i . ' " GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

GLP10-01-01. Interim Report 22: Analysis of PFOA in Groundwater Samples 

Collected at Decatur. A L for 3'" Quarter 2011 

Study Title 

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

Phase 3 Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone:610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

Maplewdod, MN 55144 

Project Identification 

GLP10-01-01-22 

Total Number of Pages 

56 

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

Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052.01. 

^ Testing that complies with this International Standard also ooerate in accordance with ISO 9001:2000. 

IACCREDITID I 

Testing Cert #2052.01 

Page 1 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

This page has been reserved for specific country requirements. 

Page 2 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

GLP CoiviPLiANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 22. Analysis of PFOA in Groundwater Samples Collected 

at Decatur, AL for 3"^ Quarter 2011 

Study: Analysis of Perfluorooctanoic Acid (PFOA) 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. 

'/I 

Gary Hohenstein/ Sponsor Representative Date 

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

Page 3 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 22. Analysis of PFOA in Groundwater Samples Collected 

at Decatur, AL for 3"^ Quarter 2011 

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

Decatur Phase 3 Site-Related Monitoring Program. 

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

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

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

Inspection Dates Pliase 

Date Re ported to 

Inspection Dates Pliase Testing Facility 

n/lanagement 

Study Director 

10/24-25/11 Interim Report 22 

Data and Report 11/1/11 11/1/11 

QAU Representative 

Page 4 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

TABLE OF CONTENTS 

GLP Compliance Statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infonnation 8 

2 Summary 9 

3 Introduction 10 

4 Test & Control Substances 11 

5 Reference Substances 11 

6 Test System 11 

7 Method Summary 12 

7.1 Methods 12 

7.2 Sample Collection 12 

7.3 Sample Preparation 12 

7.4 Analysis 12 

8 Analytical Results 13 

8.1 Calibration 13 

8.2 System Suitability 14 

8.3 Limit of Quantitation (LOQ) 14 

8.4 Continuing Calibration 14 

8.5 Blanks 14 

8.6 Lab Control Spikes (LCSs) 14 

8.7 Analytical Method Uncertainty 15 

8.8 Field Matrix Spikes (FMS) 15 

Page 5 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

9 Data Summary and Discussion 16 

10 Conclusion 23 

11 Data/Sample Retention 23 

12 Attachments 24 

13 Signatures 25 

LIST OF TABLES 

Table 1. Summarized PFOA Results (Decatur Groundwater, 3"^ Quarter 2011) 10 

Table 2. Sample Description Key Code 12 

Table 3. Instrument Parameters 13 

Table 4. Liquid Chromatography Conditions 13 

Table 5. Mass Transitions 13 

Table 6. Limit of Quantitation (LOQ) 14 

Table 7. Laboratory Control Spike Recovery 15 

Table 8. Analytical Method Uncertainty 15 

Table 9. Field Matrix Spike Concentrations 16 

Table 10. DAL GW 203L 110930 17 

Table 11. DAL GW220R110930 17 

Table 12. DAL GW 220L 110930 17 

Table 13. DAL GW 222R 110930 18 

Table 14. DAL GW 227R110922 18 

Table 15. DAL GW 227L110922 18 

Table 16. DAL GW 31 OR 110928 19 

Table 17. DAL GW 312R 110929 19 

Table 18. DALGW317L110928 19 

Table 19. DAL GW 324L110923 20 

Table 20. DAL GW 327R 110928 20 

Page 6 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Table 21. DAL GW 328R 110927 20 

Table 22. DAL GW 328L 110928 21 

Table 23. DAL GW 330R 110928 21 

Table 24. DAL GW 330L 110928 21 

Table 25. DAL GW 331S 110929 22 

Table 26. DAL GW 335R 110927 22 

Table 27. DAL GW GRS04 110930 22 

Table 28. Trip Blank 1 23 

Table 29. Trip Blank 2 23 

Table 30. Rinseate Blanks 23 

Page 7 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

Cleston Lange, Ph.D., Principal Analytical Investigator, (clange@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 Date: October 12,2011 

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 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

2 Summary 

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

representing eighteen (18) different sampling locations collected September 23 - 30,2011. A total of 

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

(PFOA) analysis, and included duplicate groundwater samples from each sampling location. Samples 

also included field matrix spike (FMS) samples for each location, two trip blanks containing Milli-QTM 

water and appropriate trip blank spikes, and two equipment rinseate blanks. The equipment rinseate 

blanks did not have FMS samples prepared for detennination of PFOA recovery. All of the samples 

were prepared and analyzed for PFOA following 3M Environmental Laboratory Method ETS-8-044.0 

and conducted under 3M project GLP10-01-01-22. 

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

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

for PFOA following 3M Environmental Laboratory Method ETS-8-044.0. Many of the groundwater 

samples required dilution to attain PFOA concentrations within the range of the curve, in some 

instances up to 100-fold dilution were required. The average measured PFOA concentrations are 

summarized in Table 1. The equipment rinseate and the trip blanks associated with GLP10-01-01-22 

were below the lower limit of quantitation (LLOQ) of 0.0240 ng/mL. Concentration results for all 

groundwater samples ranged from 0.322 ng/mL to 3580 ng/mL. The analytical uncertainty for PFOA is 

+12%. 

Page 9 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Table 1. Summarized PFOA Results (Decatur Groundwater, 3'''' Quarter 2011) 

Sample ID Avg. PFOA 

Concentration (ng/mL) 

Relative Percent 

Difference (RPD) 

DALGW203L110930 139 14% 

DAL GW220R 110930 29.3 3.4% 

DALGW220L110930 49.8 0.0% 

DAL GW222R 110930 366 [a] 3.8% 

DAL GW227R 110922 251 3.2% 

DAL GW227L 110922 144 0.70% 

DAL GW 31 OR 110928 969 1.9% 

DAL GW312R 110929 1980 2.0% 

DAL GW 317L 110928 0.322 11% 

DALGW324L110923 292 0.68% 

DALGW327R 110928 661 4.7% 

DALGW328R 110927 361 0.55% 

DAL GW328L 110928 102 3.0% 

DALGW330R110928 358 2.2% 

DAL GW330L 110928 376 5.1% 

DAL GW 331S 110929 735 2.4% 

DALGW335R110927 3580 [b] 0.0% 

DAL GWGRS04 110930 3010 3.3% 

Trip Blank (Mllli-QTM Water) - 2 sets < 0.0240 N/A 

Equipment Blank s < 0.0240 N/A 

N/A; not applicable 

The analytical method uncertainty for PFOA is +12%. 

[a] The FMS recovery did not meet acceptance criteria. Method uncertainty is expanded to 

+39% for sampling location DAL GW 222R110930. 

[b] Sampling location DAL GW335R 110927 did not have an appropriate FMS to assess 

PFOA accuracy.' 

3 Introduction 

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

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

information regarding concentrations of perfluorooctanoate (PFOA) 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 PFOA in an effort to characterize on-site groundwater conditions. 

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

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

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

Each empty container for groundwater samplings was marked with a "fill to here" line to produce a final 

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

appropriate matrix spike solution containing PFOA prior to being sent to the field for sample collection. 

