3 

GLP10-01-01 Interim Report 26: Analysis for PFOA in Sediments Collected 

from the Jeffries Property in February 2012

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

GLP10-01-01-26 

Total Number of Pages 

19
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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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
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Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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

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

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

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

LIST OF TABLES

Table 1. PFOA Results for Sediments from Jeffries Property, February 2012 ...................................... 8

Table 2. LMS PFOA Recovery Results for Sediments from Jeffries Property, February 2012 ............. 8

Table 3. 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 Jeffries Property Sediments, February 2012 .................................... 16

Table 11. Individual PFOA Results for Jeffries Property Sediments, February 2012 .......................... 16
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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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: March 02, 2012 

Interim Analytical Completion: March 23, 2012 

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 792.
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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2 Summary 

This interim report provides the PFOA concentration results for five sediments collected from the Jeffries 

property (Bert Jeffries Landfill) located in Northern Alabama. One travel blank (trip blank), containing 

approximately 10-25 grams of control soil in a sample bottle, accompanied the sample bottles to and from 

the collection site and was also analyzed. Samples were received on March 02, 2012 and logged into the 

3M Environmental Laboratory electronic LIMS system under project GLP10-01-01-26. Prior to extraction,

sediments were aliquoted from each sample bottle in triplicate into extraction vessels and accurately 

weighed. The first and second aliquot served as analytical sample and duplicate sample. The third 

replicate of each was fortified with nominal 2.00 ng of PFOA as a laboratory matrix spike (LMS). A single 

LMS for the trip blank was also prepared and fortified with nominal 1.00 ng of PFOA. Each aliquot was

extracted and analyzed per method ETS-8-053 by liquid chromatography with triple quadrapole mass 

spectrometric detection (LC/MS/MS). The PFOA recovery results from LMSs provided a measure of 

sample-specific accuracy for the results. 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 and results reported on a dry sediment weight basis. The 

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

recoveries for PFOA are summarized in Table 2. 

Table 1. PFOA Results for Sediments from Jeffries Property, February 2012 

3M LIMS ID Sample ID 

Avg. PFOA 

Concentration (ng/g; 

dry weight) 

Relative Percent 

Difference 

GLP10-01-01-26-001 JPAL SD TRIP1 0 0000 BLQ NA 

GLP10-01-01-26-002 JPAL SD ET01 0 0000 0.629 14% 

GLP10-01-01-26-003 JPAL SD ET02 0 0000 0.671 23% 

GLP10-01-01-26-004 JPAL SD ET02 DB 0000 0.819 42% 

GLP10-01-01-26-005 JPAL SD ET03 0 0000 1.06 1.4% 

GLP10-01-01-26-006 JPAL SD ET04 0 0000 2.39 11% 

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). 

NA; not applicable 

Table 2. LMS PFOA Recovery Results for Sediments from Jeffries Property, February 2012 

3M LIMS ID Sample ID 

PFOA Spike 

Concentration 

(ng/g; dry weight) 

PFOA Recovery 

(Data Accuracy) 

GLP10-01-01-26-001 LMS JPAL SD TRIP1 0 0000, LMS 1.00 ng 0.980 89.6% 

GLP10-01-01-26-002 LMS JPAL SD ET01 0 0000, LMS 2.00 ng 1.38 92.5% 

GLP10-01-01-26-003 LMS JPAL SD ET02 0 0000, LMS 2.00 ng 1.67 89.3% 

GLP10-01-01-26-004 LMS JPAL SD ET02 DB 0000, LMS 2.00 ng 1.45 85.0% 

GLP10-01-01-26-005 LMS JPAL SD ET04 0 0000, LMS 2.00 ng 2.13 91.8% 

GLP10-01-01-26-006 LMS JPAL SD TRIP1 0 0000, LMS 2.00 ng 3.34 101% 

[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 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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3 Introduction 

The 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 sediments collected from the 

Jeffries property. The samples were collected by Weston Solutions, Inc. personnel in February 2012 

and shipped to the 3M Environmental Laboratory for quantitative analysis of PFOA. One soil travel 

blank (trip blank) accompanied the sample bottles to the site, during collection and during samples 

shipment and was analyzed to evaluate for any potential contamination of samples during the sample 

shipment and collection period. 

