mL 

Data printe d by STW 

Printin g Time: 11:21:30 AM 

Page 1 o f 1 

Page 72 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS ih Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll020 a branched.rdb 

kl 11020a branctied.rdb (PFOS): "Quadratic" Regression ("1 / x" weigtiting): y = -1.54e+004 + 2.02e+006 x + 20.3 (r = 0.9999), 

4.0 4.5 5.0 5.5 

Concentration, ng/mL 

Data printe d by STW 

Wednesday, December 07, 2011 

Page 1 of 1 

Page 73 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

*ETS-Kirk Result s Name: klll020a.rd b 

kl 11020a.rdb (PFHS): "Quadratic" Regression ("1 / x" weigtiting): y = -7.53e+004 x''2 + 5.2e+006 x + 4.48e+003 (r = 1.0000) 

10 12 14 16 18 20 22 24 26 28 

Concentration, ng/mL 

30 32 34 36 38 40 

Data printe d by STW 

Wednesday, December 07, 2011 

Page 1 of 1 

Page 74 of 99 
*ETS-Kirk 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll020 a linear.rd b 

I

Sample Namo: "kl 11020a0ie" Sample ID: "10007-37-0' File: "Kl 11020a, 

Peak Name: "PFOS" Mass(es): "499.000/99.000 Da ,499.000/80.000 Da,499.000/130.00D DaComment; "2.5 ng/mL FC std tn MiH Q water" Annotation: ~ 

Sample Inden; 18 

Sample Type; Standaid 

Concentration; 1.B3 ng/mL 

Calculated Cone: 1.68 ng/mL 

Acq. Date; 10/20/2011 

Acq. Tine : 7:55:53 PH 

Modified: Ha 

Pioc. Algo i 1 tho: Specify Pacaiieters - MO 111 

Moise Petcencage; SO 

Baae. Sub. Hindow: 1.00 ni n 

Peak-Split. Factor; 2 

Report Largest Pealt: tea 

Kin . Peak Heigtit : 0.00 cps 

Min. Peak Hidth : 0.00 sec 

Smoothing Width; 0 point s 

RT Window: 30.0 sec 

Expected RT; 16.0 min 

: Reli 1 RT: No 

Heigh' 

T ype ; Va11e y 

itio n Time; 16.0 

3420726 Cl 

15.5 16.0 16.5 17.0 17.5 

I

Sample Name: "kl 11020a025- Sample ID: TN11-0356" Fie: "kl 11020a.w)rr 

Peak Name: "PFOS" Mass(e3): '499.000/99.000 Da,499.000/80.000 Da.499.000/130.000 Da" 

Comment: 'Method Blank' Annotation:" 

Sarsple Index; 25 

Sample Type; Unknown 

Calculated Cone; 0.00105 

Acq. Date; 10/20/201 

Acq. Time; • 10:25:21 

Modified : Yes 

Proc. Algorithm: Specify I 

Moise Percentage; 50 

Baae. Sub'. Hindow; l.OC 

Peak-Split. Factor: 2 

•meters - HQ I 

750-

Hin . I : Height; 

Kin . 1 

Smoothing Hidth : 

BT Window; 

Expected RT: 

Use Relative RT: 

Height: 

Start T: 

End Tim 

6.60e+002 

I

Sample Name: "kl 11D20a027* Sample ID: "LCS-111020-1" File: "kl 11020a.wirr 

Peak Name: "PFOS" Mass(e$): "499.000/99.000 Da ,499.000/80.000 Da,499.00an 30.000 Da' 

Comment; "0.2ppb LCS" Annotatton:"" 

Modified : Yes 

Proc. Algorithm; Specify Par. 

