GLP10-01-01. Interim Report 11: Analysis of PFOA in Groundwater Samples Collected at 

the Former Sludge Incorporation Area (FSIA) located in Decatur. AL in November 2010 

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 

Maplewood, MN 55144 

Project Identification 

GLP10-01-01-11 

Total Number of Pages 

53 

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 Intemational Standard also 

operate in accordance with ISO 9001:2000. 

Certificate #2052.01 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

This page has been reserved for specific country requirements. 

Page 2 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

GLP COMPLIANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 11. Analysis of PFOA in Groundwater Samples Collected 

at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 

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. 

Gary Hqraenslein, Sponsor Representative Date 

^'m 

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

Page 3 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 11. Analysis of PFOA in Groundwater Samples Collected 

at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 

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 

12/30/10 

1/27/11-1/28/11 

Phase 

In-Phase 

Data/Interim Report 

Date Reported to 

Testing Facility 

Management 

2/4/11 

2/4/11 

Study Director 

2/4/11 

2/4/11 

URepresealtativ 

/•C-^eJ ^ ;i'J''f 

QAU Representative Date 

Page 4 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Infonnation 8 

2 Summary 9 

3 Introduction 10 

4 Tests Control Substances 11 

5 Reference Substances 11 

6 Test System 12 

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 16 

8.8 Field Matrix Spikes (FMS) 16 

Page 5 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

9 Data Summary and Discussion 17 

10 Conclusion 30 

11 Data/Sample Retention 30 

12 Attachments 30 

13 Signatures 31 

LIST OF TABLES 

Table 1. Summarized PFOA Results (FSIA Groundwater, Decatur, AL, November 2010) 10 

Table 2. Instalment Parameters... 13 

Table 3. Liquid Chromatography Conditions 13 

Table 4. Mass Transitions 13 

Tables. Limit of Quantitation (LOQ) 14 

Table 6. Laboratory Control Spike Recovery 15 

Table 7. Analytical Method Uncertainty 16 

Table 8. Field Matrix Spike Levels 16 

Table 9. DAL GW130R 101105 18 

Table 10. DAL GW130S 101105 18 

Table 11. DAL GW130L 101105 18 

Table 12. DAL GW131R 101103 19 

Table 13. DAL GW131S 101103 19 

Table 14. DAL GW131L 101103 19 

Table 15. DAL GW132R 101102 20 

Table 16. DAL GW132S 101102 20 

Table 17. DAL GW132L 101103 20 

Table18. DALGW133R101102 21 

Table 19. DAL GW133S 101103 21 

Table 20. DAL GW133L 101103 21 

Page 6 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 21. DAL GW134R 101105 22 

Table 22. DAL GW134S 101105 22 

Table 23. DAL GW134L 101105 22 

Table 24. DAL GW135R 101105 23 

Table 25. DAL GW135S 101105 23 

Table 26. DAL GW135L 101105 23 

Table27. DALGW136S101103 24 

Table28. DALGW136L101103 24 

Table29. DALGW137S101109 24 

Table30. DALGW137L101109 25 

Table31.DALGW138S101110 25 

Table32. DALGW138L101110 25 

Table33. DALGWCW26R101110 26 

Table34. DALGWGVV26L101110 26 

Table35. DALGW140R101104 26 

Table36. DALGW141R101110 27 

Table37. DALGW142R101110 27 

Table38. DALGW144R101110 27 

Table 39. Trip Blank 1 28 

Table40. TripBlank2 28 

Table 41. Trip Blank 3 28 

Table42. TripBlank4 29 

Table 43. Rinseate Blanks 29 

Page 7 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari(@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

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

Susan Wolf, 3M Analyst 

Kevin Eich; Analyst 

Cheisie Grochow, Analyst 

Jonathan Steege; Analyst 

Study Dates 

Study Initiation: March 8, 2010 

Interim Report 11 Experimental Tennination: January 8,2011 

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 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

2 Summary 

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

Sludge Incorporation Area (FSIA) in Decatur, AL, representing thirty different sampling locations. A 

total of one hundred sixty-nine 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 at least two field matrix spike (FMS) samples for each location, four 

trip blank sets containing Milli-QTM water and appropriate trip blank spikes, and two equipment 

rinseates. In addition, one soil equipment rinseate blank from GLP10-01-01-12 was analyzed. The 

equipment rinseate blanks did not have FMS samples prepared for determination of PFOA recovery. 

The groundwater samples, trip blanks and two equipment rinseate blanks associated with GLP10-01-

01-10 were received from Weston personnel on November 18, 2010. The equipment rinseate blank 

associated with GLP10-01-01-12 was received from Weston personnel on October 15,2010. All of the 

samples were prepared and analyzed for PFOA following 3M Environmental Laboratory Method ETS8-044.0 under 3M project GLP-10-01-01-11. Many ofthe 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 rinseates and the trip blank were below the lower limit of quantitation (LLOQ) of 0.0250 

ng/mL, indicating adequate control of sample contamination during shipping and sample collections. 

The PFOA concentration results for all groundwaters ranged over four orders of magnitude from 0.271 

ng/mL to 2910 ng/mL. The analytical uncertainty was estimated at 100 + 23%. 

Page 9 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 1. Summarized PFOA Results (FSIA Groundwater, Decatur, AL, November 2010) 

Sample ID 

DALGW130R101105 

DALGW 1308 10 1105 

DAL GW130L 101105 

DALGW 131R 101103 

DAL GW131S 101103 

DAL GW131L 101103 

DAL GW132R 101102 

DAL GW132S 101102 

DALGW132L101103 

DAL GW133R 101102 

DALGW 1338 101103 

DAL GW133L 101103 

DAL GW134R 101105 

DALGW 1348 10 1105 

DALGW134L101105 

DAL GW135R 101105 

DALGW 1358 101105 

DALGW135L101105 

DALGW 1368 101103 

DALGW136L101103 

DALGW 1378 101109 

DALGW137L101109 

DALGW 138S 101110 

DALGW 138L 10 1110 

DAL GWCW26R 101110 

DAL GWCW26L 101110 

DAL GW140R 101104 

DALGW 141R 101110 

DALGW 142R 101110 

DALGW 144R 101110 

Trip Blanks (Milli-QTM Water) 

GLP10-01-01-11 Equipment rinseate blanks: 

DAL GW 130L and DAL GW 144R 

GLP10-01-01-12 Soil Equipment rinseate blank: 

DAL 88 607R 

Avg. PFOA 

Concentration 

(ng/mL) 

793 

174 

70.0 

2500 [a] 

24.9 

90.7 

251 

962 

404 

102 

385 

252 

1570[bl 

5.49 

520 

2910 [al 

13.7 

123 

75.4 

75.3 

0.271 

0.361 

147 

1.16 

386 

552 

121 

1.84 

47.6 

57.3 

< 0.0250 

< 0.0250 

< 0.0250 

Relative 

Percent 

Difference 

0.88% 

0.58% 

2.0% 

1.6% 

4.0% 

5.2% 

4.4% 

0.52% 

3.0% 

9.5% 

4.2% 

1.2% 

9.6% 

5.5% 

1.3% 

1.4% 

3.7% 

2.4% 

3.8% 

3.1% 

1.8% 

0.28% 

3.4% 

6.1% 

1.8% 

4.7% 

0.83% 

10% 

4.6% 

0.17% 

N/A 

N/A 

N/A 

N/A; not applicable 

The analytical uncertainty for PFOA was estimated at 100 + 23%. 

