3M Company 

St. Paul, Minnesota 

Perfluorooctanoic Acid (PFOA) 

Site Related Environmental 

Assessment Program 

3M and Dyneon LLC 

Decatur, Alabama 

Quarterly Status Report 

January 1, 2011 to March 31, 2011 

C~N!TAlNS NO CE?' 
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 
TABLE OF CONTENTS 

Section Page 

1 . 

2. 

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

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 . 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. 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 

J.\FOLDERS.0-913M-DECAT\Phase 3 Work PIan11011 Status ReportO011 Status Report FINALdoc 4/2712011 

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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. 

J.\FOLDERS.0-9\3M-DECATPhase 3 Work PIanN011 Status ReportY1O11 Status Report FINALdoc 4/27/2011 

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p. 10 

ATTACHMENT 1 

GROUNDWATER SAMPLING 

TECHNICAL PROGRESS REPORT 

JANUARY 1, 2011 - MARCH 31, 2011 

J \FOLDERS .0-9\3M-DECAT\Phase 3 Work Plan\1011 Status Report\1011 Status Report FINAL.doc 4,'27/2011 
p. 11 

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-DECATPhase 3 Work Plan\1011 Status Report\1011 Status Report FINALdoc 4/27/2011 

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p. 12 

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 

J:IFOLDERS 0-9\3M-DECATPhase 3 Work Plan\1011 Status Report\1011 Status Report FINAL.dot 4/27/2011 

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p. 13 

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 

J\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\1011 Status Report\1011 Status Report FINAL.doc 4/27/2011 

Att 1-3 
p. 14 

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 . 

J:\FOLDERS.0-9\3M-DECAT1Phase 3 Work Plan\1011 Status Reportl1011 Status Report FINAL.doo 4/2712011 

Att 1-4 
Table 1 

Fourth Quarter Former Sludge Incorporation Area Groundwater 

PFOA Concentrations 

November 2010 

Sample ID Sample 

Location 

Average PFOA 

n mL, b 

DAL GW 130R 101105 130R 793 

DAL GW 130S 101105 130S 174 

DAL GW 130L 101105 130L 70 .0 

DAL GW 131 R 101103 131 R 25001a' 

DAL GW 131 S 101103 131S 24.9 

DAL GW 131 L 101103 131 L 90.7 

DAL GW 132R 101102 132R 251 

DAL GW 132S 101102 132S 962 

DAL GW 132L 101103 132L 404 

DAL GW 133R 101102 133R 102 

DAL GW 133S 101103 133S 385 

DAL GW 133L 101103 133L 252 

DAL GW 134R 101105 134R 1570Jb1 

DAL GW 134S 101105 134S 5 .49 

DAL GW 134L 101105 134L 520 

DAL GW 135R 101105 135R 29101al 

DAL GW 135S 101105 135S 13.7 

DAL GW 135L 101105 135L 123 

DAL GW 136S 101103 136S 75 .4 

DAL GW 136L 101103 136L 75 .3 

DAL GW 137S 101109 137S 0 .271 

DAL GW 137L 101109 137L 0 .361 

DAL GW 138S 101110 138S 147 

DAL GW 138L 101110 138L 1 .16 

DAL GW CW26R 101110 CW26R 386 

DAL GW CW26L 101110 CW26L 552 

DAL GW 140R 101104 140R 121 

DAL GW 141 R 101110 141 R 1 .84 

DAL GW 142R 101110 142R 47.6 

DAL GW 144R 101110 144R 57.3 

Notes: 

Average PFOA is the average of primary and duplicate sample 

analytical results 

~a3 Sampling location did not have an appropriate FMS spike level to 

sufficiently evaluate PFOA recovery 

~bl The analytical uncertainty has been adjusted for field matrix 

spike recovery to t 31% 

p. 15 

1 :\FOLDERS.0-9\3M-DEGAT\Phase 3 Work Plan\1Q11 Status Report\Attachment 1\Table 1 FSIA GW PFOA DATA Nov 2010 .xlsx-AVG_Data 
p. 16 

Imagery Source: 

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

GeoEye, Getmapping, Aerogri(A, IGP. 2010 

hlonitoritw, Well Locations (Cliuter5) 

- :0 i -, 

Figure 1 

BFI Morris Farms Landfill 

Groundwater Sampling 

Decatur, AL 
p. 17 

Norfolk Southern Ra 

133R 

133S 

133L 

102 

385 

252 

m O 

Y 

U 

O 

N 

20/72 

Notes : 

-Average PFOA is the average of primary and 

duplicate sample analytical results m 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 feld matrix spike recovery to ± 31% 

Legend: 

Groundwater 

Sampling Location 

Daikin Property 

Note : 

R - Residuum Well 

S - Epikarst Well 

L - Bedrock Well 

800 400 0 Feet Figure 2 

Former Sludge Incorporation Area 

Groundwater PFOA Sampling 

November 2010 

Decatur, AL 
p. 18 

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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. 

1:\FOLDERSC-9-3M-DECA91Phase 3 H4,rk Plau\IQI I Stalus Rcpcxi\IQI I St-, Repom FINAL d« 4/27/201 1 
GLP10-01-01 . Interim Report 11. " Analysis of PFOA In Groundwater Samples Collected at 

the Former Sludae incorDoration Area (FSIA) located in Decatur. AL in November 2010 

Study Title 

Analysis of PerRuorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E ., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

West Chester, PA 19380 

Phone: 610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

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

Maplewood, MN 55144 

Project Identification 

GLP10-01-01-11 

Total Number of Pages 

53 

The testing reported herein meet the requirements of IS09EC 17021t-20Q8 "General 

Requirernents for the Competence of Testing and Calibration Laboratories", In accordance with the A2LA Certificate *2b62.01. Testing tdat complies with this International Standard also 

operate in accordance with ISO 9001 :2000. 

Certificate #2052.01 
p. 23 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

This page has been reserved for specific country requirements. 

Page 2 of 53 
p. 24 

GLP10-01-01 ; Intenm Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

GLP COMPLIANCE STATEMENT 

Report Title: GLP10-01-01, Interim Report 11 . Analysis of PFOA in Groundwater Samples Collected 

at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 

Study: Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program. 

This analyticat phase was conducted in compliance with Toxic Substances Control Act (TSCA) Good 

Laboratory Practice (GLP) 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 GI-Ps and the stability under 

storage conditions at the test site have not been determined under GI-Ps. 