See section 8.8 of the report for field matrix spike levels. The aqueous equipment rinseate sample was 

collected in a plain bottle without fortification. 

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". 

Page 10 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Table 1 summarizes the average PFOA concentrations for the duplicate groundwater samples 

collected, and for the two trip blanks and aqueous 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. 

5 Reference Substances 

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

Reference Substance PFOA (Linear) PFOA (Linear and Branclied) 

Chemical Name Perfluorooctanoate Perfluorooctanoate 

Chemical Formula CyFisCOQ- C7F15COO" 

Identifier CAS # 335-67-1 CAS #95328-99-7 

Use FMS Reference Standard Target Analyte and LCS 

Reference Standard 

Source Oakwood Products Wellington 

Expiration Date 01/17/2018 03/17/2014 

Storage Conditions Frozen Frozen 

Chemical Lot Number 3440 TPFOA0311 

TCR Number TCR07-0041 TCR11-0009 

Physical Description Powder Liquid 

Purity 99.1% 98.3% 

6 Tes* System 

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

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

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

Page 11 of 56 
Table 2. Sample Description Key Code. 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Example DALGW 203L DB 110930 

String Number String Descriptor Example 

1 Sampling Location DAL = Decatur, Alabama 

2 Sample Type GW= Ground water 

3 Well Identifier Example: 203L 

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 

HS = high spike 

6 Sampling Date 110930 = September30,2011 

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. Two sets 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 Q water, 

1:10 dilutions were prepared by diluting 1 mL 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 diluting 0.1 mL sample with 9.9mL of Milli Q water. 

7.4 Analysis 

All study samples and quality control samples were analyzed for PFOA 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 in Table 3, Table 4 

and Table 5. 

Page 12 of 56 
Table 3. Instrument Parameters. 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Instrument Name ETS Buster 

Analytical Method Followed ETS-8-044.0 

Analysis Dates 10/7/11 

Project GLP10-01-01-22 

Liquid Ciiromatograph Agilent 1100 

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

Analytical column Betasil 018 (2.1 mm X 100 mm), 5|i 

Injection Volume 10 nL 

IVIass Spectrometer Applied Biosystems API 4000 

Ion Source Turbo Spray 

Electrode Turbo ion electrode 

Polarity Negative 

Software Analyst 1.4.2 

Table 4. Liquid Chromatography Conditions. 

step Total Time Flow Rate PercentA PercentB 

Number (min) (fiUmin) (2 mM ammonium acetate) (MethanoO 

ETS-8-044.0 

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 

Table 5. Mass Transitions. 

Analyte 

Mass Transition 

Q1/Q3 

Reference Material 

Structure 

PFOA 

413/369 

413/219 Linear* Branched 

413/169 

Dwell time was 100 msec for each transition. The individual transitions 

were summed to produce a "total ion chromatogram" (TIC), which was 

used for quantitation. 

8 Analytical Results 

8.1 Calibration 

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

prepared by spiking known amounts of the stock solution containing PFOA (reference standard 

containing both linear and branched isomers) into Milli Q water. Standards ranging from 0.0250 ng/mL 

to 100 ng/mL (nominal) were analyzed. 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 

Page 13 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 

100±25% (100±30% for the lowest curve point) were met for all analytes. The con-elation coefficient (r) 

was greater than 0.995 for PFOA. 

8.2 System Suitability 

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

demonstrate overall system suitability. Analysis runs met 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%RSDfor PFOA. 

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 twnce those of the appropriate 

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

Table 6. Limit of Quantitation (LOQ). 

Analysis Date PFOA 

LOQ, ng/mL 

10/7/11 0.0240 

(1) Analytical LOQ wittiout sample dilution factors applied. 

8.4 Continuing Calibration 

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

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

reported samples were bracketed by CCVs that met method criteria of 100% ± 25%. 

8.5 Blanks 

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

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

evaluate method performance and to determine the LOQ for PFOA. Trip blanks reflect the shipping and 

sample collection conditions the sample bottles and samples experience. Equipment rinseate blanks 

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

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

8.6 Lab Control Spikes (LCSs) 

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

prepared by spiking known amounts of the analyte into laboratory reagent water, 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%, was met for all LCSs. 

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

1 o . r. Calculated Concentration ,,... , 

LCS Percent Recovery = * 100% 

Spike Concentration 

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

average LCS recovery 

Page 14 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 10/7/11 PFOA (Linear + Branched) 

Spiked Calculated 

Concentration Concentration 

Lab ID (ng/mL) (ng/mL) VoRecovery 

LCS-111007-1 1.91 2.04 107 

LCS-111007-2 1.91 1.92 100 

LCS-111007-3 1.91 2.02 106 

Average ± %RSD 104% ±3.6% 

LCS-111007-4 19.1 18.8 98.6 

LCS-111007-5 19.1 19.7 103 

LCS-111007-6 19.1 19.0 99.2 

Average ± %RSD 100% ±2.4% 

LCS-111007-7 47.7 45.1 94.6 

LCS-111007-8 47.7 45.2 94.8 

LCS-111007-9 47.7 46.2 96.9 

Average ± %RSD 95.4% ±1.3% 

8.7 Analytical Method Uncertainty 

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

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

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

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

which con-esponds to a confidence level of 95%. 

Table 8. Analytical Method Uncertainty 

Analyte 

PFOA 

Method 

Standard 

Deviation 

Method 

Analyte Uncertainty 

PFOA ETS-8-044.0 5.99 ±12% 

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 PFOA (reference standard containing primarily 

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

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

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

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

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

Page 15 of 56 
Table 9. Field Matrix Spike Concentrations 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Location (Well ID) Spike Level 

PFOA Spike 

Concentration 

(ng/mL) 

317L Low Spike 1 

High Spike 10 

220R, 220L, and 328L Low Spike 10 

High Spike 100 

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

324L, 327R, 330L, 331S, and 335R 

203L, 222R, 227L, 227R, 31 OR, Low Spike 100 

324L, 327R, 330L, 331S, and 335R High Spike 1000 

GRS04, 312R, and 330R Low Spike 1000 

High Spike 5000 

328R Low Spike 100 

High Spike 500 

Trip Blanks Low Spike 10 

Mid Spike 100 

Trip Blanks 

High Spike 1000 

(Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample Dup.) ^, „, FMS Recovery = -^^ — * 100% Spike Concentraton 

9 Data Summary and Discussion 

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

locations as well as the Trip Blanks and rinseate 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 222R (Table 13) - High spike recovery was 61.4%. Method uncertainty is expanded to 

±39%. 

DAL GW 335R (Table 26) - Sampling location did not have an appropriate field matrix spike level to 

accurately assess PFOA recovery. 

Page 16 of 56 
Table 10. DAL GW203L 110930 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

PFOA 

Concentration 

3MUMSID Description (ng/mL) VoRecovery 

GLP10-01-01-22-001 DAL GW203L 0110930 148 NA 

GLP10-01-01-22-002 DALGW203L DB 110930 129 NA 

GLP10-01-01-22-003 DALGW203LLS110930 241 103 

GLP10-01-01-22-004 DALGW203L HS 110930 1010 87.2 

Average Concentration (ng/mL) ± %RPD 139 ng/mL ±14% 

NA = Not Applicable 

Samples analyzed using a 1 ;50 dilution factor. 

