3 

GLP10-01-02 Interim Report 25: Analysis of PFOS, PFHS and PFBS in 

Sediments Collected from the Jeffries Property

Study Title

3M Environmental Laboratory Analytical Protocol GLP10-01-02: Analysis of Perfluorooctane 

Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in 

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

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

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

GLP10-01-02-25 

Total Number of Pages 

24
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Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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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 ........................................................................................ 10

5 Test System ....................................................................................................................................... 11

6 Method Summary .............................................................................................................................. 11

6.1 Methods ................................................................................................................................ 11

6.2 Sample Receipt .................................................................................................................... 11

6.3 Sample Preparation .............................................................................................................. 12

6.4 Percent Soil Moisture Determination ................................................................................... 13

6.5 LC/MS/MS Analysis .............................................................................................................. 13

7 Analytical Results .............................................................................................................................. 14

7.1 Calibration ............................................................................................................................. 14

7.2 Limits of Quantitation (LOQs) .............................................................................................. 16

7.3 Continuing Calibration .......................................................................................................... 16

7.4 Blanks .................................................................................................................................... 16

7.5 Laboratory Control Spikes (LCSs) ....................................................................................... 16

7.6 Laboratory Matrix Spikes (LMSs) ........................................................................................ 18

7.7 Percent Moisture Determinations ........................................................................................ 18

7.8 Individual Analytical Sample Results ................................................................................... 19
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Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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8 Conclusion ......................................................................................................................................... 22

9 Data/Sample Retention ..................................................................................................................... 23

10 List of Attachments ............................................................................................................................ 23

11 Signatures .......................................................................................................................................... 23

LIST OF TABLES

Table 1. Results for Jeffries Property Sediments ...................................................................................... 8

Table 2. LMS Recovery for Jeffries Property Sediments .......................................................................... 9

Table 4. Instrument Information ................................................................................................................ 13

Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053)....................................................... 14

Table 6. Mass Transitions ......................................................................................................................... 14

Table 7. PFOS Calibration Summary ....................................................................................................... 15

Table 8. PFHS Calibration Summary ....................................................................................................... 15

Table 9. PFBS Calibration Summary ....................................................................................................... 15

Table 10. LCS Results (PFOS, linear + branched isomer) ..................................................................... 17

Table 11. LCS Results (PFHS, linear + branched isomer) ..................................................................... 17

Table 12. LCS Results (PFBS) ................................................................................................................. 17

Table 13. Analytical Method Uncertainties ............................................................................................... 18

Table 14. Percent Moistures for Jeffries Property Sediments ................................................................. 19

Table 15. Individual PFOS Results for Jeffries Property Sediments ...................................................... 19

Table 16. Individual PFHS Results for Jeffries Property Sediments....................................................... 20

Table 17. Individual PFBS Results for Jeffries Property Sediments ....................................................... 21
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Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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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 12, 2012 

Interim Analytical Completion: May 29, 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: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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2 Summary 

This interim report provides the PFOS, PFHS and PFBS concentration results for five sediment samples 

collected in March 2012 at the Jeffries property in northern Alabama. In addition, one travel blank (trip 

blank), containing between10-25 grams of control soil in a sample bottle, accompanied the sample bottles 

to and from the site and was also analyzed for quality control purposes. Samples were logged into the 3M 

Environmental Laboratory information management system (LIMS) under project GLP10-01-01-26 and 

cross referenced to this project GLP10-01-02-25 for additional fluorochemical sulfonates analysis. Four 

aliquots of sample were removed from each sample bottle and accurately weighed for extraction. The first 

and second aliquot served as analytical sample and duplicate analytical sample. The third and fourth 

aliquots were fortified with nominal 20.0 and 200 ng each of PFOS (linear isomer), PFHS (linear isomer) 

and PFBS as a low and high laboratory matrix spike (LMS), respectively. Three aliquots of the trip blank 

were taken, with the third prepared as a single LMS that was fortified with nominal 1.00 ng each of PFOS 

(linear isomer), PFHS (linear isomer) and PFBS. Samples were extracted and analyzed per method ETS8-053 by liquid chromatography with triple quadrapole mass spectrometric detection (LC/MS/MS). The 

LMS recovery results provided a measure of the data accuracy. The relative percent difference (RPD) of 

the duplicate analytical sample results was used to assess the data precision. The percent moisture of 

each soil was also determined as part of the study. The PFOS, PFHS and PFBS concentrations are 

summarized in Table 1. The PFOS, PFHS and PFBS recoveries from the LMS samples are summarized 

in Table 2. The average data accuracy and standard deviation determined from LMS results was 107% +

7.9% for PFOS, 105% + 7.2% for PFHS and 106% + 5.2% for PFBS. The analytical method uncertainty 

(95% CI) was determined at + 7.3% for PFOS, + 10% for PFHS and + 12% for PFBS. 