Date 

~dzlbl 

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

Page 3 of 53 
p. 25 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

QUALITY ASSURANCE STATEMENT 

Report Titie: GLP10-01-01, Interim Report 11_ Analysis of PFOA in Groundwater Samples Collected 

at the Former Sludge Incorporation Area (FSIA) at Decatur, AL in November 2010 

Study: Analysis of Perfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program. 

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 

(P .I .), laboratory management and study director. 

Date Reported to 

Inspection Dates Phase Testing Facility 

Management 

Study Director 

12130(10 In-Phase 214111 214111 

1/27/11 -1128/11 Data 1 Interim Report 214111 214111 

(aAU Repres4tative 

_ 

Date 

Page 4 of 53 
p. 26 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

TABLE OF CONTENTS 

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

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

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 Limit of Gluantitation (LOQ) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . : . . . . . . . . . . . . . . . . . . . . . . .14 

8.4 Continuing CalilJraGon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . .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 

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Former Sludge Incorporation Area " November 2010 

9 Data Summary and Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .17 

10 Conclusion . . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ., . . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30 

11 Data/Sample Retention . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . 30 

12 Attachments. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30 

13 Signatures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31 

LIST OF TABLES 

Table 1 . Summarized PFOA Results (FSIA Groundwater, Decatur, AL, November 2010) . . . . . . . . . 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 

Table 9. DAL GW 130R 101105 . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .18 

Table 10. DAL GW 130S 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..18 

Table 11 . DAL GW 130L 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . .18 

Table 12. DAL GW 131R 101103 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . .19 

Table 13. DAL GW 131S 101103 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19 

Table 14. DAL GW 131L 101103 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19 

Table 15. DAL GW 132R 101102 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .20 

Table 16. DAL GW 132S 101102 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .20 

Table 17. DAL GW 132L 101103. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .20 

Table 18. DAL GW 133R 101102 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .21 

Table 19. DAL GW 133S 101103 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ., . .21 

Table 20. DAL GW 133L 101103. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .21 

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GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge incorporation Area - November 2010 

Table 21 . DAL GW 134R 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .22 

Table 22. DAL GW 134S 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .22 

Table 23. DAL GW 134L 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .22 

Table 24. DAL GW 135R 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23 

Table 25. DAL GW 135S 101105 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . ._ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . .23 

Table 26. DAL GW 135L 101105. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .23 

Table 27. DAL GW 136S 101103 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .24 

Table 28. DAL GW 136L 101103 . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .24 

Table 29. DAL GW 137S 101109 . . . . . . . . . . . . . . . . . . . . ., . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .24 

Table 30. DAL GW 137L 101109 . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .25 

Table 31. DAL GW 138S 101110 . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .25 

Table 32. DAL GW 138L 101110 . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ., . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .25 

Table 33. DAL GW CW26R 101110. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..26 

Table 34. DAL GW GW26L 101110 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . 26 

Table 35. DAL GW 140R 101104 . . .. . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .26 

Table 36. DAL GW 141R 101110 . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .27 

Table 37. DAL GW 142R 101110 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ._ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . ._ . . . . . . . . . . . . .27 

Table 38. DAL GW 144R 101110 . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ., 27 

Table 39. Trip Blank 1 . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . : . . . .. . . . . . . . . . . . . . . . . . .28 

Table 40. Trip Blank 2 . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . .28 

Table 41. Trip Blank 3 . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . ..28 

Table 42. Trip Blank 4. . . . . . . . . . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . ..29 

Table 43. Rinseate Blanks . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29 

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p. 29 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 2245W-03 

Saint Paul, MN 551441000 

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 Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55106 

Study Personnel 

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

Cleston Lange, Ph.O., Principal Analytical Investigator. (clanue Ommm.com); phone (651)-733-9860 

Susan Wolf 3M Analyst 

Kevin Eich; Analyst 

Cheisie 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 
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GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporahon Area - November 2010 

The 3M Environmental Laboratory received groundwater samples from wells located at the Former 

Sludge Incorporation Area (FSIA) in Decatur, AL, representing thirty different sampling locations. A 

total of one hundred sixty-nine sample bottles were received at the 3M Environmental Laboratory for 

perfluorooctanoate (PFOA) analysis, and included duplicate groundwater samples from each sampling 

location. Samples also included at least two field matrix spike (FMS) samples for each location, four 

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

rinseates. In addition, one soil equipment rinseate blank from GLP10-01-01-12 was analyzed . The 

equipment rinseate blanks did not have FMS samples prepared for determination of PFOA recovery. 

The groundwater samples, trip blanks and two equipment rinseate blanks associated with GLP10-01-

01-10 were received from Weston personnel on November 18, 2010. The equipment rinseate blank 

associated with GLP10-01-01-12 was received from Weston personnel on October 15, 2010. All of the 

samples were prepared and analyzed for PFOA following 3M Environmental Laboratory Method ETS8-044.0 under 3M project GLP-10-01-01-11 . 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 summarized 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 collections. 

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

ng/mL to 2910 ng/mL. The analytical uncertainty was estimated at 100 + 23%. 

Page 9 of 53 
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GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 1 . Summarized PFOA Results (FSIA Groundwater, Decatur, AL, November 2010) 

i 

~ Sample ID 

' 

Avg. PFOA ~ 

Concentration 

n mL 

Relative 

Percent 

Difference 

DAL GW 130R 101105 793 0.88% 

DAL GW 130S 10 1105 174 0.58% 

DAL GW 130L 101105 70,0 2,0% 

DAL GW 131 R 101103 2500 a 1 .6% 

DAL GW 131 S 101103 24.9 4 .0% 

DAL GW 131 L 101103 90.7 5.2% 

DAL GW 132R 101102 251 4.4°/n 

DAL GW 132S 101102 962 0.52% 

DAL GW 132L 101103 404 3.0% 

DAL GW 133R 101102 102 9.5% 

DAL GW 133S 101103 385 4.2% 

DAL GW 133L 101103 252 12% 

DAL GW 134R 101105 1570 9.6% 

DAL GW 134S 10 1105 5.49 5.5% 

DAL GW 134L 101105 520 1 .3% 

DAL GW 135R 101105 2910 a 1 .4% 

DAL GW 135S 101105 13 .7 3.7% 

DAL GW 135L 101105 123 2.4% 

DAL GW 136S 101103 75.4 3.8% 

DAL GW 136L 101103 75.3 3.1% 

DAL GW 137S 101109 0.271 1 .8% 

DAL GW 137L 101109 0.361 0.28% 

DAL GW 138S 101110 147 3.4% 

DAL GW 138L 101110 1.16 6.1 % 

DAL GW CW26R 101110 386 1,8% 

DAL GW CW26L 1011 .10 552 4 4.7% 

DAL GW 140R 101104 ~ 121 0.83% 

DAL GW 141R 101110 1 .84 10°la 

i DAL GW 142R 101110 " 47.6 4.6°l0 DAL GW 144R 101110 57.3 0.17% 

Trip Blanks Milli-QT"' Water < 0.0250 N/A 

GLP10-01-01-11 Equipment rinseate blanks : 