Moise Percentage: 50 

Base. Sub. Hindow: 1.00 

Peak-Split. Factor; 2 

Report Largest Peak; Yes 

Hin . Peak Height; O.DO 

Hin . Peak Hidth ; 0.00 

Smoothing ( 

RT Window; 30.0 

(

Sample Name: "kl l 1020a030" Sample ID: "LCS-111020-4" Fie: "klllOZOa.wifr 

Peak Name: "PFOS" Mas£(e£): "499.000/99.000 Da.499.000/80.000 03,499.000/130.000 DaComment "2ppb LCS" Anriolalion: ~ 

Sample Index; 30 

Sample Type: OC 

Concentration; 1.85 ng/raL 

Calculated Cone; 1.16 ng/mL 

Acq. Date: 10/21/2011 

Acq. Time: 12;12:10 AM 

Proc. Algorithm: Specify Pari 

Base. Sub. window; 1.00 

Peak-Spilt. Factor; 2 

Report Largest Poak: Yes 

Hin . Peak Height: 0.00 

Min. Peak Hidth : 0.00 

Smoothing Width: 0 

KT Hindow; 30.0 sf 

Expected RT; 16.0 mi 

! Relal • RT; tlo 

Int . Type; Valley 

Retention Time: 16.0 min 

Area; 2382495 counts 

Heigtit: 3.42et005 cps 

3.4e5 

3.2e5 

3.0e5 

2.8e5 

2.6e5 

2.4e5 

2.2e5 

2.0e5 

1.8e5-

1.6a5 

1,4e5 

12e5 

1.0e5 

S.0»4 

6.0e4 

4.0e4 

2.0e4 

15.5 16.0 16.5 17.0 17.5 

Data printe d by STW 

Printin g Time: 11:23:25 AM 

Page 1 o f 2 

Page 75 of 99 
GLP10-01-02; Interim Report 22 

/Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Results Name: klll020a linear.rdb 

Data printe d by STW 

Printin g Time: 11:23:25 AM 

Page 2 of 2 

Page 76 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Result s Name: klll020 a branched.rdb 

I

SampleNaffle:*klll020a018" Sample ID: "10007-37-9" I 

Peak Name: "PFOS* Mau(es): "499.000/99.000 Da,499.0(] 

Convnent "2.5 ng/mL FC std in MH O water* AnrK>Ulk)n:" 

Sampl e Index ; I B 

Sampl e Type : Standar d 

Concentration : 0.49 0 ng/n L 

Calculate d Cone ; 0.46 9 ng/ra L 

Acg . Date ; 10/20/201 1 

Modified : 

Peak-Split. Factor: 

Report Largest Peak; 

Min. Peak Height: 

Hin. Peak Hidth ; 

SiBOOthing width : 

RT Hindow: ] 

Expected RT; 

Use Relativ e RT : 

Star t Tin< 

End Time: 16.0 ni n 

4.4e5 

4.2e5 

4.0e5 

3.ee5 

3.ee5 

3.4e5 

3.2e5 

3.0e5 

2.ee5 

2.6e5 

2.4e5 

2.2e5 

2.0e5 

1.4e5 

1.2e5 

1.0e5 

15.0 15.5 16.0 16.5 17.0 17.5 18.0 

I

SampteName:-k111020a025" SamplelD:*TN1l-0356" Fle:>111020a.wiir 

Poak Name: TFOS" Ma»(es): "499.000^9.000 Da,499.000«0.000 Da ,499.000/130.000 DaComment "Method Blank" Annotation:" 

Sample Index: 25 

I Cone; 0.000137 ng/mL 

10/20/2011 

I0;25;21 PK 

l b. Windoi. 

L-Split 

Report Largest Peak: 

Hin. Peak Height: 

Min. Peak Hidth : 

Smoothing Hidth ; 

RT Window: IS 

Expected RT: 

: Reli ; RT; 

13.5 14.0 14.5 15.0 

I

Sample Name: "k111020a027" San«)le ID:'LCS-111020-1" 

Peak Name: "PFOS" Mass<es): "499.000/99.000 Da,49g.000 

Commeni: *0.2ppb LCS" Annotation: ~ 

Sample Index; 27 

Sample Type: 

:ed Cone;' 0.0320 

Base. Sub. -window; 

Peak-Split. Factor; 

Report Largest Peak; 

ig/raL 

ig/mL 

Smoothing Hidtt 

RT Hindow: 

Expected RT: 

Use Relative RI 

3.4»4 

3.2e4 

3.0e4-

2.3e4 

2.6e4 

2.4e4 

2.2e4 

2.0O4-

1.0e4 

8000.0-

6000.0 

40O0.0-

2000.0-

0.0-

I

Sample Name: 1(111020a030" Sample ID: "LCS-111020-4" File: "kl11020a.»ir 

Peak Name: TFOS" Massfes): "499.000/99.000 Da,499.000/e0.000 Da.499.000/130.000 Da" 

