3 

GLP10-01-01 Interim Report 21: Analysis for PFOA in Decatur, AL Soils 

Collected from Well Location 610 in August, 2011

Study Title

3M Environmental Laboratory Analytical Protocol GLP10-01-01: 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 

West Chester, PA 19380 

Phone: 610-701-3761 

Principal Analytical Investigator

Cleston C. Lange, Ph.D. 

3M Environmental Laboratory 

Interim Report Completion Date 

Upon Signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

St. Paul, MN 55144 

Project Identification

GLP10-01-01-21 

Total Number of Pages 

19
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 2 of 19

This page has been reserved for specific country requirements. 
study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610 

jGLP COMPLIANCE ST^|EMENT 

Report Title: GLP10-01-01 Interim Report 21: Analysis for PFOA in Decatur, AL Soils Collected 

from Well Location 610 in August 2011. 3M Environmental Laboratory Analytical Protocol GLP10-

01-01: 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: 

Exceptions to GLP compliance: 

• Test, control and reference substances were not all characterized under GLPs. 

• Samples environmental samples, there was no dosing and no specific test substance for this 

study. 

Gary Hohenstein, Sponsor Representative Date 

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

Page 3 of 19 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610 

iQuALiTY ASSURANCE STATEMENT 

Report Title: GLP10-01-01 Interim Report 21: Analysis for PFOA in Decatur, AL Soils Collected 

from Well Location 610 in August 2011. 3M Environmental Laboratory Analytical Protocol 

GLP10-01-01: Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for 

the 3M Decatur Phase 3 Site-Related Monitoring Program. 

This interim study 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. 

study Inspection 

Dates 

Phase 

Date Reported to 

study Inspection 

Dates 

Phase P.I. Study Director 

•Management 

Study Director 

Nov. 14-15,2011 Interim Report 

and Data 

11/25/2011 1/13/2012 1/13/2012 

A A. f-'/ ^ 

QAU Representative Date 

Page 4 of 19 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 5 of 19

TABLE OF CONTENTS

GLP Compliance Statement ...................................................................................................................... 3

Quality Assurance Statement .................................................................................................................... 4

Table of Contents ....................................................................................................................................... 5

List of Tables ............................................................................................................................................... 6

1 Study Information ................................................................................................................................ 7

2 Summary ............................................................................................................................................. 8

3 Introduction .......................................................................................................................................... 9

4 Test, Control and Reference Substances .......................................................................................... 9

5 Test System ....................................................................................................................................... 10

6 Method Summary .............................................................................................................................. 10

6.1 Methods ................................................................................................................................ 10

6.2 Sample Receipt .................................................................................................................... 10

6.3 Sample Preparation .............................................................................................................. 10

6.4 Percent Soil Moisture Determination ................................................................................... 11

6.5 LC/MS/MS Analysis .............................................................................................................. 11

7 Analytical Results .............................................................................................................................. 13

7.1 Calibration ............................................................................................................................. 13

7.2 Limits of Quantitation (LOQs) .............................................................................................. 14

7.3 Continuing Calibration .......................................................................................................... 14

7.4 Blanks .................................................................................................................................... 14

7.5 Laboratory Control Spikes (LCSs) ....................................................................................... 14

7.6 Laboratory Matrix Spikes (LMSs) ........................................................................................ 15

7.7 Percent Moisture Determinations ........................................................................................ 16

7.8 Individual Sample Results .................................................................................................... 16
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 6 of 19

8 Conclusion ......................................................................................................................................... 17

9 Data/Sample Retention ..................................................................................................................... 17

10 List of Attachments ............................................................................................................................ 17

11 Signatures .......................................................................................................................................... 18

LIST OF TABLES

Table 1. PFOA Results for Decatur, AL Soils from Well Location 610, August 2011 ........................... 8

Table 2. LMS Recovery for Decatur, AL Soils from Well Location 610, August 2011 ........................... 8

Table 3. Control and Reference Substances ........................................................................................... 9

Table 4. Instrument Information .............................................................................................................. 12

Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053)..................................................... 12

Table 6. Mass Transitions ....................................................................................................................... 12

Table 7. PFOA Calibration Summary (Calibrated with linear PFOA) ................................................... 13

Table 8. LCS Results .............................................................................................................................. 15

Table 10. Percent Moistures for Decatur, AL Soils from Well Location 610, August 2011 ................. 16