DAL GW 130L and DAL GW 144R ~ < 0.0250 N/A 

GLP10-01-01-12 Soil Equipment rinseate blank: 

DAL SS 607R < 0.0250 NIA 

N/A; not applicable 

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

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

b The analytical uncertain has been adjusted for field matrix spike recove ry 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 perfluorooctanoate (PFOA) in various environmental media 

Page 10 of 53 
p. 32 

GLP10-01-01; Interim Reoort 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - Novernber 2010 

such as groundwater, soils and sediments that are associated with and near the Decatur facility. This analytical study was conducted to analyze ground water samples collected from various wells located 

at the Former Sludge incorporation Area (FSAI) in Decatur, AL for PFOA in an effort to characterize regional groundwater conditions. 

The 3M Environmental Laboratory prepared sample bottles (250 mL high-density polyethylene) which 

were shipped to Decatur, AL Weston personnel prior to field sampling . Sample bottle sets for each 

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 "fit 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 Perfluorinated 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 prepared 

and analyzed with the samples are reported and discussed elsewhere in this report. 

4 Test 8 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 SLibstanc® PFOA PFOA 

Chemical Name Perfluorooctanoate Perfluorooctanoate 

Chemical Formula C,F,5COOH C7F;5C00- 

Identifier CAS # 335f7-1 Ammonium Salt 

CAS # 335-67-1 

Source Oakwood Products 3M 

Expiration Date 0912912012 02127/2017 

Storage Conditions Frozen Frozen 

Chemical Lot Number 3440 332 

TCR Number TCR07-0041 TCR-123 

Physical Description Powder White Powder 

Purity 99.5'Yo 95% 

Page 11 of .°i3 
p. 33 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

There was not a test system for this study in the classic sense of a GLP study. This study was 

conducted for analysis of ground water samples collected from wells located in Decatur, AL by Weston 

Solutions, Inc. personnel. Samples for this study are "real world" environmental samples. 

Sample Description Key Code. 

Stri ng Number Sfty Descriptor Exampl e 

Example DAL 132R 0101102 

1 Sample Locaaton DAL= Decear, Alabama 

wen to Eranple:1sz 

Well Level R - Rasld+an shallow water-beadng zone 

L = Bedrock water-bearing zkre 

S = Epikarst mirkBe water-beading zone 

s Sampling Daft 101102- n+owamlm z 2010 

Sample Type O--Pdmaiy sample 

1=dupllcate sample 

LS a low Spike 

US mid spike 

I HS = high spike 

7.1 Methods 

Analysis for all analytes was completed following 3M Environmental Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds In Water by High Performance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis°. 

7.2 Sample Collection 

Samples were collected in 250 mL Nalgene~" (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory . Sample bottles associated with GLP10-01-01-11 were returned to the laboratory at ambient conditions on November 18, 2010. The equipment rfnseate blank associated with GLP10-01-01-12 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 in an autov'ral for analysis. 

Samples that required dilution were prepared by dilutions 1 mL sample with 9 mLs of Milli-Q water (dilution 1 :10) . Some sampling locations were diluted 1 :100 by diluting the 1 :10 and additonal with Mil6- Q water. 

7.4 Analysis 

All study samples and quality control samples were analyzed for PFOA using high performance liquid chromatography/ tandem mass spectrometry (HPLC/MSIMS). Detailed instrument parameters, the 

Page 12 of 53 
p. 34 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

liquid chromatography gradient program, and the specific mass transitions analyzed are described in the 

raw data hard copies placed in the final data packet, and are briefly described below in Table 2, Table 3 and Table 4. 

Table 2. Instrument Parameters. 

InstrumetrtNwne ETS Buster 

Ana cal Method Fo(Icwed ETS..8.04q .0 

Ana Date 1/dJ11 - 1l8/11 

Liq uid Chrom ra lent 1100 

Guard column Prism RP 2.1 mm X 50 mm 5 

An I column Betasi C18 2.1 mm X 100 mm), 51, 

I ection Volume 2 or 10 L 

Masa fed Blos API 4000 

[on Source Turbo S 

Electrode Turbo lon electrode 

Po N tive 

Ana 1 .4.2 

Table 3. Liquid Chromatography Conditions . 

Step 

Number 

TOW 7-me 

(min) 

Flow Raft 

(fd./rrrln) 

PencentA 

mM ammonium scalate 

Percent a ' 

0 0 300 . 97 .0 3.0 

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 13.6 300 97.0 3.0 

5 j 17.0 ~ 300 ~ 97.0 3.0 

Table 4. Mass Transitions. 

Anal te Mass Transrtlon y ctvQ3 

4131'Jti9 

PFOA 413319 

4131169 

DWe1 time was 100 msec for each transition, 

The Individual transitions were summed to 

produce a "lotal ion chromatogram' (TIC), 

which was used for quantftation. 

8.1 Calibration 

Samples were analyzed against an extemal standard calibration curve. Calibration standards were prepared by spiking known amounts of the stock solution containing the target anatytes into a laboratory- Mi11i Q water. A total of fifteen spiked standards ranging from 0.025 ng/ml to 100 ng/mL (nominal) were 

Page 13 of 53 
p. 35 

G1 .P10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

prepared. The two highest curve points were disabled to meet linearity criteria . A quadratic, 1/x weighted, calibration curve of the peak area counts was used to fit the data for PFOA. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area confirmed accuracy of each curve point. 

Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 100t25% (100t30% for the lowest curve point) were met for all 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 criteria 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 met for PFOA. 

8.3 Limit of Quantitation (LOQ) 

The LOQ for this analysis is the lowest non-zero calibration standard in 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 (LOO). 