Comment •2ppb LCS" Annotathyi: -

Sample Index: 

Sample'Type; 

Calculated Cone; 

Data printe d by STW 

Wednesday, December 07, 2011 

Page 1 o f 2 

Page 77 of 99 
*ETS-Kirk 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll020 a branched.rd b 

I

SamplaName:-k111020a033' Sampio ID: "LCS-111020-r Fite:•k11l020a.svfr 

Peak Name: "PFOS" Massfes): "499.000/99.000 Da.499.000ffl0.000 Da,499.000/130.000 Da* 

Common!: •20ppb LCS" Annolation:" 

Sample Index; 33 

Sample Type; OC 

Concentration: 18.5 ng/raL 

Calculated Cone; 3.52 ng/mL 

Acq. Date: 10/21/2011 

Xcq. Time: 1:16;H AH 

Modified: 

Proc. Algo. 

tloise Percentage; 

Base. Sub. Hindox: 

Peak-Split. Factor: 

Report Largest Peak 

Min. peak Height; 

Min. Peak Hidth ; 

Smoothing Width: 

RT Window; 

Expected RT; 

Use Relativ e RT: 

Specify Parameters 

Valle y 

i e: 15.» 

693193B ct 

Height; 

Star t Time: 

End Time: 

Data printe d by STW 

Wednesday, December 07, 

Sub. Mindok 

Min. Peak Width; 

Smoothing Width: 

RT Window: 

Expected RT: 

Sample Name: "k111020a050" Sample ID; "GLPl 0-01-02-22-065* File: •kl11020a. 

Peak Name: "PFOS" Mass(Bs): "499.000/99.000 Da,499.000/80.000 Da,499.000/130.000 Da' 

Comment "DAL GW 335R 0" Annotation: ~ 

Sample Index; 50 

Sample Type: Unknown 

on; Il/A 

Cone; 2080. ng/nL 

-ttun; Specify Poramotei 

:age; 50 

9.73e+005 cps 

Page 2 o f 2 

Page 78 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll020a.rd b 

I Sample Name: •k111O20aO18* Sample ID: "10007-37-9" File: "kill020a. 

Peak Name: "PFHS" Massfes): '399.000/99.000 Da.399.00D/80.000 Da' 

I Commeni: *2.5 ng/mL FC atd In MD Q water* Annotation: -

ampl e Index : IS 

ampl e Type ; Standar d 

oncentcation : 2.5 0 ng/n L 

alculate d Cone : 2.5 1 ng/m L 

e q . Date : 10/20/201 1 

Acq. Tin 7:55:5 3 PM 

Modified: 

Proc. Algorithm: £ 

Iloise Percentage; 

Peak-Split. Factoi 

Report Largest Pee 

Min. Peak Height: 

Min. Peak Hidth; 

Smoothing Hidth: 

RT Window: 

Expected RT: 

Use Relative RT: 

Ho 

I

Sample Name: "kl 11020a025" Sample ID; TN11-0356" F»«: "kl 11020a,w 

Peak Narrw: "PFHS" Mass(ea): "399.000/99.000 Da.399.000/80.000 Da' 

Comment "MettKxJ Blank" Annotatkin: ~ 

Sample Index: 25 

Saraple Type; 

Min. Peak Height: 

Min, Peak Hidth ; 

Smoothing Hidth ; 

Base To Base 

Height; 

Star t Ti t 

End Time: 

17.0 17.5 

I

Sampte Name: T(111020a027' Sample ID: "LCS-111020-1' File: "kllH 

Peak Name: "PFHS" Mass(es): "399.000/99.000 Da,399.000/30.000 Da" 

CommenL "0.2ppb LCS' Annotation: ~ 

Sample Index: 27 

Sample Type: QC 

Concentration; 0.200 ng/rsL 

Calculated Cone: 0.174 ng/mL 

lifl i 

ttoii 

Algor Specify Paramet 

Sub. HindOH: 

Peak-Split. Factor: 

Report Largest Peak; 

Min. Peak width; 

1 RT; 

I

Samide Name: "k111020a030" Sample ID: "LCS-111020-4" File: 'kllio : 