Table 1. Results for Jeffries Property Sediments 

3M LIMS ID [d] Sample ID Average Concentration (ng/g; dry) 

PFOS PFHS PFBS 

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

GLP10-01-01-26-002 JPAL SD ET01 0 0000 3.95 BLQ BLQ 

GLP10-01-01-26-003 JPAL SD ET02 0 0000 8.59 BLQ BLQ 

GLP10-01-01-26-004 JPAL SD ET02 DB 0000 10.0 BLQ BLQ 

GLP10-01-01-26-005 JPAL SD ET03 0 0000 12.1 BLQ BLQ 

GLP10-01-01-26-006 JPAL SD ET04 0 0000 23.8 BLQ BLQ 

All LMS recovery results were within acceptance criteria of 100 + 30% 

Average concentration of duplicate analytical result reported; RPDs of duplicates were less than 10% 

The analytical method uncertainty was determined from LCS results at + 12% for PFBS, + 10% for PFHS and + 7.2% for PFOS 

Concentration values are shown at 3 significant figures, but more precise data was used for data calculations. 

BLQ; analyte response was lower than the analyte response of the lowest standard (LLOQ) which was the nominal 0.500 ng 

calibration standard (i.e. less than nominal 0.50 ng/g) 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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Table 2. LMS Recovery for Jeffries Property Sediments 

3M LIMS ID [b] Sample ID LMS Recovery (%) 

PFOS PFHS PFBS 

GLP10-01-01-26-001 Low JPAL SD TRIP1 0 0000 LMS 130% 125% 105% 

GLP10-01-01-26-002 Low JPAL SD ET01 0 0000 LMS Low 102% 105% 114% 

GLP10-01-01-26-002 High JPAL SD ET01 0 0000 LMS High 103% 103% 103% 

GLP10-01-01-26-003 Low JPAL SD ET02 0 0000 LMS Low 104% 102% 110% 

GLP10-01-01-26-003 High JPAL SD ET02 0 0000 LMS High 104% 105% 103% 

GLP10-01-01-26-004 Low JPAL SD ET02 DB 0000 LMS Low 105% 100% 105% 

GLP10-01-01-26-004 High JPAL SD ET02 DB 0000 LMS High 104% 103% 98.5% 

GLP10-01-01-26-005 Low JPAL SD ET03 0 0000 LMS Low 111% 105% 108% 

GLP10-01-01-26-005 High JPAL SD ET03 0 0000 LMS High 108% 107% 104% 

GLP10-01-01-26-006 Low JPAL SD ET04 0 0000 LMS Low 105% 108% 115% 

GLP10-01-01-26-006 High JPAL SD ET04 0 0000 LMS High 104% 97.0% 101% 

Average Recovery 107% 105% 106% 

Standard Deviation 7.9% 7.2% 5.2% 

RSD 7.4% 6.8% 4.9% 

LMSs were fortified with PFOS, PFHS and PFBS (linear isomers only) at nominal 20.0 ng (low) and 200 ng (high). 

The LMS for the trip blank was fortified at nominal 1.0 ng each of PFOS, PFHS and PFBS 

Recovery values are shown at 3 significant figures, but more precise data was used for data calculations. 

3 Introduction 

The soil analyses results 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 perfluorooctane sulfonate 

(PFOS), perfluorohexane sulfonate (PFHS) and perfluorobutane sulfonate (PFBS) in various 

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

the Decatur facility. 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 PFOS, PFHS and PFBS. 

