3 

GLP10-01-02 Interim Report 21: Analysis for PFOS, PFHS and PFBS in 

Decatur, AL Soils Collected from Well Location 610 in August, 2011

Study Title

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

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

GLP10-01-02-21 

Total Number of Pages 

23
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 2 of 23

This page has been reserved for specific country requirements. 
study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610 

GLP COMPLIANCE STATEMENT 

Report Title: GLP10-01-02 Interim Report 21: Analysis for PFOS, PFHS and PFBS in Soils 

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

Protocol GLP-10-01-02: 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. 

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: 

• The reference substances were not all characterized under GLPs. 

• Because these are environmental samples and the study analytical in nature only, there was 

no specific test substance or control substance for this study. 

Gary Hohenstein, Sponsor Representative 

Date 

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

Page 3 of 23 
study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610 

QUALITY ASSURANCE STATEMENT 

Report Title: GLP10-01-02 Interim Report 21: Analysis for PFOS, PFHS and PFBS in Soils 

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

Protocol GLP-10-01-02: 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. 

This interim analytical 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 

QAU Represerjfative Date 

Page 4 of 23 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 5 of 23

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 ....................................................................................................................................... 11

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

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

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

6.3 Sample Preparation .............................................................................................................. 11

6.4 Percent Soil Moisture Determination ................................................................................... 12

6.5 LC/MS/MS Analysis .............................................................................................................. 12

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

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

7.2 Limits of Quantitation (LOQs) .............................................................................................. 15

7.3 Continuing Calibration .......................................................................................................... 15

7.4 Blanks .................................................................................................................................... 15

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

7.6 Laboratory Matrix Spikes (LMSs) ........................................................................................ 17

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

7.8 Individual Sample Results .................................................................................................... 18
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

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8 Conclusion ......................................................................................................................................... 21

9 Data/Sample Retention ..................................................................................................................... 22

10 List of Attachments ............................................................................................................................ 22

11 Signatures .......................................................................................................................................... 22

LIST OF TABLES

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

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

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

Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053)..................................................... 13

Table 6. Mass Transitions ....................................................................................................................... 13

Table 7. PFOS Calibration Summary ..................................................................................................... 14

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

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

Table 10. LCS Results (PFOS, linear + branched isomer) ................................................................... 16

Table 11. LCS Results (PFHS, linear + branched isomer) ................................................................... 16

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

Table 13. Analytical Method Uncertainties ............................................................................................. 17

Table 14. Percent Moistures for Decatur, AL Soils from Well Location 610 ........................................ 18

Table 15. Individual PFOS Results for Decatur, AL Soils from Well Location 610 .............................. 18

Table 16. Individual PFHS Results for Decatur, AL Soils from Well Location 610 .............................. 19

Table 17. Individual PFBS Results for Decatur, AL Soils from Well Location 610 .............................. 20
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 7 of 23

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 analytical reference standard reserve 

samples are archived at the 3M Environmental Laboratory according to 40 CFR Part 79
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 8 of 23

2 Summary 

This interim report provides the PFOS, PFHS and PFBS concentration results for the four soils collected 

in August 2011 near well location 610, located 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 3M Environmental 

Laboratory information management system (LIMS) under project GLP10-01-01-21. Four aliquots of soil 

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

aliquot served as sample and duplicate sample. The third and fourth replicates were fortified with nominal 

5.00 and 50.0 ng of PFOS (linear isomer), PFHS (linear isomer) and PFBS as a low and high laboratory 

matrix spike (LMS), respectively. A single LMS for the trip blank was fortified with nominal 1.00 ng of 

PFOS (linear isomer), PFHS (linear isomer) and PFBS. 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 recovery results provided a measure of data accuracy. 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 

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. 