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

PFOA recovery. 

[b] The analytical uncertainty has been adjusted for field matrix spike recovery to ± 31 %. 

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 

Page 10 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area • November 2010 

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 

at the Former Sludge incorporation Area (F8AI) in Decatur, AL for PFOA in an effort to characterize 

regional groundwater conditions. 

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

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

groundwater sampling location included a field sample, field sample duplicate, and a minimum of two 

field spike samples. Each empty container for groundwater samplings was mari<ed 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. 

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

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

Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis". 

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

collected, the trip blank, and equipment rinseate samples. Tables 9-43 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. 

1 Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOA 

Perfluorooctanoate 

C7F15COOH 

CAS # 335-67-1 

Oakwood Products 

09/29/2012 

Frozen 

3440 

TCR07-0041 

Powder 

99.5% 

PFOA 

Perfluorooctanoate 

C7F15COOAmmonium Salt 

CAS # 335-67-1 

3M 

02/27/2017 

Frozen 

332 

TCR-123 

White Powder 

95% 

Page 11 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

6 Test System 

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

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

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

Sample Description Key Code. 

string Number 

Example 

1 

2 

3 

4 

5 

string Descriptor 

DAL 132R 0101102 

Sampie Location 

Weil ID 

Weil Level 

Sampling Date 

Sampie Type 

Example 

DAL= Decatur, Alaliama 

Example: 132 

R = Residum shallow water-bearing zone 

L = Bedrock water-bearing zine 

S = Epikarst middle water-bearing zone 

101102- November 2,2010 

0=primary sample 

1=duplicate sample 

LS = low spike 

MS = mid spike 

HS = high spike 

7 Method Summar y 

7.1 Methods 

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

"Determination of Perfluorinated Compounds In Water by High Perfonnance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

-TM , 

7.2 Sample Collection 

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

Environmental Laboratory. Sample bottles associated with GLP10-01-01-11 were retumed to the 

laboratory at ambient conditions on November 18, 2010. The equipment rinseate blank associated with 

GLP10-01 -01 -12 was returned to the laboratory at ambient conditions on October 15,2010. 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 each cooler of sample collection bottles. 

7.3 Sample Preparation 

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

analysis. 

Samples that required dilution were prepared by dilutions ImL sample with 9 mLs of Milli-Q water 

(dilution 1:10). Some sampling locations were diluted 1:100 by diluting the 1:10 and additonal with MilliQ water. 

7.4 Analysi s 

All study samples and quality control samples were analyzed for PFOA using high perfonnance liquid 

chromatography/tandem mass spectrometry (HPLC/MS/MS). Detailed instrument parameters, the 

Page 12 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area • November 2010 

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

raw data hard copies placed in the final data packet, and are briefly described below in Table 2, Table 3 

and Table 4. 

Table 2. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Date 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETS Buster 

ETS-8-044.0 

1/3/11-1/8/11 

Agilent 1100 

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

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

2or10nL 

/Applied Biosystems API 4000 

Turbo Spray 

Turbo ion electrode 

Negative 

Analyst 1.4.2 

Table 3. Liquid Chromatography Conditions. 

step 

Number 

0 

1 

2 

3 

4 

5 

Total Time 

(min) 

0 

2.0 

11.5 

13.5 

13.6 

17.0 

Flow Rate 

(nUmin) 

300 

300 

300 

300 

300 

300 

Percent A 

(2 mM ammonium acetate) 

. 97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

Percent B 

(Methanol) 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Table 4. Mass Transitions. 

Analyte 

PFOA 

Mass Transition 

Q1/Q3 

413/369 

413/219 

413/169 

Dwell time was 100 msec for each transition. 

The individual transitions w/ere 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 ofthe stock solution containing the target analytes into a laboratoryMilli Q water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL (nominal) were 

Page 13 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

prepared. The two highest curve points were disabled to meet linearity criteria. A quadratic, 1/x 

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

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

peak area confinned accuracy of each curve point. 

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

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

analytes. The con-elation coefficient (r) was greater than 0.995 for PFOA. 

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 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 twice those ofthe appropriate 

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

Table 5. Limit of Quantitation (LOQ). 

Analysis Date 

1/3/11 

PFOA 

LOQ, ng/mL 

0.0250 

8.4 Continuing Calibration 

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

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

CCVs met method criteria of 100% ± 25% for PFOA. 

8.5 Blanks 

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

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

performance to determine the LOQ for PFOA. Trip blanks reflect the shipping and sample collection 

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

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

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

8.6 Lab Control Spiltes (LCSs) 

Low, mid, and high-level lab control spikes were prepared and analyzed in triplicate with each 

preparation set. LCSs were prepared by spiking known amounts ofthe analyte into 40 mL of laboratory 

Milli Q 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 <2i3/o, were met for the linear PFOA LCS samples. 

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

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

and branched PFOA were prepared at three concentrations to evaluate the potential for analytical bias. 

The average recovery of the linear and branched LCS at the low and high levels met method 

acceptance criteria. The mid-level linear and branched LCS had an average recovery of 123%. Ail LCS 

samples were used in the determination of method uncertainty in section 8.7. 

Page 14 of 53 
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Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

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

LCS Percent Recovery = 

Calculated Concentration, 

Spike Concentration 

100% 

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

average LCS recovery 

Table 6. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Analyzed 1/3/2011 

Lab ID 

LCS-101230-1 

LCS-101230-2 

LCS-101230-3 

Average ±%RSD 

LCS-101230-4 

LCS-101230-5 

LCS-101230-6 

Average ±%RSD 

LCS-101230-7 

LCS-101230-8 

LCS-101230-9 

Average ±%RSD 

Linear PFOA 

Spiked 

Concentration 

(ng/mL) 

0.497 

0.497 

0.497 

Calculated 

Concentration 

(ng/mL) 

0.580 

0.557 

0.590 

VoRecovery 

117 

112 

119 

116% ±3.1% 

4.97 

4.97 

4.97 

5.83 

5.69 

5.69 

117 

115 

114 

115% ±1.3% 

29.9 

29.9 

29.9 

25.6 

25.8 

25.7 

85.6 

86.3 

85.9 

85.9% ±0.41% 

ETS-8-044.0 

Analyzed 1/3/2011 

Lab ID 

LCS-101230-10 ECF 

LCS-101230-11 ECF 

LCS-101230-12 ECF 

Average ±%RSD 

LCS-101230-13 ECF 

LCS-101230-14 ECF 

LCS-101230-15 ECF 

Average ±%RSD 

LCS-101230-16 ECF 

LCS-101230-17 ECF 

LCS-101230-18 ECF 

Average ±%RSD 

Linear + Branched PFOA 

Spiked 

Concentration 

(ng/mL) 

0.498 

0.498 

0.498 

Calculated 

Concentration 

(ng/mL) 

0.546 

0.553 

0.541 

YoRecovery 

110 

111 

109 

110% ±0.91% 

4.99 

4.99 

4.99 

6.29 

6.03 

612 

126 

121 

123 

123% ±2.0%'" 

29.9 

29.9 

29.9 

31.3 

30.8 

30.6 

105 

103 

102 

103% ±1.5% 

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

Page 15 of 53 
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Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

8.7 Analytical Method Uncertainty 

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

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

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

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

con-esponds to a confidence level of 95%. 