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 PFOS, PFHS and PFBS in the sediment samples that 

were received. Additionally, included in this report are the assessment of the analytical precision 

and accuracy for the reported PFOS, PFHS and PFBS concentration results based on duplicate 

analytical sample results and laboratory matrix spike (LMS) recovery results, respectively. The 

recovery results for a stable isotope labeled 13C4-PFOS surrogate recovery standard (SRS) that was 

added to each soil aliquot prior to extraction, and the determined percent moisture content of each 

soil, are also included herein. 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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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. Reference Substances 

Reference ID PFOS (linear) PFOS (linear + branched) PFHS (linear) 

Chemical Name n-Perfluorooctane-1-

Sulfonate Potassium Salt 

Perfluorooctane Sulfonate 

Potassium Salt 

n-Perfluorohexane-1-sulfonate 

Sodium Salt 

Chemical Formula n-C8F17SO3 K C8F17SO3 K n-C6F13SO3 Na 

Use Reference Standard for 

Calibration and LMSs Reference Standard for LCSs Reference Standard for Calibration and LMSs 

Source Wellington Laboratories 3M Wellington Laboratories 

Expiration Date 10/18/18 12/14/16 3/25/18 

Storage Conditions Frozen Frozen Frozen 

Chemical Lot Number LPFOSKBM06 171 LPFHxSAM08 

TCR Number TCR08-0001-1/1 TCR-696 TCR08-0018-1/1 

Physical Description Crystalline White Powder Crystalline 

Purity 98% 86.4% >98% 

Reference ID PFHS (linear + 

branched) 

PFBS (predominantly 

linear) 

13C4-PFOS 

Chemical Name n-Perfluorohexane-1-

sulfonate Potassium Salt 

Perfluorobutane-1-sulfonate 

Potassium Salt 

[1,2,3,4-13C4]-Perfluorooctane1-Sulfonate Sodium Salt 

Chemical Formula n-C6F13SO3 K n-C4F9SO3 K 13C4

12C4F17SO3 Na 

Use Reference Standard for 

LCSs 

Reference Standard for All 

PFBS Surrogate 

Source 3M 3M Wellington Laboratories 

Expiration Date 2/12/17 1/10/17 9/8/2013 

Storage Conditions Frozen Frozen Frozen 

Chemical Lot Number NB 120067-69 101 MPFOS0910 

TCR Number TCR-083 TCR-121 TCR10-0044-2/9 

Physical Description White Powder White Powder Liquid; Methanol solution 

Purity 98.6% 96.7% >98% [a]
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Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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Reference ID 13C8-PFOS 13C3-PFHS 18O2-PFBS 

Chemical Name [

13C8]-Perfluorooctane-1-

Sulfonate Sodium Salt 

[

13C3]-Perfluorohexane-1-

Sulfonate Sodium Salt 

[

18O2]-Perfluorobutane-1-

Sulfonate Ammonium Salt 

Chemical Formula 13C8F17SO3 Na 13C3

12C3F13SO3Na C4F9S

18O2

16O NH4

Use Internal Standard for 

PFOS Internal Standard for PFHS Internal Standard for PFBS 

Source Wellington Laboratories Wellington Laboratories RTI International 

Expiration Date 9/28/2013 9/28/2013 3/9/15 

Storage Conditions -20 ̊C -20 ̊C -20 ̊C 

Chemical Lot Number 092310 092310 11546-107-2 

TCR Number TCR10-0048-3/16, 4/16 TCR10-0048-3/16, 4/16 TCR-1042 

Physical Description Liquid; Methanol solution Liquid; Methanol solution Liquid; Methanol solution 

Purity >98% [a] >98% [a] >99% [a]

[a] The commercially provided material was a methanol solutions and labeled with a weight/volume concentration 

purity value. However, the concentration of further dilutions was based on the certified concentration of the stock 

material. 

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 method 

ETS-8-053.0. The results reported herein were obtained from analytical run j120507b. Two analytical runs 

were conducted as o120312a and o120313a, but result not used due to QC results that did not meet 

method acceptance criteria. 

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 Jeffries Property, formerly the Bert Jeffries landfill. Following the sample 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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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 PFOS, 

PFHS and PFBS. 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 

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 PFOS (linear isomer), PFHS (linear isomer) 

and PFBS 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 for analysis. An accurately 

measured volume of each supernatant was analyzed by LC/MS/MS. 

During preparation, each sample and quality control sample received nominal 3.0 ng of a stable isotope

labeled 13C4-PFOS surrogate recovery standard (SRS). 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 and sediment 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 Tables 15, 16 and 17 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 PFOS, PFHS and PFBS 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 analyte level in the equivalent non-fortified soil/sediment sample, and 

the fortification of 20 ng and 200 ng was sufficient in at least one of the LMSs to be considered appropriate 

for determination of the data accuracy for PFOS, but was greater than 10-times the PFBS and PFHS 

endogenous levels which were less than the LLOQ (BLQ) in all samples. 