Table 11. DAL GW 220R 110930 

PFOA 

Concentration 

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

GLP10-01-01-22-005 DAL GW220R 0110930 28.8 NA 

GLP10-01-01-22-006 DALGW220R DB 110930 29.8 NA 

GLP10-01-01-22-007 DALGW220RLS110930 37.1 NC 

GLP10-01-01-22-008 DALGW220R HS 110930 113 83.7 

Average Concentration (ng/mL) ± %RPD 29.3 ng/mL ±3.4% 

NA = Not Applicable 

NC = Not Calculated; ttie sample concentration is greater ttian 2x ttie spil<e level. 

Samples analyzed using a 1:5 dilution factor. 

Table 12. DAL GW 220L 110930 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-009 DAL GW220L 0110930 49.8 NA 

GLP10-01-01-22-010 DALGW220L DB 110930 49.8 NA 

GLP10-01-01-22-011 DALGW220LLS 110930 57.6 NC 

GLP10-01-01-22-012 DALGW220L HS 110930 133 83.2 

Average Concentration (ng/mL) ± %RPD 49.8 ng/mL ±0.0% 

NA = Not /\pplicable 

NC = Not Calculated; the sample concentration is greater Uian 2x the spil<e level. 

Samples analyzed using a 1:5 dilution factor. 

Page 17 of 56 
Table 13. DAL GW 222R 110930 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-013 DAL GW222R 0110930 359 NA 

GLP10-01-01-22-014 DALGW222R DB 110930 373 NA 

GLP10-01-01-22-015 DALGW222RLS 110930 462 NC 

GLP10-01-01-22-016 DALGW222R HS 110930 980 61.4<^> 

Average Concentration (ng/mL) ± %RPD 366 ng/mL ±3.8%'^ 

NA = Not /Applicable 

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

Samples analyzed using a 1:50 dilution factor. 

(1) FMS recovery did not meet acceptance criteria of 100 ± 30%. 

(2) Mettiod uncertainty has been expanded to ±39%. 

Table 14. DAL GW 227R 110922 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-017 DAL GW227R 0110922 247 NA 

GLP10-01-01-22-018 DALGW227R DB 110922 255 NA 

GLP10-01-01-22-019 DALGW227R LS 110922 345 NC 

GLP10-01-01-22-020 DALGW227R HS 110922 1040 78.9 

Average Concentration (ng/mL) ± %RPD 251 ng/mL ±3.2% 

NA = Not /Applicable 

NC = Not Calculated; the sample concentiBtion is greater than 2x the spil^e level. 

Samples analyzed using a 1:20 dilution factor 

Table 15. DAL GW 227L 110922 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-021 DAL GW227L 0110922 143 NA 

GLP10-01-01-22-022 DALGW227L DB 110922 144 NA 

GLP10-01-01-22-023 DALGW227LLS110922 224 80.5 

GLP10-01-01-22-024 DALGW227LHS 110922 918 77.5 

Average Concentration (ng/mL) ± VoRPD 144 ng/mL ±0.70% 

NA = Not/Applicable 

Samples analyzed using a 1;20 dilution factor. 

Page 18 of 56 
Table 16. DAL GW 31 OR 110928 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-025 DAL GW310R 0110928 978 NA 

GLP10-01-01-22-026 DALGW31 OR DB 110928 960 NA 

GLP10-01-01-22-027 DALGW31 OR LS 110928 1050 NC 

GLP10-01-01-22-028 DALGW31 OR HS 110928 1770 80.1 

Average Concentration (ng/mL) ± VoRPD 969 ng/mL ±1.9% 

NA = Not Applicable 

NO = Not Calculated; Uie sample concent^tion is greater than 2x the spike level. 

Samples analyzed using a 1:100 dilution factor. 

Table 17. DAL GW 312R 110929 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-029 DAL GW312R 0110929 1960 NA 

GLP10-01-01-22-030 DALGW312R DB 110929 2000 NA 

GLP10-01-01-22-031 DALGW312R LS 110929 2700 72.0 

GLP10-01-01-22-032 DALGW312R HS 110929 6560 91.6 

Average Concentration (ng/mL) ± VoRPD 1980 ng/mL ±2.0% 

NA = Not Applicable 

Sample, sample duplicate, and LS vmre analyzed using a 1:100 dilution fector. The HS was analyzed using a 1:500 dilution factor. 

Table 18. DAL GW 317L 110928 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-033 DAL GW 317L 0110928 0.340 NA 

GLP10-01-01-22-034 DALGW317L DB 110928 0.304 NA 

GLP10-01-01-22-035 DALGW 317LLS 110928 1.18 85.8 

GLP10-01-01-22-036 DAL GW317LHS 110928 9.37 90.5 

Average Concentration (ng/mL) ± VoRPD 0.322 ng/mL ±11% 

NA = Not Applicable 

Page 19 of 56 
Table 19. DAL GW 324L 110923 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-037 DAL GW324L 0110923 293 NA 

GLP10-01-01-22-038 DALGW324LDB 110923 291 NA 

GLP10-01-01-22-039 DALGW324L LS 110923 378 NC 

GLP10-01-01-22-040 DALGW324L HS 110923 1110 81.8 

Average Concentration (ng/mL) ± VoRPD 292 ng/mL ±0.68% 

NA = Not /Applicable 

NC = Not Calculated; the sample concenti^ition is greater than 2x ttie spike level. 

Samples analyzed using a 1:50 dilution factor. 

Table 20. DAL GW 327R 110928 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-041 DAL GW327R 0110928 645 NA 

GLP10-01-01-22-042 DALGW327R DB 110928 676 NA 

GLP10-01-01-22-043 DALGW327RLS110928 771 NC 

GLP10-01-01-22-044 DALGW327R HS 110928 1400 74.0 

Average Concentration (ng/mL) ± VoRPD 661 ng/mL ±4.7% 

NA = Not /Applicable 

NC = Not Calculated; ttie sample concenti^tion is greater ttian 2x ttie spike level. 

Samples analyzed using a 1:50 dilution factor 

Table 21. DAL GW 328R 110927 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-045 DAL GW328R 0110927 362 NA 

GLP10-01-01-22-046 DALGW328R DB 110927 360 NA 

GLP10-01-01-22-047 DALGW328RLS 110927 425 NC 

GLP10-01-01-22-048 DALGW328R HS 110927 715 70.8 

Average Concentration (ng/mL) ± %RPD 361 ng/mL ± 0.55% 

NA = Not Applicable 

NC = Not Calculated; the sample concenti^tion is greater ttian 2x the spike level. 

Samples analyzed using a 1:20 dilution factor. 

