Perfluorooctanoic Acid (PFOA) 

Site Related Environmental 

Assessment Program

3M and Dyneon LLC

Decatur, Alabama 

Quarterly Status Report 

January 1, 2011 to March 31, 2011

11P-0094-v1-1

3M Company

St. Paul, Minnesota

®
Perfluorooctanoic Acid (PFOA) Site Related

Environmental Assessment Program

3M Decatur, Alabama Site

Quarterly Status Report

January 1, 2011 to March 31, 2011 

Prepared for

3M Company and Dyneon LLC

By

WESTON SOLUTIONS, INC.

West Chester, Pennsylvania 19380

W.O. No. 02181.129.118.0001 
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i 

TABLE OF CONTENTS

Section Page 

1. BACKGROUND ............................................................................................................ 1-1

2. SUMMARY OF ACTIVITIES ..................................................................................... 2-1

ATTACHMENTS

Attachment Title

1 GROUNDWATER SAMPLING TECHNICAL PROGRESS REPORT 

2 SOIL AND SEDIMENT SAMPLING TECHNICAL PROGRESS 

REPORT
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1-1 

1. BACKGROUND

In accordance with the Phase 3 Work Plan for Sampling Environmental Media

(WESTON, 2009) and the Memorandum of Understanding (MOU) (3M, 2004) with 

EPA, 3M and Dyneon LLC are undertaking a Perfluorooctanoic Acid (PFOA) SiteRelated Environmental Monitoring and Assessment Program at their Decatur, Alabama, 

plant. Per the agreement between EPA and 3M, this report represents the status report of 

this effort as required by the MOU for the January 1, 2011 through March 31, 2011 time 

period. For brevity, and following previous convention, this report will be referred to as 

the March 31, 2011 Quarterly Status Report. 
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2-1 

2. SUMMARY OF ACTIVITIES 

The Phase 2 Work Plan and MOU were finalized on October 25, 2004. Phase 2 of the 

monitoring program has been completed and Phase 3 commenced on November 19, 2009 

with EPA’s acceptance of the Phase 3 Work Plan. This report represents the fifth

quarterly status report under Phase 3. It covers the January 1, 2011 to March 31, 2011 

timeframe and includes a description of activities completed under the Phase 3 Work 

Plan. In addition to Phase 3 MOU activities, 3M is performing other non-MOU studies 

related to PFOA to provide data for itself, the Alabama Department of Environmental 

Management (ADEM) and/or EPA Region 4. Where relevant, non-MOU data may be 

incorporated in the revised Screening Level Human Exposure Assessment. This nonMOU information will also be described and provided in these quarterly status reports. 

Details on activities completed during this reporting period are as follows: 

Groundwater Technical Progress

• Off-site well construction – Arrangements for access to the remaining 

groundwater monitoring locations for well construction are ongoing. It is 

anticipated that the agreements will be finalized in the second quarter of 2011. 

• Off-site groundwater sampling at the BFI Morris Farms Landfill – Groundwater 

samples were collected from 14 active monitoring wells at the BFI Morris Farms

Landfill on March 21 through 23, 2011 for PFOA analysis. Detailed descriptions 

of the activities associated with the sampling activities are provided in the 

Groundwater Sampling Technical Progress Report (Attachment 1). 

• On-site groundwater – Analyses of PFOA in routine groundwater monitoring 

samples collected in November 2010 from wells in the Former Sludge 

Incorporation Area have been completed. Analytical results are summarized in the 

Groundwater Sampling Technical Progress Report (Attachment 1). 

Groundwater sampling was performed during the weeks of March 21 and 28, 

2011 at 17 locations in the chemical plant area and northeast of the closed landfill 

at the Decatur site as part of routine quarterly monitoring for conventional 

constituents. This effort included the collection of samples for PFOA analysis. 

The routine groundwater monitoring locations included 16 individual wells and 

the combined groundwater discharge from maintenance pumping wells at the 
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2-2 

closed landfill prior to treatment at the on-site groundwater treatment plant. The 

routine on-site groundwater monitoring is not a MOU-related activity. Analytical 

results for PFOA will be provided in a subsequent quarterly status report. 

• On-site Avenue A area groundwater – On January 27, 2011, two on-site 

temporary wells were installed in the Avenue A drainage ditch area. These 

temporary wells were installed to obtain additional data for the Remedial Action 

Agreement Program being undertaken by 3M under the ADEM NPDES program. 

This is not part of the MOU activities. Groundwater sampling was performed on 

January 27 and 28, 2011 at the two temporary wells and at one permanent well 

(210R). When finalized, PFOA analytical results will be provided in a subsequent 

quarterly status report. Detailed descriptions of the activities associated with the 

additional Avenue A sampling activities are provided in the Groundwater 

Sampling Technical Progress Report (Attachment 1) and the Soil and Sediment 

Technical Progress Report (Attachment 2).

Soil and Sediment Technical Progress

• On-site Avenue A area sediment and soil – Between January 26 and 28, 2011, 

samples of sediments, surface and subsurface soils were collected at additional 

locations within the Avenue A area to obtain data for the Remedial Action 

Agreement Program being undertaken by 3M under the ADEM NPDES program. 

This was not a MOU-related activity. When finalized, PFOA analytical results 

will be provided in a subsequent quarterly status report. Detailed descriptions of 

the activities associated with the additional Avenue A sampling activities are 

provided in the Soil and Sediment Technical Progress Report (Attachment 2). 

Phase 3 Status Meeting and Technical Consultation

• Phase 3 Status – 3M provided a summary of the status of Phase 3 investigations in 

a presentation to EPA on March 28, 2011. The briefing included the display and 

discussion of PFOA analytical results from on-site and off-site Phase 3 sample 

collection and from on-site non-MOU related sampling activities.

• Vegetative Uptake Study – Based on review of the Phase 3 off-site soil PFOA 

concentrations from sampling of surface soils at ten locations within 

approximately 3 miles of the Decatur facility and surface soils from the new 

Phase 3 off-site well borings, a maximum concentration of 8 ng/g was established 

for the vegetative uptake study. The test species of tomato, turnip greens and 

potato were selected on the basis of the home gardening survey conducted in the 

Decatur Area of the most commonly grown produce in the fruiting vegetable, 

leafy vegetable and root vegetable categories.
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Expanded summaries of these activities, where applicable, are included as attachments to 

this status report and provide additional details on the work which has been completed. 

For utility and clarity of communication, each attachment has been constructed as a 

separate report on a different media and/or study area. 
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ATTACHMENT 1

GROUNDWATER SAMPLING 

TECHNICAL PROGRESS REPORT 

JANUARY 1, 2011 – MARCH 31, 2011
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Att 1-1 

GROUNDWATER

TECHNICAL PROGRESS REPORT

3M AND DYNEON DECATUR, ALABAMA

The following subsections describe groundwater sampling activities completed during the 

first quarter of 2011 and summarize the results of analyses for PFOA. Analytical data 

packages for Interim Report 11 are provided in Appendix A. Full analytical data 

packages including raw data, chromatograms and correspondence are provided in the 

Raw Data Appendix to this quarterly status report.

OFF-SITE ACTIVITIES

BFI Morris Farms Landfill Groundwater Sampling

Groundwater samples were collected from 14 existing monitoring wells at the BFI Morris 

Farms Landfill between March 21 and 23, 2011 (Figure 1). The sampling was conducted 

to evaluate the potential presence of PFOA in the local groundwater system. Wells were 

selected based on a review of previous groundwater monitoring data for the facility to 

provide an upgradient control and suitable downgradient coverage of the primary waste 

disposal areas. 

Wells at the facility are constructed in clusters to monitor different depths within the 

groundwater system. The BFI Morris Farms Landfill well nomenclature differs from that 

established for the 3M facility in that identification of the groundwater zone monitored is

no suffix in the well ID for shallow (residuum) groundwater and the suffix “D” for

deeper bedrock groundwater.

Groundwater samples were collected by WESTON after completion of a routine 

quarterly groundwater monitoring event conducted by Analytical Services, Inc. (ASI) on 

behalf of Republic Services, Inc., the owner / operator of Morris Farms Landfill. ASI

purged the monitoring wells and collected the facility samples prior to WESTON’s 

sampling for PFOA analysis. 