Calibration standards were prepared by spiking known quantities of PFOS (linear isomer), PFHS (linear 

isomer), PFBS and 13C4-PFOS 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 PFOS (mixed 

linear + branched isomers), PFHS (mixed linear + branched isomers) and PFBS. The LCS results were 

used to estimate the analytical method uncertainty. 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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6.4 Percent Soil Moisture Determination 

The percent moisture of sediment samples was determined by gravimetric analysis. Dry weights were 

determined from separate weighings than the sample aliquot weighings used for extractions. To 

determine the percent moisture, duplicate aliquots of each soil sample were removed and the accurate 

“wet” weight determined for each. Each aliquot was then dried at > 100°C until no further mass loss 

occurred from water evaporation, at which time the accurate dry sample weights were determined. The 

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

original sample. The averaged percent moisture result for each was then used to report the PFOS, 

PFHS and PFBS concentration on a dry weight basis. 

6.5 LC/MS/MS Analysis 

The analysis of sample extracts for PFOS, PFHS and PFBS was performed by LC/MS/MS as 

described in method ETS-8-053.0. The relative percent difference (RPD) of duplicate prepared 

sample results was used as a measure of the analytical precision. The determined recovery of 

fortified PFOS, PFHS and PFBS from LMS samples was used as a measure of analytical 

accuracy. Surrogate recoveries are reported in Tables 15, 16 and 17, but were not used for 

evaluating analyte recovery for this study. The surrogate data was collected as part of an on-going 

evaluation of surrogate recovery from environmental field samples for supporting a method 

validation of ETS-8-053. 

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-Jonas (j) 

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 μm) 

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 5000 

Ion Source TurboIon Spray 

Polarity Negative 

Software Analyst 1.4.2 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

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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 

PFBS 299>99, 299>80 

18O2-PFBS (IS) 303>84 

PFHS 399>99, 399>80 

13C3-PFHS (IS) 402>80 

PFOS 499>130, 499>99, 499>80 

13C8-PFOS (IS) 507>80 

13C4-PFOS (Surrogate) 503>80 

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

analyte. 

7 Analytical Results 

Concentration values are rounded to three significant figures according to EPA rounding rules. 

Because of rounding some calculated values may vary slightly from those found in the raw data. 

Samples with RPDs for duplicate results of less than 50% and LMS results meeting the method 

criterion of within 100 ± 30% demonstrated that the method was appropriate for those samples and 

were reported without footnotes in results tables. The nominal 20.0 ng and 200 ng fortified quantities 

of PFOS, PFHS and PFBS into LMSs for field samples were at an appropriate level for evaluating 

sample-specific analyte recoveries for PFOS. Results for PFHS and PFBS were all less than the 

LLOQ (BLQ) and therefore LMS fortifications were greater than 10-times the endogenous level 

measured in the samples.

7.1 Calibration 

A set of calibration standards were prepared by spiking varying known quantities of PFOS (linear), PFHS 

(linear), PFBS and surrogate (13C4-PFOS), and a fixed quantity of stable isotope labeled internal 

standards, into one cubic centimeter (1 cc, 1 mL) aliquots of 3M Environmental Laboratory control soil

TCR-455 (nominal soil mass of 1.0 g/mL). A total of twelve (12) calibration standards were prepared as 

a set. The prepared standards were fortified from nominal 0.200 ng to 500 ng in 1 cubic centimeter of
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 15 of 24

control soil TCR-455; equivalent to nominal 0.200 ng/g to 500 ng/g in soil TCR-455. Following analysis 

of the calibration standards, the concentration of each standard was plotted against the measured 

analyte /IS peak area ratio. A quadratic equation with 1/x weighting was used to fit the data for each 

analyte. Calibration curves were not forced through zero. Determining the standard concentration using 

the resultant calibration curve and comparing to the known concentration confirmed accuracy of each 

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

0.999 for all calibration curves, and the coefficient of determination (r2) was greater than 0.990. 

Calibration results for PFOS, PFHS and PFBS are summarized in Table 7, Table 8 and Table 9, 

respectively. 