Table 11. Individual PFOA Results for Decatur, AL Soils from Well Location 610, August 2011 ....... 16
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 7 of 19

1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary A. Hohenstein 

Environmental Manager 

Special Projects, EHS Operations 

Bldg 224-5W-03 

St. Paul, MN 55144 

Phone: (651) 737-3570 

gahohenstein@mmm.com

Study Director

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

West Chester, PA 19380 

Study Analytical Testing Facility 

3M EHS Operations 

Environmental Laboratory 

Building 260-5N-17 

St. Paul, MN 55144 

Study Personnel (3M Environmental Laboratory) 

Cleston C. Lange, Ph.D., Principal Analytical Investigator 

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

Patrick Kenney, Laboratory Technician (Pace Analytical, Professional Services) 

Marlene Heying, Laboratory Technician (Pace Analytical, Professional Services) 

Study Dates 

Study Initiation: March 08, 2010 

Interim Analytical Initiation: September 12, 2011 

Interim Analytical Completion: October 19, 2011 

Interim Report Completion: Upon final Signatures 

Location of Archives 

All original raw data and analytical reports 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 79
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 8 of 19

2 Summary 

This interim report provides the PFOA concentration results for the four soils collected in August 2011 at 

well location 610 near the 3M facility at Decatur, AL. One travel blank (trip blank), containing 

approximately 16 grams of control soil in a sample bottle, accompanied the sample bottles to and from the 

site and was also analyzed. Samples were logged into the laboratory information management system 

(LIMS) under project GLP10-01-01-21. Four aliquots of each soil were removed from each sample bottle 

and accurately weighed. The third and fourth replicates of each sample were fortified with nominal 5.00 

and 50.0 ng of PFOA as a low and high laboratory matrix spiked (LMS), respectively. A single LMS for the 

trip blank was fortified with nominal 1.00 ng of PFOA. Sample were extracted and analyzed per method 

ETS-8-053 which employs analysis by liquid chromatography with triple quadrapole mass spectrometric 

detection (LC/MS/MS). The LMS results provided a measure of PFOA recovery from individual samples. 

The relative percent difference (RPD) of the duplicate sample results was used to assess the analytical 

precision of the sample results. The percent moisture of each soil was also determined as part of the

study. The PFOA concentrations and RPDs are summarized in Table 1. The PFOA fortification levels 

and recoveries of PFOA from the LMS samples are summarized in Table 2. 

Table 1. PFOA Results for Decatur, AL Soils from Well Location 610 

3M LIMS ID Sample ID Avg. PFOA Concentration 

(ng/g; dry weight) 

Relative Percent 

Difference 

GLP10-01-01-21-001 DAL-SB-610S-0-0000 4.57 10% 

GLP10-01-01-21-002 DAL-SB-610S-0-0010 10.3 7.0% 

GLP10-01-01-21-003 DAL-SB-610S-0-0040 6.21 2.9% 

GLP10-01-01-21-004 DAL-SB-610S-0-0150 BLQ N/A 

GLP10-01-01-21-005 TRIP BLANK-1 BLQ N/A 

BLQ; The integrated peak area response for PFOA in the sample was below the PFOA peak area response for the lowest 

standard that was used to construct the calibration curve (< nominal 0.200 ng/g). 

Data Accuracy determined from LMS results was within 100+ 29%, and RPD (precision) determined for analytical duplicates 

was <15%. 

N/A; not applicable 

The analytical method uncertainty determined from LCSs was + 13%; determined at the 95% CI. 

Table 2. LMS Recovery for Decatur, AL Soils from Well Location 610 

3M LIMS ID Sample ID 

PFOA Spike 

Concentration 

(ng/g; dry 

weight) 

PFOA Recovery 

(Data Accuracy) 

GLP10-01-01-21-001 Low DAL-SB-610S-0-0000 Lab Matrix Spike Low 6.07 103% 

GLP10-01-01-21-001 High DAL-SB-610S-0-0000 Lab Matrix Spike High 58.9 102% 

GLP10-01-01-21-002 Low DAL-SB-610S-0-0010 Lab Matrix Spike Low 5.60 98.7% 

GLP10-01-01-21-002 High DAL-SB-610S-0-0010 Lab Matrix Spike High 57.2 112% 

GLP10-01-01-21-003 Low DAL-SB-610S-0-0040 Lab Matrix Spike Low 5.05 129% 

GLP10-01-01-21-003 High DAL-SB-610S-0-0040 Lab Matrix Spike High 52.4 111% 

GLP10-01-01-21-004 Low DAL-SB-610S-0-0150 Lab Matrix Spike Low 4.90 94.8% [a] 