Existing monitoring wells at the Morris Farms Landfill are constructed as 4-inch wells 

with dedicated Grundfos pumps. As a standard practice, the wells are purged and 
J:\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\1Q11 Status Report\1Q11 Status Report FINAL.doc 4/28/2011

Att 1-2 

sampled by ASI through the pumps. According to ASI, the pumps are assembled with 

Teflon tubing to the surface. Due to the presence of the Teflon tubing and Teflon seals in 

the pumps, sampling for PFOA was performed with disposable polyethylene bailers. All 

of the wells were purged by ASI using the dedicated Grundfos pumps with the exception 

of MW-02, which, due to low yield and high turbidity, was purged using a peristaltic

pump and low-flow purging techniques. To ensure consistency with the Phase 2 and 

Phase 3 sampling procedures, the MW-02 well was purged to dryness using the dedicated 

pump following completion of the ASI sampling. The well was then allowed to recharge 

approximately 12 hours before sampling for PFOA occurred.

The groundwater was poured from the disposable polyethylene bailers into laboratoryprepared containers, labeled, and placed into an ice chest for shipment to the laboratory. 

The sample information was also recorded onto a Chain of Custody which accompanied 

the samples to the laboratory. One rinseate blank was obtained from the disposable bailer 

prior to use in sampling MW-01. A trip blank was also prepared and accompanied the 

sample containers throughout the sampling process. The samples were packed and 

shipped to the 3M Environmental Laboratory in St. Paul, MN for PFOA analysis. When 

complete, analytical results will be provided in a subsequent quarterly status report. 

ON-SITE ACTIVITIES

Former Sludge Incorporation Area Monitoring Wells

3M implemented a groundwater monitoring program as part of the Former Sludge 

Incorporation Area (FSIA) capping program to establish current conditions at the site and 

to provide adequate coverage for continued monitoring. This is not a MOU-related 

activity but is being undertaken by 3M under a NPDES Remedial Action Agreement with 

ADEM. The current FSIA groundwater program includes 29 existing monitoring wells 

and five wells (140R, 141R, 142R, 143R and 144S) recently constructed to enhance 

monitoring coverage. The November 2010 sampling of the FSIA wells was described in 

the December 31, 2010 Quarterly Status Report. Analyses of PFOA in groundwater 

samples have been completed and the results are summarized in Table 1 and shown in 

Figure 2. A copy of the final analytical data package, Interim Report 11, is provided in 
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Att 1-3 

Appendix A and the full analytical data package including raw data, chromatograms and 

correspondence are provided in the Raw Data Appendix to this quarterly status report. 

On-site Chemical Plant and Closed Landfill Groundwater Results

Groundwater sampling was performed during the weeks of March 21 and 28, 2011 at 17 

locations in the chemical plant area and northeast of the closed landfill at the Decatur site 

as part of routine quarterly monitoring. Monitoring locations included 16 individual wells 

and the combined groundwater discharge from the maintenance pumping wells at the 

closed landfill prior to treatment at the on-site groundwater treatment plant. The wells 

sampled included 203L, 220R, 220L, 222R, 227R, 227L, 310R, RW312R, 317L, 324L, 

RW327R, 328R, 328L, 330R, 330L, RW331S and the combined groundwater treatment 

plant landfill extraction wells sample GRS04. This was not a MOU-related activity. Once 

finalized, PFOA analytical results will be provided in a subsequent quarterly status report. 

On-site Avenue A Area Groundwater and Surface Water

Groundwater sampling was performed at the two temporary wells and at one permanent 

well (210R) at locations throughout the Avenue A drainage ditch area on January 27, 

2011 for PFOA analysis. The Avenue A assessment is intended to obtain additional data 

for the NPDES Remedial Action Agreement being undertaken by 3M for the ADEM 

NPDES program and is not an MOU-related activity. 

Monitoring locations included two samples collected from soil sampling locations in the 

marsh area, west of the inactive landfill, and one sample was collected from monitoring 

well 210R, located southwest of the fire training area. The well locations are identified on 

Figure 3. 

Prior to sampling at the marsh locations, the soil borings were advanced to 

approximately 4 feet below ground surface and a temporary five foot screen was inserted 

to facilitate groundwater sample collection. After these locations stabilized, depth to 

water measurements were recorded at 10 inches below grade and 6 inches below grade 

for location S22 and S24, respectively. Additional information regarding the soil 
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Att 1-4 

sampling locations is provided in Attachment 2. The depth to groundwater was measured 

at 3.65 feet below ground surface in monitoring well 210R. This well was sampled on 

January 28, 2011 in accordance with standard monitoring well sampling procedures. 

All groundwater samples for PFOA analysis were collected using disposable 

polyethylene bailers. Appropriate volumes of groundwater were placed into laboratoryprepared containers which were sealed, labeled, and placed into an ice chest along with 

completed chain-of-custody forms for shipment to the 3M Environmental Laboratory in 

Maplewood, MN. Once finalized, PFOA analytical results will be provided in a 

subsequent quarterly status report.

GROUNDWATER ELEVATIONS – NOVEMBER 2010

Groundwater elevation data collected from various on-site and off-site groundwater 

collection activities conducted in November 2010 were compiled to produce groundwater 

elevation contours. Residuum groundwater elevation contours are shown in Figure 4 and 

bedrock groundwater elevation contours are shown in Figure 5. 

&<

&<

&< &<

&<

&<

&<

MW-01

MW-02

MW-03

MW-13 MW-04

MW-05

MW-10

&<

&<

&< &<

&<

&<

&<

MW-01

MW-02

MW-03

MW-13 MW-04

MW-05

MW-10

Figure 1

BFI Morris Farms Landfill 

Groundwater Sampling μ Decatur, AL

File: \\fsfed01\tig\3MDec\MXD\BFI_Morris_Farm_landfill.mxd, 20-Apr-11 16:42, ricksc

Imagery Source:

ESRI, i-cubed, USDA FSA, USGS, AEX, 

GeoEye, Getmapping, Aerogrid, IGP. 2010

Legend 0 375 750 Feet

&< Monitoring Well Locations (Clusters)
..!!

.!..!!

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!!

..!!!.

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.!

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Field 12

Field 13

Finley Island Road

Field 9

State Docks Road

Field 10

Field 11

Field 5

Nebo Road

Highway 20/72

Field 14

Field 8c

500-gal No. 2 

Fuel Oil AST

207L

217D

217R

217S

Norfolk Southern Railroad

Field 8b

138-R

134S

136S

130S

133L

132S

131R

137S

135-R

140R

141R

144R

142R

CW26

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Field 12

Field 13

Finley Island Road

Field 9

State Docks Road

Field 10

Field 11

Field 5

Nebo Road

Highway 20/72

Field 14

Field 8c

500-gal No. 2 

Fuel Oil AST

207L

217D

217R

217S

Norfolk Southern Railroad

Field 8b

138-R

134S

136S

130S

133L

132S

131R

137S

135-R

140R

141R

144R

142R

CW26

Figure 2

Former Sludge Incorporation Area 

Groundwater PFOA Sampling

November 2010

Decatur, AL

File: \\fsfed01\tig\3MDec\MXD\FSIAGW_gw_PFOA_nov2010.mxd, 22-Apr-11 15:43, ricksc

Notes:

-Average PFOA is the average of primary and 

 duplicate sample analytical results in ng/mL (ppb).

-[a] Sampling location did not have an 

 appropriate FMS spike level to sufficiently 

 evaluate PFOA recovery.

-[b] The analytical uncertainty has been 

 adjusted for field matrix spike recovery to ± 31%

Legend:

Groundwater 

Sampling Location .!