Page 20 of 56 
Table 22. DAL GW 328L 110928 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

PFOA 

Concerttration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-049 DAL GW328L 0110928 100 NA 

GLP10-01-01-22-050 DALGW328L DB 110928 103 NA 

GLP10-01-01-22-051 DALGW328L LS 110928 109 NC 

GLP10-01-01-22-052 DALGW328L HS 110928 179 77.5 

Average Concentration (ng/mL) ± VoRPD 102 ng/mL ±3.0% 

NA = Not /Applicable 

NO = Not Calculated; Uie sample concentration is greater than 2x ttie spike level. 

Samples analyzed using a 1:10 dilution factor. 

Table 23. DAL GW 330R 110928 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-053 DAL GW330R 0110928 362 NA 

GLP10-01-01-22-054 DALGW330R DB 110928 354 NA 

GLP10-01-01-22-055 DALGW330RLS 110928 1210 85.2 

GLP10-01-01-22-056 DALGW330R HS 110928 4820 89.2 

Average Concentration (ng/mL) ± VoRPD 358 ng/mL ±2.2% 

NA = Not Applicable 

NC = Not Calculated; the sample concentration is greater than 2x ttie spike level. 

Sample, sample duplicate, and LS were analyzed using a 1:100 dilution factor The HS was analyzed using a 1:500 dilution factor. 

Table 24. DAL GW 330L 110928 

PFOA 

Concentration 

3M LIMS ID Description (n^mL) VoRecovery 

GLP10-01-01-22-057 DAL GW330L 0110928 366 NA 

GLP10-01-01-22-058 DALGW330L DB 110928 385 NA 

GLP10-01-01-22-059 DALGW330L LS 110928 520 NC 

GLP10-01-01-22-060 DALGW330LHS 110928 1270 89.5 

Average Concentration (ng/mL) ± VoRPD 376 ng/mL ±5.1% 

NA = Not /Applicable 

NC = Not Calculated; the sample concenfation is greater than 2x ttie spike level. 

Samples analyzed using a 1:50 dilution factor 

Page 21 of 56 
Table 25. DAL GW 331S 110929 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-061 DAL GW331S0 110929 744 NA 

GLP10-01-01-22-062 DALGW331SDB110929 726 NA 

GLP10-01-01-22-063 DALGW331SLS 110929 808 NC 

GLP10-01-01-22-064 DAL GW331SHS 110929 1440 70.5 

Average Concentration (ng/mL) ± VoRPD 735 ng/mL ±2.4% 

NA = Not /Applicable 

NC = Not Calculated; the sample concenti'ation is greater than 2x ttie spike level. 

Samples analyzed using a 1:50 dilution factor. 

Table 26. DAL GW 335R 110927 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-065 DAL GW335R 0110927 3580 NA 

GLP10-01-01-22-066 DALGW335R DB 110927 3580 NA 

GLP10-01-01-22-067 DALGW335R LS 110927 3530 NC 

GLP10-01-01-22-068 DALGW335R HS 110927 4250 NC 

Average Concentration (ng/mL) ± VoRPD 3580 ng/mL ±0.0%'^' 

NA = Not Applicable 

NC = Not Calculated; the sample concenti^tion is greater than 2x ttie spike level. 

Samples analyzed using a 1:50 dilution factor. 

(1) Sampling location does not have an appropriate matrix spike level to assess accuracy. 

Table 27. DAL GW GRS04110930 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-069 DAL GWGRS04 0110930 3060 NA 

GLP10-01-01-22-070 DAL GW GRS04 DB 110930 2960 NA 

GLP10-01-01-22-071 DAL GW GRS04 LS 110930 3720 NC 

GLP10-01-01-22-072 DAL GW GRS04 HS 110930 6990 79.6 

Average Concentration (ng/mL) ± VoRPD 3010 ng/mL ±3.3% 

NA = Not Applicable 

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

Sample, sample duplicate, and LS were analyzed using a 1:100 dilution factor. The HS was analyzed using a 1:500 dilution factor. 

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

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Table 28. Trip Blank 1 

PFOA 

Concentration 

3M LIMS ID Description (ng/mL) VoRecovery 

GLP10-01-01-22-074 DAL GW TRIP01 0 <0.0240 NA 

GLP10-01-01-22-075 DAL GW TRIP01 LS 8.50 85.0 

GLP10-01-01-22-076 DAL GW TRIP01 MS 85.6 85.6 

GLP10-01-01-22-077 DAL GW TRIP01 HS 913 91.3 

NA = Not Applicable 

Table 29. Trip Blank 2 

PFOA 

3M LIMS ID Descnptfon 

Concentration 

(ng/mL) %Recovery 

GLP10-01-01-22-078 DALGWTRIP02 0 <0.0240 NA 

GLP10-01-01-22-079 DALGWTRIP02LS 8.55 85.5 

GLP10-01-01-22-080 DALGWTRIP02MS 94.0 94.0 

GLP10-01-01-22-081 DALGWTRIP02HS 1000 100 

NA = Not /Applicable 

Table 30. Rinseate Blanks 

PFOA 

3M LIMS ID Description 

Concerttration 

(ng/mL) 

GLP10-01-01-22-082 DALGW203L RB 110930 <0.0240 

GLP10-01-01-22-083 DALGW220L RB 110930 <0.0240 

10 Conclusion 

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

accuracy and precision for PFOA. Analysis was successfully completed following 3M Environmental 

Laboratory method ETS-8-044.0 described herein. 

11 Data/Sample Retention 

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

to 3M Environmental Laboratory standard operating procedures. 

Page 23 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

12 Attachments 

Attachment A: Protocol Amendment 22 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method ETS-8-044.0 

Attachment D: Method Deviation 

Page 24 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

13 Signatures 

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

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

1 

Gary Hohenstein, Sponsor Representative 

z. 

Date 

Jaisimha Kesari, Study Director Date 

Page 25 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 26 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Analytical Protocol: GLP10-01-01 

Amendment 22 

Study Title 

Analysis of Perfluorooctanoic Acid (PFOA) in Gribundwater, 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 

IVIaplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-01 

Sampling Event 

Decatur 3"^ Quarter Groundwater Sampling 

Page 1 of 7 

Page 27 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

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 prdtOGpl 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 thie 3M Environmental Labbratory LIMS 

as project GLP10-01-01-22 and reported as Interim report GLP10-^01-01-122, (reflecting study GLPiO-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 collectiop 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 28 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Analytical Protocol: GLP10-01-01 

Arriendmeht 22 

Amendment Approval 

Gary Hohen; tein, Sponsor Representative Date 

7}i4jzill 

Cleston C. Lange, Principal Analytical Investgator Date 

William Reagen, EHC Opns Environmental Lab Management Date 

Jaisimha I Dat^ Kes; E, Study Director 

Page 3 of 7 

Page 29 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Analytical Protocol: GLP10-01-01 

Anhendment22 

<«J|VI Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Qpns 

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, MN 55144-1000 

Phone: (651)737-3570 

aahohenstein®mmrn.com 

3IW Environmental Laboratory Management 

William K. Reagen 

3M EHS opns, Environmental Lalwratory 

250-5N-17 

651 733-9739 

Contacts wkreaaen® mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanoe®mmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinak®westonsolutions.com 

Phone; (334)-332-9123 

Lab Request Number GLP10-01-01-22 

Six Digit Departrlient Number Dept #530711, Project #0022674449 

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

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

Page 4 of 7 

Page 30 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

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 groundvyater 

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

conducted under the GLP requirerfients 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 1.9, 2011. The 3M Environmental Laboratory will prepare the sample bottles with all required 

spikes to ensure that results for PFOA are of a known precisibn 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"fiirto here" line 

on each 250 mL Nalgene bottle will be 2.00 mL. Two sete of trip blank spikes consisting of reagent-grade water, 

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

the 3M Environmerital Laboratory and sent to the sampling location with the other bottles. Results from 

GLP10-01-01-02, GLP10-O1-O1-O9, and GLP 10-01-01-17 were used to determine the field matrix spike levels 

forGLP10-01-01-22 listed in Table 1. 