Peak Name; "PFHS" . Mass(as): -399.000^9.000 Da.399.000re0.000 Da" 

Comment "2ppb LCS" Annotation:" 

Sanple Index: 30 

Sample Type: QC 

Concentration: 2.00 ng/nL 

Calculated Cone: 1.76 ng/mL 

Acq. Date: 10/21/2011 

Acq. Time: 12:12:10 AM 

Proc. AlgorJ 

Base. Sub. window: 

Peak-Split. Factor; 

Report Largest Peak: 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindow: 30 

Expected RT: 11 

1906055 C 

1.26e+006 

15.0 

1.25e6-

1.20e6-

1.15e6-

I.IOee1.05*6-

i.oooe9.50e5-

9.00o5-

8.5005-

8.00«5-

7.50e5-

7.00e5-

, 6.50e5-

S.00e5-

5.50e5-

5.00e5-

4.50e5 

4.00e5 

3.50e5' 

3.00e5 

2.50eS2.00e5 

1.50e5 

1.00e5 

5.00e4 

0.00 

13.0 13.5 14.0 17.0 17.S 

Data printe d by STW 

Printin g Time: 11:19:20 AM 

.Page 1 of 2 

Page 79 of 99 
*ETS-Kirk 

GLPl 0-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Results Name: kH1020a.rd b 

Data printe d by STW 

Printin g Time: 11:19:20 AM 

Page 2 of 2 

Page 80 of 99 
GLPl 0-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll024a.rd b 

Data printe d by STW 

Wednesday, December 07> 2011 

Page 1 o f 1 

Page 81 of 99 
*ETS-Kirk 

GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll024a.rd b 

(

Sample Name: "kl l 1024a017' Sample ID: "11 003-40-r Fie: "kl 11024a.w«r 

Peak Name: "13C6PFOS-IS(ISr MaM(es): "507.000/80.000 Da" 

Comment "1.0 n^ftnL FC std In Synth. Watof" Annotation; -

Sanple Index: 17 

Sample Type: Standard 

Concentration; 0.960 ng/oL 

Calculated Cone; H/A 

Acq. Date: 10/21/2011 

Acq. Time: 7:42;41 PM 

Modified; Ves 

Proc. Algorithm: Specify Parameters - HQ II I 

tloise Percentage: 50 

Base. Sub. Hindow; 1.00 min 

Peak-Split. Factor; 2 

Report Largest Peak: ^ea 

Min. Peak Height; O.OO cps 

Min. Peak Hidth : O.OO sec 

(idth ; 

RT Window: 

14.0 15.0 15.5 18.0 16.5 

I

SamiJe Name: "kl l 1024aO25" Sample ID:* 

Peak Name: "13CePFOS^S(ISr Mass(BS): *! 

Comment "Method Blank" Annotation;" 

Sample Index; 25 

. Algorithm; Specify Pan 

Peak Height; 

iight : 

;act Time: 

id Time; 

I

Sample Name: 1(1110243027" Sampio ID: "LCS-111024-1" File: "kl11024a.iMr 

Peak Name: "13CBPFOS4S(iS)" M8»s(e»): "507,000/80.000 Da" 

Comment "0.2ppb LCS" Annotation:"" 

Sanple Index: 27 

Sample Type; QC 

Concentration; 0.953 ng/nL 

Calculated Cone: M/A 

Acq. Date; 10/24/2011 

Acq. Tine: 11:16:23 PM 

. Sub. Kindox: 

-Split . Factoi 

::t Largest Pei 

Sisoothing WidI 

RT Window; 

Expected RT; 

Height; 

Star t Tir 

End Time: 

Valle ; 

(19456 

I

Sample Name: •k111024a030" Sampte ID: "I 

PeakName:"13C8PFOS-IS(IS)" Masa{es);"l 

Comment•2ppbLCS" Annotation:"" 

Sanple Index: 30 

Sample Type; OC 

Concentration; 0.953 n. 