GLP10-01-01-21-004 High DAL-SB-610S-0-0150 Lab Matrix Spike High 49.5 114% [a] 

GLP10-01-01-21-005 LMS Trip Blank-1 Lab Matrix Spike Low 1.01 102% [a] 

[a] Samples with an endogenous PFOA level of BLQ were treated as a concentration of zero to calculate recovery. 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 9 of 19

3 Introduction 

The soil analyses reported herein were conducted as part of the Phase 3 Environmental Monitoring 

and Assessment Program for the 3M facility located in Decatur, Alabama. The objective of the 

overall program is to gain information regarding concentrations of perfluorooctanoate (PFOA) in 

various environmental media such as groundwater, soils and sediments that are associated with and 

near the Decatur facility. Reported herein are the results from analysis of soils from near well 

location 610, located near the 3M facility in Decatur, AL. The samples were collected by Weston 

Solutions, Inc. personnel in August 2011 and shipped to the 3M Environmental Laboratory for 

quantitative analysis of PFOA. One soil travel blank (trip blank) was also analyzed. 

This report describes the sample shipment, receipt, extraction and quantitative LC/MS/MS analysis 

procedures conducted for determination of PFOA in the soils for project GLP10-01-01-21. 

Additionally, included in this report are the assessment of the analytical precision and accuracy for 

the reported PFOA concentration results, the recovery results for a stable isotope labeled surrogate 

(

13C4-PFOA) that was added to each soil aliquot prior to extraction, and the determined percent 

moisture content of each soil. 

4 Test, Control and Reference Substances 

This study does not have a test substance in the classic sense of a GLP study because this study 

was purely analytical in nature. The reference and control substances are listed in Table 3. 

Table 3. Control and Reference Substances 

Test 

Substance 

PFOA (linear 

isomer), free acid 

Technical PFOA 

(linear + branched 

isomers), 

ammonium salt 

13C4-PFOA 13C8-PFOA 

Use Calibration & LMSs LCSs Surrogate Internal Standard 

Source Oakwood 3M Wellington Labs Wellington Labs 

Expiration Date 9/29/2012 2/27/2017 10/22/2012 10/22/2012 

Storage 

Conditions Frozen Frozen Frozen Frozen 

Chemical Lot 3440 332 MPFOA1009 M8PFOA0408 

TCR Number TCR07-0041 1/1 TCR-123 TCR09-0075 2/9 TCR09-0067 5/9 

Physical 

Description Powder White Powder Methanol Solution [a]

Methanol Solution 

[a]

Purity 99.5% 95% >98% 97.9% 

[a] Stable isotope labeled materials are typically provided as methanolic solutions by the vendor (source) and are 

treated as 100% pure; the vendor’s reported methanol stock concentration is used for calculating concentrations of 

diluted standards made from them. 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 10 of 19

5 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 off-site soils collected near well location 610, near the 3M facility in 

Decatur, AL. Samples for this study are “real world” environmental samples. 

6 Method Summary 

6.1 Methods 

Soil extractions and quantitative LC/MS/MS analysis were performed following validated method 

ETS-8-053.0. The analysis conducted for reporting results was performed on October 5, 2011 as 

analytical run s111005a. 

6.2 Sample Receipt 

On August 23, 2011 four (4) empty 250-mL HDPE NalgeneTM sample bottles, and one travel 

blank (trip blank) containing approximately 16 grams of a control soil TCR-842, were sent from the 

3M Environmental Laboratory to Weston Solutions, Inc. field personnel for collection of soils from 

well location 610. Following the soil sample collections by Weston Solutions, Inc. personnel, 4 

soil-filled sample bottles and the trip blank were sent to the laboratory for analysis. The samples 

were received with sample chains of custody numbers 16926 on September 12, 2011. A 

discrepancy between the date of bottle order sent to Decatur (8/23/2011) and the listed date of 

collection of the soils (8/19/2011) indicated samples were collected prior to receiving the bottles 

and trip blank. Charles Young of Weston, Inc. who oversaw the soil collections at Decatur was 

notified and indicated that the trip blank likely did not accompany the samples during collection in 

Decatur since other bottles apparently were used than those sent on 8/23/2011. However, the trip 

blank did accompany the samples when shipped back to 3M. A protocol deviation regarding this 

was written and is maintained in the study folder for project GLP10-01-01-21. Any impact on the 

study sample results for the soils collected under GLP10-01-01-21 was regarded as minimal. 