Because soil and sediment weights can vary significantly for a 1 cc (1 mL) field sample, depending on 

composition and moisture content, the instrument response was calibrated for the known concentrations 

of target analytes based on the mass quantity of reference substance added to a 1 cc soil (1 mL) 

calibration standard prior to extraction (e.g. calibrated in this study for a range of 0.500 ng to 500 ng 

PFOS, PFHS and PFBS; the 0.200 ng standard was excluded). Because a 1cc aliquot of control soil 

TCR-455 weighs nominally 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 500 ng/g. However, because sample 

soil aliquots may weigh more than 1.0 gram and contain significant moisture, the determined 

concentrations during the analysis on an ng per sample aliquot basis from the calibration curve and then 

adjusted for the accurate determined weight and percent moisture so they could be reported on a ng/g 

(dry weight) basis.

Table 7. PFOS Calibration Summary 

Analytical 

Run 

PFOS (ng) 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 0.199 0.499 0.748 0.997 2.49 4.99 9.97 24.9 49.9 99.7 199 499 N/A 

s111007a excluded 0.478 0.791 0.888 2.51 5.42 10.1 24.5 50.6 98.9 199 499 0.9999 

Recovery N/A 95.8% 106% 89.1% 101% 109% 101% 98.4% 101% 99.2% 100% 100% N/A 

Table 8. PFHS Calibration Summary 

Analytical 

Run 

PFHS (ng) 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 0.200 0.500 0.750 1.00 2.50 5.00 10.0 25.0 50.0 100 200 500 N/A 

s111007a excluded 0.473 0.801 0.908 2.41 5.57 9.95 26.2 47.5 99.9 201 500 0.9998 

Recovery N/A 94.6% 107% 90.8% 96.4% 111% 99.5% 105% 95.0% 99.9% 101% 100% N/A 

Table 9. PFBS Calibration Summary 

Analytical 

Run 

PFBS (ng) 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 0.200 0.500 0.750 1.00 2.50 5.00 10.0 25.0 50.0 100 200 500 N/A 

s111007a excluded 0.415 0.773 0.944 2.54 5.90 9.76 25.5 51.5 97.7 199 501 0.9998 

Recovery N/A 83.0% 103% 94.4% 102% 118% 97.6% 102% 103% 97.7% 99.5% 100% N/A 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 16 of 24

7.2 Limits of Quantitation (LOQs) 

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

the linearity and accuracy requirement for a low standard (100 + 35%) and for which the area counts 

were at least twice that of the average response determined for the method blank injected just prior to 

the calibration standards . The LLOQ for this study was the nominal 0.500 ng calibration standard 

(nominal 0.500 ng/g in soil TCR-455) for PFOS, PFHS and PFBS. All sample analyte responses less 

than the response of the 0.500 ng calibration standard were reported as BLQ (below the limits of 

quantitation). The upper limit of quantitation (ULOQ) was the nominal 500 ng calibration standard. 

7.3 Continuing Calibration 

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

injection of a mid-level calibration standard after approximately every 15th sample injected 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-455 and were spiked with IS and surrogate; travel blanks (trip blanks) prepared from 

aliquots of soil TCR-455 sealed in s ample bottle that accompanied the bottle order to and from the 

sampling site; and solvent blanks containing extraction solvent. The different blank results were 

reviewed to evaluate potential contamination during shipment, and to evaluate method performance 

parameters such as injector carry over and to establish the LLOQ. All blanks were below the LLOQ 

(BLQ) 

7.5 Laboratory Control Spikes (LCSs) 

Laboratory control spikes were prepared by spiking know quantities of PFOS (linear + branched), PFHS 

(linear + branched) and PFBS into 1 cc aliquots of soil TCR-455, fortified at nominal 3.0 ng and 30 ng

and 300 ng levels, with each level prepared in triplicate. The results of the LCS analyses and calculation 

of analyte measurement accuracies (percent recovery) for PFOS, PFHS and PFBS are shown in Table 

10, Table 11 and Table 12 respectively. The analytical method uncertainty calculated from LCS results 

is shown in Table 13. 

*100%

Spike Concentration

(Determine d Concentration of LCS) LCS Recovery =
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 17 of 24

Table 10. LCS Results (PFOS, linear + branched isomer) 

Sample ID PFOS Recovery 

3.00 LCS 30.0 LCS 300 LCS 

LCSs (j120507b) 

114% 109% 118% 

112% 109% 117% 

108% 114% 113% 

Average Recovery 111% 111% 116% 

Std Dev. 2.9% 3.1% 2.8% 

RSD 2.6% 2.8% 2.4% 

Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFOS (linear + branched isomers), each prepared and 

analyzed in triplicate. 