Daikin Property

Note:

R - Residuum Well

S - Epikarst Well

L - Bedrock Well μ 800 400 Feet 0

130R 793

130S 174

130L 70.0

131R 2500[a]

131S 24.9

131L 90.7

132R 251

132S 962

132L 404

133R 102

133S 385

133L 252

134R 1570[b]

134S 5.49

134L 520

135R 2910[a]

135S 13.7

135L 123

136S 75.4

136L 75.3

137S 0.271

137L 0.361

138S 147

138L 1.16

CW26R 386

CW26L 552

140R 121

141R 1.84

142R 47.6

144R 57.3
"/

"/

&<

Tennessee River

Finley Island Road

State Docks Road

SS22

SS24

210R

0

μ250 500Feet

3M Decatur, AL Facility

Figure 3

Additional Avenue A

Groundwater Sampling

January 2011

File: \\fsfed01\tig\3MDec\MXD\Additional_AvenueA_gw_Jan2011.mxd, 21-Apr-11 15:41, ricksc

Imagery Source:

ESRI, i-cubed, USDA FSA, USGS, AEX, 

GeoEye, Getmapping, Aerogrid, IGP. 2010

Legend

&< Monitoring Well

"/ Temporary Well
&<

&<

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Wheeler Reservoir

Morgan County Landfill

Bakers

Creek

330R

556.25

510R

560.72

204L

579.58 212R

578.65

227R

228R 560.04

578.73

138-R

587.32

602-R

569.47

603R

560.2

604R

558.1

605-R

130R

584.95

131R

600.38

132R

608.96

133R

614.05

134R

594.69

135R

575.12

136R

567.87

MW-1

571.42

MW-3

573.87

MW-4

568.13

MW-13

633.04

140R

599.14 141R

142R

555.51

143R

555.53

144R

590.08

611R

564.45

609R

572.89

607R

594.11

590

580

570

562

575

566

560

600

590

585

580

556

590

610 600

588

630

620

562

560

559 558

558

0

μ

1,250 2,500

Feet

Legend:

Monitoring Well Location with 

Groundwater Elevation

(feet above mean sea level).

3M Decatur, AL Facility

Figure 4

Residuum Groundwater

Elevation Contour Map

November 2010

File: \\fsfed01\tig\3MDec\MXD\residuum_gw_elev_1110.mxd, 21-Apr-11 17:02, ricksc

Groundwater Elevation Contour 

(feet above mean sea level)

Imagery Source: ESRI Bing 

Mapping Service 2010

Note: Water levels were recorded

in November 2010

100

Facility Boundary

&<

604R

558.1
&<

&<

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&<

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Wheeler Reservoir

Morgan County Landfill

Bakers

Creek

137

555.33

607

557.11

609

577.08

611

573.1

MW-4

565.15

MW-1

574.12

136

563.76

135

556.69

134

564.31

133

588.66

132

567.54

131

592.13

130

552.15

MW-13

583.27

605

561.74

604

557.1 603

558.22

602

556.16 138

562.49

MW-2

565.21

MW-3

569.08

212

579.66

228

578.88

227

559.45

206L

579.6

204

560.65

510

562.24

330

557.78

566

560

564

570

568 574

558

580

556

554

590 570

568

566

556

568

564

560

570

558

556

0

μ

1,250 2,500Feet

Legend:

Monitoring Well Location with 

Groundwater Elevation

(feet above mean sea level).

3M Decatur, AL Facility

Figure 5

Bedrock Groundwater

Elevation Contour Map

November 2010

File: \\fsfed01\tig\3MDec\MXD\Bedrock.gw_elev_1110.mxd, 21-Apr-11 17:04, ricksc

Groundwater Elevation Contour 

(feet above mean sea level)

Imagery Source: ESRI Bing 

Mapping Service 2010

Note: Water levels were recorded

in November 2010

100

Facility Boundary

&<

604R

558.1
J:\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\1Q11 Status Report\1Q11 Status Report FINAL.doc 4/28/2011

APPENDIX A TO ATTACHMENT 1

GLP10-01-01 INTERIM REPORT 11

The full data package, including raw data, is provided in the Raw Data Appendix. 
Analysis of Perfiuorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3

Site-Related Monitoring Program

Data Requirement

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792

Study Director

Jasimha Kesari RE, DEE

Weston Solutions, Inc.

1400 Weston Way

West Chester, PA 19380

Phone: 610-7014761

Author

Susan Wolf

3M Environmental Laboratory

Interim Report Completion Date

Date of signing

Performing Laboratory

3M Envfronmentai Health and Safety Operations

Enwonmental Laboratory

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

Maplewood, MN 55144

Project Identification

GLP1O-01-01-1 1

Total Number of Pages

53

The testing reported hereis meet the requirements of ISOAEC 17025-2005 Oenera1

Requirements for the Competence of Testing and Calibration Laboratories”, in accordance with

the A2LA Certlilcata #2052.01. Testing that compiles with this International Standard also

operate in accordance with ISO 9001 :2000.

Certificate #2052.01
Page 2 of 53
g 

g

This analytical phase was conducted in compliance with Toxic Substances Control Act (TSCA) Good Laboratory Practice (Gil’) Standards, 40 CFR 792, with the exceptions listed below:

• These are environmental samples where there is no specific test substance, no specific test

system and no dosing of a test system.

• The reference substances have not been characterized under the GLPs and the stability under

storage conditions at the test site have not been determined under GLPs.

Jaisimha Kesan, RE., DEE, Study Director Date

Page 3 of 53
g 

g

This report and the accompanying data were audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), as indicated below. The findings were reported to the principal investigator (P1), laboratory management and study director.

Date Renorted to

Inspection Dates Phase Testing Facility Diter Management

12/3C10 In-Phase 2)4111 2)4/11

1127/11—1/28111 Data!lnterimReport 214/11 2/4/11

QAU

cd

Repres1tative Date

Page 4 of 53
Table of Contents 5

List of Tables 6

1 Study Information 8

2 Summary 9

3 Introduction

... 10

4 Test & Control Substances 11

5 Reference Substances 11

6 Test System 12

7 Method Summary 12

7.1 Methods 12

7.2 Sample Collection 12

7,3 Sample Preparation 12

7.4 Analysis 12

8 Analytical Results 13

8.1 Calibration 13

8.2 System Suitability 14

8.3 Lwnit of Quantitation (LOQ) 148.4 Continuing Calibration 14

8.5 Blanks 14

8.6 Lab Control Spikes (LCSS) 14

8.7 Analytical Method Uncertainty 16

8.8 Field Matrix Spikes (FMS) 16

Page 5 of 53
13 Signatures 31

LIST OF TABLES

Table 1. Summanzed PFOA Results (FSIA Groundwater, Decatur, AL. November2010) 10

Table 2. Instrument Parameters 13

Table 3. Liquid Chromatography Conditions 13

Table 4. Mass Transitions 13

Table 5. Limit of Quantitation (LOQ) 14

Table 6. Laboratory Control Spike Recovery 15

Table 7. Analytical Method Uncertainty 16

Table 8. Field Matrix Spike Levels 16

Table9. DALGW13OR 101105 18

Table 10. DALGW13OS 101105 18

Table 11. DAL GW13OL 101105 18

Table 12. DALGW131R 101103 19

Tablel3. DALGWI31S 101103 19

Table 14. DALGW131L 101103 19

TablelS. DALGWI32R 101102 20

TablelG. DALGWI32S 101102 20

Table 17. DAL GW 1321 101103 20

Tablel8.DALGWI33R1OIIO2 21

Tablel9. DALGWI33S1OIIO3 21

Table2O. DALGW133L1O11O3 21

Page 6 of 53
Table25. DALGW135S 101105 23

Table26. DALGW135L1O11O5

Table27.DALGW136S1O1IO3 24

Table 28. DAL GW 13&. 101103 24

Table29.DALGWI37SIOI1O9 24

Table 30. DAL GW137L 101109 25

Table 31. DALGW138S 101110 25

Table32. DALGW138L1OI1IO 25

Table33. DALGWCW26R 101110 26

Table 34. DALGWGW26L 101110 26

Table 35, DALGWI4OR 101104 26

Table 36. DALGW14IR 101110 27

TabIe37, DALGW142R 101110 27

Table 38. DALGW144R 101110 27

Table39. TripBlankl 28

TabIe4O. Trip Blartk2 28

Table4t Trip Blank 3 28

Table 42. Trip Blank 4 29

Table 43. Rinseate Blanks 29

Page? of 53
Sponsor Representative

Gary Hohenstern

3M EHS Operations

3M Building 224-5W-03

Saint Paul, MN 55144-1000

Phone: (651) 737-3570

Study Director

Jaisimha Kesari, P.E., DEE

Weston Solutions, Inc.