Tabid . 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 TOO 

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

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

203L, 222R, 227R, 227L, 31 OR, 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 31 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

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 "Detennination of Perfluorinated 

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

Analysis". Dueto previous data for these sampling locations (GLP10-01-01-02, GLP10r01-01-09, and GLPlO01-01-17), 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 the target analytes with an analytical accuracy of 100±30%. Field matrix spikes not 

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

adjusted accordingly. 

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

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

Calibration curves used for both ETS-8^044.0 and ETS-8r110.1 vvill be cohstmcted using a reference material 

containing both linear and branched isomers of PFOA. Field matrix spikes will be prepai-ed with a solution 

prepared with a reference material containing predominantly linear PFOA Laboratory control sahnples (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 the sample,, sample duplicate, and the field 

matrix spikes. Trip blariksets 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 willialso be 

reported and used to evaluate the overall method accuracy and precision. Method blanks of reagent water 

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

matrix spikes that may be prepared will also be included In the final report. 

7 Email Correspondenc e 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 32 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

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, Martin; Johnson, Kevin A.; Missildine, BretC. 

Subject: Bottles - GW sampling Decatur, AL 

Charlie, 

The S"' quarter GW sampling will begin next Monday at Decatijr. The sampling for PCs will be inside this 

time and include the following: 

203L 

220R 

220L 

.222R 

227R 

227L 

31QR 

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 33 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

ATTACHMENT B : REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S) 

Page 34 of 56 
»** Buster J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batch Name: blllOOTa.dab 

b111007a.rdb (PFOA): "Quadratic" Regression ("1 / x" weighting): y = -2.44e+003 x"! + 6.94e+005 x + 2.25e+004 (r = 0.9995) 

40 45 50 55 

Concentration, ng/mL 

Data printe d by STW 

Printin g Time: 10:12:41 AM 

Printin g Date: Thursday, November 03, 2011 

Page 1 of 1 

Page 35 of 56 
Buster J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batch Name: blll007a.dab 

I

SampIo Name: "bl 11007b018' Sampla IDr "10007-27-9" Fila: "bl 11007b,w 

Peak Name: 'PFOA' Mass(es): MlS.O/SeS.O aimj.413.0/219.0 amu.413.(V16! 

Comment -2.5 ng/mL FC std In MD Q Water" Annolatior: ~ 

Sanpla Index : 18 

Modified : Yea 

Proc. Algocithm: IntelliQ i 

Mill . Peak Height: 0.00 

Min . Pea): Width : 0.00 

Smooching Width : 0 

RT Window: 30.0 

Expected RT: 

I • Sar 

I Pea 

• Cor 

! Rela • RT: 

14.8 15.0 

2819^ 2857 

Sample Name: "bl 11007a029' Sample ID: 'Solvent Blank' File: "bl 11007a.wifr 

Peak Name: TFOA' Mass{es):'413.0/369.0 amu,413.0/219.0amu,413.Cl/169.0 

Comment 'MIDI Q Water TN11 -0333* Annotation: -

Modified : 

Proc. Algorithm : I n 

Min . Peak Width : 

Smoothing Width : 0 

RT Window: 

Expected RT: 

! Relal 

Retention ' 

Area: 

Height: 

! RT: 

I Sample Name: •b111007a030' Sample ID:'LCS-111007-r FOe: "bl l 1007a.wtfr 

Peak Name: 'PFOA' Mass{ett): '413.0/369.0 a) 

• Comment '2ppb LCS" Annotatwn: ~ 

Sanpla Index: 30 

SADple Type: OC 

Concentration : 1.91 ng/mL 

Calculate d Cone: 2.80 ng/mL 

Acq. Date: 10/8/2011 

Acq. Time: 2:27:25 AM 

^.413.0/169.0 amu' I

Sample Name: •b111007a033' Sample ID: 'LCS-111007-4' File: "bl 11007a.wir 

Peak Name: 'PFOA* Mas5(es): '413.0/369.0 amu,413.0«19.0 amu,413.0/169,0 amu 

Comment '20ppb LCS* Annotation; ~ 

i l f ie . Yea 

Peoc. Algorithm : InColliQua n 

Min. Peak Height : 0.00 

Min. Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30.0 

Expected BT: 14.9 

cps 

! Reli 

Height: 

Start Ti 

End Tiro< 

I RT : Ho 

4 .00e*005 cp9 

14.7 min 

15.0 min 

3.6e5 

3.4e5 

3.2eS 

3.0eS 

2.ee6 

2.6e5 

2.4e5 

2.2e5 

2.0e5 

6.0e4 

4.0e4 

2.0e4 

^4.07 14.24^ 14.30 14.55^4.56 

.0 14.2 14.4 

i6 2704 2742 

RT windot 

Height: 

Start TJ 

End Tira« 1.6e6 

1.4e6 

1.2e6 

. 15.73 15.90^.^ 

15.0 

2819 2857 

Time, min 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 2011 

Page 1 of 7 

Page 36 of 56 
Buster J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batch Name: blll007a.dab 

I

Samp*eName:T)111007a036' Sample ID: •LCS-111007-7' File: 1>111007a.wir 

Peak Name: *PFOA* Mas9(es): '413.0/369.0 8mu.413.0/2ig.O amu.413.0/169.0 an 

Comment 'SOppb LCS* Anrwtation: "" 

Sample Index: 36 

Sample Type: OC 

Concentration : 47.7 ng/mL 

Calculate d Cone: 62.0 ng/mL 

Acq. Date: lO/B/2011 

Acq. Time: 4:34:02 AH 5.0e6 

Modified : Yea 

Proc. Algorithm : IntelliQua n - IQJ 

Min. Peak Height : 0.00 cps 

Min. Peak Width: 0.00 sec 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 

Expected RT: 

Relal [ RT: 

Retentio i 

Height : 

Star t Tir 

End Time 

14.9 

3701204 1 

5.44eiO06 

Sample Name: "bl 11O07aO43' Sample ID: 'GLP10-01-01-22-082- Fie: 'b111007a.wiff' I

Peak Name:'PFOA- Mass{esJ:*413. 