Table 11. LCS Results (PFHS, linear + branched isomer) 

Sample ID PFHS Recovery 

3.00 LCS 30.0 LCS 300 LCS 

LCSs (j120507b) 

118% 109% 108% 

116% 107% 113% 

103% 107% 105% 

Average Recovery 113% 108% 109% 

Std Dev. 8.3% 1.1% 3.9% 

RSD 7.4% 0.99% 3.5% 

Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFHS (linear + branched isomers), each prepared and 

analyzed in triplicate. 

Table 12. LCS Results (PFBS) 

Sample ID PFBS Recovery 

3.00 LCS 30.0 LCS 300 LCS 

LCSs (j120507b) 

116% 106% 98.3% 

117% 114% 112% 

113% 109% 106% 

Average Recovery 116% 110% 106% 

Std Dev. 2.1% 4.2% 7.0% 

RSD 1.8% 3.8% 6.6% 

Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFBS, each prepared and analyzed in triplicate. 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 18 of 24

Table 13. Analytical Method Uncertainties 

Sample ID LCS Results 

PFOS PFHS PFBS 

3.00 LCSs 

114% 118% 116% 

112% 116% 117% 

109% 103% 113% 

30.0 LCSs 

109% 109% 106% 

109% 107% 114% 

115% 107% 109% 

300 LCSs 

119% 108% 98.3% 

118% 113% 112% 

113% 105% 106% 

Average Recovery 113% 110% 110% 

Std Dev. 3.7% 5.1% 6.1% 

RSD 3.3% 4.7% 5.5% 

Method Uncertainty (2 x Std. Dev.); 95% CI 7.3% 10% 12% 

7.6 Laboratory Matrix Spikes (LMSs) 

Laboratory matrix spikes (LMSs) were generated by adding a known quantity of PFOS (linear), PFHS 

(linear) and PFBS to an aliquot of sediment sample, and then preparing the sample the same as nonspiked samples. Spikes for this study, LMSs were spiked at levels that were appropriate for the 

endogenous analyte levels in the soils, determined from screening analysis and fortified with the target 

analytes from 0.5-times to 10-times the endogenous analyte levels determined in the soil/sediment 

samples during the range finding analysis. The LMS method acceptance criterion of within 100 ± 30% 

were met for all LMS recoveries. The LMS recovery results are summarized in Table 2. The nominal 

20.0 ng and 200 ng fortified quantities of PFOS, PFHS and PFBS into LMSs for field samples were at an 

appropriate level for evaluating sample-specific analyte recoveries for PFOS. Results for PFHS and 

PFBS were all less than the LLOQ (BLQ) and therefore LMS fortifications were greater than 10-times the

endogenous level measured in the samples. The PFOS, PFHS and PFBS recovery calculations for 

LMSs used the following equation: 

*100%

Spike Concentration

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

=

7.7 Percent Moisture Determinations 

The percent moisture was determined for each soil sample. Duplicate aliquots of each were taken and 

accurately weighed to determine the “wet” weight. Then each aliquot was dried at > 100°C until no 

further loss in mass occurred due to water evaporation, after which the dry weight was accurately 

determined. The average percent moisture and RPD of the duplicate determinations for each soil are 

reported in Table 14. The percent moisture was calculated by the following equation: 

*100%

OriginalSoil Wet Mass

(OriginalSoil Wet Mass DriedSoil Mass) Percent Moisture −

= 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 19 of 24

Table 14. Percent Moistures for Jeffries Property Sediments 

LIMS ID Sample ID Average Percent 

Moisture (w/w) [a]

Relative Percent 

Difference [a]

GLP10-01-01-26-001 JPAL SD TRIP1 0 0000 2.7% 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 sample aliquots taken from each sample bottle 

7.8 Individual Analytical Sample Results 

The individual analytical sample results for PFOS, PFHS and PFBS concentrations are shown in Table 

15, Table 16 and Table 17, respectively. 