Analysis Date PrcoA 

LOQ, n 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 100% t 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 LOQ 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 coilections 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 triplicate with each preparation set. LCSs were prepared by spiking known amounts of the analyte into 40 mL of laboratory Milli Q 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 level should be within 100% 120% with an RSD 52Qio, 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°l0 . All LCS samples were used in the determination of method uncertainty in section 8.7 . 

Page 14 of 53 
p. 36 

GLP10"01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

The following calculations were used to generate data in Table 6 for laboratory control spikes: 

LGS Percent Recovery Calculated Concentration , = 1009t, 

Spike Concentration 

LCS% RSD = 

standard deviation LCS replicates ,100% 

average LCS recovery 

Table 6. Laboratory Control Spike Recovery . 

ETS-S&044 .0 

Analyzed i13f2011 Linear PFOA 

Spiked Calculated 

Concw*ndbn Concentration 

Lab ID (09~M-9 n mL %Recov 

LCS-101230-1 0.497 0.580 117 

LCS-101230-2 0.497 0.557 112 

LCS-101230-3 0.497 0.590 119 

Ave rage t%RSD 11s%ta.1% 

LCS-101230-4 4.97 5.83 117 

LCS-101230-5 4.97 5.69 

I 

115 

LCS-101230-6 4.97 5.69 114 

Average t %RSD 115°ti tt .3% 

LCS-101230-7 29.9 25.6 85.6 

LCS-101230-8 29.9 25.8 86.3 

LCS-101230-9 29.9 25.7 85.9 

,Ave go t %RSD 85.9°i6 t 0.41% 

ETS-8-044.0 

An 11312011 Linear t Branched PF;OA 

Spiked Calculated 

Concenba8on ConcenbaSon 

Lab ID mL n mL ~ %Recove 

LCS-101230-10 ECF 0.498 0.546 110 

LCS=101230-11 ECF 0.498 0.553 111 

LCS-101230-12 ECF 0.498 0.541 109 

AvBra x %RSO 11100/0±0110% 

LCS-101230-13 ECF 4.99 6.29 126 

LCS-101230-14 ECF 4.99 6.03 121 

LCS-101230-15 ECF 4.99 6.12 123 

A t °1sRSD 123'/a t 2.0% 

LCS-101230-16 ECF 29.9 31.3 105 

LCS-101230-17 ECF 29 .9 30 .8 103 

LCS-101230 -18 ECF 29 .9 30 .6 102 

Average t %RSD 101% t 1 .5'1e 

(1) Laboratory control sample average recovery did not meet method acceptance criteria of 100% t 20%. 

Page 15 of 53 
p. 37 

GtP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

8.7 ~ Analytical Method Uncertainty 

Analytical uncertainty is based on historical QC data that is control charted and used to evaluate 

method accuracy and precision. The method uncertainty is calculated following ETS-12-012 .2 . The 

standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The 

expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which 

corresponds to a confidence level of 95%. 

Table 7. Analytical Method Uncertainty . 

Analyte Method Standard Deviatfon Method 

Uncertain ty 

PFOA E78-8-044.0 11 .3 t 23% 

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 container spiked by the laboratory with the target analytes prior to shipping 

sample containers for sample collection . Field matrix spike recoveries within method acceptance criteria 

of 100t30% confirm that 'unknown" components in the sample matrix do not significantly interfere with 

the extraction and analysis of the analytes of interest. Field matrix spike concentrations must be 50°!0 of 

the sample concentration to be considered an appropriate field spike. Field matrix spikes are presented 

in section 9 of this report. 

Table 8. Field Matrix Spike Levels. 

Sampling Location Spike Level PFOA, nglmL 

Low 0.0991 

136R, 137R, 137s, 137L, 138L Mid 0.991 

High 9.91 

Low 0.991 

13oL, 131 L, 131 S, 1331R, 134S, 135S, 136S Mid 9.91 

High 99 .1 

130R, 130S, 132R, 132L. 132S, 133S, 133L, Low 9.91 

134L, 135L, 1361, 138S, 138R, CVV28R, CW26L, Mid 99.1 

140R, 141R, 142R, 143R, 144R Hig h 991 

3 R 134R 35R 

Low 99.1 1 1 , , 1 High 991 

Low 0.991 ' 

T i Bl k Mid 9.91 r p an Mid-Hi 99 .1 

I High ~ - 991 

FMS Recovery = 

(S ample Concentration of FMS--Average Concentration : Field Sample & Field Sample Dup.) 100% 

Spike Concentraton 

Page 16 of 53 
p. 38 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

y 

~Daf

-, -im 1 1 .1111, a, Suna,r~"aryFa d , Discus 

The tables below summarize the sample results and field matrix spike recoveries for the sampling 

locations as well as the Trip Blanks and rinseate blanks. Results and average values are rounded to 

three significant figures according to EPA rounding rules. Because of rounding, values may vary slightly 

from those listed in the raw data . 

Field matrix spike recoveries meeting the method acceptance criteria of t 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 t 31 %. 

DAL GW 131 R 101103 - 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 . 

DAL GW 135R 101108 -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 17 of 53 
p. 39 

GLP10-01-01; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 9. DAL GW 130R 101105 

PFOA 

Concentration ' 

3M LAWS ID Desc ' 'on mL %Recov 

GLP10-01-01-11-001 DAL GW 130R 0 101105 789 NA 

GLP10-01-01-11-002 DAL GW 130R DB 101105 796 NA 

GLP10-01-01-11-003 DAL GW 130R LS 101105 805 NC 

GLP10-01-01-11-OD4 DAL GW 130R MS 101105 895 NC 

GLP10-01-01-11-005 DAL GW 130R HS 101105 1680 89.6 

Ave Concerlftdon mL t %RPD 793 n mL :t Q88% I 

NA = Not Applicable 

NC = Not Calculated-, Endogenous sample concentration greater than 2x spike level . 