Soil samples from Decatur, AL are regulated and were appropriately shipped in accordance with 

USDA/APHIS soil permit number P330-09-00125. 

Sample nomenclature follows the form DAL-SB-610x-xx-xxxx where the first string defines the Decatur 

Alabama (DAL) project area, the second string defines the sample media (i.e., SB= soil boring), the third 

string defines the specific well identity (well 610). The fourth string defines the sample type (0 = primary 

sample, DB = field duplicate, RB = equipment rinseate blank). The fifth string indicates the sampling

depth range (0040 indicates 4.0 ft to 4.5 ft interval soil sample). 

6.3 Sample Preparation 

Sample preparation was conducted as a single batch on October 4-5, 2011. 

Each soil extraction involved removal of a 1 cubic centimeter (1 cc; 1 mL) soil aliquot (typically ~ 1 gram) 

from each sample bottle using a fixed volume 1 cc spoon, transferring it to a 15 mL conical centrifuge

tube, followed by accurate weight determination of the aliquot on a 5-place balance. Then, nominal 3.0 

ng of internal standard (IS; nominal 3.0 ng) was added to each soil aliquot. Then the soil aliquot was 

extracted by addition of 8 mL of a 4:1 acetonitrile:water solution followed by sonication for 1 to 2 hours 

and then centrifugation to remove solids. The supernatant from each was then transferred to an autovial 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 11 of 19

for analysis. An accurately measured volume of each supernatant was analyzed by LC/MS/MS. 

For a few samples, the 1cc aliquot resulted in only ~0.65 gram of soil, therefore, extra soil was used in 

those extractions in order to be closer to 1 gram of sample. In those few instances the inclusion of extra 

sample ensured adequate sensitivity for target analytes was achieved for the final extract. 

During preparation, each sample received nominal 3.0 ng of a stable isotope labeled surrogate recovery

standard (SRS) as 13C4-PFOA. Although not included as part of the data accuracy assessment for this 

study, SRS recovery determinations were included as part of an ongoing method validation aspect for 

SRS behavior in environmental soil samples for potential future applications. The SRS was quantified 

from a SRS calibration curve constructed from analysis of calibration standards prepared from the SRS 

in calibration standards. The SRS recovery was determined based on the calculated concentration of 

SRS from the analysis and recovery of SRS from each sample is included in Table 10, but was not used 

for evaluation of data accuracy for this study and is otherwise excluded from the discussions in the 

report. 

Each analytical sample was prepared in duplicate for analysis of PFOA in the soil sample. Additionally, 

a third and fourth replicate was weighed out and used to prepare a low- LMS and high-LMS, fortified 

with nominal 5.0 ng and 50.0 ng of PFOA (linear isomer), respectively. LMS results were used for 

determination of data accuracy. RPD of duplicate samples results was used for determination of data 

precision. 

Calibration standards were prepared by spiking known quantities of PFOA (linear isomer) into 1-cubic 

centimeter (1 cc, 1 mL) aliquots of 3M Environmental Laboratory control soil TCR-842. The nominal 

mass of 1 cc of control soil TCR-842 is 1.0 gram (dry). The nominal calibration standard range prepared 

and analyzed was 0.200 ng/g to 500 ng/g. 

Laboratory control spike (LCS) samples were prepared with each sample preparation batch; prepared at 

three levels (nominal 3.00 ng/g, 30.0 ng/g and 300 ng/g) and each level in triplicate. The LCSs were 

prepared using control soil TCR-842, same as calibration standards, and were fortified with technical 

PFOA (linear + branched isomer). The LCS results were used to estimate the analytical method 

uncertainty. 