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 GLP10-01-01-26. 

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 13C4-PFOA 

surrogate recovery standard (SRS) 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 analytical reference substances are listed in Table 3. 

Table 3. 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 Jan.17, 2018 Feb. 27, 2017 Dec. 07, 2013 May 24, 2014 

Storage Conditions Frozen Frozen Frozen Frozen 

Chemical Lot 3440 332 MPFOA1210 052411 

TCR Number TCR07-0041-1/1 TCR-123 TCR11-0001-11/14 TCR11-0016-13/17 & 

TC R11-0016-14/17 

Physical Description Powder White Powder Methanol Solution [a] Methanol Solution [a]

Purity 99.6% 95% >98% >98% 

[a] Stable isotope labeled materials are typically provided as methanol solutions by the commercial vendor 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 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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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 sediments collected from the Jeffries property that is located in Northern 

Alabama. Samples for this study are “real world” environmental samples. 

6 Method Summary 

6.1 Methods 

The sample extractions and quantitative LC/MS/MS analyses were performed following validated method 

ETS-8-053.0. Two analytical batches were prepared for this study as o120309c and o120316a. The result 

for the trip blank was reported from batch o120309c and results for field samples were reported from run 

120316a. 

6.2 Sample Receipt 

On February 21, 2012 seven empty 250-mL HDPE NalgeneTM sample bottles, and one travel blank 

(trip blank) containing approximately 10-25 grams of a control soil TCR-455, were sent from the 3M 

Environmental Laboratory to Weston Solutions, Inc. field personnel for collection of sediments from 

the property known as the Bert Jeffries landfill. Following the sample collections by Weston 

Solutions, Inc. personnel, five sediment-filled sample bottles and the trip blank were returned in the

bottles to the 3M Environmental Laboratory for quantitative analysis of PFOA. The samples were 

received with sample chains of custody numbers 15290 on March 02, 2012. 

Soil samples from Alabama are regulated and the sediments for this study were shipped in 

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

Sample nomenclature follows the form JPAL-SD-ET-xxxx where the first string defines the Jeffries 

Property Alabama (JPAL), the second string defines the sample media (i.e., SD= sediment, SB –field 

sample duplicate), the third string defines the site location (ET = eastern tributary), the fourth string defines 

the field sample (1,2,3... or DB = duplicate field sample) . The fourth string defines the sediment sampling 

depth (0000 = 0 ft to 0.5 ft interval). 

6.3 Sample Preparation 

Sample preparation was conducted as two analytical batches, o120309c and o120316a. The first batch 

was prepared with LMSs fortified at 20 and 200 ng of PFOA, which was later determined to be too high for 

a proper evaluation of PFOA recovery from the sediments which contained much lower PFOA levels. The 

trip blank was prepared with a 1 ng PFOA LMS and was reported from that batch. The samples were 

prepared a second time as o120316a with a 2 ng fortified LMS for each sample, and the sample results 

reported from that batch. 

Each soil or sediment extraction involved removal of a 1 cubic centimeter (1 cc; 1 mL) aliquot of field 

sample (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) and 3.0ng of surrogate recovery standard 

(SRS) was added to each soil aliquot and a known quantity of PFOA was added to each LMS. Then each 

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

followed by centrifugation to remove solids. The supernatant from each was then transferred to an autovial 
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

Page 11 of 19

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

During preparation, each sample additionally 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 sample. Additionally, a third 

and/or fourth replicate was weighed out and used to prepare LMSs. The LMS results were used for 

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

precision. Appropriate LMS levels are considered those that are within 0.5-times to 10-times the measured 

endogenous PFOA level in the equivalent non-fortified soil/sediment sample. 