West Chester, PA 19380

Phone: (610) 701-3761

Fax: (610) 701-7401

j.kesari@westonsolutions.com

Study Location

Testing Facility

3M EHS Operations3M Environmental Laboratory

Building 260-5N-17

Maplewood, MN 55106

Study Personnel

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

Cleston Lange, Ph.D., Principal Analytical Investigator. (clangemmm.com); phone (851 )-733-9860 Susan Wolf 3M Analyst

Kevin Eich: Analyst

Chelsie Grochow, Analyst

Jonathan Steege; Analyst

Study Dates

Study Initiation: March 8, 2010

Interim Report 11 Experimental Termination: January 8, 2011

Interim Report Completion: Date of Interim Report Signing

Location of Archives

All original raw data and the analytical report have been archived at the 3M Environmental

Laboratory according to 40 CFR Part 792. The test substance and analytical reference standard

reserve samples are archived at the 3M Environmental Laboratory according to 40 CFR Part 792

Page 8 of 53
location, Samples also included at least two field matrix spike (FMS) samptes for each location, four

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

nnseates. In addition, one soil equqnlent rinseate blank from GLPIO-01-01-12 was an&yzed. The

equipment nnseate blanks did not have FMS samples prepared for determination of PFOA recovery.The groundwater samples, trip blanks arid two equipment nnseate blanks associated with GLPI 0-01 -

01-10 were received from Weston personnel on November18, 2010. The equipment nnseate blank

associated with GLP1O-01-01-12 was received from Weston personnel on October15, 2010. All of the

samples were prepared and analyzed for PFOA following 3M Environmental Laboratory Method ETS8-044.0 under 3M project CLP-10-01-01-1 1. Many of the groundwater samples required dilution to

attain PFOA concentrations within the range of the curve, in some instances up to 100-fold dilution

were required. The average measured PFOA concentrations are surriahzed in Table 1. The

equipment rinseates and the trip blank were below the lower limit of quantitation (LLOQ) of 0.0250

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

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

ngfmL to 2910 nglmL The a,alytkal uncertainty was estimated at 100 ± 23%.

Page 9of53
DALGW 130L 101106 70.0 2.0%

DALGW 131R 101103 22.11_.__. - 1.6% DALGW 131S 101103 24.9 4.0%

DALGW131L1O11O3 90.7 52%

DALGW 132R 101102 251 4.4%

DALGW 132S 101102 962 0.52%DALGW 132L 101103 404 3.0%

DALGW133R 101102 102 9.5%

DALOW 133S 101103 385 4.2%

DALGW 133L 101103 252 1DALGW134R 101105 15701b] 9.6%

DALGW 1345 101105 5.49 5.5%

DALGWI34LIO1IO5 520 1,3%

DALGW135R1O11O5 1.4%

DAL GW 135S 101105 13.7 3.7%DALGW135LIO11O5 123 2.4%

DALGW 1365 101103 75.4 3.8%

DALGW136L1O11O3 75.3 3.1%

OALGW 137S 101109 0.271 1.8%

OALGW 1371 101109 0,361 0.28%

DALGWI38S1O1I1O 147 3.4%

DALGW138LIOI1IO 1.16 6.1%

DALGWCW2BR 101110 386 1.8%DALGWCW26L 101110 552 4.7%

DALGW14OR1OI1O4 121 0.83%

DALGW141R1OI1IO 1,84 10%

DALGW 142R 101110 47.6 4.6%

DAL GW 144R 101110 57.3 0.17%

,lanks(Milli-Q Water) < 0.0250 N/A

GLP1O-01-01-1 1 Equipment rinseate blanks:

DALGW13OLartdDALGWI44R <0 0250 N/A

GLPIO-01-O1-12 Soil Equipment rinseate blank:

< 0 0250 N/A DAL SS 607R

N/A; not apphcable

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

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

PFQA recovery.

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

3 Introduction

This analytical study was conducted as part of the Phase 3 Environmental Monitoring and Assessment

Program for the 3M facility located in Decatur, Alabama. The objective of the overall program is to gain

information regarding concentrations of pertluorooctanoate (PFOA) in various environmental media

Page 10 of 53
groundwater sampling location included a field sample, field sample duplicate, and a minimum of two

field spike samples. Each empty container for groundwater samplings was marked with a “fill to here”

line to produce a final sample volume of 200 mL. Containers designated for field matrix samples were

fortified with an appropriate matrix spike solution containing PFOA prior to being sent to the field for

sample collection. See section 8.8 of the report for field matrix spike levels.

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

Laboratory method ETS-8-044.0 “Determination of Perfiuorinated Compounds in Water by High

Performance Liquid Chromatography/Mass Spectrometry Direct Injection Analysis”.

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

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

sample results and the associated FMS recoveries. All results for the quality control samples preparedand analyzed with the samples are reported and discussed elsewhere in this report.

4 Test & Control Substances

There was not a test substance or control substances in the classic sense of a GLP study. This study

was purely analytical in nature.

5 Reference Substances

The analytical reference substances used for this study are listed below.

Reference Substance PFOA PFOA

Chemical Name Perfluorooctanoate PerfiuorooctanoateChemical Formula C7FCOOH C,F 5OO

Identifier CAS # 33567-1

Source Oakwood Products 3MExpiration Date 09/29/2012 02127/2017

Storage Conditions Frozen Frozen

Chemical Lot Number 3440 332

TCR Number TCRO7-0041 TCR-123

Physical Description Powder White Powder

Purity 995% 95%

Page 11 of 53
Sample Description Key Code.

Strtr Number Strg Desaipt xaie&le DALI32ROIOIIO2

I Sample Location DAL Decatur, Alabama

2 4IID &ie: 132

3 We Level R Resldum shaow wele”be8thIg zone

1. Bedrock water-bearing zine

S Ep#rs1mkidJeter-beadngzone

4 Sampling Date 101102-Noven,ber2, 2010

5 Sample 77se Opdmaiy sample

Idupficate sampleLS low spike

MS amidspike _________________ HS high spike

7.1 Methods

Analysis for all anaMes was completed following 3M Environmental Laboratory method ETS-8-044.O

‘Determination of Perfiuonnated Compounds In Water by High Performance Liquid

ChromatographylMass Spectrometiy Direct Injection Analysis’.

7.2 Sample Collection

Samples were collected in 250 mL Nalgene (high-density polyethylene) bottles prepared at the 3MEnvironmental Laboratory. Sample bottles associated with GLPIO-01-01-1 1 were returned to the

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

GLP1O-O1-01-1 2 was returned to the laboratory at ambient conditions on October 15, 2010. Samples

were stored refrigerated at the laboratory after receipt. A set of laboratory prepared Trip Blank and Trip Blank field matrix spikes were sent with each cooler of sample collection bottles.

7.3 Sample Preparation

Samples were prepared by removing an aliquot of the well mixed sample and placing it ‘i an autovial for

analysis.

Samples that required dilution were prepared by dilutions I mL sample with 9 mLs of Milti-Q water

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

Q water.

7.4 Analysis

AU study samples and quality control samples were analyzed for PFOA using high performance liquid chromatogrhyI tandem mass spectrometry (l-4PLC/MS/MS), Detailed instrument parameters, the

Page 12o153
Analytical Mstiod Followed ETS-8-044.0Analysis Oats 113/11 -1/8/11

Liquid Chroniatogtaph AlenI 1100Guard cok,mn Prism RP (2.1 mmX 50 nsn), 5

Anyt)cal column Betas4 C18 2.1 rmi X 100 mm), 5i

lrrØctlon Volume 2 or 10 iL

Mass Spectrometer ied Blosyslerns API 4000Ion Source Tixbo SprayElectrode Turbo Ion etedrode

Polarity NegativeSoftware Arralystl.4.2

Table 3. LIquid Chromatography Conditions.

St Totalre Flow Rate PecentA percent B

Nuner (mm) (pUmh7) (2 mM amrnoniom acetate) (Methw,ol)

0 0 300 97.0 30

1 2.0 300 97.0 3.0

2 11.5 300 5.0 95.0

3 13.5 300 5.0 95.0

4 136 300 97.0 3.0

5 17.0 300 97.0 30

Table 4. Mass Transitions.

8.1 Calibration

Samples were analyzed against an external standard calibration curve. CalIbration standards were

prepared by spiking known amounts of the stock solution containing the target anatytes into a laboratoryMliii Q water. A total of fifteen spiked standards ranging from 0.025 ng/mL to 100 ng/mL (nominal) were

Mass Transition

Analyte Q1/Q3

4131369

PFOA 4131219

4131169

Dwd time was 100 msec loreadi transition.