6.4 Percent Soil Moisture Determination 

The percent moisture of soils was used to calculate the dry weight of the wet soils weighed during 

sample preparations for PFOA analysis, and was determined by gravimetric analysis. Dry weights were 

determined for separate weighings than the weighings used for PFOA extraction and analysis 

procedures. To determine the percent moisture, duplicate aliquots of each soil sample were removed 

and the accurate “wet” weight determined for each. All aliquots were dried at > 100°C until no further 

mass loss occurred from water evaporation, at which time the accurate dried weights were determined. 

The difference in mass, attributed to water evaporation, was used to calculate the percent moisture of

the original soil. The averaged percent moisture result for each was then used to calculate the soil 

PFOA concentration on a dry weight basis, and is reported for each soil in Table 9. 

6.5 LC/MS/MS Analysis 

The LC/MS/MS analysis was performed on October 5, 2011 as analytical run S111005a and was 

performed by as described in method ETS-8-053.0 

The relative percent difference (RPD) of the duplicate sample results was used as a measure of 

the analytical precision. The determined recovery of fortified PFOA from the LMS samples was 

used as a measure of sample-specific analytical accuracy. Recovery of the surrogate (13C4-PFOA) 

is included within this report in Table 10 as an indirect measure of analytical data accuracy, and is 

not considered in the accuracy assessment for this study and is only included as part of an ongoing method validation aspect in which surrogate recovery behavior is being evaluated in “real 

world” environmental samples for possible future applications. 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 12 of 19

Details of the specific instrument parameters, the liquid chromatography gradient program, and the 

specific mass transitions analyzed are detailed in the raw data, and are briefly described below in 

Table 4, Table 5 and Table 6. 

Table 4. Instrument Information 

Instrument Name ETS-Stan 

Analytical Method ID ETS-8-053.0 

Liquid Chromatograph Agilent 1100 with Binary Pump 

Guard column Pre-Autosampler; Prism RP (2.1 x 50 mm, 5 μ) 

Extraction column Oasis HLB (3 x 20 mm, 25 μ); 30°C 

Analytical column Betasil C18 (2.1 x 100 mm, 5μ) 

Injection Volume 25 μL 

Mass Spectrometer API 4000 

Ion Source TurboIon Spray 

Polarity Negative 

Software Analyst 1.4.2 

Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053) 

Step 

Number 

Total Time 

[min] 

Flow Rate 

[mL/min] 

Percent A 

[2 mm Aqueous 

Ammonium Acetate] 

Percent B 

[ Acetonitrile] 

1 0.0 0.400 97.0 3.0 

2 3.0 0.400 97.0 3.0 

3 3.5 0.400 70.0 30.0 

4 17.0 0.400 40.0 60.0 

5 17.5 0.400 10.0 90.0 

6 19.5 0.400 10.0 90.0 

7 20.0 0.400 97.0 3.0 

8 23.0 0.400 97.0 3.0 

Table 6. Mass Transitions 

Analyte Mass Transitions Monitored 

PFOA 413>169, 413>219, 413>369 

13C4-PFOA (Surrogate) 417>169, 417>219, 417>372 

13C8-PFOA (IS) 421>172, 421>223, 421>376 

Note: Multiple mass transitions are summed to give the instrument response for that 

analyte. 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 13 of 19

7 Analytical Results 

All results are rounded to three significant figures according to EPA rounding rules. Because of 

rounding, values may vary slightly from those found in the raw data. All results were calculated from

accurate values in the raw data. Laboratory matrix spikes (LMS) meeting the method acceptance 

criteria of 100 ± 30%, demonstrate that the method was appropriate. The 5.00 ng spiked 

concentrations for the low LMS were the most adequate with respect to the endogenous PFOA 

measured in the samples.

7.1 Calibration 

Calibration standards were prepared by spiking varying known quantities of PFOA (linear isomer) and 

surrogate, and a fixed quantity of internal standard, into separate 1-cubic centimeter (1 cc, 1 mL) 

aliquots of 3M Environmental Laboratory matrix soil TCR-842 (nominal 1.0 gram per mL). A total of 

eleven (11) soil matrix calibration standards ranging from nominal PFOA concentration 0.200 ng/g to 200 

ng/g were prepared for the definitive analysis. Following the analysis of calibration standards, the 

nominal concentration of each standard was plotted versus the measured analyte peak area/IS peak 

area response ratio. A quadratic equation with 1/x weighting was used to fit the calibration response

data. Calibration curves were not forced through zero. Calculating the determined standard 

concentration using the resultant calibration curve and comparing to the known concentration confirmed

accuracy of each curve point within 100 ± 30% (+ 35% at the LLOQ). The correlation coefficient (r) was 

greater than 0.999, and coefficient of determination (r2

) was greater than 0.990. Calibration results for 

PFOA are summarized in Table 7. 