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

3M LIMS ID [d] Sample ID 

Analyte Concentration (ng/g; 

dry) 

PFOS PFHS PFBS 

GLP10-01-01-21-001 DAL-SB-610S-0-0000 36.1 0.586 0.991 

GLP10-01-01-21-002 DAL-SB-610S-0-0010 19.5 0.690 0.439 

GLP10-01-01-21-003 DAL-SB-610S-0-0040 3.00 1.11 0.572 

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

GLP10-01-01-21-005 TRIP BLANK-1 BLQ BLQ BLQ 

LMS results were within acceptance criteria of 100 + 30% 

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

RPD values were less than 50% for all duplicate sample results unless otherwise indicated 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.200 ng/g low standard 

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

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

PFOS PFHS PFBS 

GLP10-01-01-21-001 Low DAL-SB-610S-0-0000 Lab Matrix Spike Low [a] 91.3% 93.8% 

GLP10-01-01-21-001 High DAL-SB-610S-0-0000 Lab Matrix Spike High 97.8% 102% 109% 

GLP10-01-01-21-002 Low DAL-SB-610S-0-0010 Lab Matrix Spike Low [a] 103% 110% 

GLP10-01-01-21-002 High DAL-SB-610S-0-0010 Lab Matrix Spike High 93.0% 95.0% 101% 

GLP10-01-01-21-003 Low DAL-SB-610S-0-0040 Lab Matrix Spike Low 112% 103% 112% 

GLP10-01-01-21-003 High DAL-SB-610S-0-0040 Lab Matrix Spike High 111% 97.6% 109% 

GLP10-01-01-21-004 Low DAL-SB-610S-0-0150 Lab Matrix Spike Low 98.1% 92.3% 91.5% 

GLP10-01-01-21-004 High DAL-SB-610S-0-0150 Lab Matrix Spike High 87.4% 91.6% 100% 

GLP10-01-01-21-005 LMS Trip Blank-1 Lab Matrix Spike Low 97.4% 102% 115% 

LMSs were fortified with PFOS, PFHS and PFBS (linear isomers only) at nominal 5.0 ng (low) and 50.0 ng (high). 

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

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

[a] LMS fortification level was too low relative to the endogenous analyte level to make an accurate determination of recovery. 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 9 of 23

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 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 PFOS, PFHS and PFBS. 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 PFOS, PFHS and PFBS in the soil samples received. 

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

reported PFOS, PFHS and PFBS concentration results. 

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 -20 ̊C -20 ̊C -20 ̊C 

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% 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 10 of 23

Table 3. Reference Substances 

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 -20 ̊C -20 ̊C -20 ̊C 

Chemical Lot Number NB 120067-69 101 MPFOS0910 

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

Physical Description White Powder White Powder Methanol solution, sealed 

ampoule 

Purity 98.6% 96.7% >98% [a]

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 C4F9S18O216O 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 

Mixed IS methanol 

solution in sealed 

ampoule 

Mixed IS methanol solution 

in sealed ampoule 

Methanol solution, sealed 

ampoule 

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. 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 11 of 23

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 7, 2011 as 

analytical run s111007a. 

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. 

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 each stable isotope labeled internal standard (IS) was added to each soil aliquot. Internal 

standards 13C4-PFOS, 13C3-PFHS and 18O2-PFBS are described in Table 3. Each 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: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 12 of 23

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-PFOS. 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 15, Table 16 and 

Table 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 soil 

sample. Additionally, a third and fourth replicate was weighed out and used to prepare a low- LMS and 

high-LMS, fortified with PFOS (linear), PFHS (linear) and PFBS at nominal 5.0 ng and 50.0 ng each, 

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 PFOS (linear isomer), PFHS (linear 

isomer) and PFBS 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 3.0 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 

PFOS (mixed linear and branched isomer), technical PFHS (mixed linear and branched isomers) and 

PFBS. 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 PFOS, PFHS and PFBS analysis, and was determined by gravimetric analysis. 

Dry weights were determined for separate weighings than the 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. 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 PFOS, PFHS and 

PFBS concentration on a dry weight basis. 