Table 7. Analytical IVIethod Uncertainty. 

Analyte 

PFOA 

Method 

ETS-8-044.0 

Standard Deviation 

11.3 

Method 

Uncertainty 

± 23% 

8.8 Field Matrix Spikes (FMS) 

A minium of two 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 the target analytes 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 8. Field Matrix Spike Levels. 

Sampling Location 

136R, 137R, 137s, 137L, 138L 

130L, 131L, 131S, 133R, 134S, 135S, 136S 

130R, 130S, 132R, 132L, 132S, 133S, 133L, 

134L, 135L, 136L, 138S, 138R, CW26R, CW26L, 

140R, 141R, 142R, 143R, 144R 

131R, 134R, 135R 

Trip Blank 

Spike Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

PFOA, ng/mL 

0.0991 

0.991 

9.91 

0.991 

9.91 

99.1 

9.91 

99.1 

991 

99.1 

991 

0.991 

9.91 

99.1 

991 

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

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

Spike Concentraton 

Page 16 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

9 Data Summary and Discussion 

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

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

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

from those listed in the raw data. 

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

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

DAL GW 134R101104 - The high-level FMS did meet method acceptance criteria with a recovery of 

69.1%. The low-level FMS was not appropriate as compared to the sample concentration. The 

analytical uncertainty has been adjusted for PFOA to ± 31 %. 

DAL GW 1 SIR 101103 - Due to the high concentration of PFOA detected in the sample, this sampling 

location did not have an appropriate FMS spike level to sufficiently evaluate PFOA recovery. 

DAL GW 135R101105 - Due to the high concentration of PFOA detected in the sample, this sampling 

location did not have an appropriate FMS spike level to sufficiently evaluate PFOA recovery. 

Page 17 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Tables. DALGW 130R 101105 

3MUIVISID 

GLP10-01-01-11-001 

GLP10-01-01-11-002 

GLP10^1-01-11-003 

GLP10-01-01-11-004 

GLP10-01-01-11-005 

Description 

DAL GW130R 0101105 

DALGW130RDB101105 

DALGW130RLS101105 

DALGW130RMS101105 

DALGW130RHS101105 

Average Concentration (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

789 

796 

805 

895 

1680 

YoRecovery^ 

NA 

NA 

NC 

NC 

89.6 

793 ng/mL ±0.88% 

NA = Not Applicable 

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

Table 10. DALGW 1303 101105 

3M LIMS ID 

GLP10-01-01-11-006 

GLP10-01-01-11-007 

GLP10-01-01-11-008 

GLP10-01-01-11-009 

GLP10-01-01-11-010 

Description 

DAL GW130S 0101105 

DAL GW130SDB 101105 

DALGW130SLS101105 

DALGW130SMS101105 

DAL GW130SHS 101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

174 

173 

183 

270 

1150 

YoRecovery 

NA 

NA 

NC 

97.4 

98.5 

174 ng/mL ±0.58Yo 

NA = Not Applicable 

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

Table 11. DALGW 1 SOL 101105 

3M LIMS ID 

GLP10-01-01-11-011 

GLP10-01-01-11-012 

GLP10-01-01-11-013 

GLP10-01-01-11-014 

GLP10-01-01-11-015 

Description 

DAL GW130L 0 101105 

DALGW130LDB101105 

DALGW130LLS101105 

DALGW130LMS101105 

DALGW130L HS 101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

69.3 

70.7 

71.0 

73.3 

162 

YoRecovery 

NA 

NA 

NC 

NC 

92.8 

70.0 ng/mL 12.0Yo 

NA = Not Applicable 

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

Page 18 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 12. DAL GW 131R101103 

3M LIMS ID 

GLP10-01-01-11-017 

GLP10-01-01-11-018 

GLP10-01-01-11-019 

GLP10^1-01-11-020 

Description 

DAL GW131R0 101103 

DAL GW131RDB 101103 

DAL GW131RLS 101103 

DAL GW131RHS 101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

2520 

2480 

2b/U 

3240 

YoRecovery^ 

NA 

NA 

NC 

NC 

2500 ng/mL ±1.6Yo'^^ 

NA = Not /Applicable 

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

(1) Sampling location did not have an appropriate spike level to evaluate PFOA recoveiy. 

Table 1S. DAL GW 1 SI S 10110S 

3M LIMS ID 

GLP10-01-01-11-021 

GLP10-01-01-11-022 

GLP10-01-01-11-023 

GLP10-01-01-11-024 

GLP10-01-01-11-025 

Description 

DAL GW131S 0101103 

DALGW131SDB 101103 

DALGW131SLS 101103 

DALGW131S MS 101103 

DALGW131SHS 101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

25.4 

24.4 

25.3 

34.6 

127 

YoRecovery 

NA 

NA 

NC 

NC 

103 

24.9 ng/mL ±4.0Yo 

NA = Not /Applicable 

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

Table 14. DAL GW 131L 10110S 

3M LIMS ID 

GLP10-01-01-11-026 

GLP10-01-01-11-027 

GLP10-01-01-11-028 

GLP10-01-01-11-029 

GLP10-01-01-11-030 

Description 

DAL GW 131L 0101103 

DAL GW131LDB 101103 

DAL GW131LLS 101103 

DAL GW 131L MS 101103 

DAL GW131LHS 101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

88.3 

93.0 

87.7 

96.9 

179 

YoRecovery 

NA 

NA 

NC 

NC 

89.2 

90.7 ng/mL ±5.2Yo 

NA = Not Applicable 

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

Page 19 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 15. DALGW 1S2R101102 

3M LIMS ID 

GLP10-01-01-11-031 

GLP10-01-01-11-032 

GLP10-01-01-11-033 

GLP10-01-01-11-034 

GLP10-01-01-11-035 

Description 

DAL GW132R 0101102 

DALGW132RDB101102 

DALGW132RLS101102 

DALGW132RMS101102 

DAL GW132RHS 101102 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

256 

245 

267 

356 

1160 

YoRecovery 

NA 

NA 

NC 

NC 

91.8 

251 ng/mL ±4.4Yo 

NA = Not /Applicable 

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

Table 16. DALGW 1328 101102 

3M LIMS ID 

GLP10-01-01-11-036 

GLP10-01-01-11-037 

GLP10-01-01-11-038 

GLP10-01-01-11-039 

GLP10-01-01-11-040 

Description 

DAL GW132S 0101102 

DALGW132SDB 101102 

DALGW132SLS 101102 

DALGW132SMS101102 

DALGW132SHS101102 

Average Concentration (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

959 

964 

926 

1020 

1810 

YoRecovery 

NA 

NA 

NC 

NC 

85.6 

962 ng/mL ±0.52Yo 

NA = Not Applicable 

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

Table 17. DALGW 1S2L101103 

3M LIMS ID 

GLP10-01-01-11-041 

GLP10-01-01-11-042 

GLP10-01-01-11-043 

GLP10-01-01-11-044 

GLP10-01-01-11-045 

Average Cone 

Description 

DAL GW132L 0101103 

DALGW132LDB101103 

DALGW132LLS101103 

DALGW132LMS101103 

DAL GW132LHS 101103 

entration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

398 

410 

451 

482 

1290 

YoRecovery 

NA 

NA 

NC 

NC 

89.4 

404 ng/mL ±3.0Yo 

NA = Not Applicable 

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

Page 20 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 18. DAL GW 1SSR 101102 