Table 10. DAL GW 130S 101105 

PFpA 

Concenbadon 

3M UMS ID Descri tion m %Recove 

GLP10-01-01-11-006 DAL GW 130S 0101105 174 NA 

GLP10-01-01-11-007 DAL GW 130S DB 101105 173 NA 

GLP10-01-01-11-008 DAL GW 130S LS 101105 183 NC 

GLP10-01-01-11-009 DAL GW 130S MS 101105 270 97.4 

GLP10-01-01-11-010 DAL GW 130S HS 101105 1150 98.5 

Average Concentfadon (nWmL) t %RPD T 1 74 ng/mt t 0.58'rd 

NA = Not Applicable 

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

Table 11. DAL GW 130L 101105 

PFOA 

Concentratlon 

3MLtMSID Descrf Bon n m IRecove 

GLP10-01-01-11-011 DAL GW 130L 0 101105 69.3 NA 

GLP10-01-01-11-012 DAL GW 130L DB 101105 70.7 NA 

GLP10-01-01-11-013 DAL GW 130L LS 101105 71 .0 NC 

GLP10-01-01-11-014 DAL GW 130L MS 101105 73.3 NC 

GLP10-01-01-11-015 DAL GW 130L HS 101105 162 92.8 

Average Concentradon (ng/mL) t %RPD 70.0 ngdnrL t 2.0"i6 

N A= Not Applicable 

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

Page 1 8 of :53 
p. 40 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 12. DAL GW 131R 101103 

PFOA 

COncenfl'dLOn 

3M LfMS ID Descrf !!on mL %Recov 

GLP10-01-01-11-017 DAL GW 131 R 0 101103 2520 NA 

GLP10-01-01-11-018 DAL GW 131 R DB 101103 2480 NA 

GLP10-01-01-11-019 DAL GW 131 R LS 101103 2570 NC 

GLP10-01-01-11-020 DAL OW 131 R HS 101103 3240 NC 

Average Concentration (nglrnL) t V.RPD 2500 nghrrL t 1.6% n~ 

NA = Not Applicable 

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

(1) Sampling location did not have an appropriate spice level to evaluate PFOA recovery . 

Table 13. DAL GW 131 S 101103 

PFOA 

Concenfration 

3M LH14S ID Descri tlon n roL %Recov 

GLP1G`-01-01-11-021 DAL GW 131 S 0101103 25.4 NA 

GLP10-01-01-11-022 DAL GW 131 S DB 101103 24.4 NA 

GLP10-01-01-11-023 DAL GW 131 S LS 101103 25.3 NC 

GLP10-01-01-11-024 DAL GW 131S MS 101103 34.6 NC 

GLP10-01-01-11-02 5 DAL GW 131S HS 101103 127 103 

Average Concentradon (ngimL) t %RPD ~ 24.9 n94mL t 4.0'/ 

NA = Not Applicable 

NC = Not Calculated: Endogenous sample cancentration greater than 2x spike Level . 

Table 14. DAL GW 131 L 101103 

PFOA 

Concenfvadon 

3M LIMS ID Descri tlon mL I Recove 

Gt-P10-01-01-11-026 DAL GW 131 L 0 101103 88.3 NA 

GLP10-01-01-11-027 DAL GW 131L DB 101103 93 .0 NA 

GLP10-01-01-11-028 DAL GW 131 L LS 101103 87.7 NC 

GLP10-01-01-11-029 DAL GW 131 L MS 101103 96.9 NC 

GLP10-01-01-11-03 0 DAL GW 131L HS 101103 179 89 .2 

Average Concentrafton (ng/rnL) t %RPD 90.7 ng/mL t 5.2"/ 

NA = Not Applicable 

NC a Not Calculated ; Endogenous sample coricentradon greater than 2x spike level. 
p. 41 

G1F10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge incorporation Area - November 2010 

Table 15. DAL GW 132R 101102 

PFOA 

Concenbation 

3M LJJbS ID ' D=2 don n mL %Reco 

GLP10-01-01-11-031 DAL GW 132R 0101102 256 NA 

GLP10-01-01-11-032 DAL GW 132R DB 101102 245 NA 

GLP10-01-01-11-033 DAL GW 132R LS 101102 267 NC 

GLP10-01-01-11-034 DAL GW 132R MS 101102 356 NC 

GLP10-01-01-11-035 DAL GW 132R HS 101102 1160 91 .8 

Average Concentmtion (nglmL) t %RPD l 251 no/ML t 4.4% I 

NA - Not Applicable 

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

Table 16. DAL GIN 132S 101102 

PFOA 

Concentration 

3M LIlNS 1D Descri on n mL %Reco i 

GLP10-01-01-11-036 DAL GW 132S 0101102 959 NA 'i 

GLP10-01-01-11-037 DAL GW 132S DS 101102 964 NA 

GLP10-01-01-11-038 DAL GW 132S LS 101102 926 NC 

GLP10-01-01-11-039 DAL GW 132S MS 101102 1020 NC 

GLP1 0 _ _ -01-01-11-040 DAL GW 132S HS 101102 1810 85 .6 

Average Concerrbatforr (ng4nL) t %RPD 962 ngftL t Q 5Y.6 

NA = Not Applicable 

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

Table 17. DAL GI N1321-101103 

PFOA 

Concentraffon 

3M UMS 1D Description n rn %Recove 

GLP10-01-01-11-041 DAL GW 132L 0101103 398 NA 

GLP10-01-01-11-042 DAL GW 132L 08 101103 410 NA 

GLP10-01-01-11-043 DAL GW 132L LS 101103 451 NC 

GLP10-01-01-11-044 DAL GW 132L MS 101103 482 NC 

GLP10-01-01-11-045 DAL GW 132L HS 101103 1290 89.4 

Average Concenbaffon (ng/mL) t %RPD 404 ng/mt t 3_0-/ 

NA = Not Applicable 

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

Page 20 of 53 
p. 42 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 18. DAL GW 133R 101102 

PFOA ' 

Concentration 

3M LIMS ID Descrf tfon mL %Recove 

GLP10-01-01-11-046 DAL GW 133R 0101102 107 NA 

GLP10-01-01-11-047 DAL GW 133R DB 101102 97.3 NA 

GLP10-01-01-11-048 DAL GW 133R LS 101102 102 NC 

GLP10-01-01-11-049 DAL GW 133R MS 101102 108 NC 

GLP10-01-01-1 1-050 DAL GW 133R HS 101102 193 91 .7 

Average ConcentraUon (nglmL) t %.RPD 102 nallmL t 9.5% 

NA = Not Applicable 

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

Table 19. DAL GW 133S 101103 

PFOA 

Concentration 

3M UMS !D Desc ' on n ML oReco 

GLP10-01-01-11-051 DAL GW 1333 0101103 393 NA 

GLP10-01-01-11-052 DAL GW 133S DB 101103 377 NA 

GLP10-01-01-11-053 DAL GW 133S LS 101103 407 NC 

GLP10-01-01-11-054 DAL GW 133S MS 101103 485 NC 

GLP10-01 -01-11-055 DAL GW 133S HS 101103 1260 B8.3 

Average Concentraffon (ng/mL) t %RPD 385 ng/mL t 4.2'/ 

NA = Not Applicable 

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

Table 20. DAL GW 133L 101103 

PFOA 

Concentration 

3M L1MS ID Descrtr Uon n mL %Recove 

GLP10-01-01-11-056 DAL GW 133L 0 101103 253 NA 

GLP10-01-01-11-057 DAL GW 133L DB 101103 250 NA 

GLP10-01-01-11-058 DAL GW 133L LS 101103 265 NC 

GLP10-01-01-11-059 DAL GW 133L MS 101103 355 NC 

GLP10-01-01-11-060 DAL GW 133L HS 101103 1190 94.7 

Av Concentration n m t I RPD 252 n mL t 1 .2% 

NA = Not Applicable 

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

Page 21 of 53 
p. 43 

GLP10-01-01 ; interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 21 . DAL GW 134R 101105 