6.5 LC/MS/MS Analysis 

The analysis of soil 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 Table 10, 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. 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 13 of 23

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 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 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 

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. 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 14 of 23

7 Analytical Results 

Concentration results 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 associated LMS results meeting the 

method acceptance criteria of 100 ± 30% demonstrated that the method was appropriate for those 

samples and were reported without footnotes in results tables. The nominal 5.00 ng and 50.0 ng 

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

for evaluating sample-specific analyte recoveries, with respect to the endogenous levels 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-842 (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

control soil TCR-842; equivalent to nominal 0.200 ng/g to 500 ng/g in soilTCR-842. 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 weights can vary significantly for a 1 cc (1 mL) field sample, depending on soil type 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 0.200 ng/mL to 500 ng/mL PFOS, 

PFHS and PFBS). Because a 1cc aliquot of control soil TCR-842 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 the sample soil aliquots typically weigh more than 

1.0 gram and contain significant moisture, the determined concentrations during the analysis on an 

ng/mL basis from the calibration curve were 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 0.200 0.500 0.750 1.00 2.50 5.00 10.0 25.0 50.0 100 200 500 N/A 

s111007a 0.202 0.482 0.725 1.09 2.45 4.91 9.56 24.7 53.8 101 195 502 0.9997 

Recovery 101% 96.4% 96.6% 109% 98.2% 98.2% 95.6% 98.8% 108% 101% 97.5% 100% N/A 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 15 of 23

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 0.234 0.491 0.746 0.96 2.37 4.84 9.9 24.6 49.8 99.9 202 499 1.000 

Recovery 117% 98.2% 99.4% 96.0% 95.0% 96.8% 99.0% 98.3% 99.6% 99.9% 101% 99.8% 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 0.199 0.47 0.802 0.989 2.41 5.00 9.96 26.1 50.3 102 195 502 0.9999 

Recovery 99.3% 94.1% 107% 98.9% 96.3% 99.9% 99.6% 105% 101% 102% 97.4% 100% N/A 

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 2X 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 0.200 ng calibration standard (nominal 

0.200 ng/g in soil TCR-842), and was the lowest prepared calibration standard. All sample analyte 

responses less than the response of the 0.200 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-842 and were spiked with IS and surrogate; travel blanks (trip blanks) prepared from 

aliquots of soil TCR-842 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) 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 16 of 23

7.5 Laboratory Control Spikes (LCSs) 

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

PFHS (linear + branched) into 1 cc aliquots of soil TCR-842, fortified with nominal 3.0 ng and 30 ng 

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

measurement accuracies (percent recovery) for PFOS and PFHS are shown in Table 10, Table 11 and 

Table 12 respectively. The analytical method uncertainty determined from LCS results is shown in 

Table 13. 

*100%

Spike Concentration

(Determine d Concentration of LCS) LCS Recovery =

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

Sample ID PFOS Recovery 

3.01 LCS 30.1 LCS 301 LCS 

LCSs (S111007a) 

126% 130% 128% 

125% 127% 134% [a]

139% [a] 118% 119% 

Average Recovery 130% 125% 127% 

Std Dev. 7.7% 6.4% 6.6% 

RSD 5.9% 5.1% 5.2% 

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. 

[a] LCS result was outside of 100 + 30%, but included in statistical calculations 

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

Sample ID PFHS Recovery 

3.00 LCS 30.0 LCS 300 LCS 

LCSs (S111007a) 

110% 103% 100% 

108% 106% 112% 

107% 104% 108% 

Average Recovery 108% 104% 107% 

Std Dev. 1.3% 1.3% 6.1% 

RSD 1.2% 1.3% 5.8% 

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. 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 17 of 23

Table 12. LCS Results (PFBS) 

Sample ID PFBS Recovery 

3.01LCS 30.1 LCS 301 LCS 

LCSs (S111007a) 

101% 97.3% 88.4% 

105% 102% 96.3% 

105% 96.0% 92.7% 

Average Recovery 103% 98.6% 92.5% 

Std Dev. 2.1% 3.3% 4.0% 

RSD 2.0% 3.4% 4.3% 

Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/g and 300 ng/g of PFBS, each prepared and analyzed in triplicate. 