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-455. The nominal mass 

of 1 cc of control soil TCR-455 is 1.0 gram (dry), therefore, 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-455, 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 sediments and soils were used to calculate the dry weight of the wet soil and 

sediment samples 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 wate r 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 sample in Table 9. 

6.5 LC/MS/MS Analysis 

The LC/MS/MS analysis was performed 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 on-going 

method validation aspect in which surrogate recovery behavior is being evaluated in “real world” 

environmental samples for possible future applications. 

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. 
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

Page 12 of 19

Table 4. Instrument Information 

Instrument Name ETS-Ollie 

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 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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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. 

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-455 (nominal 1.0 gram per mL). A total of twelve (12) soil 

matrix calibration standards ranging from nominal PFOA concentration 0.200 ng/g to 500 ng/g were 

prepared and analyzed. 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 0.998, 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-455 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 and 

sediments can vary in moisture content, composition and density, 1 cc aliquots of field soil and sediment 

samples typically weigh more or less 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 0.750 1.00 2.50 5.00 9.99 25.0 50.0 100 200 500 N/A 

o120309c excluded 0.342 0.651 1.01 2.78 5.13 11.9 27.2 53.5 101 183 512 0.9984 

o120316a 0.166 0.511 0.763 0.911 2.62 5.45 10.4 26.3 51.7 96.8 198 502 0.9998 

Average (ng) 0.166 0.427 0.707 0.961 2.70 5.29 11.2 26.8 52.6 98.9 191 507 0.9991 

Avg. Recovery 

(%) 83.0% 85.3% 94.3% 96.1% 108% 106% 112% 107% 105% 98.9% 95.3% 101% NA 

NA; not applicable 

[a] PFOA concentrations are nominal ng/g (dry soil wt) concentration based on a nominal mass of 1.0 gram (dry wt.) for each 1 cubic centimeter 

of control soil used to prepare each calibration standard. 
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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 analytical run o120309c, from 

which the trip blank result was reported, was nominal 0.500 ng/g calibration standard. The LLOQ for 

analytical batch o120316a, from which the study sample results were reported, was nominal 0.200 ng/g. 

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). 

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 for PFOA from CCVs were used to confirm that the instrument 

response and the initial calibration curve were still in control. All CCVs flanking reported PFOA data met 

the method criteria of 100% ± 30% accuracy, except for in o120309c where one of the CCVs for PFOA 

was at 131% and the PFOA result for the trip blank in that run reported with a method deviation. 

7.4 Blanks 

Three types of blanks were analyzed during this analysis: solvent blanks; and method blanks, which were 

prepared with blank matrix soil TCR-455 and were spiked with IS and surrogate; and travel blanks (trip

blanks) prepared from aliquots of soil TCR-455 contained in sealed sample bottles that accompanied the

bottle order to Decatur, AL and the collection site, and returned with the sample shipment back to 3M 

Environmental Laboratory. 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-455, 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 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

Page 15 of 19

Table 8. LCS Results 

Sample ID 

PFOA Recovery 

3.00 ng LCS 30.0 ng LCS 300 ng LCS 

LCSs (o120309c) 

114% 114% 129% 

97.0% 108% 104% 

108% 110% 107% 

LCSs (o120316a) 

89.7% 93.7% 102% 

97.0% 93.7% 95.0% 

95.3% 88.3% 96.3% 

Average Recovery 100% 101% 106% 

Std Dev. 9.1% 10% 12% 

RSD 9.1% 10% 12% 

Overall Average 102% 

Overall Std. Dev. 10% 

Overall RSD 10% 

Method Uncertainty (95% 

CI) = 2 x Std Dev. all levels 21% 

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-455 equal to nominal 1.0 gram; dry weight). 

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/sediment sample and then preparing the sample the same as regular non-fortified samples. 