The irttMduai transitions ware sunvned to

pmdu a otal ion c)romatogram’ (riC),

wtiidi was used for quantilalion,

Page 13 of 53
analytes. The correlation coefficient (r) was greater than 0.995 for PFOA

8.2 System Suitability

A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. The acceptance critena of less than or equal to 5% relative

standard deviation (RSD) for peak area and retention time criteria of less than or equal to 2% RSD was metfor PFOk

8.3 Limit of Quantitation (LOQ)

The LOQ for this analysis is the lowest non-zero calibration standard iii the curve that meets linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate blanks. The nominal LOQ for all analytes can be found in Table 5.

Table 5. LImit of Quantitation (LOQ).

Ana.ysJs Date PFOA

LOQ, ng/mL.

1/3/11 0.0250

8.4 Continuing Calibration

During the course of each analytical sequence, continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. All

CCVs met method criteria of 1 00% ±25% for PFOA.

8.5 Blanks

Three types of blanks were prepared and analyzed with the samples: solvent blanks, trip blanks and equipment rinseate blanks, Solvent blank results were reviewed and used to evaluate method

performance to determine the LOO for PFOA. Trip blanks reflect the shipping and sample collection conditons the sample bottles and samples experience. Equipment rinseate blanks are aqueous samples that reflect the efficiency of equipment cleaning in the field between different sample cdiections and are proof of no cross contamination of samples from the equipment

8.6 Lab Control Spikes (LCSs)

Low, mid, and high-level lab control spikes were prepared and analyzed in tnplicate with each preparation set. LCSs were prepared by spiking known amounts of the arralyte into 40 mL of laboratory Milli 0 water, to produce the desired concentration. The spiked water samples were then analyzed in the same manner as the samples. The method acceptance criteria, average of LCS at each levelshould be within 100% ± 20% with an RSD 2%, were met for the linear PFOA LCS samples,

As the reference materials used for quantitation of PFOA is predominantly linear, and the PFOA present in the water samples are comprised of linear and branched isomers, additional LCS samples of linear and branched PFOA were prepared at three concentrations to evaluate the potential for analytical bias. The average recovery of the linear and branched LCS at the low and high levels met method

acceptance criteria. The mid-level linear and branched LCS had an average recovery of 123%. All LCS samples were used in the determination of method uncertainty in section 8.7.

Page 14 of 53
Tabte 6. Laboratory Control Spike Recovery.

ETS-8-044.0

j1j__ Linear PFOA

Spiked Calculated

Concentration Concentaiion

Lab ID (nglmL) (nWrnL) %Recovey

LCS-101230-1 0.497 0580 117

LCS-101230-2 0,497 0.557 112LCS-101230-3 0.497 0.590 119Average± %RSD 116% ± 3.1%

LCS-101230-4 4.97 5.83 117

LCS-101230-5 4.97 5.69 115

LCS-101230-6 4.97 5.69 114

Avege±%RSD 116%±1.3%

LCS-.101230-7 29.9 25.6 85.6LCS-101230-8 29.9 25.8 86.3LCS-101230-9 29.9 25,7 85.9

Average± %RSD 85.9% ± 0.41%

ETS4-044.0

Arrafyzed 1t301 i Linear• B,nched PFOA

Spiked Calculated

Concentration Concentration

Lab ID (ng/niL) (ng’mL) %Recovesy

LCS-101230-1OECF 0.498 0.546 110LCS101230-1 1 ECF 0.498 0.553 111

LCS-101230-12 ECF 0.498 0.541 109

Avaagat%RSO 110% ±0.91%

LCS-101230-13ECF 4.99 6.29 126LCS.101230’-14 ECF 4.99 603 121

LCS-101230-15 ECF 4.99 8.12 123

Aveiage ± %R.SD 123% ± 2.0%

LCS-101230-16 ECF 29.9 31.3 105

LCS-101230-17 ECF 29.9 30.8 103

LCS-101230-18ECF 29.9 30.6 102

Average±%RSD 103%±1.5%

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

Page 15 of 53
Table 7. Analytical Method Uncertainty.

Method I Analyte Method Standard Deviation I Uncertainty I I I PFOA I ETS-8444.O 11.3 ± 23% I

8.8 Field Matrix Spikes (FMS)

A minium of two field matrix spikes were collected at each sampling point to verify that the analytical

method is applicable to the collected matrix. Field matrix spikes were generated by adding a measured

volume of field sample to a containerspiked by the laboratory with the target analytes prior to shipping

sample containers for sample collection. Field matrix spike recoveries within method acceptance criteriaof 100t30% confirm that unknown” coniponents in the sample matrix do not significantly interfere withthe extraction and analysis of the analytes of interest. Field matrix spike concentrations must be 50% of

the sample concentration to be considered an appropriate field spike. Feki matrix spikes are presented in section 9 of this report.

Table 8. Field Matrix Spike Levels.

Sampling Location Spike Level PFOA ngmL

Low 0.0991

136R, 137R, 137s, 137L 1381 Mid 0.991

High 9,91

Low 0.991

1301, 131L, 1315, 133R, 134S, 1355, 1355 Mid 9.91

High 99.1

13CR, 1305, 132R, 1321, 1325, 1335, 133L, Low 9.91

134L 1351,1361, 1385, 138R, CW26R, CW26L, Mid 99.114CR, 141R, 142R, 143R, 144R i1E 991

131R,134R135R 1gh

Low 0.991

T’ Blnk Mid 9.91 np a Mid-High 99.1

High 991

(SampleConcentration of FMS-Average Concentration FicidSample& FicldSample Dup.) FMS Recovery 100% Spike Concentraton

Page 18oi53
from those listed in the raw data.

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

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

DAL GW 134R 101104- The high-level FMS did meet method acceptance criteria with a recovery of

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

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

DAL GW 1 31R 101103 — Due to the high concentration of PFOA detected in the sample, this samplinglocation did not have an appropriate FMS spike level to sufficiently evaluate PFOA recovery.

DAL GW 135R 101105—Due to the high concentration of PFOA detected in the sample, this sampling

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

Page 17of53
GLPIO-01-01-1 1-002 OAt. GW 130R DB 101105 798 NA

OLP1O-O1-01-11-003 DAL.GW13ORLS 101105 805 NC

GLP1O-C1-01-11-004 DALGW13ORMS1OI1O5 895 NC

GLP1O-01-01-11-005 DAL GW 130R HS 101105 1680 89.6

Average Concentration (n’mL) ± %RPD 793 ng/mL ± CL88%

NA Not Apçftcable

NC = Not Caated: Encogenous sample concentration greater than 2x spike lev.

Table 10. DAL. GW 130S 101105

PFOA

Concentration

3MLIMS ID Descnption (ng’mL) %Recove,y

GLPIO-01-01-11-006 DALGW13OSO1O11O5 174 NA

GLPIO-01-01-11-007 DALGWI3OSDB 101105 173 NA

GtJ’10-01-01-11-008 OALGWI3OSLS1OIIO5 183 NC

GLP1O-01-01-11-009 DAL GW 130S MS 101105 270 97.4

GLP101-01-11-010 DAL OW 130S HS 101105 1150 98.5

Average Concentration (nnL) ± %RPD 174 ng/mL ± 0.58%

NA = Not AppUcab4e

NC = Not Calciialed; Endogenous sample concentration greater than 2x sp4te tevel.

Table 11. DAL GW 130L 101105

PFOA

Concentration

3MLIMS ID DeseMption (ng/mL) %Recovesy

GLP1O-01-01-11-011 DALGWI3OLOIO1IO5 69.3 NA

GLP1O-01-01-1 1-012 DAt. GW 130L 08 101105 70.7 NA

GLP1O-01-01-11-013 DALGW13OLLS 101105 71.0 NCGLP1O-01-01-11-014 DALGWI3OLMSIOIIO5

, 73.3 NC

GLPIO-01-01-11-015 DALGWI3OL HS1O11O5 162 92.8

Average Concentration (ngfmL) ± %RPD 70.0 n9mL ± 20%

NA Not Apllcab1e

NC = Not CaIcated: Endogenous sanp4e concentration greater than 2x spike level.