Table 13. Analytical Method Uncertainties 

Sample ID LCS Results 

PFOS PFHS PFBS 

3.00 LCSs 

126% 110% 101% 

125% 108% 105% 

139% 107% 105% 

30.0 LCSs 

130% 103% 97.3% 

127% 106% 102% 

118% 104% 96.0% 

300 LCSs 

128% 100% 88.4% 

134% 112% 96.3% 

119% 108% 92.7% 

Average Recovery 127% 106% 98.2% 

Std Dev. 6.6% 3.6% 5.5% 

RSD 5.2% 3.4% 5.6% 

Method Uncertainty (2 x Std. Dev.); 95% CI 13% 7.3% 11% 

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

branched isomers) and PFBS; each LCS level was prepared and analyzed in triplicate. 

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 soil sample, and then preparing the sample the same as non-spiked 

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 PFOS, PFHS and PFBS 

recovery calculations for LMSs used the following equation: 

*100%

Spike Concentrat ion

(Determine d Concentrat ion of LMS Determined Concentrat ion of Field Sample) LMS Recovery −

=
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 18 of 23

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%

Original Soil Wet Mass

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

= 

Table 14. 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 results for PFOS, PFHS and PFBS are shown in Table 15, Table 16 and 

Table 17, respectively. 

Table 15. Individual PFOS Results for Decatur, AL Soils from Well Location 610 

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 (%) 

GLP10-01-01-21-001 108% 

N/A 

29.8 

N/A 36.1 

GLP10-01-01-21-001 Dup 105% 42.5 

GLP10-01-01-21-001 Low LMS 110% 5.58 43.7 137% [a]

35% 

GLP10-01-01-21-001 High LMS 102% 57.5 92.4 97.8% 

GLP10-01-01-21-002 114% 

N/A 

21.1 

N/A 19.5 

GLP10-01-01-21-002 Dup 106% 17.9 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 19 of 23

Table 15. Individual PFOS Results for Decatur, AL Soils from Well Location 610 

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 (%) 

GLP10-01-01-21-002 Low LMS 103% 5.06 30.9 226% [a]

17% 

GLP10-01-01-21-002 High LMS 101% 48.5 64.6 93.0% 

GLP10-01-01-21-003 100% 

N/A 

2.94 

N/A 3.00 

GLP10-01-01-21-003 Dup 102% 3.05 

GLP10-01-01-21-003 Low LMS 108% 5.07 8.66 112% 

3.7% 

GLP10-01-01-21-003 High LMS 120% 55.2 64.1 111% 

GLP10-01-01-21-004 107% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-004 Dup 116% BLQ 

GLP10-01-01-21-004 Low LMS 118% 4.66 4.58 98.1% 

N/A 

GLP10-01-01-21-004 High LMS 94% 59.7 52.2 87.4% 

GLP10-01-01-21-005 108% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-005 Dup 107% BLQ 

GLP10-01-01-21-005 LMS 105% 0.990 0.965 97.4% N/A 

N/A; not applicable 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.200 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 16. Individual PFHS Results for Decatur, AL Soils from Well Location 610 

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 (%) 

GLP10-01-01-21-001 108% 

N/A 

0.449 

N/A 0.586 

GLP10-01-01-21-001 Dup 105% 0.723 

GLP10-01-01-21-001 Low LMS 110% 5.58 5.68 91.3% 

47% 

GLP10-01-01-21-001 High LMS 102% 57.5 59.3 102% 

GLP10-01-01-21-002 114% 

N/A 

0.720 

N/A 0.690 

GLP10-01-01-21-002 Dup 106% 0.660 

GLP10-01-01-21-002 Low LMS 103% 5.06 5.87 103% 

8.7% 

GLP10-01-01-21-002 High LMS 101% 48.5 46.8 95.0% 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 20 of 23

Table 16. Individual PFHS Results for Decatur, AL Soils from Well Location 610 

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 (%) 