3M LIMS ID 

GLP10-01-01-11-046 

GLP10-01-01-11-047 

GLP10-01-01-11-048 

GLP10-01-01-11-049 

GLP10-01-01-11-050 

Description 

DAL GW133R 0101102 

DAL GW133RDB 101102 

DALGW133RLS101102 

DALGW133RMS101102 

DALGW133RHS101102 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

107 

97,3 

102 

108 

193 

YoRecovery 

NA 

NA 

NC 

NC 

91.7 

102 ng/mL ±9.5Yo 

NA = Not Applicable 

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

Table 19. DALGW 1SSS 101103 

3M LIMS ID 

GLP10-01-01-11-051 

GLP10-01-01-11-052 

GLP10-01-01-11-053 

GLP10-01-01-11-054 

GLP10-01-01-11-055 

Description 

DAL GW133S 0101103 

DALGW133SDB101103 

DALGW133SLS101103 

DALGW133SMS101103 

DALGW133SHS101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

393 

377 

407 

485 

1260 

YoRecovery 

NA 

NA 

NC 

NC 

88.3 

385 ng/mL ±4.2Yo 

NA = Not Applicable 

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

Table 20. DALGW 1 SSL 101103 

3M LIMS ID 

GLP10-01-01-11-056 

GLP10-01-01-11-057 

GLP10-01-01-11-058 

GLP10-01-01-11-059 

GLP10-01-01-11-060 

Description 

DAL GW133L 0101103 

DALGW133LDB101103 

DALGW133LLS101103 

DAL GW133L MS 101103 

DALGW133LHS101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

253 

250 

265 

355 

1190 

252 ng/mL 

YoRecovery 

NA 

NA 

NC 

NC 

94.7 

± 7.2% 

NA = Not /Applicable 

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

Page 21 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 21. DAL GW 1S4R 101105 

3M LIMS ID 

GLP10-01-01-11-061 

GLP10-01-01-11-062 

GLP10-01-01-11-063 

GLPiaO1-01-11-064 

Description 

DAL GW134R 0101105 

DALGW134RDB101105 

DALGW134RLS101105 

DALGW134RHS101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

1640 

1490 

1620 

2250 

YoRecovery 

NA 

NA 

NC 

69.1 <^' 

1570 ng/mL ±9.6Yo 

NA = Not Applicable 

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

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

Table 22. DAL GW 1S4S 101105 

3M LIMS ID 

GLP10-01-01-11-065 

GLP10-01-01-11-066 

GLP10-01-01-11-067 

GLP10-01-01-11-068 

GLP10-01-01-11-069 

Description 

DAL GW134S 0101105 

DALGW134SDB101105 

DALGW134SLS101105 

DALGW134SMS101105 

DALGW134SHS101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

5.64 

5.34 

6.95 

16.6 

102 

YoRecovery 

NA 

NA 

NC 

112 

97.4 

5.49 ng/mL ±5.5Yo 

NA = Not /Applicable 

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

Table 23. DALGW 1S4L 101105 

3M LIMS ID 

GLP10-01-01-11-070 

GLP10-01-01-11-071 

GLP10-01-01-11-072 

GLP10-01-01-11-073 

GLP10-01-01-11-074 

Description 

DAL GW134L 0101105 

DALGW134LDB101105 

DALGW134LLS101105 

DALGW134LMS101105 

DALGW134LHS101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

523 

516 

530 

599 

1390 

YoRecovery 

NA 

NA 

NC 

NC 

87.8 

520 ng/mL ±1.3Yo 

NA = Not /Applicable 

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

Page 22 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 24. DAL GW 1 SSR 101105 

3M LIMS ID 

GLP10-01-01-11-075 

GLP10-01-01-11-076 

GLP10-01-01-11-077 

GLP10-01-01-11-078 

Description 

DAL GW135R 0101105 

DAL GW135RDB 101105 

DAL GW135RLS 101105 

DALGW135RHS101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

2930 

2890 

2930 

3840 

YoRecovery 

NA 

NA 

NC 

NC 

2910 ng/mL ±1.4Yo'^' 

NA = Not Applicable 

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

(1) Sampling location did not have an appropriate spike level to evaluate PFOA recovery. 

Table 25. DAL GW 1353 101105 

3M LIMS ID 

CJ) O •<- CN CO t^ 00 CO CO CO 2 2 2 2 2 

IIII I 

9 9 9 9 9 mil 

a. a. a. a. a. _i _i _i _i _i 

CD CD CD CD CD 

Description 

DAL GW135S 0101105 

DAL GW135SDB 101105 

DAL GW135SLS 101105 

DALGW 1358 MS 101105 

DALGW135SHS101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

13.9 

13.4 

14.5 

24.2 

110 

YoRecovery 

NA 

NA 

NC 

106 

97.2 

13.7 ng/mL ±3.7Yo 

NA = Not Applicable 

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

Table 26. DAL GW 1S5L 101105 

3M LIMS ID 

GLP10-01-01-11-084 

GLP10-01-01-11-085 

GLP10-01-01-11-086 

GLP10-01-01-11-087 

GLP10-01-01-11-088 

Description 

DAL GW135L 0101105 

DALGW135LDB101105 

DAL GW135LLS 101105 

DALGW135LMS101105 

DAL GW135LHS 101105 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

124 

121 

129 

226 

1070 

YoRecovery 

NA 

NA 

NC 

104 

95.6 

123 ng/mL ±2.4Yo 

NA = Not /Applicable 

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

Page 23 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 27. DAL GW 1S6S 101103 

3M LIMS ID 

GLP10-01-01-11-089 

GLP10-01-01-11-090 

GLP10-01-01-11-091 

GLP10-01-01-11-092 

GLP10-01-01-11-093 

Description 

DAL GW136S 0101103 

DALGW136SDB101103 

DALGW136SLS101103 

DALGW136SMS101103 

DALGW136SHS101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

73.9 

76.8 

77.6 

86.1 

166 

YoRecovery 

NA 

NA 

NC 

NC 

91.5 

75.4 ng/mL ± 3.8Yo 

NA = Not Applicable 

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

Table 28. DAL GW 1S6L 101103 

3M LIMS ID 

GLP10-01-01-11-094 

GLP10-01-01-11-095 

GLP10-01-01-11-096 

GLP10-01-01-11-097 

GLP10-01-01-11-098 

Description 

DAL GW136L 0101103 

DALGW136LDB101103 

DAL GW136LLS 101103 

DALGW136LMS101103 

DAL GW136LHS 101103 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

74.1 

76.4 

86.2 

169 

1030 

YoRecovery 

NA 

NA 

NC 

94.6 

96.3 

75.3 ng/mL ± 3.1Yo 

NA = Not Applicable 

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

Table 29. DAL GW 1S7S 101109 

3M LIMS ID 

GLP10-01-01-11-099 

GLP10-01-01-11-100 

GLP10-01-01-11-101 

GLP10-01-01-11-102 

GLP10-01-01-11-103 

Description 

DAL GW137S 0101109 

DAL GW137SDB 101109 

DALGW137SLS101109 

DAL GW137S MS 101109 

DAL GW137SHS 101109 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

0.273 

0.268 

0.350 

1.32 

10.9 

YoRecovery 

NA 

NA 

NC 

106 

107 

0.271 ng/mL ± I.8Y0 

NA = Not Applicable 

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

Page 24 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table SO. DAL GW 137L 101109 