Because soil weights vary significantly for a 1 cc (1 mL) soil sample, depending on soil type and moisture 

content, the instrument response was calibrated for the known concentrations of PFOA based on the 

mass quantity of PFOA added to each 1 cc soil calibration standard prior to extraction (e.g. calibrated in 

this study for a range of 0.200 ng/g to 200 ng/g PFOA). Because a 1cc aliquot of control soil TCR-842

weighs approximately 1.0 gram (dry weight) and has less than 5% moisture content, the nominal 

concentration range of the calibration was essentially 0.200 ng/g to 200 ng/g. However, because the 

sample soils vary in moisture content and soil composition and density, 1 cc aliquots of field soil samples 

typically weigh more than 1.0 gram. Therefore, the final measured results from the analysis were 

adjusted for the accurate determined dry weight of the 1 cc sample aliquot that was extracted. 

Table 7. PFOA Calibration Summary (Calibrated with linear PFOA)

Analytical 

Run 

PFOA (ng) [a]

r STD 

1 

STD 

2 

STD 

3 

STD 

4 

STD 

5 

STD 

6 

STD 

7 

STD 

8 

STD 

9 

STD 

10 

STD 

11 

STD 

12 

Actual Conc. 0.200 0.500 0.749 0.999 2.50 5.00 9.99 25.0 50.0 99.9 200 500 N/A 

S111005a 0.185 0.505 0.722 1.01 2.52 5.08 10.5 25.7 50.8 96.2 202 500 0.9999 

Recovery (%) 92.5 101 96.3 101 101 102 105 103 102 96.2 101 100 N/A 

N/A; not applicable 

[a] PFOA concentrations are nominal ng/g (dry wt.) and based on a nominal mass of1.0 gram (dry wt.) for each 1 cubic centimeter (1 mL) of 

control soil used to prepare each calibration standard. 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 14 of 19

7.2 Limits of Quantitation (LOQs) 

The lower limit of quantitation (LLOQ) was the lowest non-zero calibration standard in the curve that met 

linearity and accuracy requirements (100 + 35%) and for which the area counts were at least 2X that of 

the average response determined from the method blanks. The LLOQ for this study was nominal 

concentration 0.200 ng/g, and was the lowest prepared calibration standard. All sample analyte 

responses less than the response of the 0.200 ng/g calibration standard were reported as BLQ (below 

the limits of quantitation). The upper limit of quantitation (ULOQ) was nominal concentration 200 ng/g. 

7.3 Continuing Calibration 

During the course of each analysis, continuing calibration verifications (CCVs) was performed by regular 

injection of a mid-level calibration standard after approximately every 15 samples in the analytical run. 

The back calculated concentration results were used to confirm that the instrument response and the 

initial calibration curve were still in control. All CCVs flanking reported data met the method criteria of 

100% ± 30% accuracy. 

7.4 Blanks 

Three types of blanks were analyzed during this analysis: method blanks were prepared with blank 

matrix soil TCR-842 and were spiked with IS and surrogate; travel blanks (trip blanks) prepared from 

aliquots of soil TCR-842 contained in sealed bottles that accompanied the bottle order to Decatur, and

sample shipment back to 3M Environmental Laboratory; and solvent blanks containing extraction 

solvent. The different blanks results were reviewed to evaluate potential contamination during shipment 

and sampling, to evaluate method performance parameters such as injector carry over and also to 

establish the LLOQ and the performance of the blanks were considered in the reporting of all results. 