Page 18 of 53
GLPIO-01-01-11-018 DALGWI3IRDS 101103 2460 NA

SLP1G-0101-11-019 DAL GW 131R LS 101103 2570 NC

GLP1O-O1M1-11020 DALGW131RHS 101103 3240 NC

Average Concentration (ngfmL) ± %RPD 2500 ng/mL ± 1.6%

NA Not Applicable

NC = Not Calailated; Endogenous sante corntration greater than 2x sptke level

(1) Sang location dic not have an appropriate spe level to evaluate PFOA recovery.

Table 13. DAI GW 13IS 101103

PFOA_______

Concentration

3M LIMS ID Description (ng(mL) %Recoverg

GLPIO.01-01.11.021 DALGW131SO1OI1O3 25.4 NA

GLP10-0101 -11-022 DAL GW 131$ D8 101103 24.4 NA

GLP1O-01-01-11-023 DAL GW 1315 IS 101103 25.3 NC

GLP1O-01-01-11-024 DAL GW 1315 MS 101103 34.6 NCGLP1O-01-01-1 1-025 DAL GW 131S HS 101103 127 103

Average Concentration (ng/mL) t %RPD 24.9 ng’mL ± 4.0%

NA Not Applicable

NC Not Cala.iated; Endogenous sample concentration greater than Zx spike level.

Table 14. DAL. GW 131L 101103

_____________ PFQA______

Concentration

3MUMS ID Description (ngfmL) %Recovery

GLP1O-01-01-11-026 DAI GW 13110101103 88.3 NA

GLPIO-01-01-11-027 DALGW 1311 08 101103 93.0 NA

GLP1O-01-01-11-028 DALGW13ILLS 101103 87.7 NC

GLP10-0101-11-029 DALGWI31LMS 101103 96.9 NC

GLP1O-01-.0l-11-030 DAL GW 1311 HS 101103 179 89.2

Average Concentration (ng/mL) ± %RPD 90.7 ng/mL ± 5.2%

NA = Not ApplIcable

NC Not Calculated; Endogenous sarople concentration greater Than 2x spike level.

Page 19 of 53
3M LIMS ID Description (ng’mL) %Recovety

GLP1O.0l-01-l1-031 DALGWI32ROIOI1O2 256 NA

GIPIO-O1-01-1 1-032 DAL SW 132R DB 101102 245 NAGIPIO-01..0i-l1-033 DAL (3W 132R IS 101102 267 NC

GLPIO-01-01-11-034 DALGWI32RMS 101102 356 NC

GLPIO-01-01-1 1-035 DAL (3W 132R HS 101102 1160 91.8

Averaqe Concentration (nWL) ± %RPD 251 nWmL ± 4.4%

NA Not AppkcableNC Not Calculated; Endogenous sample concentration greaterthan 2spike level.

Tablel8. DALGWI32SIOIIO2

PFOA_______

Concentration

3M LIM$ ID Dewip*fon (n’mL) %Pecove’y

GLPIO-01-01-1 1-036 DAL (3W 132$ 0101102 959 NA

GLPIO-01-01-11-037 C)AL SW 132$ DB 101102 964 NAGLP1O-01-01-1 1-038 DAL GW 132$ LS 101102 926 NCGLPIO-01-01-11-039 DALGWI32SMSIOIIO2 1020 NCGLP1O.01.01-11-040 DALGWI32SHSIOIIO2 1810 85.8

Avereqa Concentration (nnL) ± %RPD 962 ng’mL ± 032%

NA = Not Akable

NC Not Calculated; Endogenous sample ccneer*allon greaterthan 2x spike level,

Table 17. DAL GW 132L101103

PFCA_______

Concentration

3MLIMS ID Description (n9’mL) %Recovery

GLP1O.01.01-11-041 DALGWI32LO 101103 398 NAGIP1001-01-11-042 DALGWI32LDB 101103 410 NA

GLPIO-01-01-1 1-043 DAL GW 132L LS 101103 451 NCGIPIO-01-01-11-044 DALGWI32LMS 101103 482 NCGLP1O-01-01-11-045 DALGW132LHS 101103 1290 89.4

Avemge Concentration (nq/rnL) ± %RPD 404 ng/mL ± 3.0%

NA = Not pltcatleNC = Not Calculated; Endogenous sample concentratIon greater than 2x spike level.

Page 20 of 53
GLP1O-01.01-11-047 DALGW133RDBIO1IO2 973 NA

GLP1O-01-01-11-048 DALGW133RLSIO11O2 102 NC

GLP1O-01-01-11-049 DALGW133RMS 101102 108 NC

GLP1O-01.01-11-050 DAL GW 133R HS 101102 19 91.7

Average Concentration (nWmL) ± %RPD 102 nWmL ± 9.5%

NA Not Appltcable

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

Table 19. DAL GW 133S 101103

PFOA_______

Concentration

3M UMS lD Description (nglmL) %Recoveiy

GLP1O-0141-11-051 DALGW133SO1OI1O3 393 NA

GLP1O-01-01-11-052 DALOW133SD8IOIIO3 377 NAGLP1O-01-01-11-053 DAL GW 133S LS 101103 407 NC

GLPIO-01-01-11-054 DALGWI33SMSIOI1O3 485 NC

GLP1O-01-01-11-055 DALGW133SHSIO11O3 1260 88.3

Avge Concentration (n’mL) ± %RPD 385 n’mL ± 4.2%

NA = Not ApplIcable

NC = Not Calc*dated; Endogenous sample concentration greater than 2x spike level.Table 20. DAL GW 133L 101103

PFOA________

Concentration

3M LIMS ID Description (n/mL) %Recoverj

GLP1O-01..01-11-056 DAI..GW133L0101103 253 NAGLP1O-01-01-11-057 DAL GW 133L DB 101103 250 NA

GLPIO-01-01-11-058 DAL GW 133L LS 101103 265 NC

GLP1001.01-11-059 DAL GW 133L MS 101103 355 NCGLP1O010111060 DALGWI33LHS 101103 1190 941

Average Concentration (ng/mL) ± %RPD 252 ngfmL ±1.2%

NA = Not ApplicableNC = Not Calculated; Endagenous sample concentration greaterthan 2x spike level.

Page2l of 53
GLPIO-01-01-l1-062 DALGW134ROB1O1IO5 1490 NA

GLPIO-OIM1-11-063 DAL GW 134R LS 101105 1620 NCGLP1O-O1-01-11-064 DALGWI34RHS 101105 2250 69.1

Average Concentration (ng4nL) ± %RPD 1570 ng’mL ± 9.6%

NA Nc Applcat4e

NC = Not Calculated; Endogenous sample concentration greater than 2x spike level(1) Field matrix spike did not meet method acceptance criteria of 100% ± 30%.

Table 22, DAL GW 134S 101105

PFOA

concentmiion

3M LIMS ID Description (ng’mL) %Recove,y

GLP1O-01-01-11-065 DALGW134.S0 101105 5.64 NAGLP1O-01-01-11-066 DALGWI34SDB 101105 5.34 NAGLPIO.01-O1-11-067 DALGW134SLS1OIO5 6.95 NC

GLP1O-O1-01-11-068 DAL GWI34S MS 101105 15.6 112

GLP1O-O1-01-11-069 DALGW1S4SHS1OI1O5 102 97.4

Average Concentration (nq/mL) ± %RPD 5.49 nWmL ± 5.5%

NA = Nc App4cableNC = N± Calo.ialed: Endogenous sample concentration greater than 2x spike level,

Table 23. DALGW 134L 101105

PFOA

J Concentration

3M LIMS ID j Description (n’mL) %Recove,y

GLP10-O1-01-11-70 DAI..GW134L0101105 523 NAGLPIO-01-01-11-071 DALGWI34LDB 101105 516 NA

GLP10-0101-114)72 DALGWI34LLS1O11O5 530 NC

GLP1O-O1-01-11-073 DALGW134LMS 101105 599 NC

GLP1O.01.01-11-074 DALGWI34LHS 101105 1390 87.8

Average Concentration (n’mL) ± %RPD 520 nWmL *1.3%

NA = Not Apphcae

NC Not Calculated; Endogena.Js sample concentration greater than 2x ske level

Page 22 of 53
GLP10101i147 DALGW135RDB1O11O5 2890 NA

GLP1O.0l-0l-l1-077 DALGW135RLS1O11O5 2930 NC

GLP1O-O1-01-11-078 DAL GW 135R HS 101105 3840 NC

Average Concentration (ng/mL) * %RPD 2910 n’mL ± 1.4% “

NA Not Applicable

NC - Not CalcUated; Endogenous sampte cc nlraUor greater than 2x spike level

(1) SamplIng location did not have an appropnate spike level to evaluate PFOA recovery.