Table 15. Individual PFOS Results for Jeffries Property Sediments 

Sample Description 

Surrogate 

(

13C4-PFOS) 

Recovery 

LMS Spike 

Concentration 

(ng/g; dry 

weight) 

Measured PFOS 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

Average PFOS 

Concentration 

(ng/g; dry wt.) 

and RPD (%) 

GLP10-01-01-21-001 109% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-001 Dup 110% BLQ 

GLP10-01-01-21-001 LMS 105% 1.04 1.35 130% N/A 

GLP10-01-01-21-002 101% 

N/A 

3.81 

N/A 3.95 

GLP10-01-01-21-002 Dup 103% 4.09 

GLP10-01-01-21-002 Low LMS 102% 14.6 18.8 102% 

7.0% 

GLP10-01-01-21-002 High LMS 104% 143 152 103% [a]

GLP10-01-01-21-003 106% 

N/A 

8.99 

N/A 8.59 

GLP10-01-01-21-003 Dup 110% 8.20 

GLP10-01-01-21-003 Low LMS 107% 15.0 24.1 104% 

9.1% 

GLP10-01-01-21-003 High LMS 103% 151 166 104% [a]

GLP10-01-01-26-004 106% 

N/A 

9.8 

N/A 10.0 

GLP10-01-01-26-004 Dup 104% 10.2 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 20 of 24

Table 15. Individual PFOS Results for Jeffries Property Sediments 

Sample Description 

Surrogate 

(

13C4-PFOS) 

Recovery 

LMS Spike 

Concentration 

(ng/g; dry 

weight) 

Measured PFOS 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

Average PFOS 

Concentration 

(ng/g; dry wt.) 

and RPD (%) 

GLP10-01-01-26-004 Low LMS 105% 16.6 27.5 105% 

3.6% 

GLP10-01-01-26-004 High LMS 105% 152 168 104% [a]

GLP10-01-01-21-005 104% 

N/A 

11.9 

N/A 12.1 

GLP10-01-01-21-005 Dup 106% 12.2 

GLP10-01-01-21-005 Low LMS 104% 19.6 33.8 111% 

2.9% 

GLP10-01-01-21-005 High LMS 104% 198 227 108% [a]

GLP10-01-01-21-006 104% 

N/A 

23.5 

N/A 23.8 

GLP10-01-01-21-006 Dup 102% 24.1 

GLP10-01-01-21-006 Low LMS 106% 35.8 61.4 105% 

2.5% 

GLP10-01-01-21-006 High LMS 104% 380 418 104% 

N/A; not applicable 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.500 ng/g low standard. 

[a] LMS fortification level was greater than 10-times the endogenous analyte level. 

Table 16. Individual PFHS Results for Jeffries Property Sediments 

Sample Description 

Surrogate 

(

13C4-PFOS) 

Recovery 

LMS Spike 

Concentration 

(ng/g; dry 

weight) 

Measured PFHS 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

Average PFHS 

Concentration 

(ng/g; dry wt.) 

and RPD (%) 

GLP10-01-01-21-001 109% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-001 Dup 110% BLQ 

GLP10-01-01-21-001 LMS 105% 1.04 1.30 125% N/A 

GLP10-01-01-21-002 101% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-002 Dup 103% BLQ 

GLP10-01-01-21-002 Low LMS 102% 14.6 15.3 105% [a]

N/A 

GLP10-01-01-21-002 High LMS 104% 144 148 103% [a]

GLP10-01-01-21-003 106% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-003 Dup 110% BLQ 

GLP10-01-01-21-003 Low LMS 107% 15.1 15.4 102% [a]

N/A 

GLP10-01-01-21-003 High LMS 103% 151 158 105% [a]
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 21 of 24

Table 16. Individual PFHS Results for Jeffries Property Sediments 

Sample Description 

Surrogate 

(

13C4-PFOS) 

Recovery 

LMS Spike 

Concentration 

(ng/g; dry 

weight) 

Measured PFHS 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

Average PFHS 

Concentration 

(ng/g; dry wt.) 

and RPD (%) 

GLP10-01-01-26-004 106% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-26-004 Dup 104% BLQ 

GLP10-01-01-26-004 Low LMS 105% 16.7 16.7 100% [a]

N/A 

GLP10-01-01-26-004 High LMS 105% 153 157 103% [a]

GLP10-01-01-21-005 104% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-005 Dup 106% BLQ 

GLP10-01-01-21-005 Low LMS 104% 19.7 20.7 105% [a]

N/A 

GLP10-01-01-21-005 High LMS 104% 199 212 107% [a]

GLP10-01-01-21-006 104% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-006 Dup 102% BLQ 

GLP10-01-01-21-006 Low LMS 106% 36.0 38.7 108% [a]

N/A 

GLP10-01-01-21-006 High LMS 104% 382 371 97.0% [a]

N/A; not applicable 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.500 ng/g low standard. 