•25/201 

12;20;30 

Specify Parameti 

Expected RT: 

15.0 15.5 16.0 16.5 15.0 15^ 16.0 16.5 17.0 17.5 18.0 18.5 

Data printe d by STW 

Wednesday, December 07, 2011 

Page 1 o f 4 

Page 82 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

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Result s Name: klll024a.rd b 

I

SamploName:"k111024a033* Sample ID: "LCS-111024-r Fite:"k111024a.wtfP 

Peak Name: "13C8PFO&^S(IS)• Ma»s{es): "507.000«0.000 Da" 

Comment "10ppb LCS" AnnolaOon: ** 

Sample Index; 33 

Modified ; 

RT Window; 

Expected RT 

Use Relativ i 

Int . Type: 

Height; 

End rime; 

15.5 16.0 16.5 

I

Sampte Name: "k111024a040" Sample ID; "GLPl 0^1-02-22-033" File: 

Peak Name: "ISCSPFOS-ISllSr Ma3»(e9): "507.000/80.000 DaComment "DAL GW317L0" Annotation:-

Sample Index; 40 

Sanple Type; Unknown 

Concentration; 0.955 ng/mL 

Calculated Cone: H/A 

Acq. Date; 10/25/2011 

Acq. Tirae: 3;51:12 AM 

liti i 

Area: 

Height; 

in; Specify Paran 

,ge: 50 

idow; 1.00 r 

773931 cc 

l.lSetOOS 

16.0 

15.0 15.5 16.0 16.5 17.0 17.5 

I

SamploName:"k111024aO44* Sample ID: "GLPl0-01-02-22-049' Fite:"k111024a.w(r 

Peak Name: "13C6PFOS4S(ISJ" Mas4(es): "507.000/30.000 Da" 

Commeni: "DAL GW328L0* Annotation:"" 

Sample Index; 11 

Sample Type: Unknown 

Concentration; 0.955 ng/mL ^ 

Calculated Cone: N/A 

ic. Algori 

.se Percer 

le. Sub. V 

ik-SpliC, 

Hin . Poak Hidth ; 

Smoothing Hidth ; 

RT Hindow: 

: Specify Paramet 

Height: 

Start Til 

End Time 

I

Sample Name; "kl 11024a0ir Sampte ID: "11 003-40^" 

Peak Name; TFOS- Mass(es); "499.000^9.000 Da.499.01 

Cofranent "1.0 ng/mL FC std In Synth. Water Annolation;" 

Sample Index; 17 

Proc. Algor i 

Base. Sub . ( 

:-Spli< Fact 

Report Largest Peak; 

Min. Peak Hidth : 

Smoothing Width: 

RT Window; 3( 

Expec 

; Relal 

I RT: 

; RT; 

Retention Tii 

Area: 

Height: 

1.00e5-

9.50e4' 

9.0ae4' 

8.50e4' 

8.00e4' 

7.50e4-

7.00©4-

6.50e4' 

S.00e4 

g 5.50e4-

j 5.00e4-

- 4.50M 

4.00e4' 

3.50e4 

3.00*4-

2.S0»4 

2.00e4 

1.50e4 

1.00e4-

5000.00 

0.00 

15.0 15.5 16.0 16,5 17.0 17.5 

Data printe d by STW 

Wednesday, December 07, 

Page 2 o f 4 

Page 83 of 99 
*ETS-Kirk 

GLPl 0-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

Results Name: klll024a.rd b 

Data printe d by STW 

Wednesday, December 07, 2011 

Page 3 o f 

Page 84 of 99 
GLPl 0-01-02; Interim Report 22 

Analysis of PFBS, PFHS. and PFOS in Groundwater 

3rd Quarter Sampling - 2011 

Result s Name: klll024a.rd b 

(

Sample Name ; >111024aO40 " Sample ID; "GLP l 0-01-02-22-033" File: 

Peak Name : "PFOS" Mass(es): "499.000/99.000 Da,499.000/80.000 Da.-

Comment:"DALGW317L0 ' AnnotatJon;-

Sampl e Index ; 40 

Sampl e Type ; Unknow n 

Concentration : N/A 

Calculate d Cone : 0.21 1 ng/n L 

Acq. Date; 10/25/2011 ). 