7.5 Laboratory Control Spikes (LCSs) 

Laboratory control spikes were prepared by spiking known quantities of PFOA (linear + branched 

isomers) into 1 cc aliquots of soil TCR-842, fortified with nominal 3.0 ng, 30 ng and 300 ng PFOA (linear 

+ branched isomer). The linear + branched isomer quantitation using a linear PFOA calibration curve 

provided a measure of accuracy in quantifying the sum of potential linear + branched PFOA isomers that

are commonly associated with environmental samples. Each LCS level was prepared in triplicate. The 

averaged results of the LCS analyses are shown in Table 8 and calculated analytical method uncertainty 

is shown in Table 9. The method acceptance criteria of 100 ± 30% was met for all LCSs. The LCS 

recoveries were calculated using the following equation: 

*100%

Spike Concentration

(Determine d Concentration of LCS) LCS Recovery =
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 15 of 19

Table 8. LCS Results 

Sample ID PFOA Recovery 

3.00 ng LCS 30.0 ng LCS 300 ng LCS 

LCSs (S111005a) 

91.0% 86.0% 86.3% 

84.7% 92.3% 88.3% 

93.0% 90.3% 107% 

Average Recovery 89.6% 89.6% 93.9% 

Std Dev. 4.4% 3.2% 11% 

RSD 4.9% 3.6% 12% 

LCS concentrations were 3.00 ng, 30.0 ng and 300 ng of PFOA (linear + branched isomers) added to each nominal 1 gram of 

control soil used to prepare the LCSs (1 cc of soil TCR-842 equal to nominal 1.0 gram; dry weight). 

Table 9. Analytical Method Uncertainty Determination 

Sample ID PFOA Recovery (%) 

3 ng LCS in TCR-842, replicate 1 91.0% 

3 ng LCS in TCR-842, replicate 2 84.7% 

3 ng LCS in TCR-842, replicate 3 93.0% 

30 ng LCS in TCR-842, replicate 1 86.0% 

30 ng LCS in TCR-842, replicate 2 92.3% 

30 ng LCS in TCR-842, replicate 3 90.3% 

300 ng LCS in TCR-842, replicate 1 86.3% 

300 ng LCS in TCR-842, replicate 2 88.3% 

300 ng LCS in TCR-842, replicate 3 107% 

Average 91.0% 

Standard Deviation 6.7% 

RSD 7.3% 

Analytical Method Uncertainty (2 x Std. Dev.); 95% CI 13% 

7.6 Laboratory Matrix Spikes (LMSs) 

Laboratory matrix spikes (LMSs) were generated by spiking a known quantity of PFOA (linear) to an 

aliquot of each soil sample and then preparing the sample the same as regular non-spiked samples. 

For this study, two LMSs were prepared for each field sample, fortified with 5.00 ng and 50.0 ng of PFOA 

as a low LMS and high LMS, respectively. One LMS was prepared for the trip blank an fortified with 

nominal 1.00 ng PFOA The LMS recoveries for PFOA from samples are shown in Table 2 and ranged 

from 94.8% to 129%. The method acceptance criteria of 100 ± 30% was met for all LMSs. The PFOA 

recovery calculations for LMS samples used the following equation: 

*100%

Spike Concentration

(Determine d Concentration of LMS Determined Concentration of Field Sample) LMS Recovery −

=
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 16 of 19

7.7 Percent Moisture Determinations 

The percent moisture was determined in duplicate for each soil sample. For each replicate, a sample 

aliquot is accurately weighed to determine the “wet” weight. Then the aliquot is dried at > 100°C unt il no 

further loss in mass occurs (due to water evaporation), and then the dry weight is accurately determined. 

The average percent moisture and RPD of the duplicate determinations for each is reported in Table 10. 

The percent moisture was calculated by the following equation: 

*100%

Original Soil Wet Mass

(Original Soil Wet Mass Dried Soil Mass) Percent Moisture −

= 

Table 10. Percent Moistures for Decatur, AL Soils from Well Location 610 

LIMS ID Sample ID Average Percent 

Moisture (w/w) [a]

Relative Percent 

Difference [a]

GLP10-01-01-21-001 DAL-SB-610S-0-0000 13.0% 2.1% 

GLP10-01-01-21-002 DAL-SB-610S-0-0010 9.46% 0.53% 

GLP10-01-01-21-003 DAL-SB-610S-0-0040 12.8% 14% 

GLP10-01-01-21-004 DAL-SB-610S-0-0150 19.4% 0.32% 

GLP10-01-01-21-005 TRIP BLANK-1 1.97% 16% 

 [a] Percent moisture determined for duplicate samples of soil taken from each sample bottle 

7.8 Individual Sample Results 

. The individual sample concentration results are shown in Table 11. 