3M LIMS ID 

GLP10-01-01-11-104 

GLP10-01-01-11-105 

GLP10-01-01-11-106 

GLP10-01-01-11-107 

GLP10-01-01-11-108 

Description 

DAL GW137L 0101109 

DALGW137LDB101109 

DALGW137LLS101109 

DALGW137LMS101109 

DALGW137LHS101109 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

0.360 

0.361 

0.458 

1.40 

10.7 

YoRecovery 

NA 

NA 

NC 

105 

104 

0.361 ng/mL ±0.28Yo 

NA = Not Applicable 

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

Table 31. DAL GW 1383 101110 

3M LIMS ID 

GLP10-01-01-11-109 

GLP10-01-01-11-110 

GLP10-01-01-11-111 

GLP10-01-01-11-112 

GLP10-01-01-11-113 

Description 

DAL GW138S 0101110 

DALGW138SDB 101110 

DALGW138SLS 101110 

DALGW138SMS101110 

DALGW138SHS101110 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

149 

144 

162 

230 

1020 

YoRecovery 

NA 

NA 

NC 

84.3 

88.1 

147 ng/mL ±3.4Yo 

NA = Not /Applicable 

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

Table S2. DAL GW 1 SSL 101110 

3M LIMS ID 

GLP10-01-01-11-114 

GLP10-01-01-11-115 

GLP10-01-01-11-116 

GLP10-01-01-11-117 

GLP10-01-01-11-118 

Description 

DAL GW138L 0101110 

DAL GW138LDB 101110 

DAL GW138LLS 101110 

DAL GW138L MS 101110 

DAL GW138LHS 101110 

Average Concentrati'on (ng/mL) ± %RPD 

PFOA 

Concentration 

(ng/mL) 

1.19 

1.12 

1.24 

2.18 

11.2 

YoRecovery 

NA 

NA 

NC 

103 

101 

1.16 ng/mL ±6.1Yo 

NA = Not Applicable 

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

Page 25 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table SS. DAL GW CW26R 101110 

3M LIMS ID 

GLP10-01-01-11-119 

GLP10-01-01-11-120 

GLP10-01-01-11-121 

GLP10-01-01-11-122 

GLP10-01-01-11-123 

Description 

DAL GWCW26R 0101110 

DAL GWCW26RDB 101110 

DAL GW CW26R LS 101110 

DAL GWCW26R MS 101110 

DAL GWCW26RHS 101110 

Average Concentrati'on (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

382 

389 

395 

450 

1290 

YoRecovery 

NA 

NA 

NC 

NC 

91.3 

386 ng/mL ± 1.8 Yo 

NA = Not /Applicable 

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

Table 34. DAL GW CW26L 101110 

3M LIMS ID 

GLP10-01-01-11-124 

GLP10-01-01-11-125 

GLP10-01-01-11-126 

GLP10-01-01-11-127 

GLP10-01-01-11-128 

Description 

DAL GWCW26L 0101110 

DAL GWCW26L DB 101110 

DAL GW CW26L LS 101110 

DAL GW CW26L MS 101110 

DAL GW CW26L HS 101110 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

565 

539 

552 

623 

1480 

YoRecovery 

NA 

NA 

NC 

NC 

93.6 

552 ng/mL ± 4.7 Yo 

NA = Not Applicable 

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

Table 35. DAL GW 140R 101104 

3M LIMS ID 

GLP10-01-01-11-129 

GLP10-01-01-11-130 

GLP10-01-01-11-131 

GLP10-01-01-11-132 

GLP10<31-01-11-133 

Description 

DAL GW140R 0101104 

DALGW140RDB101104 

DALGW140RLS101104 

DALGW140RMS101104 

DALGW140RHS101104 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

121 

120 

128 

217 

973 

YoRecovery 

NA 

NA 

NC 

97.4 

86.0 

121 ng/mL ± 0.83 Yo 

NA = Not /Applicable 

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

Page 26 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 36. DAL GW 141R 101110 

3M LIMS ID 

GLP10-01-01-11-134 

GLP10-01-01-11-135 

GLP10-01-01-11-136 

GLP10-01-01-11-137 

GLP10-01-01-11-138 

Description 

DAL GW141R0 101110 

DALGW 141 RDB 101110 

DALGW 141 RLS 101110 

DALGW 141 RMS 101110 

DALGW 141 RHS 101110 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

2.13 

1.55 

11.4 

95.5 

908 

YoRecovery 

NA 

NA 

96.5 

94.5 

91.4 

1.84 ng/mL ± 10 Yo 

NA = Not Applicable 

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

Table 37. DAL GW 142R 101110 

3M LIMS ID 

GLP10-01-01-11-139 

GLP10-01-01-11-140 

GLP10-01-01-11-141 

GLP10-01-01-11-142 

GLP10-01-01-11-143 

Description 

DAL GW142R0 101110 

DALGW142RDB101110 

DAL GW142RLS 101110 

DAL GW142R MS 101110 

DAL GW142RHS 101110 

Average Concentration (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

465 

48.7 

55.3 

143 

925 

YoRecovery 

NA 

NA 

NC 

96.3 

88.5 

47.6 ng/mL ± 4.6 Yo 

NA = Not /Applicable 

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

Table 38. DAL GW 144R 101110 

3M LIMS ID 

GLP10-01-01-11-144 

GLP10-01-01-11-145 

GLP10-01-01-11-146 

GLP10-01-01-11-147 

GLP10-01-01-11-148 

Description 

DAL GW144R 0101110 

DALGW144RDB101110 

DALGW144RLS101110 

DALGW144RMS101110 

DALGW144RHS101110 

Average Concentrati'on (ng/mL) ± YoRPD 

PFOA 

Concentration 

(ng/mL) 