Acq. Tine: 3:54;12 AM 

Hodifif 1.7e4 

; Specify Paranetei 

Base. Sub. Window; l.DO 

Peak-Split. Factor: t 

Report Largest Peak: Yes 

Hin. Peak Height; 0.00 

Use Relativ i 

Retention T: 

Height: 

§" 1.0e4-

I 9000.0-

8000.0-

7000.0-

6000.0-

5000.0 

4000.0-

3000.0-

2000.0-

10D0.0 

0.0-

17.0 17.5 18.0 18.5 

I

Sampte Name : "k111024aO44" Sampte ID: "GLP l Wll-02-22-049 " File;"k111024a.w« r 

Pea k Name : "PFOS" M3*s(es); "499.OO(V99.O0O Oa ,499.000/80.000 Da,499.000/130.000 Da -

Commen t "DAL G W 328L 0" Annolation: " 

Sanpl e Index : 44 

Sanpl e Type ; Unknow n 

Peak-Split. Factoi 

Report Largest Pel 

Hin. Peak Height: 

Min. Peak Width: 

Smoothing width; 

RT Window: 

Expected RT; 

0,0 0 cp s 

7.0e4 

! Relal 

Height: 

Start Tin 

End Time; 

; RT; 

Data printe d by STW 

Wednesday, December 07, 2011 

Page 4 of 4 

Page 85 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

ATTACHMENT C : ANALYTICAL METHOD(S) 

Page 86 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

3IVI Eiwironmental Laboratory 

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^y'o'7 

Approved By: 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Page 87 of 99 
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Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

1 Scope and Application 

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

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

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

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

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

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

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

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

Performance Liquid Chromatography/Mass Spectrometry". 

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

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 Method Summary 

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 predeteirnined 

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 interi'erences are present in the field environment. This sample is also refen-ed to as a Trip Blank. 

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 88 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

3.4 Field Duplicate Sample (FDS, Field Dup) 

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

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

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

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

3.5 Field Matrix Spike (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 determine if the method is in control and 

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

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

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

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

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

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

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

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

quantitated within the specified limits of precision and accuracy during roufine 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 

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GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

3.11 Method Blank 

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

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

blank is used to determine 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-anaiyte prepared in the laboratory with an assayed reference 

compound. 

3.14 Surrogate 

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

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

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

control samples. Surrogate(s) are added to quantitatively evaluate the entire analytical procedure 

including sample collection, preparation, and analysis. Inclusion of a surrogate 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 detemnined; 

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

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

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

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

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

4.2 Cautions 

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

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

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

5 Interferences 

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

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

conditions of analysis by running method blanks. 

ETS-8-044.0 Page 4 of 11 

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

Injection Analysis 

Page 90 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

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

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

caps, autovial caps, HPLC parts, etc. 

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

calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Equipment 

6.1 Instrumentation and Equipment 

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

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

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25|JL, 50pL, lOOpL, 250pL, 500ML, 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: 

Flow Rate 

Time (min) %A % B (mL/min) 

0.0 97 3 1.0 

0.5 97 3 1.0 

11.0 5 95 1.0 

13.5 5 95 1.0 

13.6 97 3 1.0 

17.0 97 3 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 

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GLPl 0-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

6.3 MS/MS System 

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

Analyte Transition Monitored 

PFBA 213^ 169 

PFPeA 263^219 

PFHA 313^269 and 313^ 119 

PFHpA 363 ^ 319, 363 ^ 169 and 363 -» 119 

PFOA 413 ^ 369, 413 -» 219 and 413 169 

PFNA 463 419, 463 ^ 169 and 463 ^219 

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

PFUnA 563 ^ 519, 563 269 and 563 -» 219 

PFDoA 613 ^ 569, 613 ^ 169 and 613 319 

PFBS 299 80 and 299 ^ 99 

PFHS 399 80 and 399 99 

PFOS 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, altemate instnjments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfluorooctanoic Acid (PF0A-C8 acid); 3M 

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

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

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

ETS-8-044.0 Page 6 of 11 

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

Analysis 

Page 92 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

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

used. 

7.3 Reagent Preparation 

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

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

100 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 con-ection is given below for PFOS. 

X- r X molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

499 

PFOS (K"" )salt correction factor = — = 0.9275 

538 

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

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

flask and bring up to volume with solvent. 