Table 11. Individual PFOA Results for Decatur, AL Soils from Well Location 610 

Sample Description 

Surrogate 

(

13C4-PFOA) 

Recovery [a] 

LMS Spike 

Concentratio

n (ng/g; dry 

weight) 

Measured 

PFOA 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

(Data 

Accuracy) [b]

Average PFOA 

Concentration 

(ng/g; dry wt.) and 

RPD (Data 

Precision) 

GLP10-01-01-21-001 119% N/A 4.80 N/A 4.57 

GLP10-01-01-21-001 Dup 123% 4.33 

GLP10-01-01-21-001 Low LMS 108% 6.07 10.8 103% 

10% 

GLP10-01-01-21-001 High LMS 108% 58.9 64.5 102% 

GLP10-01-01-21-002 116% N/A 10.6 N/A 10.3 

GLP10-01-01-21-002 Dup 109% 9.91 

GLP10-01-01-21-002 Low LMS 108% 5.60 15.8 98.7% 

7.0% 

GLP10-01-01-21-002 High LMS 113% 57.2 74.2 112% 

GLP10-01-01-21-003 124% N/A 6.11 N/A 6.21 

GLP10-01-01-21-003 Dup 109% 6.30 

GLP10-01-01-21-003 Low LMS 118% 5.05 12.7 129% 

2.9% 

GLP10-01-01-21-003 High LMS 104% 52.4 64.1 111% 

GLP10-01-01-21-004 123% N/A BLQ N/A BLQ 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 17 of 19

Table 11. Individual PFOA Results for Decatur, AL Soils from Well Location 610 

Sample Description 

Surrogate 

(

13C4-PFOA) 

Recovery [a] 

LMS Spike 

Concentratio

n (ng/g; dry 

weight) 

Measured 

PFOA 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

(Data 

Accuracy) [b]

Average PFOA 

Concentration 

(ng/g; dry wt.) and 

RPD (Data 

Precision) 

GLP10-01-01-21-004 Dup 109% BLQ 

GLP10-01-01-21-004 Low LMS 111% 4.90 4.64 94.8% [c]

N/A 

GLP10-01-01-21-004 High LMS 114% 49.5 56.2 114% [c]

GLP10-01-01-21-005 118% N/A BLQ N/A BLQ 

GLP10-01-01-21-005 Dup 117% BLQ 

GLP10-01-01-21-005 LMS 115% 1.01 1.03 102% [c]N/A 

N/A; not applicable 

[a] Surrogate recovery determined for samples fortified with 3.0 ng of 13C4-PFOA and quantified from a 13C4-PFOA calibration curve, 

but otherwise not used for data accuracy assessments for the study. 

[b] LMSs prepared using PFOA (linear isomer). 

[c] Values below the LLOQ (BLQ) were treated as a concentration of zero for LMS recovery calculations 

8 Conclusion 

Analysis of the Decatur, AL soils collected from near well location 610 was successfully completed 

following 3M Environmental Laboratory method ETS-8-053.0 and conducted as 3M study GLP10-01-

01-21. The average PFOA concentration results for the soil samples are summarized in Table 1 and 

associated LMS recoveries are summarized in Table 2. The PFOA results for each individual 

sample replicate are provided in Table 10. 

All sample results were reported with acceptable LMS recoveries within 100 + 30%, and all gave 

acceptable RPDs of less than 50% for duplicate determined results. The travel blank that 

accompanied the sample bottles shipments was below the low limit of quantitation (BLQ, less than 

nominal 0.200 ng/g) , indicating there was not any contamination of samples during sample 

shipment, storage and preparation for analysis.

9 Data/Sample Retention 

All soil samples and associated project data (hardcopy and electronic) will be archived as project GLP10-

01-01-21according to 3M Environmental Laboratory standard operating procedures. 

10 List of Attachments 

Attachment A: Preparation Forms, Raw Data and Chromatograms 
study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610 

i11 Signatures 

Report Approval: 

'•A:i 

Cleston C. Lange, Ph.D., Principal Analytical Investigator Date 

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

f2-

Gary A. Hoheristein, Sdbnsor Representative Date 

Jaisimha Kesari, Study Director Ddte 

Page 18 of 19 
Study: GLP10-01-01, Interim Report 21 

Analysis for PFOA in Decatur, AL Soils Collected from Well Location 610

Page 19 of 19

Attachment A 

Preparation Forms, Raw Data and Chromatograms