57.2 

57.3 

67.6 

142 

966 

YoRecovery 

NA 

NA 

NC 

85.5 

91.7 

57.3 ng/mL ± 0.17 Yo 

NA = Not /Applicable 

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

Page 27 of 53 
Table 39. Trip Blank 1 

NA = Not Applicable 

Table 40. Trip Blank 2 

NA = Not Applicable 

Table41. Trip Blanks 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

3M LIMS ID 

GLP10-01-01-11-150 

GLP10-01-01-11-151 

GLP10-01-01-11-152 

GLP10-01-01-11-153 

GLP10-01-01-11-154 

Description 

TRIP BLANK 1 0 

TRIP BLANK 1 LS 

TRIP BLANK 1 MS 

TRIP BLANK 1 MHS 

TRIP BLANK 1 HS 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

1.08 

10.6 

99.1 

1040 

%Recovery 

NA 

109 

107 

100 

105 

3M LIMS ID 

GLP10-01-01-11-155 

GLP10-01-01-11-156 

GLP10-01-01-11-157 

GLP10-01-01-11-158 

GLP10-01-01-11-159 

Description 

TRIP BLANK 2 0 

TRIP BLANK 2 LS 

TRIP BLANK 2 MS 

TRIP BLANK 2 MHS 

TRIP BLANK 2 HS 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

1.08 

10.9 

96.9 

1020 

%Recovery 

NA 

109 

110 

97.8 

103 

3M LIMS ID 

GLP10-01-01-11-160 

GLP10-01-01-11-161 

GLP10-01-01-11-162 

GLP10-01-01-11-163 

GLP10-01-01-11-164 

Description 

TRIP BLANK 3 0 

TRIP BLANK 3 LS 

TRIP BLANK 3 MS 

TRIP BLANK 3 MHS 

TRIP BLANK 3 HS 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

1.07 

10.4 

101 

1050 

YoRecovery 

NA 

108 

105 

102 

106 

NA = Not Applicable 

Page 28 of 53 
Table 42. Trip Blank 4 

NA = Not Applicable 

Table 43. Rinseate Blanks 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

3M LIMS ID 

GLP10-01-01-11-165 

GLP10-01-01-11-166 

GLP10-01-01-11-167 

GLP10-01-01-11-168 

GLP10-01-01-11-169 

Description 

TRIP BLANK 4 0 

TRIP BLANK 4 LS 

TRIP BLANK 4 MS 

TRIP BLANK 4 MHS 

TRIP BLANK 4 HS 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

1.06 

10.4 

95.4 

985 

YoRecovery 

NA 

107 

105 

96.3 

99.4 

3M LIMS ID 

GLP10-01-01-11-016 

GLP10-01-01-11-149 

GLP10-01-01-12-009 

Description 

DALGW130LRB101105 

DAL GW144RRB 101110 

DAL SS 607R RB 0040 

PFOA 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

<0.0250 

YoRecovery 

NA 

NA 

NA 

NA = Not Applicable 

Page 29 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

10 Conclusion 

Laboratory cx)ntrol spikes and field matrix spikes were used to determine the analytic^al 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. 

12 Attachment s 

Attachment A: Protocol Amendment 11 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method - ETS-8-044.0 

Attachment D: Method Deviation 

Page 30 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

13 Signatures 

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

5^/6^;gf ^o/ / 

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

1. 

Date 

Gary Hohenstein, 3M Sponsor Representative 

OM/il 

2 m

_ 

Date 

2Ml 

Jaisimha Kesaffi, Study Director Jate 

Page 31 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Attachment A Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-01 

Amendment 11 

Study Title 

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

3M Decatur Pliase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 11 

Amendment Date: 

October 20, 2010 

Performing Laboratory 

SIVI Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

IVIaplewood, IVIN 55144-1000 

Laboratory Project Identification 

GLP10-01-01 

Sampling Event 

Former Sludge Incorporation Area (FSIA) Groundwater 

Page 1 of 7 

Page 32 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

AttachmentA 'Trf^Fy>tl^W P?S&!''b'tm'^8nr ^°'° 

Amendment 11 

This amendnnent 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 ofthe 3M Decatur Phase 3 Program for PFOA (GLP10-01-01). 

The anticipated sample collection will occur around the timeframe of October 25, 2010. The groundwater 

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

GLP10-01-01-11 and reported as interim report GLP10-01-01-11, (reflecting study GLP10-01-01 and 

amendment-11). 

Reason: 

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

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

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

Page 2 of 7 

Page 33 of 53 
Attachment A 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater '%%imi^r8i^csmm^sn^'''°'° 

Amendment 11 

Amendment Approval 

%i-. '10 

Gary Hohenstein, Sponsor Representative Date 

Cleston C. Lange, Principal Analytical Investigator Date 

? / OC/ i^o/ 0 

William Reagen, EHS Opns Environmental Lab Management 

Jaisimha Kesatf P.E., DEE, Study Director 

Date 

# 

Page 3 of 7 

Page 34 of 53 
Attachment A 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Amendment 11 

ovember2010 

wIVI Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

To: Gary Hohenstein, 3M EHS&Opns 

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

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

Cliffton Jacoby, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

Charles Young, Weston Solutions 

Tim Frinak, Weston Solutions 

Date October 20, 2010 : 

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

Decatur Phase 3 Site-Related Monitoring Program; GLP Interim Report 11 - Former Sludge 

Incorporation Area (FSIA) Groundwater 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project Schedule/Test Dates 

3M Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

aahohensteinSJmmm.com 

3M Environmental Laboratory Management 

William K. Reagen 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaaen@mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

cclanae(5)mmm.com 

Sampling Coordinator 

Timothy Frinak 

Weston Solutions 

Timothv.frinak(a)westonsolutions.com 

Phone: (334)-332-9123 

GLP10-01-01-11 

Dept #530711, Project #0022674449 

Sampling scheduled for the week of October 25, 2010 

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

Page 4 of 7 

Page 35 of 53 
Attachment A 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former.Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-01 

Amendment 11 

2 Background Information and Project Objective(s) 

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

samples collected from twenty-seven groundwater wells for Perfluorooctanoic Acid (PFOA) from the 

Former Sludge Incorporation Area (FSIA). Analyses will be conducted under the GLP requirements of 

EPA TSCA Good Laboratory Practice Standards 40 CFR 792. 

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

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

spikes to ensure that results for 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 GLP10-01-01-11. 

3 Project Schedule 

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

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

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

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

The targeted limit of quantitation will be 0.025 ng/mL (ppb) for PFOA. 

A total of thirty-four sampling locations have been specified. For each sampling location, a sample, sample 

duplicate and a minimum of two field matrix spikes will be collected. Table 1 indicates the well ID and 

con-esponding field spike levels. The "fill to here" line on each 250 mL Nalgene bottle will be 200 mL. Four sets 

of trip blanks consisting of reagent-grade water, a low-level trip blank spike, mid-level field spike, mid-high field 

spike, and a high-level trip blank spike will be prepared at the 3M Environmental Laboratory and sent to the 

sampling location with the other bottles. Two additional bottles will be prepared to be used for the preparation 

ofthe equipment rinseate blanks. A total of 189 sample bottles will be prepared. 

Table 1. Sampling Locations and Field Matrix Spil<e levels. 

Well No. 

136R,137R,137S,137L, 138L 

130L. 131L, 131S, 133R, 134S, 

135S.136S 

130R, 130S,132R,132L, 132S, 

133S, 133L, 134L, 135L, 136L, 

138S. 138R, CW26R, CW26L, 

140R, 141R, 142R, 143, and 144R 

131R, 134R, 135R 

TripBlankSet1,2, 3, and4 

Sample Level 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

Mid 

High 

Low 

High 

Low 

Mid 

Mid-High 

High 

Spike Cone. (ng/mL) 

0.1 

1.0 

10 

1 

10 

100 

10 

100 

1000 

100 

1000 

1 

10 

100 

1000 

Page 5 of 7 

Page 36 of 53 
GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

, „ . , . Former Sludge Incorporation Area-November 2010 

AttachmentA Analytical Protocol: GLP10-01-01 

Amendment 11 

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 Performance Liquid Chromatography/Mass Spectrometry Direct Injection 

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

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

in the report and the final accuracy statement may be adjusted accordingly. Based on the results from 

previously collected samples from the FSIA (GLP10-01-01-07), most sampling locations will require dilution with 

laboratory reagent water prior to sample analysis by ETS-8-044.0. 

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

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

Chromatography/Mass Spectrometry". 

6 Reporting Requirements 

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

spikes. Trip blank and trip blank spikes will be reported for the sampling event as will any equipment/rinseate 

blanks prepared in the field. Laboratory control spikes of reagent water prepared at the time of sample 

preparation will also be reported and used to evaluate the overall method accuracy and precision. Method 

blanks of reagent water prepared at the time of sample preparation will be used to determine the method 

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

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

final report. 