GLP10-01-01-21-003 100% 

N/A 

1.070 

N/A 1.11 

GLP10-01-01-21-003 Dup 102% 1.152 

GLP10-01-01-21-003 Low LMS 108% 5.07 6.33 103% 

7.3% 

GLP10-01-01-21-003 High LMS 120% 55.2 54.9 97.6% 

GLP10-01-01-21-004 107% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-004 Dup 116% BLQ 

GLP10-01-01-21-004 Low LMS 118% 4.66 4.31 92.3% 

N/A 

GLP10-01-01-21-004 High LMS 94% 59.7 54.7 91.6% 

GLP10-01-01-21-005 108% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-005 Dup 107% BLQ 

GLP10-01-01-21-005 LMS 105% 0.990 1.01 102% N/A 

N/A; not applicable 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.200 ng/g low standard. 

Table 17. Individual PFBS Results for Decatur, AL Soils from Well Location 610 

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 (%) 

GLP10-01-01-21-001 108% 

N/A 

0.804 

N/A 0.991 

GLP10-01-01-21-001 Dup 105% 1.18 

GLP10-01-01-21-001 Low LMS 110% 5.58 6.23 93.8% 

38% 

GLP10-01-01-21-001 High LMS 102% 57.5 63.7 109% 

GLP10-01-01-21-002 114% 

N/A 

0.470 

N/A 0.439 

GLP10-01-01-21-002 Dup 106% 0.408 

GLP10-01-01-21-002 Low LMS 103% 5.06 6.02 110% 

14% 

GLP10-01-01-21-002 High LMS 101% 48.5 49.7 101% 

GLP10-01-01-21-003 100% 

N/A 

0.609 

N/A 0.572 

GLP10-01-01-21-003 Dup 102% 0.536 

GLP10-01-01-21-003 Low LMS 108% 5.07 6.24 112% 13% 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 21 of 23

Table 17. Individual PFBS Results for Decatur, AL Soils from Well Location 610 

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 120% 55.2 60.8 109% 

GLP10-01-01-21-004 107% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-004 Dup 116% BLQ 

GLP10-01-01-21-004 Low LMS 118% 4.66 4.27 91.5% 

N/A 

GLP10-01-01-21-004 High LMS 94% 59.7 59.5 100% 

GLP10-01-01-21-005 108% 

N/A 

BLQ 

N/A BLQ 

GLP10-01-01-21-005 Dup 107% BLQ 

GLP10-01-01-21-005 LMS 105% 0.990 1.14 115% N/A 

N/A; not applicable 

BLQ; analyte response was lower than the analyte response of the LLOQ which was nominal 0.200 ng/g low standard. 

8 Conclusion 

Soils collected from near groundwater well location 610 in August 2011 were successfully analyzed 

for PFOS, PFHS and PFBS following 3M Environmental Laboratory method ETS-8-053.0 and 

conducted as 3M study GLP10-01-02-21. 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 to the 

laboratory. 

The accuracy of the results based on LMS recoveries were within acceptance criteria of 100 + 30%; 

when the appropriate level of fortified LMS was evaluated relative the endogenous analyte level 

measured. 

The analytical method uncertainties were determined by statistical examination of the LCS results for 

PFOS, PFHS and PFBS and were determined to be + 13% for PFOS, + 7.3% for PFHS and + 11% 

for PFBS, respectively; determined at the 95% confidence interval (CI).
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610 

9 Data/Sample Retention 

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

01-02-21 according to 3M Environmental Laboratory standard operating procedures. 

10 List of Attachments 

Attachment A: Preparation Forms, Raw Data and Chromatograms 

i ll Signatures 

Report Approval: 

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

/fJi^de//A^ 

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

2-

Gary A. Hohenstein, Sponsor Representative Date 

Jaisimha Kesari, Study Director Dife 

Page 22 of 23 
Study: GLP10-01-02, Interim Report 21 

Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 23 of 23

Attachment A 

Preparation Forms, Raw Data and Chromatograms