Comment 'DAL GW 203L RB* Annotation: 

Sampl e Index : 43 

Sampl e Type ; 

iu.413.0/219.0 amu.413.0/169.0 ai 

Unknown 

N/A 

Modified : 

Proc. Algorithmi 

Min . Peak Height 

Min . Peak Widthi 

ig Widthi 

RT Wli 

1 RT: 

Height: 

Start Tin 

14.8 15.0 

2819 2657 

I SampleName:-b111OO7a059' Sample ID: •GLP1^01-01-22.00r Fle:'b111007a.wtfr 

Peak Name: 'PFOA' Mass(es}: '413.0/369.0 ai 

• ConunenC 'DAL GW 203L 0' Annotation: * 

Sample Index: 61 

Sample Type: Unknown 

itelliQua i 

0.00 1 

0.00 ! 

j,413.0/219.0 amu.413.0/169.0 amu' 

3.8e5-

3.6e5-

3.4e5-

3.2e5-

3.0e5-

23e5-

2.6e5-

2.4e5 

2.2e5 

2.0e5-

1.8e5-

1.6e5 

1.4e5-

1.2e5-

1.0e5-

(

Sample Name: •b111007a063* Sampte ID: 'GLP10-01-01-22-005' Flle:'b111007a.wir 

Peak Name: TFOA' Mass{es): '413.0/369.0 amu,413.0/219.0 amu,413.0/169.0 amu' 

Comment 'DAL GW 220R 0" Anwtation: -

Sample Index: 65 

Sample Type: Unknown 

8.0e4 

6.0e4 

4.0e4 

2.0e4 

14.06^14.17.., 14.23 

Calculate d Cone: 28.8 ng/mL 

Acq. Date: 10/9/2011 

Acq. Time: 12:44:29 PM 

Modified : Yes 

Proc. Algorithm : IntelliQua n - IQA 

Min, Peak Height: 0.00 cps 

Min. Peak Width: 0.00 sec 

Smoothing Width: 0 point s 

RT Window: 30.0 sec 

Expected RT: 

Relal ! RT: No 

Area: 3940537 counts 

Height : 7.22e*005 cps 

Start Time: 14.4 rain 

7.0e5 

6.5e5 

6.0e5 

5.5e5 

5.0e5 

4.5e5 

4.0e5 

3.5e5 

3.0e5 

2.5e5 

2.0eS 

1.5eS 

1.0eS 

15.46 ^15.56 15.76 

14.8 15.0 

2819 2857 

Time, min 

14.8 

2819 2857 

Time, min 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 

Page 2 of 7 

Page 37 of 56 
*** Buste r J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batc h Name: blllOOVa.da b 

Fie: •b111007a.wtfr 

IntelliOua r 

: 0.00 1 

0.00 i 

I SampleName:"bll1DO7a071' Sample ID:'GLP1CM)1-01-22-009-

Peak Name:'PFOA' Mass[es):'413.0/369.0 amu.413.0/219.0 amu,413.0/169.0 amu' 

I Comment-DAL GW 220L 0' Annotation: " 

1.20e6-

1.15e6-

1.10e6-

1.05e6-

1.00e6 

9.50e5 

9.0Oe5-

8.50e5-

e.00eS7.50e5-

7.00e5-

g- 6.50eS-

^ 6.00e5-

I 5.50e5 

5.00e5 

4.50e5-

4.00e5-

3.50e5 

3.00e5 

2.50e5 

2.00e5 

1.50e5-

1.00e5 

5.0064 

0.00 

I

Sampte Name: t i 11007a075' Sample ID; 'GLPKM) 1-01-2 

Peak Name: TFOA' Mawfes): '413.0/369.0 amu,413.0/219 

Comment 'DAL GW 222R 0' /^nfwtatwn: ~ 

Sample Index: ^^ 

Sample Type: Unknown 

Calculate d Cone: 359. ng/mL 

Acq. Date: 10/9/2011 

Acq. Time: 4:57:34 PM 

Modified : Yes 

Proc. Algorithm : IntolliQua n - IQA 

Min. Peak Height: 0.00 cps 

Hln . Peak width ; 

Smoothing Width: 

RT Window: 

0. 00 

0 

30.0 

14.9 

Height: 

End Tin 

15.0 

2819 2857 

Time, min 

I

Sample Name: •b111007a083' Sarr^e ID: •GLPl(W)1-01-22-017' Fie: •b111007a.wttr 

Peak Name: 'PFOA' MassfesJ: '413.0/369.0 amu,413.0/219.0 amu.413.0/169.0 amu' 

Comment *DAL GW 227R 0' Annolatkw:" 

Calculate d Cone: 247. 

Acq. Date: 10/9/2011 

Acq. Time: 7:46:14 1 

Modified : Yes 

Proc. Algorithm : IntelliQ i 

Min. Peak Height : 0.00 

Min. Peak Width: 0.00 

Smoothing Width: 0 

RT Window: 30.0 

Expected RT: 

• Relai • RT: 

Height; 

Start 

End Tit 

1.3e6 

1.2e6 

9.0e5 

8.0eS 

3.065 

2.0e5 

I

Sample Name: •b111007a087' Sampte ID: •GLP10^1-01-22-02r File: •b11l007a.w«r 

Peak Name: "PFOA' Mass(8s): '413.0/369.0 amu,413.0/219.0 amu,413.0/169.0 amu' 

Comment "DAL GW 227L 0' Annotation: " 

Modified : 

Min 

RT Window: 

Expected RT: 

Use Relativ e 

Retention T i 

Area: 

Height: 

star t Time: 

IntelJiCJu; 

L Height: 0.00 

: Width: 0.00 

I Width: 0 f 

• : 30.0 

RT: 

9.10o*005 cps 

15.0 

2819 2857 

Time, min 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 2011 

Page 3 of 7 

Page 38 of 56 
Buste r J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batc h Name: blll007a.da b 

1"^ . Peak Name:'PFOA* Ma3s(es):'413.0/369.0 ai 

Comment "DAL GW 310R 0' Annotatkjn:' 

Sample 

I Sample Name: ti l 1007a095' Sampte ID: •GLP1O^1-01-22-025' Fle:-b111007a.witr 

' - • • 119.0amu,413.0/169.0amu' 

Type: 

Calculate d Cone: 

Acq. Date; 

Acq. Time: 

Modified : 

Proc. Algorithm : 

Min. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Unkni 

N/A 

! Relal • RT: 

1.15e6 

1.10e6 

1.0Se6 

1.00e6 

9.50e5 

9.00e5 

8.50e5 

6.00e5 

7.5065 

7.00e5 

§• 6.50e5 

^ 6.00e5 

I 5.50e5 

5.0005 

4.50e5 

4.00e5 

3.50e5 

3.00e5 

2.50e5 

2.00e5 

1.50e5 

1.00e5 

5.00e4 

0.00 

14.6 15.0 

2619 2857 

Time, n 

Sample Name: "bl 11007a099' Sampte ID: "GLP10-01-01-22-029* File: "bl 11007a.wir I

Peak Name: 'PFOA' Mass(es): '413.0/369.0 

Comment 'DAL GW 312R 0" Annotation: ~ 

Sample Index: 101 

Sample Type: 

Calculate d Cor 

Acq. Date: 

Acq. Time: 

Modified : 

Unknown 

H/A 

19 60. I 

10/10/2011 

1:24:05 AM 

IntelliQ i 

0 .00 

0 . 00 

Expected RT: 