7 Email Correspondence 

Attachment A: Sampling Bottle Request 

Page 6 of 7 

Page 37 of 53 
Attachment A 

Attachment A 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Analytical Protocol: GLP10-01-01 

Amendment 11 

Bottle Request 

Decatur Groundwater Sampling 

On-site FSIA Wells 

0218L129.145.0004 

DATE REQUESTED: 18 October 2010 DATE REQUIRED: 25 October 2010 

This request addresses the bottle requirements for the following wells: 

130R 

130S 

130L 

131R 

131S 

131L 

132R 

132S 

132L 

133R 

133S 

133L 

134R 

134S 

134L 

135R 

135S 

135L 

136R 

136S 

136L 

137R 

137S 

137L 

138R 

138S 

138L 

CW26R 

CW26L 

140R 

141R 

142R 

143R 

144R 

Total Wells: 34 

Sample Summary 

No. of Samples Sample Type Comment 

34 

2 

4 

Groundwater 

Rinseate Sample 

Trip Blanks 

Will need HPLC water 

Anticipate 1 per cooler 

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

SHIPPING INFORMATION 

Please ship to the following address: 

Martin Smith \ Weston Field Office 

3M Decatur Plant 

1400 State Docks Road 

Decatur, AL 35601 

256-552-6189 

Page 7 of 7 

Page 38 of 53 
Buster J2930203 

Attachment B 

GLP10-01-01; Interim Report 11 

Former Sludge Incorporation Area - November 2010 

b110103a.rdb (PFOA): "Quadratic" Regression ("1 / x" weighting): y = -1.02e+004 x'^2 + 1.32e+006 x + 7.38e+003 (r = 0.9996) 

6.2e7 

6.0e7 

5.5e7 

5.0e7 

4.5e7 

4.0e7 

3.5e7 

" 3.0e7 

of 

< 

2.5e7-

2.0e7 

1.5e7-

1.0e7 

5.0e6 

0.0 / 

O 

o 

/ 

/ / 

/ 

0 5 10 15 20 25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 80 85 90 95 100 

Data worked up by STW 

Printing Time: 12:41:02 PM 

Printing Date: Tuesday, February 08, 2011 

Page 1 of 1 

Page 39 of 53 
"** Buster J2930203 

Attachment B 

GLP10-01-01; Interim Report 11 

Former Sludge Incorporation Area - November 2010 

I

Sampla Name: -b110103a021" Sample ID: -08008-194-8- File: -bllOIOSa.tMT 

Peak Name: 'PFOA' Mass(ee): '413.0/369.0 •rTHj,413.0/219.0 arT)u,413.CV169.0 amuComment *2.5 nghnL FC eld in Mill Q V\btBr* Anrwtation: 

Sample Type: Standard 

Cancsntration : 2.50 ny/mL 

Calculate d Cone: 2.65 nq/mL 

ftcq. Data : 1/3/2011 

Acq. Tin<e: 5:28:0?! PM 

Modified : 

BT Wind'jw: 

Expacta d RT: 

I'se Ralativ e 

Int . Type : 

Retentior . Ti 

Area : 

Height : 

?tar t Time : 

Er.d Tima : 

RT: 

H 2 

S 

Vas 

30. 0 

14 . e 

No 

Manual 

i^. e 

°B56 CO 

349*00 5 

U . 7 

15. 0 

mi 

cp 

mi 

mi 

m Sample Name:-b1101O3aO37- Sample ID:-LCS-1D123C>6' 

I Peak Name: 'PFOA' hAass(ea): "413.0/369.0 amu,413.(V219 

• Comment "Sppb LCS" Annotation: •" 

Sampl e Inde_l: 37 

Sampl e Type ; QC 

Concentration : 4.9 7 nq/mL 

Calcul:ste d Cone : 5.6 9 ng/mL 1.6e6 

Acq. Date : 1/3/201 1 

Acq. Time : 11:05:1' ' PM 

1.5e6 

File:-bllOl03a.wir 

D amu.413.(V169.0 amu* 

Modified : Ho 

Ptoc . Al^';rithrii : Int^lliQua n -

Ba^e. Sub. Window: 1.00 ra 

Peak-Split . Factor: 2 

Raport Larges t PaaK: No 

nul l 

Hln . Peak Width : 0.00 

Smoottiing Width : 0 

RT Window: 30.0 sac 

I'se Relativ e RT: No 

Int . Type: Valle y 

R.itei.tio n Tirr-e: 1J.& min 

Area : 7181731 coMnts 

Haiglit : l.eje.OO e cp3 

Star t Time: 1J.7 min 

ec 

poi n s 

^ 

f 

F 

1.4e6 

1.3e6 

1.1e6 

I.OeS 

9.0e5 

7.0*5 

6.0e5 

5.0e5 

4.0e5 

3.0e5 

2.0eS 

l.OeS 

16 18 

I SamplaName:-b110103a049' Sample ID;-LCS-10123D-13- FBe: tllDloaa.wifr 

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

• Comment 'Sppb LCS ECF* Anrwtation: *" 

Sampl e Index : 49 

Sampi e Type : OC 

Concentration : 4.&5 ng/» L 

Calculate d Core : 6.3 9 ng/mL 

Acq. DatB: 1/4/201 1 

Acq. Tima : 3:19:2 9 AH 

iu.413.0/169.0amif I

Sample Name:-b110103a069- Sampto ID: 'Solvent Blank (MilliQ Elemerrt)' File: -b110103a.wtfr 

Peak Name: "PFOA" Mass(ea): "413.0/369.0 amu,413.a/219.Damu,413.0/169.0 amu" 

Comment "MilE Q Wtater TNlO-0475" /^notation: " 

RT Windov : 

Expecte d RT: 

Use Relativ e RT: 

l;it . Tvp« : 

Retentio n Time : 

Area : 76? 

Heigtit : ! 

Star t Time : 

End Tim? : 

30. 0 

H . 8 

No 

Manual 

H . 8 

6783 c 

.626+00 5 

14. 5 

15. 0 

1.6e6 

1.5e6 

1.4e6 

1.3aE 

1.2e6 

1.1e6 

I.Oee 

9.0eS 

a.OeS 

7.0e5 

e.0e5 

5.0e5 

4.0e5 

3.De5 

ZOeS1.0e5-

14 

14.66.... 1 

79 

M. _4^- ^ 

sample Type: I'nkr 

i: H/A 

)nc: 0.00332 

ate : 

ime : 

e d : 

Algcrithm : 

Percentag e 

Sub . Windo 

1/4/201 1 

10:20:3 4 

No 

IntalliQ' j 

: 90 

u : 1.00 

Smoothing Wid 

Expected RT: 

5.2e4 

5.0e4 

4.ae4 

4.6e4' 

4.4e4 

4.2e4 

4.0e4 

3.8o4 

3.6e4 

3.4«4 

3.2e4 

3.0«4 

2.8e4 

Z6e 4 

2.4e4 

2.2e4 

2.0e4 

1.4e4 

1.2e4 

1.0e4 

8000.0 

6000.0-

4000.0 

2000.0-

0.0 nwllli MK^ff***^"'' 