PFOA 

ConcentYaflion 

3M L1MS ID Descrf don n mL %Recov 

GLP10~01-01-11-061 DAL GW 134R 0 101105 1640 NA 

GLP10-01-01-11-062 DAL GW 134R DB 101105 1490 NA 

GLP10-01-01-11-063 DAL GW 134R LS 101105 1620 NC 

GLP10-01-01-11-064 DAL GW 134R HS 101105 2250 69.1 «1 

Average CorncentraLion (ng/mL) t %RPD 1570 ng(mL 19.6% 

NA = Not Applicable 

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

(1) Field matrbc spike did not meet method acoeptance criteria of 100% t 30%. 

Table 22. DAL GW 134S 101105 

PFOA 

Concentration 

3M UMS fD DescN on n mL %Recov 

GLP10-01-01-11-065 DAL GW 134S 0101105 5.64 NA 

GLP10-01-01-11-066 DAL GW 134S DB 101105 5.34 NA 

GLP10-01-01-11-067 DAL GW 134S LS 101105 6.95 NC 

GLP10-01-01-11-068 DAL GW 134S MS 101105 16.6 112 

GLP10-01-01-11-069 

- 

DAL GW 134S HS 101105 102 97.4 

Average Concentration (n L) t %RPD 5.49 ng/mL t 5 5% 

NA = Not Applicable 

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

Table 23. DALGW 134L 101105 

PFOA ' 

ConcentYatYon 

3M LfMS ID Descd tlon n mL %Recove 

GLP10-01-01-11-070 DAL GW 134L 0101105 523 NA 

GLP10-01-01-11-071 DAL GW 134L DB 101105 516 NA 

GLP10-01-01-11-072 DAL GW 134L LS 101105 530 NC 

GLP10-01-01-11-073 DAL GW 134L MS 101105 599 NC 

GLP10-01-01-11-074 DAL GW 134L HS 101105 1 390 87.8 

Average Concentyatlort (no/mL) 3 %RPD ~ 

_ 

520 ncymL t 13% I 

NA = Not Applicable 

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

Page 22 of 53 
p. 44 

GLP10-01-01 ; Interim Report 11 

Ana" of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 24. DAL GW 135R 101105 

PFOA 

Conceniradon 

3M LIMS 1D Descrtr tlon nrL ~Recov 

GLP10-01-01-11-075 DAL GW 135R 0101105 2930 NA 

GLP10-01-01-11-076 DAL GW 135R DB 101105 2890 NA 

GLP10-01-01-11-077 DAL GW 135R LS 101105 2930 NC 

GLP10-01-01-11-078 DAL GW 135R HS 101105 3840 NC 

Average Conceittra8on (ng(mL) t %RPD 1 2910 ngumL t 1.4% (1) 

NA - Not Applicable 

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

(1) Sampling location did not have an appropriate spike level to evaluate PFOA recovery. 

Table 25. DAL GW 135S 101105 

PFOA 

Concentration 

3M LIMS W Descri on mL I Recov 

GLP10-01-01-11-079 DAL GW 135S 0 101105 13 .9 NA 

GLP10-01-01-11-080 DAL GW 135S DB 101105 13.4 NA 

GLP10-01-01-11-081 DAL GW 135S LS 101105 14 .5 NC 

GLP10-01-01-11-082 DAL GW 135S MS 101105 24.2 105 

GLP10-01-01-11-083 DAL GW 135S HS 101105 110 97.2 

Ave ConcentraNon L t %RPD 13.7 n mL t 3.T/ 

NA = Not Applicable 

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

Table 26. DAL GW 135L 101105 

PFOA 

Concenbadon 

3M LOS ID Descri tlon mt %Recov 

GLP10-01-01-11-084 DAL GW 135L 0 101105 124 NA 

GLP10-01-01-11-085 DAL GW 135L DB 101105 121 NA 

GLP10-01-01-11-086 DAL GW 135L LS 101105 129 NC 

GLP10-01-01-11-087 DAL GW 135L M5101 105 226 104 

GLP10-01-01-11-088 DAL GW 135L HS 101105 1070 95.6 

Average Concenbatfon (naJmL) t %RPD ~ 123 nadmL t 2.4% 

NA - Not Applicable 

NC = Net Calculated ; Endogenous sample concentration greater than 2x spike level. 

Page 23 of 53 
p. 45 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 27. DAL GW 136S 101103 

PFOA 

ConcentYaBon 

3M LIMS !D Desc tfon n m %Recov 

GLP10-01-01-11-089 DAL GW 136S 0101103 73.9 NA 

GLP10-01-01-11-090 DAL GW 136S 08 101103 76.8 NA 

GLP10-01-01-11-091 DAL GW 136S LS 101103 77.6 NC 

GLP10-01-01-11-092 DAL GW 136S MS 101103 86 .1 NC 

GLP10-01-01-11-093 DAL GW 136S HS101103 166 91 .5 

Average ConcentYdtion (nghnt) t %RPD 75.4 nqVmL t 3.8"4 

NA = Not Applicable 

NC = No( Calculated : Endogenous sample Conoentration greater than 2x spike level. 