For this study, LMSs were prepared for each field sample at 20 and 200 ng PFOA as a low LMS and high 

LMS, respectively, in run o120309c. However, those LMS levels were too high and samples re-prepared 

in o120316a with LMSs fortified with 2 ng PFOA. One LMS was prepared for the trip blank and fortified 

with nominal 1.00 ng PFOA in run o120309c and was reported from that run. The LMS recoveries for 

PFOA are shown in Table 2. 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 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

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 Jeffries Property Sediments, February 2012 

LIMS ID Sample ID Average Percent 

Moisture (w/w) [a]

Relative Percent 

Difference [a]

GLP10-01-01-26-001 JPAL SD TRIP1 0 0000 2.72% 2.5% 

GLP10-01-01-26-002 JPAL SD ET01 0 0000 28% 0.78% 

GLP10-01-01-26-003 JPAL SD ET02 0 0000 30% 1.5% 

GLP10-01-01-26-004 JPAL SD ET02 DB 0000 30% 0.78% 

GLP10-01-01-26-005 JPAL SD ET03 0 0000 40% 3.6% 

GLP10-01-01-26-006 JPAL SD ET04 0 0000 61% 0.096% 

 [a] Percent moisture determined for duplicate samples of soil/sediment 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 Jeffries Property Sediments, February 2012 

Sample Description 

Surrogate 

(

13C4-PFOA) 

Recovery [a]

LMS Spike 

Concentration 

(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) 

JPAL SD TRIP1 0 0000 101% NA 

BLQ 

NA BLQ 

JPAL SD TRIP1 0 0000 Duplicate 113% BLQ 

JPAL SD TRIP1 0 0000 LMS [c] 113% 0.980 0.878 89.6% NA 

JPAL SD ET01 0 0000 98.2% NA 0.671 NA 0.629 

JPAL SD ET01 0 0000 Duplicate 103% 0.586 

JPAL SD ET01 0 0000 LMS 94.5% 1.38 1.91 92.5% 14% 

JPAL SD ET02 0 0000 109% NA 0.592 NA 0.671 

JPAL SD ET02 0 0000 Duplicate 106% 0.749 

JPAL SD ET02 0 0000 LMS 97.2% 1.67 2.16 89.3% 23% 

JPAL SD ET02 DB 0000 96.2% NA 0.990 NA 0.819 
Study: GLP10-01-01, Interim Report 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

Page 17 of 19

Table 11. Individual PFOA Results for Jeffries Property Sediments, February 2012 

Sample Description 

Surrogate 

(

13C4-PFOA) 

Recovery [a]

LMS Spike 

Concentration 

(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) 

JPAL SD ET02 DB 0000 Duplicate 94.5% 0.649 

JPAL SD ET02 DB 0000 LMS 104% 1.45 2.05 85.0% 42% 

JPAL SD ET03 0 0000 109% NA 1.07 NA 1.06 

JPAL SD ET03 0 0000 Duplicate 104% 1.05 

JPAL SD ET03 0 0000 LMS 101% 2.13 3.02 91.8% 1.4% 

JPAL SD ET04 0 0000 100% 

NA 

2.25 

NA 2.39 JPAL SD ET04 0 0000 Duplicate 108% 2.53 

JPAL SD ET04 0 0000 LMS 104% 3.34 5.76 101% 11% 

NA; Not applicable 

BLQ; Below the lower limit of quantitation 

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

[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 sediments collected from the Jeffries property was successfully completed following 

3M Environmental Laboratory method ETS-8-053.0 and conducted as 3M study GLP10-01-01-26. 

The average PFOA concentration results for the samples and trip blank are summarized in Table 1

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

analytical sample replicate used for reporting are provided in Table 10. 

All sample results were reported with LMS recoveries within 100 + 15%, and duplicate results gave 

RPDs of less than 50%. The travel blank that accompanied the sample bottles shipments was below 

the low limit of quantitation (BLQ, less than nominal 0.500 ng/g), indicating there wasn’t 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-

01-01-26 according 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 26 

Analysis for PFOA in Sediments Collected from the Jeffries Property, Feb. 2012

Page 19 of 19

Attachment A 

Preparation Forms, Raw Data and Chromatograms