10 12 14 18 18 

Timg. min 

Data worked up by STW 

Printing Time: 12:43:02 PM 

Printing Date: Tuesday, February 08, 2011 

Page 1 of 2 

Page 40 of 53 
*** Buster J2930203 

Attactiment B 

GLP10-01-01; Interim Report 11 

Ba t AP^?i l :°f ffi9fbi?a9SJ'i"«*'"a'er 

Former Sludge Incorporation Area - November 2010 

Data worked up by STW 

Printing Time: 12:43:02 PM 

Printing Date: Tuesday, February 08, 2011 

Page 2 of 2 

Page 41 of 53 
Document may beGLF*'o-oi-ui mter.mfieFw-114 days from 02/08/20" 

Analysis of PFOA in Groundwater 

Attactiment 0 Fomier Sludge Incorporation Area - November 2010 

3M Environmenfal LaixxrafDiy 

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 i^^f^^^ j 

Approved By: 

^yyjyo •> 

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 42 of 53 
Document may beGUBtoM,i-:6i;:irit€-nrnHefKv-ri14 days from 02/08/20' 

Analysis of PFOA in Groundwater 

Attactiment C Former Sludge Incorporation Area - November 2010 

1 Scope and Application 

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

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

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

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

and 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 IVIethod Summar y 

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

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

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

This is a perfonnance-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 detennined 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 detemnine the statement of 

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

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

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

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

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

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

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

a measure ofthe 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 ofthe FB is to determine if test substances or 

other interferences 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 43 of 53 
Document may bewh'!0^o^^^cimmr!\ke^m•^i4 days from 02/08/2011 

Analysis of PFOA in Groundwater 

Attachment C Former Sludge Incorporation Area - November 2010 

3.4 Field Duplicate Sample (FDS, Field Dup) 

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

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

procedures. Analysis ofthe FDS compared to that ofthe first sample gives a measure ofthe 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 ofthe 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 ofthe 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 ofthe 

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

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

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

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

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

3.7 Laboratory Control Sample (LCS) 

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

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

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

exactly like a laboratory sample to 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 detennined in a separate aliquot and the measured values in the LMS con^ected 

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

3.9 Laboratory Sample 

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

3.10 Limit of Quantitation (LOQ) 

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

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

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

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

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

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

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

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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 materiail intended to represent the original source 

material. 

3.13 Stock Standard Solution (SSS) 

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

compound. 

3.14 Surrogate 

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

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

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

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

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

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

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

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

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

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 ofthe 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 infonnation 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). 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, 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 Chromatographi c System 

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

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

Temperature: 10°C 

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

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mUmin) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 pL. 

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

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: Electrospnay Negative ion, MRM mode, monitoring the following transitions: 

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263-> 219 

313-> 269 and 313 ^119 

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

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

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

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

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

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

299 ^ 80 and 299 -» 99 

399 -> 80 and 399 -> 99 

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

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

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

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

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

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

7 Reagents and Standards 

7.1 Chemicals 

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

Methanol - HPLC grade 

Ammonium Acetate - A.C.S. Reagent Grade 

7.2 Standards 

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

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

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

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

Products, Inc 

Perfluorooctanoic Acid (PFOA - 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 

Periluorododecanoic Acid (PFDoA-CI2 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 ofthe solvent to solute ratios are maintained. 

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

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

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

when diluting stock solutions to appropriate levels. 

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

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

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

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

procedure. An example of purity and salt con-ection is given below for PFOS. 

,. X- r 1 molecular weight of anion 

salt correction factor = 

moclecular weight of salt 

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

538 

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

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

flask and bring up to volume with solvent. 

250 ng/mL mixed working standard—Add 1.25mL ofthe 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 ofthe 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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rom 02/08/2011 

7.5 Calibration Standards 

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

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

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

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS./d. 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in ASTIVI Type 1 Water, 

or other suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

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

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

sample aliquot, or filtered. 

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

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

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

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

Prepare at least five method blanks. 

9 Sample Analysi s - LC/MS/MS 

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

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

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

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

thoroughly documented in the raw data. 

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

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

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

The coefficient of detemnination {f) value for the calibration curve must be greater than or equal to 0.990. Each 

point in the curve must be within ±25% ofthe theoretical concentration with the exception ofthe 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, perform routine maintenance or prepare a new standard 

curve (if necessary) and reanalyze. 

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

mid-range calibration standard, one ofthe 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 ofthe analytical mn. 

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

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

the mean area counts ofthe method blanks exceed 50% ofthe 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 ofthe 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% ofthe 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 Analysi s 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. 

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

Analyte added (ng/mL) 

12 Method Performance 

Any method perfonnance parameters that are not achieved must be considered in the evaluation ofthe data. 

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

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

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

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

discussed in the text ofthe report. 

12.1 System Suitability 

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

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

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

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

have area counts with an RSD of S5% and a retention time RSD of S2% to be compliant. 

12.2 Quantitation 

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

equal to 0.990. Each point in the curve must be within ±25% ofthe 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 ofthe calibration curve. The accuracy of 

each curve point must be within 25% ofthe 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 evaluafion of appropriate blanks and the accuracy ofthe low-level calibration curve points. Refer 

to Section 10 for addifional details. 

12.4 Accurac y 

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

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

spikes and laboratory matrix spikes. 

12.5 Precision 

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

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

requirement for replicates excludes field blanks or rinse blanks. 

Section 10 contains additional 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 reconstnjction ofthe 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 (instalment batch records, instalment acquisition 

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

15 Affected Document s 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

ETS-8-044.0 Page 11 of 11 

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

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GLP10-01-01; Interim Report 11 

3M Confidential Analysis of PFOA in Groundwater 

Attachment D __. __ .. . Former Sludge Incorporation Area-November 2010 

RECORD OF DEVIATION/NONCONFORMANCE 

/, Identification 

Study / Project No. Date(s) of Occurrence: Document Number: 

GLP10-01-01-11 1-3-11 ETS-8-044.0 

Deviation type 0 SOP D Equipment Procedure D Method 

(Check one) D Protocol O GPO D Other: 

//. Description (attach extra pages as needed) 

Method Requirements: 

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

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

Actual procedure/process: 

1. The average PFOA recovery for the 5 ppb ECF LCS was 123%. 

2. The high FMS recovery for sample DAL GW 134R was 69.1%. 

///. Actions Taken 

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

Corrective Action (D Yes 0 No) Reference: 

Acceptability of tfie nonconforming work: 

1. Low, mid, and high sets of linear, and linear + branched (ECF) LCS samples were prepared and analyzed 

with the samples. All sets met rriethod acceptance criteria with the exception of the mid level ECF LCS. 

The linear + branched PFOA LCS, when quantitated against calibration curve point prepared from linear 

PFOA, have been quantitating around 5-15% higher. The recovery for the 5 ppb ECF LCS (123%) will be 

flagged in the final report. All LCS were used in the determination of method analytical uncertainty. 

2, The FMS recovery for the sample outside the acceptance criteria will be flagged in the final report. The 

method uncertainty for PFOA will be adjusted according. 

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

0 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: /} ^^ Date:, , 

^l^/ l '^0 Study Director (if GLP): M Vj.J>^^'{K/vC>^ Date?-

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

Technical Reviewer (optional): NA Date: NA 

Laboratory Department Manager Approval: Date: 

IV. Authorization to Resume Work 

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

Laboratory Department Manager Approval; -. Date: A. 

Deviation No. 

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

Attachment A ETS-4-008.7 • Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing Page 53 of 53