Table 28. DAL GW 136L 101103 

PPOA 

Concentration 

3M LIMS ID D!rc t9on mL %Recov 

GLP10-01-01-11-094 DAL GW 136L 0101103 74.1 NA 

GLP10-01-01-11-095 DAL GW 136L DB 101103 76.4 NA 

GLP10-01-01-11-096 DAL GW 136L LS 101103 86.2 NC 

GLP10-01-01-11-097 DAL GW 136L MS 101103 169 94.6 

GLP10-01-01-11-098 DAL GW 136L HS 101103 1030 96.3 

Average Concentraldon (n!gVmL) t %RPD 75.3 nymL t 3.1% 

NA - Not Applicable 

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

Table 29. DAL GW 137S 101109 

PFOA 

ConcemYaNon 

3M LJMS ID Descri 'on I mL %Recov 

GLP10-01-01-11-099 DAL GW 137S 0101109 0 .273 NA 

GLP10-01-01-11-100 DAL GW 137S DB 101109 0 .268 NA 

GLP10-01-01-11-101 DAL GW 137S LS 101109 0.350 NC 

~GLP10-01-01-11-102 DAL GW 137S MS 101109 1 .32 105 

IGLP10-01-01-11-103 DAL GW 137S HS 101109 10.9 107 

Average Concenfradon n mL t %RPD 0.271 n mL t 1 .8% 

NA - Not Applicable 

NC m Not Calculated ; Endogenous sample concentration greater than 2x spike level. 
p. 46 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 30. DAL GW 137L 101109 

PFOA 

Concenbation 

3M UMS ID Descri don n mL %Recove 

GLP10-01-01-11-104 DAL GW 137L 0 101109 0.360 NA 

GLP10-01-01-11-105 DAL GW 137L 08 101109 0.381 NA 

GLP10-01-01-11-106 DAL GW 137L LS 101109 0.458 NC 

GLP10-01-01-11-107 DAL GW 137L MS 101109 1 .40 105 

GLP10-01-01-11-108 DAL GW 137L HS 101109 10 .7 104 

Average Concentxadan (ng/mt) t %RPD 0.361 ng~mL t 0.28% 

NA = Not Applicable 

NG = Not Calculated; Endogenous sample concentration greater than 2x spike levet. 

Table 31 . DAL GW 138S 101110 

PFOA 

Concenfiatlon 

3M LOS ID Descri on n mL %Recove 

GLP10-01-01-11-109 DAL GW 138S 0 101110 149 NA 

GLP10-01-01-11-110 DAL GW 138S DB 101110 144 NA 

GLP10-01-01-11-111 DAL GW 138S LS 101110 162 NC 

GLP10-01-01-11-112 DAL GW 138S MS 101110 230 84.3 

G_LP10-01-01-11-113 DAL GW 138S HS 101110 1020 88.1 

Average Concentration (ng/mL) t %RPD 147 n9mL t 3.4% 

NA = Not Appucable 

NC = Not Caiadated; Endogenous serrVe concentration greater than 2x spike level. 

Table 32. DAL GW 138L 101110 

PFOA 

Concen&adon 

3M L1MS ID Descri tion n ML %R2= 

GLP10-01-01-11-114 DAL GW 138L 0 101110 1 .19 NA 

GLP10-01-01-11-115 DAL GW 138L DB 101110 1 .12 NA 

GLP10-01-01-11-118 DAL GW 138L LS 101110 1 .24 NC 

GLP10-01-01-11-117 DAL GW 138L MS 101110 2.18 103 

GLP10-01-01-11-118 DAL GW 138L HS 101110 11 .2 101 

A ConcerrtraGion n m t I RPD 1 .16 nglmL t 6.1 % 

NA = Not Applicable 

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

Page 25 of 53 
p. 47 

GLP10-01-01 ; Intenm Report 11 

Analysis of PFOA in Groundwater 

Former Sludge incorporation Area - November 2010 

Table 33. DAL GW CW26R 101110 

PFOA 

Concentratlon 

3M LIMS !D Descrf tlon mL %Recove 

GLP10-01-01-11-119 DAL GW CW26R 0101110 382 NA 

GLP10-01-01-11-120 DAL GW CW26R 08 101110 389 NA 

GLP10-01-01-11-121 DAL GW CW26R LS 101110 395 NC 

GLP10-01-01-11-122 DAL GW CW26R MS 101110 450 NC 

GLP10-01-01-11-123 DAL GW CW26R HS 101110 1290 91 .3 

Average ConcentraHon (ng/mL) t %RPD 386 mL 11. 8 % 

NA = Not Applicable 

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

Table 34. DAL GW CW26L 101110 

PFOA I 

Concentranfon 

3M L1MS ID Descrf 8on m %Recov 

GLP10-01-01-11-124 

_ __-- 

~DAL GW CW26L 0101110 565 NA 

GLP10-01-01-11-125 DAL GW CW26L DB 101110 539 NA 

GLP10-01-01-11-126 DAL GW CW26L LS 101110 552 NC 

GLP10-01-01-11-127 DAL GW CW26L MS 101110 523 NC 

GLP10-01-01-11-128 DAL GW CW26L HS 101110 1480 93.6 

Average Concentradon n mL i %RPD 552 mL t 4.7 0 

NA - Not Applicable 

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

Table 35. DAL GW 140R 101104 

Pr-OA 

Concentratfon 

3M LIMS !D Descn' 8on rnL I Recove 

GLP10-01-01-11-129 DAL GW 140R 0 101104 121 NA 

GLP10-01-01-11-130 DAL GW 140R DB 101104 120 NA 

GLP10-01-01-11-131 DAL GW 140R LS 101104 128 NC 

GLP10-01-01-11-132 ~ DAL GW 140R MS 101104 217 97 .4 

GLP10-01-01-11-133 DAL GW 140R HS 101104 973 86.0 

Average Concenbetlon n mL f %RPO 121 n mL t 0.83 % 

NA = Not Applicable 

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

Page 26 of 53 
p. 48 

GLP10-01-01 ; Intenm Report 11 

Analysis of PFOA in Groundwater 

Farmer Sludge Incorporation Area - November 2010 

Table 36. DAL GW 141R 101110 

PFOA 

Concentration 

3M LtMS ID Descr! tlon n mL %Recove 

GLP10-01-01-11-134 DAL GW 141 R 0 101110 2.13 NA 

GLP10-01-01-11-135 DAL GW 141R DB 101110 1 .55 NA 

GLP10-01-01-11-136 DAL GW 141 R LS 101110 11 .4 96.5 

GLP10-01-01-11-137 DAL GW 141 R MS 101110 95 .5 94.5 

GLP10-01-01-11-138 DAL GW 141 R HS 101110 908 91 .4 

Avera ConcenOratlon n m t %RPD 1.84 n mL t 10 % 

NA a Not Applicable 

NC " Not Calculated; Endogenan sample concentration greater than 2x spike level, 

Table 37. DAL GW 142R 101110 

PFOA 

Concentration 

3M LIMS !D Descr! on n rnL %.Recov 

GLP10-01-01-11-139 DAL GW 142R 0101110 46.5 NA 

GLP10-01-01-11-140 DAL GW 142R DB 101110 48.7 NA 

GLP10-01-01-11-141 DAL GW 142R LS 101110 55 .3 NC 

GLP10-01-01-11-142 DAL GW 142R MS 101110 143 96.3 

GLP10-01-01-11-143 DAL GW 142R HS 101110 925 88.5 

Average Concentradon (na/mL) t %RPD ~ 47. 6 ncymL t 4. 6 % 

NA = Not Applicable 

NC = Not Calculated : Endogenous sample concentration greater than Dc spike level . Table 38. DAL GW 144R 101110 