Table 25, DAL GW 135S 101105 

PFOA

Concentration

3M LIMS ID Description (n’mL) %Recovey

GLPIO-O1-01-11-079 DALGW135SO 101105 139 NA

GLP10-0101-11-080 DALGW135SD8 101105 13.4 NA

GLP1O-0101-11-081 DAL GW 1358 LS 101105 14,5 NCGLPIO-01-01-11-082 DALGW135SMS1O11O5 24.2 106

GLPIO-01.01-11-083 DALGW135SHS1O1IO5 110 97.2

Average Concentration (nnL) ± %RPD 13.7 n’mL ± 3.7%

NA Not Açpeicable

NC Not Calaiated; Endogenous sample concentration greaterthan 2x spice level

Table 26. DAL GW 135L 101105

PFOA_______

Concentration

3M LIMS ID Description (ngfmL) %Recovery

GLP10-0101-11.084 DALGW135LO 101105 124 NAGLP10-01-0111085 DALGW135LDB 101105 121 NA

GLP10-01.01-11086 DALGW135LLS 101105 129 NCGLP10-01-01-11087 DALGWI35LMS1O11O5 228 104

GLPIO-01-01-11-088 DALGWI3SLHS 101105 1070 958

Average Concentration (ngfmL) ± %RPD 123 n’mL ± Z4%

NA - Not Applicable

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

Page 23 of 53
GLPIO-01-01-11-090 DALGW136SDB 101103 76B NAGLP1O-01-01-11-091 DALGW136SLS1O11O3 77.6 NC

GLP1O-01-01-11-092 DALGWI36SMS 101103 86.1 NC

GLP1O-01-01-11-093 DALGW136SHS1O11O3 166 91 5

Average Concentration (nmL) ± %RPD 75.4 n’mL ± 3.8%

NA = Not ApplicableNC g Not Calculated; Endogenous sample C n rtation greater than 2x spike lemL

Table 28. DAL (3W 136L 101103

PFOA

Concentration

3M LIMS ID Description (ng’mL) %Recovesy

GLP1O.Oi-01-11-094 DAL GW 136L 0101103 74,1 NA

GLP1O-01-01-11-095 DALGWI38LDB1OI1O3 76.4 NA

GLP1O-01-O1-11-C98 DALGWI38LLS 101103 86.2 NCGLPIO-01-C1-11-0G7 DALGW136LMS1O1IO3 169 94.8

CLP1O-01-O1-11-098 DALGWI36LHS 101103 1030 96.3

Average Concentration (nnL) ± %RPD 75.3 n.fmL ± 3.1%

NA Not ApplicableNC - Not CaI4ated; Endogenous sample concaniration greater thai 2x spike Ievd.

Table 29. DAL GW ‘t37S 101109

F’FOA

ConcentIon

3M LIMS ID Description (n’mL) %Recovesy

GLPIO-01-01-11-099 DALGW137SOIO11O9 0.273 NA

GLP1O-01-01-11-100 DALGW137SDB1OI1O9 0.268 NA

GLP10-01-0111-101 DAL GW 137S LS 101109 0.350 NC

GLP1O-O101-11-102 DAL GW137S MS 101109 1.32 108GLPIOQ1-Q1-11-103 DALGW137SHS1O11O9 10,9 107

Average Concentration (ngfmL) ± %RPD 0.271 n’mL ± 1.8%

NA Not Applicable

NC Not CalcJated; Endogenous samp4e concentralion greater than 2x spike level.

Page 24 0153
NA = Not Appcab

NC = Not Calculaled Endogenous sample concitrion greater than 2x sp4ke level.

GLP1O-01-01-11-105 DALGW137LDB 101109 0.361 NAGLP1O-01-01-11-108 DALGWI37LLS 101109 0.458 NCGLP1O-01.01-11-107 GAL GW 137L MS 101109 1,40 105

!GLP1O-01-01-11-108 GAL GW1371 KS 101109 10.7 104

A’w8qe Concentration (nq/mL,) ± %RPD 0.361 nWmL ± 0.28%

NA = Not ApplicableNC Not Caated; Endogencus sanle concentration geater than 2x splice level.

Table 31. DAL OW 138S 101110

. PFOA_______

Concenti’atlon

3M LIMS 10 Description (ng’mL) %Recovery

GLP1O-01-01-11-109 GAL GW 13850 101110 149 NA

GLP10-1-01-11.-110 GAL GW 138S GB 101110 144 NAGLP1O-01-01-11-111 DALGWI38SLSIOIIIO 162 NC

G1.P10-0101-11-112 GAL GW 1385 MS 101110 230 84.3

GLP1O-01-01-11-113 GAL GW 138$ KS 101110 1020 86.1

Ave,ge Concentration (ng4,,L,) * %RPD 147 ,g/mL ± 3.4%

NA Not ApØcableNC = Not CaiaAated: Err.iogenous sante ccn*ation greater thai 2x spike level.

Table 32. DAL GW 138L 101110

PFOA

Concentration

3MLIMS ID Description (ng’mL) %Recove,y

GLPIO-01-01-11-114 GAL GW138L0 101110 119 NA

GLP1O-01-01-11-115 DALGWI38LDB1OII1O 1.12 NA

GLP10-0101-11-118 OALGWI38LLS1OI11O 124 NCGLP1O-01-01-1 1-117 DAL GW 138L MS 101110 2 18 103GLPIO-01-01-11-118 DALGWI38LHS 101110 11.2 101

Average Concentration LnwPi1± %RPD 1.16 nmL ± 6.1%

Page 25 of 53
GLP1C-01.01-11-120 DALGWCW26RDB 101110 389 NAQLP1O-01-Q1-11-121 DALGWCW26RLS 101110 395 NCGLP1C-01-01-11-122 OALGWCW26RMS 101110 450 NC

GLPIO-O1-01-11-123 DALGWCW26RHSIO11IO 1290 913

Average Concentration (ng’mL) ± %RPD 386 n’mL ±1.8%

NA = Not ApplicableNC = Not CalcJated; Endogenous sample concentration greaterthan 2x spike leveL

Table 34. DAt. GW CW26L 101110

PFOA______

Concentration

3M LIMS ID Description (ng(mL) %Recove,y

GLP10-01-41-11-124 DALGWCW26LO1OI1IO 565 NA

GLP1O-01-01-11-125 DALGWCW2SLOB 101110 539 NAGLP1O-01-01-11-126 DALGWC6LLS 101110 552 NCGLP1O-01-01-11-127 CAL GWCW26L MS 101110 623 NC

GLP1O-01-01-11-126 DALGWCW26LHS 101110 1480 93.6

Average Concentration (ng4nL) ± %RPD 552 ng/mL ± 47 %

NA - Not Applicable

NC = Not Calculated: Endogenous sample concentration great than 2x spike leveL

Table 35. DAL GW 140R 101104

PFOA_______

Concentration

3M LIMS ID Description (n’mL) %Recovery

GLP1O-01-01-11-129 OALGW14ORO1O11O4 121 NAGLP10-01-1-11-130 DALGW 14CR 08 101104 120 NAGLP1001.01-11-131 CAL GWI4OR LS 101104 128 NC

GLP100101-11132 !OALGW 14CR MS 101104 217 97.4

GLP10-0101-11-133 DALGWI4ORHS 101104 973 8&0

Average Concentration (ng/mL) ± %RPD 121 nqfmL ± 0.83 %

NA Not Applicable

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

Page 26 of 53
GLP1O-01-01-11-135 DAL GW 141R DS 101110 1.55 NA

GLPIG-01-01-11-136 DAL GW141R LS 101110 11.4 96.5

GLPIO-01-01-11-137 DAL SW 141R MS 101110 965 94,5

GLP1O-01-01-11-138 DAL SW 141R HS 101110 908 91.4

Average Concentration (ng/mL) ± %RPD 1.84 ng’mL ±10 %

NA Not Applicable

NC - Not Calculated; Endogenous sarrle concentration greater than 2x spike leveL

Table 37. DAL GW t42R 101110

PFOA

Concentration

3M LIMS ID Description (nfn,L) %Recove,y

GLP1O-01-01.11-139 DALGWI42ROIO1IIO 46.5 NAGLP1O-el-O1-1 1-140 DAL OW 142R DB 101110 4.8.7 NA

GLP1O-O1-01-11-141 DALGW142RLS 101110 55.3 NC

GLP1O-01-01-11-142 DALGW142RMS 101110 143 96,3

GLP1O-01-01-1 1-143 DAL GW 142R HS 101110 925 88.5

Average Concentration (nlmL) ± %RPD 47.6 ng’mL ± 46 %

NA — Not ApplicableNC Not Calculated; Endogenous sample concerrabon greater than 2x spike level.