[a] LMS fortification level was too low relative to the endogenous analyte level to make an accurate determination of recovery.

Table 17. Individual PFBS Results for Jeffries Property Sediments 

Sample Description 

Surrogate 

(

13C4-PFOS) 

Recovery 

LMS Spike 

Concentration 

(ng/g; dry 

weight) 

Measured PFBS 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

Average PFBS 

Concentration 

(ng/g; dry wt.) 

and RPD (%) 

GLP10-01-01-21-001 109% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-001 Dup 110% BLQ 

GLP10-01-01-21-001 LMS 105% 1.04 1.09 105% N/A 

GLP10-01-01-21-002 101% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-002 Dup 103% BLQ 

GLP10-01-01-21-002 Low LMS 102% 14.6 16.6 114% [a]

N/A 

GLP10-01-01-21-002 High LMS 104% 144 148 103% [a]

GLP10-01-01-21-003 106% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-003 Dup 110% BLQ 

GLP10-01-01-21-003 Low LMS 107% 15.1 16.6 110% [a] N/A 
Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 22 of 24

Table 17. Individual PFBS Results for Jeffries Property Sediments 

Sample Description 

Surrogate 

(

13C4-PFOS) 

Recovery 

LMS Spike 

Concentration 

(ng/g; dry 

weight) 

Measured PFBS 

Concentration 

(ng/g; dry 

weight) 

LMS 

Recovery 

Average PFBS 

Concentration 

(ng/g; dry wt.) 

and RPD (%) 

GLP10-01-01-21-003 High LMS 103% 151 148 103% [a]

GLP10-01-01-26-004 106% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-26-004 Dup 104% BLQ 

GLP10-01-01-26-004 Low LMS 105% 16.7 17.4 105% [a]

N/A 

GLP10-01-01-26-004 High LMS 105% 153 150 98.5% [a]

GLP10-01-01-21-005 104% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-005 Dup 106% BLQ 

GLP10-01-01-21-005 Low LMS 104% 19.7 21.2 108% [a]

N/A 

GLP10-01-01-21-005 High LMS 104% 199 206 104% [a]

GLP10-01-01-21-006 104% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-006 Dup 102% BLQ 

GLP10-01-01-21-006 Low LMS 106% 36.0 41.4 115% [a]

N/A 

GLP10-01-01-21-006 High LMS 104% 382 384 101% [a]

N/A; not applicable 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.500 ng/g low standard. 

8 Conclusion 

Sediments collected from the Jeffries Property in March 2012 were successfully analyzed for PFOS, 

PFHS and PFBS following 3M Environmental Laboratory method ETS-8-053.0 and conducted as 3M 

study GLP10-01-02-25. The average PFOS, PFHS and PFBS concentration results for the soil 

samples are summarized in Table 1 and the LMS recoveries are summarized in Table 2. The 

individual analytical sample results are shown in Table 15, Table 16, and Table 17 for PFOS, PFHS 

and PFBS, respectively. The soil trip blank that accompanied the sample bottles to the site and then 

accompanied samples back to the laboratory was sufficiently devoid of PFOS, PFHS and PFBS, 

indicating that no contamination of the samples occurred during sample shipment or sample to the 

laboratory. The PFHS and PFBS levels in the samples were all less than the 0.5 ng/g calibration 

standard that defined the lower limit of quantitation. The PFOS concentrations in the sediment 

samples ranged from 3.95 ng/g to 23.8 ng/g. 

The data accuracy was within 100 + 30% and the data precision was excellent with RPDs less than 

10%. 

The analytical method uncertainties (95% CI) were determined by statistical examination of the LCS 

results for PFOS, PFHS and PFBS and were + 7.3% for PFOS, + 10% for PFHS and + 12% for 

PFBS, respectively, at the 95% confidence interval (95% CI).

Study: GLP10-01-02, Interim Report 25 

Analysis for PFOS, PFHS & PFBS in Sediments Collected from the Jeffries Property

Page 24 of 24

Attachment A 

Preparation Forms, Raw Data and Chromatograms