PFOA 

Concentration 

3M L1MS 1D Descrl 8on n mL %Recove 

GLP10-01-01-11-144 DAL GW 144R 0 101110 57.2 NA 

GLP10-01-01-11-145 DAL GW 144R DB 101110 57.3 NA 

GLP10-01-01-11-146 DAL GW 144R LS 101110 67.6 NC 

GLP10-01-01-11-147 DAL GW 144R MS 101110 142 85.5 

GLP10-01-01-11-148 DAL GW 144R HS 101110 g6g 91 .7 

Average ConcenbaLlon n m t %RPD 57.3 n mL t 0.17 % 

NA = Not Applicable 

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

Page 27 of 53 
p. 49 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 39. Trip Blank 1 

PFOA 

ConcentraGfon 

3M UMS ID Descri on & *M 11%, ecov 

GLP10-01-01-11-150 TRIP BLANK 1 0 <0.0250 NA 

GLP10-01-01-11-151 TRIP BLANK 1 LS 1 .08 109 

GLP10-01-01-11-152 TRIP BLANK 1 MS 10 .6 107 

GLP10-01-01-11-153 TRIP BLANK 1 MHS 99 .1 100 

GLP10-01-01-11-154 TRIP BLANK 1 HS 1040 105 

NA = Not Applicable 

Table 40. Trip Blank 2 

PFOA 

Concentradon 

3M LJMS ID Descrl Llon n %Recove 

GLP10-01-01-11-155 RIP BLANK 2 0 <0 .0250 NA 

GLP10-01-01-11-156 TRIP BLANK 2 LS 1 .08 109 

GtP10-01-0i-1 i-157 RIP BLANK 2 MS 10 .9 110 

GLP10-01-01-11-158 TRIP BLANK 2 MHS 96.9 97.8 

GLP10-01-01-11-159 TRIP BLANK 2 HS 1020 103 

NA = Not Applicable 

Table 41 . Trip Blank 3 

PFOA 

Concenfradon 

3M LIMS f0 Descri don n mL %R ecove 

GLP10-01-01-11-160 TRIP BLANK 3 0 <0.0250 NA 

GLP10-01-01-11-161 TRIP BLANK 3 LS 1 .07 108 

GLP10-01-01-11-162 TRIP BLANK 3 MS 10.4 105 

GLP10-01-01-11-163 TRIP BLANK 3 MHS 101 102 

GLP10-01-01-11-164 TRIP BLANK 3 HS 1050 106 

NA = Not Applicable 

Page 28 of 53 
p. 50 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Table 42. Trip Blank 4 

' PFOA 

i 

~ ConcentraUon 

3M LOS ID Descal tlon ~ n mf. I Recov 

GLP10-01-01-11-165 TRIP BLANK 4 0 <0.0250 NA 

GLP10-01-01-11-166 TRIP BLANK 4 LS 1 .06 107 

GLP10-01-01-11-167 TRIP BLANK 4 MS 10.4 105 

GLP10-01-01-11-168 TRIP BLANK 4 MHS 95 .4 96 .3 

GLP10-01-01-11-169 TRIP BLANK 4 HS 985 99,4 

NA a Not Applicable 

Table 43. Rinseate Blanks 

PFOA 

Concent3ra8on 

3M L1MS ID Descri don n m %Recove 

GLP10-01-01-11-016 DAL GW 130L RB 101105 <0.0250 NA 

GLP10-01-01-11-149 DAL GW 144R RB 101110 <0.0250 NA 

GLP10-01-01-12-009 DAL SS 607R RB 0040 <0.0250 NA 

NA = Not AppIicable 

Page 29 of 53 
p. 51 

GLP10-01-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

0 C ~r~luslon~~ ` 

Laboratory control spikes and field matrix spikes were used to determine the analytical method 

accuracy and precision for PFOA. Analysis was successfully completed following 3M Environmental Laboratory mett-od ETS-8-044 .0 described herein . 

' i . : . ~ s~ ~ ~h - ~_.alSampte~Reteiltio ,"rt~.~-~ 

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 B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytfcal Method - ETS-8-044.0 

Attachment D: Method Deviation 

Page 30 of 53 
p. 52 

GLP10-Ot-01 ; Interim Report 11 

Analysis of PFOA in Groundwater 

Former Sludge Incorporation Area - November 2010 

Cleston Lange, Ph.D., 3M Principal Analytical Investigator Date 

q~0-'.t,r~ Do// 

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

4 U W7yfZ//TL 

2 

I-MA 

Gary Hohe*ein, 3M Sponsor Representative Date- 

, Study Director 

2/zillI 

0ate 

Page 31 of 53 
p. 53 

ATTACHMENT 2 

SOIL AND SEDIMENT SAMPLING 

TECHNICAL PROGRESS REPORT 

JANUARY 1, 2011 - MARCH 31, 2011 

1 \EOLDERS .0~9\7M-DECA7Th- 3 w'ork Pl .um\IQI I Slams Repon\IQI I Stems Rcpcvt FINALdh, J/p7/2p11 
p. 54 

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 l . 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 (SS 10 - 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 l . 

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 

1 .VOLDERS .0-9\3M -DECAiIPhaee 3 Work Plan\IQI I Siems RepcKt\IQI I Ststue Rep- FINAL.Joc a/28L1011 

Att 2-1 
p. 55 

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 . 

1 :\FODERS .0-9\3M-DECA71Phau 3 Wirck Pivm\IQI I Sin ., Repx,\IQI I Siuw, Rel,. FINALAc J/27/2011 

Att 2-2