Use Relativ e 

Int . Type: 

I

Sample Name: ti l 1007a10r Sampte ID: •GLP10-01-01-22-033' Fie: •b111007a.wifr 

Peak Name: 'PFOA' Mass(e5l: *413.0/369.0 amu.413.0/219.0 amu,413.0/169.0 amu" 

Comment *DAL GW 317L 0' Annotation; ~ 

Sample Index: 109 

Sample Type; Unknown 

Concentration ; (J/A 

Calculate d Cone: 0.340 ng/roL 

Acq. Date: 10/10/2011 

Acq. Time: 4;13;17 AM 

itelliOua i 

0.00 1 

0.00 : 

Snoothinc 

I SampleName:"bll1007a1ir Sampte ID:'GLP10-01-01-22-03r Filo:t111007a.wir 

Sample Type: 

Concentratio n 

Calculate d Coi 

Smoothing Wic 

RT Window: 

Expected RT: 

Height: 

Start Tlr 

End Time: 

14.6 15.0 

2819 2857 

Time.,min , 

7.5eS7.0e5-

6.5e5-

6.0e5-

5.5e5 

5.0e5-

4.5e5-

4.0e5 

3.5e5 

3.0e5 

2.5e5 

2.0o5 

1.5e5-

1.0e5-

5.0e4 

0.0-

15.50 ^15.59 15.79 

15.0 

2819 2857 

TImg. min 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 2011 

Page 4 of 7 

Page 39 of 56 
Buster J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batch Name: blll007a.dab 

I SampteName:t111007a119' Sampte ID:'GLP1tM)1-01-22-041* Fie: t111007a.w«r 

Peak Name:*PFOA* Mass(es):'413.0/369.0ai 

• Comment-DAL GW 327R 0' Annotatton:' 

Sample Index; 121 

Sample Type: Unknown 

Concentration : M/A 

Calculate d Cone: 645. ng/mL 

Acq. Date: 10/10/2011 

Acq. Time: 8:26;55 AM 

Modified : Ves 

Proc. Algorithm : IntelliOua n - IQA 

Min . Peak Height: 0.00 cps 

Min . Peak Width; 0.00 sec 

Smoothing Width : 0 points 

iu,413.0/169.0emu' 

RT [indoi 

1.2e6' 

1.1»6 

Height: 

Start Time: 

End Time; 

14.8 15.0 

2819 2857 

Time, min 

I

Sample Name: t i 11O07a123' Sampte ID: 'i 

Peak Name:'PFOA* MaM(es):'413.0/369.0 

Comment 'DAL GW 32eR 0' Annotatwn: 

Sample Index; 125 

Sample Type: Unknown 

Modified ; 

Proc. Algorithm : Ii 

Min. Peak Height: 

Min . Peak Width : 

Smoothing Width ; ( 

RT Window: 

Expected RT; 

2.1e6 

2.0e6 

1.8e6 

1.7e6 

7.0e5 

6.0e5 

5.0e5 

4.0e5 

3.0e5 

2.0e5 

15.0 

2619 2857 

I

Sampte Name: t111007a131' Sampte ID:'( 

Peak Nanw:'PFOA' Mass(esJ:'413.0/369.0 

Comment 'DAL GW 328L 0' Annotation: ~ 

Sample Index: 133 

Sample Type; Unknown 

Concentration : N/A 

Calculate d Cone: 100. ng/mL 

Acq. Date: 10/10/2011 

Acq. Time: 12:40:22 PM 

Modified : 

, Algorithm : 

Peak Height; 

Peak Width: 

ihln g Width : 

itelliQu ) 

0.00 

0.00 

Start Time: 

1.10e6-

1.05e6 

1.00e6 

9.50e5 

9.00e5 

8.S0e5 

8.00e5 

7.50e5 

7.00e5 

6.S0e5 

6.00e5 

5.50e5 

5.00e5 

4.50e5 

4.00e5 

3.50e5 

3.00e5 

2.50e5 

2.00e5 

1.50e5 

1.00e5 

5.00e4 

0.00 

I

Sampte Name: t i 11007a135' Sampte ID: '< 

Peak Nanw:-PFOA' Mass(e9):'413.0/369.0 

Comment 'DAL GW 330R 0' Annotetten: -

Sample Index; 137 

Acq. Time: 

Modified ; 

Proc. Algorith m 

Min. Peak Heigh( 

Min. Peak Width 

Smoothing Width 

itelliQua n • 

0.00 cp[ 

0.00 set 

I RT: 

4.8e5 

4.6e5 

4.4e5 

4.2&5 

4.0e5 

3.8e5 

3.6e5 

3.4e5 

3.2e5 

3.0e5 

2.8e5 

2.6e5 

2.4e5 

2.2e5 

2.0e5 

1.8e5 

1.6e5 

1.4o5 

1.2e5 

1.0e5 

8.0e4 

6.0e4 

4.0»4 

2.0e4 

14.6 15.0 

2619 2857 

Time, min 

15.0 

2819 2857 

Time, min 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 

Page 5 of 7 

2011 

Page 40 of 56 
Buste r J2930203 

GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Batc h Name: blll007a.da b 

I SampteName:t111007a143' Sampte ID:'GLP1{M)1-01-22-O5r Fie: t111007a.witr 

Peak Name: "PFOA* Mass(es): '413.0/369.0 a 

• Comnrtent "DAL GW 330L 0' Annotafion: "" 

Sample Index: 145 

Sample Type: Unknown 

Concentration : N/A 

Calculate d Cone: 366. ng/mL 

Acq. Date: 10/10/2011 

Acq. Time: 4:S3;32 PM 

Modified : Ves 

Smoothing width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Height; 

End Time: 

iu,413.0/219.0 amu,413.0/169.0 ai 

6.5o5 

6.0e5 

7.5e5 

7.0c5 

6.5e5 

6.0e5 

5.5e5 

5.0e5 

4.5e5 

4.0e5 

3.5e5 

3.0e5 

2.5e5 

2.0e5 

1.5e5 

1.095-

5.0e4 

14.8 15.0 

2819 2857 

Time, min 

Sampte Name: t111007a14r Sampte ID: •GLP10-01-01-22-061' FJe:t111007a.wifr I

Peak Name: 'PFOA' Massfes): *413.i 

Comment 'DAL GW 331S 0" Annolatton: 

Sample Index; 149 

Sample Type: Unknown 

Concentration : K/A 

Calculate d Cone: 744. ng/raL 

Acq. Date: 10/10/2011 

Acq. Time: 6:18:16 PM 

Modified : Yes 

Proc. Algorithm : IntelliQua n - IQJ 

Min . Peak Height: 0.00 cps 

Min . Peak Width : 0.00 sec 

Smoothing Width : 0 points 

RT Window; 30.0 sec 

Expected RT: 14.9 min 

Use Relativ e RT: No 

Height: 

iu,413.0/219.0 amu,413.0/169.0 amu' 