TabLe 38. DAL GW 144R 101110

PFOA

Concentration

3MLIMS ID Description (n,,L) %Recovery

GLPIO-01-01-11-144 DALGWI44RO1OII1O 57,2 NA

GLP1G-01-01-1 1-145 DAL SW 144R D8 101110 57.3 NA

GLP1OO1-01-1 1-146 DAL SW 144R LS 101110 67.6 NC

GLPIO-01-01-1 1-147 ‘ DAL SW 144R MS 101110 142 85.5

GLP10O1-01-11-148 DAL SW 144R HS 101110 966 91,7

Average Concentration (ng’mL) ± %RPD 57.3 nge’mL ± 0.17 %

NA = Not Applicable

NC Not Calculated; Endogenous sarrple concentration greater than 2x splke level.

Page 27 of 53
GLP1O-01-01-11-151 TRIP BLANK 1 LS 1.08 109GLP1O-01-01-11-152 TRIP BLANK I MS 10.6 107

GLP1O-01-01-11-153 TRIPBLANK1MHS 99.1 100

GLPIO-01-O1-11-154 TR1PBLANKIHS 1040 105NA = Nat Applicable

Table 40. Trip Blank 2

PFQA

ConcenbitIon

3M LIMS ID Description (nglmL) %Recove,y

GLP1O-01-O1-11-155 rRIPBLANK20 <0,0250 NA

GLPIO-01-01-11-156 TRIP BLANK2LS 1.08 109

GLPIO-01-01-11-157 TRIP BLANK2MS 10.9 110

GLPIO-01-01-11-158 TRIP BLANK 2 MHS 96.9 97.8GLP1O-01-01-11-159 RIPB1ANK2HS 1020 103

NA = Not ApphcatAe

Table 41. Trip Blank 3

PFOA

Concentration

3M UMS 10 Description (ng’mL) %Recovesy

GLP1O-01-01-1 1-160 TRIP BLANK 30 <0.0250 NAGLPIO-01-01-1 1-161 TRIP BLANK 3 LS 1.07 108GLP1O-01-01-11-162 TRIP BLANK3MS 10.4 105

1

GLP1O-01-01-1 1-163 TRIP BLANK 3 MHS 101 102

GLP1O-01-01-1 1-164 TRIP BLANK 3 HS 1050 106

NA = Not ApØicable

Page 28 of 53
GLP1O-O1-0l-1 1-166 TRIP BLANK 4 LS 106 107

GLP1O-01-O1i1-167 TRIP BLANK 4 MS 10.4 105

GLP1O-01-01-11-168 TRIP 8LANK4MHS 95.4 96.3

GLPIO-O1-01-11-189 TRIP BLANK4HS 985 994

NA Not Apicable

Table 43. Rinseate Blanks

PFOA

Concentration

3M LIMS ID Description (ng’mL) %Recove,y

GLPIO-O1-01-11-016 DAL GW 130L RB 101105 <00250 NA

GLP1O-01-01-11-149 DAt.. GW 144R RB 101110 <00250 NA

GLP1O-01-01-12-009 DAL SS 607R RB 0040 <00250 NA

NA = Not Appficabe

Page 29 of 53
All remaining samples and associated project data (hardcopy and electronic) will be archived according

to 3M Environmental Laboratory standard operating procedures.

-

Attachment A: Protocol Amendment 11 (General Project Outline)

Attachment 8: Representative Chromatograms and Caliration CurvesAttachment C: Analytical Method -ETS-8-O44OAttachment 0: Method Deviation

Page 30 of 53
2/p/i01/ — Cleston Lange, Ph.D., 3M Principal Analytical Investigator Date

0/I

William K. Reageri, Ph.D., 3M Environmental Laboratory Manager Date

,M12tt

Gary Hohe tein, 3M Sponsor Representative Date

jQAIiLAi

Jaisirnha K Study Director ate

Page 31 of53
J:\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\1Q11 Status Report\1Q11 Status Report FINAL.doc 4/28/2011

ATTACHMENT 2 

SOIL AND SEDIMENT SAMPLING

TECHNICAL PROGRESS REPORT 

JANUARY 1, 2011 – MARCH 31, 2011
J:\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\1Q11 Status Report\1Q11 Status Report FINAL.doc 4/28/2011 

Att 2-1 

SOIL AND SEDIMENT SAMPLING

TECHNICAL PROGRESS REPORT

3M AND DYNEON DECATUR, ALABAMA

The following subsection describes soil and sediment sampling activities completed 

during the first quarter of 2011. The analytical results will be summarized in a subsequent 

quarterly status report

OFF-SITE ACTIVITIES

On-Site Avenue A Area Sediment and Soil Sampling

Twenty six locations within the Avenue A area were sampled between January 26 and 28, 

2011. The 26 locations are identified on Figure 1. Soil samples were collected at 20 of these 

locations and sediment samples were collected at the remaining 6 locations. At all twenty 

six locations the following samples were collected using a hand auger: surface soil/sediment 

(0 – 0.5 ft), shallow subsurface soil (0.5 – 1.0 ft) and subsurface soil (1.5 – 2 ft). 

Eleven of the soil sampling locations (SS10 – SS20) were established within the fire 

training area. These samples were collected in order to better define the lateral extent of

PFOA distribution in the vicinity of the fire training area. 

Nine soil sampling locations (SS21, SS22 and SS24 – SS30) and six sediment sampling 

locations (SD18 – SD23) were located within the marsh area to the west of the closed

landfill area. These samples were collected to better define the lateral extent of the PFOA 

distribution associated with the drainage feature. At the time of sampling most of the 

sediment sampling locations were inundated and thus sediment was collected using 

disposable sample scoops, stainless steel hand augers, and polyethylene tubing. Two of 

the soil sampling locations in the marsh area were sampled for groundwater; this 

sampling is discussed in Attachment 1. 

The Avenue A assessment is intended to obtain additional data for the Remedial Action 

Agreement Program being undertaken by 3M under the ADEM NPDES program and is 
J:\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\1Q11 Status Report\1Q11 Status Report FINAL.doc 4/28/2011 

Att 2-2 

not a MOU-related activity. The analysis of samples was not completed in time for the 

March 31, 2011 Quarterly Status Report and will be discussed in a subsequent report. 
!( !(!(

!(!(

!(!(!(

!(

!( !(

!(

!(

!( #*

#*

#*

"/

!( #*

!( "/

!( !( #*

#*

Tennessee River

Finley Island Road

State Docks Road

Avenue A

Closed

Landfill

SD19

SD20

SD23

SS28

SS27

SS22

SS21

SS24

SD26

SD21

SD22

SS25 SS30

SS29

SS19

SS12 SS20

SS18

SS14 SS17

SS15

SS13

SS16

SS10

SS11

SD18

0

μ250 500Feet

3M Decatur, AL Facility

Figure 1

Additional Avenue A

Soil and Sediment Sampling

January 2011

File: \\fsfed01\tig\3MDec\MXD\Additional_AvenueA_sampling.mxd, 22-Apr-11 15:32, ricksc

Imagery Source:

ESRI, i-cubed, USDA FSA, USGS, AEX, 

GeoEye, Getmapping, Aerogrid, IGP. 2010

Legend

#* Sediment Sampling Locations

!( Soil Sampling Locations

"/ Soil Sampling/Groundwater 

Sampling Locations