250 ng/mL mixed 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 93 of 99 
GLP10-01-02; Interim Report 22 

Analysis of PFBS, PFHS, and PFOS in Groundwater 

Srd Quarter Sampling - 2011 

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 worthing standards may 

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL Volume of WS, pL 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTM Type 1 Water, 

or other suitable water 

125 10 50 0.025 

125 15 50 0.0375 

125 20 50 0.050 

125 30 50 0.075 

250 20 50 0.100 

250 50 50 0.250 

250 100 50 0.500 

250 200 50 1.00 

5000 25 50 2.50 

5000 50 50 5.00 

5000 100 50 10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

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

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

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

Prepare at least five method blanks. 

9 Sample 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 detennination (r^) value for the calibration curve must be greater than or equal to 0.990. Each 

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

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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, perfomri 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 njn. 

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 fleld blanks. 

10.4 Surrogate Spikes 

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

10.5 Lab Control Sample 

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

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

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

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

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

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

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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 1 f J / ; 1X (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. 

Recove - '^'^'^^^^'^^^'^'^^'^^'^^'^'S^^'^^'^'^^^^'^^^'^^^ xlOO 

Analyte added (ng/mL) 

12 Method Performance 

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

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

If criteria listed in this method performance 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 

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

calitiration 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 S2% to be compliant. 

12.2 Quantitation 

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

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

the LLOQ, which may be within ±30%. 

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

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

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

bracketed by CCVs not meeting these criteria must be reanalyzed. 

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

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

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

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

to Section 10 for additional details. 

12.4 Accuracy 

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

Section 10 contains additional infomiation 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 information 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 information for reconstmction of the data. 

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

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

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

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ATTACHIVIENT D: DEVIATION(S) 

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RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

Study / Project No. 

GLP10-01-02-22 

Date(s) of Occurrence: 

b l l 1012a, kin020 a 

Document Number: 

ETS-8-044.0 

Deviation type • SOP • Equipment Procedure 0 Method 

(Check one) • Protocol • GPO • Other: 

/ / . Description (attach extra pages as needed) 

Method Requirements: 

1. System Suitability area counts with RSD <5% (section 12.1). 

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

3. LCS recovery within ±20% (section 10.5). 

4. CCV recovery within ±25% (section 12.2). 

Actual procedure/process: 

1. The system suitability area count RSD for PFOS was 7.5% for 'b111012a PFOS sum' and 9.1% for 

'kl l 1020a PFOS sum'. 

2. The following sampling locations had FMS samples outside method acceptance criteria for run bl 11012a: 

DAL GW 220R for PFOS HS (61.9%), DAL GW 220L for PFOS MS (61.9%), DAL GW 222R for PFBS MS 

(66.8%), PFHS HS (65.1%), and PFOS HS (56.9%), DAL GW 327R for PFBS HS (65.4%) and PFHS HS 

(69.1%), DAL GW 330L for PFBS (66.1%), DAL GW 3318 for PFBS (68.5%), DAL GW 335R for PFBS 

(69.1%), DAL GW GRS04 for PFOS LS (63.0%), TRIP01 for PFOS MS (68.0%), and TRIP02 for PFOS 

MS (65.9%) and HS (68.9%). 

3. The 0.2ppb LCSs had an average recovery of 74.1 % and the 2ppb LCSs had an average recovery of 

78.1% for PFOS in run bl l 1020a (summed). 

4. Five CCVs for PFOS (summed) in run b111012a had recoveries greater than 125% (127% -135%). 

///. Actions Taken) 

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

Corrective Action (• Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

The system suitability results for PFOS will be noted in the final report. 

Sampling locations with FMS recoveries outside method acceptance criteria will be flagged in the report 

and the analytical uncertainty adjusted for the samples where the non-compliant FMS was the most 

appropriate spiking concentration. The trip blanks were also relatively low, especially for PFOS, which 

may explain why several sample FMSs are low. 

The non-compliant LCSs will be flagged in the final report. 

The accuracy of the CCVs for PFOS increased throughout the run, which suggests instrument drift. 

However, since the sample concentrations are similar to that of previous studies performed in the past for 

this sample set, samples were not re-analyzed. 

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

0 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: 

Study Director (if GLP): 

Sponsor Approval (for GLIv protocol deviations): NA 

Date: 

Date: 

Date: 

Technical Reviewer (optional): NA Date: NA 

Laboratory Department Manager Approval: 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 Date: NA 

Deviation No. 

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

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