I.7e6 

1.6e6 

1.5e6 

1.4e6 

13e6 

1.206 

1.1e6 

1.0e6 

9.0e5 

8.0e5 

7.0e5 

6.0e5 

5.0eS 

4.0e5 

3.0eS 

2.0e5 

1.0e5-

0.0-

14.8 15.0 

2819 2857 

Time, min 

I

SampteName:t1l1007al55' Sample ID: •GLP10«1-01-22-065' Flo:t111007a.w«r 

Peak Name: "PFOA' Mass(es): "413.0/369.0 amu,413.0/219.0 amu.413.0/169.0 amu' 

Comment 'DAL GW 335R 0' Annotation:" 

Sample Index: 157 

Sample Type; Unltnown 

9:07:19 PM 

(

Sample Name: t111007a159' Sampte ID: *GLP10-01-01-22-069' FIte: t111007a.wir 

Peak Name: -PFOA' Mass{es): -413.0/359.0 amu,413.0/219.0 amu.413.0/169.0 amu" 

Comment'DAL GW GRS04 0* Amolatian:-

Smoothlng Width : 

IntelliQua n - IQA 

Min . Peak Width; 

Expected BT: 

Retentio n Tin 

End Time: 

2.91e+006 cps 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 2011 

Page 6 of 7 

Page 41 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

Buster J2930203 Batch Name: blll007a.dab 

f

Sample Name: t111007t>00r Sample ID:'LCS-111010-01' Fite:-b111007b. 

Peak Name: *PF0A' Mass(«a): '413.0/369.0 amu,413.0/219.0 amu.413.0/169.0 amu' 

Comment: 'SOOppb LCS' Annotation: " 

Sample Index; 2 

Sample Type: QC 

Concentration ; 500. ng/mL 

Calculate d Cone: 478. ng/mL 

Acq. Date; 10/11/2011 

Acq. Time: 1:41:49 AM 

Peak Height: 

Smoothing 1 

RT Window; 

Expected R: 

Height: 

Star t Ti l 

End Time 

7.69e»005 

14.8 15.0 

2819 2857 

Time, min 

Data printe d by STW 

Printin g Time: 10:11:09 AM 

Printin g Date: Thursday, November 03, 

Page 7 of 7 

Page 42 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

ATTACHMENT C: ANALYTICAL METHOD(S) 

Page 43 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA In Groundwater Samples 

3rd Quarter 2011 Sampling 

3IVI Environmental 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 ^^rg y/<3 7 

Approved By: 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

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

Injection Analysis Page 44 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

1 Scope and Application 

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

PerfiuorohexanoicAcid (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 Perfonnance 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 altemate 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 predeteimined 

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

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

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

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

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

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

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

ETS-8-044.0 Page 2 of 11 

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

Injection Analysis 

Page 45 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

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 quantities of target analytes are added 

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

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

sample matrix must be determined in a separate aliquot and the measured values in the LMS con^ected 

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

ETS-8-044.0 Page 3 of 11 

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

Injection Analysis 

Page 46 of 56 
GLP10-01-01; Interim Report 22 

Analysis of PFOA in Groundwater Samples 

3rd Quarter 2011 Sampling 

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-analyte prepared in the laboratory with an assayed reference 

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

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

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

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

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

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

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

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

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

4.2 Cautions 

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

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

appropriate equipment procedure or operator manual for additional infomnation 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. 

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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). 1 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

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

Gas tight syringes, 25pL, 50pL, lOOpL, 250pL, 500pL, lOOOpL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

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

6.2 Chromatographic System 

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

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

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

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. 

RunTime: ~ 17minutes. 

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

provided that data quality objectives are met. 

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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, alternate instruments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

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

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

PerfiuorohexanoicAcid (PFHA-C6 acid); Oakwood Products, Inc 

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

Products, Inc 

Perfluorooctanoic Acid (PFOA - C8 acid); 3M 

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

Perfluorodecanoic Acid (PFDA - CI 0 acid); Oakwood Products, Inc 

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

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

Perfluorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfluorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfluorooctanesulfonate (PFOS - C8 sulfonate); 3M 

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

used. 

7.3 Reagent Preparation 

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

water. 

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

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

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

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

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

^. , ^ molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

499 

PFOS (K"')salt correction factor = — = 0.9275 

538 

10 mg CSFITSO/K" with purity 90% = 8.35mg CSFITSOS" (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 10mL volumetric 

flask and bring up to volume with solvent. 

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

volumetric flask and bring up to volume with solvent. 

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

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and 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. 

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7.5 Calibration Standards 

Using the wori<ing standards described above, prepare calibration solutions in ASTM Type 1 water, HPLC water, or 

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

ofWS, ng/mL Volume of WS, fd. 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTIVI 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 

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

Dilute sample, if necessary, with ASTM Type 1, HPLC water, or other suitable water. 

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

Prepare at least five method blanks. 

9 Sample Analysis - LC/MS/MS 

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

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

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

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

thoroughly documented in the raw data. 

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

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

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

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

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

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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 construct the calibration curve. 

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

curve (if necessary) and reanalyze. 

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

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

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

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

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

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

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

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

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

the raw data and footnoted in the final report. 

10.2 Method Blanks 

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

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

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

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

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

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

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

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

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

10.3 Sample Replicates 

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

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

replicates excludes field blanks. 

10.4 Surrogate Spikes 

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

10.5 Lab Control Sample 

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

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

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

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

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

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

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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 detennine the statement of accuracy for analytical results. 

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

11 Data Analysis and Calculations 

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

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

Analyte found (ng/mL) = (Peak Area-Intercept) ^ 

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. 

Recovery - ^"^'y*® found (ng/mL) - Average analyte found in sample (ng/mL) ^^QQ 

Analyte added (ng/mL) 

12 Method Performance 

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

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

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

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

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

discussed in the text of the report. 

12.1 System Suitability 

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

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

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

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

have area counts with an RSD of <5% and a retention time RSD of ^2% 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 infomnation regarding the required accuracy of laboratory control spikes, field matrix 

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

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

13 Pollution Prevention and Waste Management 

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

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

14 Records 

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

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

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

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

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

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ATTACHMENT D: DEVIATION(S) 

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RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

study / Project No. 

GLP10-01-01-22 

Date(s) of Occurrence: 

b111007a 

Document Number: 

ETS-8-044.0 

Deviation type • SOP 

(Check one) • Protocol 

• Equipment Procedure 0 Method 

• GPO • Other: 

//. Description (attach extra pages as needed) 

Method Requirements: 

1. FMS (ETS-8-044.0 section 10.6): recoveries within 100% ± 30%. 

Actual procedure/process: 

1. Sampling location DAL GW 222R HS recovery for PFOA was 61.4%. 

///. Actions Taken (such as amendment issued, SOP revision, etc.) 

Corrective Action (• Yes 0 No) Reference: 

Acceptability of the nonconforming work: 

1. The non-compliant DAL GW 222R HS will be flagged in the final report. The method uncertainty will be 

expanded for PFOA to ±39%. 

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

0 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: Susan 

Study Director (if GLP): 

Sponsor Approval (for GLP proTOCordeviations): NA 

Date:/ , 

Date: N 

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) 

Attachment A ETS-4-008.7 Page l^of J 

Documentation of Deviations and Control of Nonconforming Testing Page 56 of 56