# 3M

Company St. Paul, Minnesota



# PerfluorooctanoicAcid (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 NOCE?'

# Perfluorooctanoic Acid (PFOA) Site Related Environmental Assessment Program 3MDecatur, 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 GROUNDWATERSAMPLING TECHNICAL PROGRESS REPORT 2 SOIL AND SEDIMENT SAMPLING TECHNICAL PROGRESS

REPORT

J,\FOLDERS 0-9\3M-DECATPhase3Work Plan\1011 Status ReportN011 Status Report FINALdoo 4/2712011 1

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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, 3Mand Dyneon LLC are undertaking a Perfluorooctanoic Acid (PFOA) SiteRelated Environmental Monitoring and Assessment Programat their Decatur, Alabama, plant . Per the agreement between EPA and 3M, this report represents the status report of this effort as required by the MOUfor 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 MOUactivities. 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 Programbeing 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 fromon-site and off-site Phase 3 sample collection and fromon-site non-MOU related sampling activities . " Vegetative Uptake Study - Based on reviewof 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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### GROUNDWATER TECHNICAL PROGRESS REPORT 3M ANDDYNEON 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 rawdata, 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 from14 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 reviewof 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 fromthat 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

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### 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 lowyield and high turbidity, was purged using a peristaltic pump and low-flowpurging 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 fromthe 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 fromthe disposable bailer prior to use in sampling MW-01 . Atrip 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 Form er Sludge Incorporation Area Monitoring Wells 3Mimplemented 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 programincludes 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, InterimReport 11, is provided in

J:IFOLDERS0-9\3M-DECATPhase 3 Work Plan\1011 Status Report\1011 Status Report FINAL .dot 4/27/2011 

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### Appendix Aand 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 AArea 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 Aassessment is intended to obtain additional data for the NPDES Remedial Action Agreement being undertaken by 3Mfor the ADEM NPDES programand is not an MOU-related activity. Monitoring locations included two samples collected fromsoil sampling locations in the marsh area, west of the inactive landfill, and one sample was collected frommonitoring 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 belowgrade for location S22 and S24, respectively. Additional information regarding the soil

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### sampling locations is provided in Attachment 2 . The depth to groundwater was measured at 3.65 feet belowground 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 - NOVEMBER2010 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 . Residuumgroundwater elevation contours are shown in Figure 4 and bedrock groundwater elevation contours are shown in Figure 5.

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### 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 3Work Plan\1Q11 Status Report\Attachment 1\Table 1 FSIA GW PFOA DATA Nov 2010.xlsx-AVG_Data

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Imagery Source: ESRI, i-cubed, USDA FSA, USGS, AEX, GeoEye, Getmapping, Aerogri(A, IGP . 2010

hlonitoritw, Well Locations (Cliuter5) - :0i -, Figure 1 BFI Morris Farms Landfill Groundwater Sampling Decatur, AL

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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 mng/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 - ResiduumWell S - Epikarst Well L - Bedrock Well 800 400 0 Feet Figure 2 Former Sludge Incorporation Area Groundwater PFOA Sampling November 2010 Decatur, AL

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# APPENDIX A TOATTACHMENT 1 GLP10-01-01 INTERIMREPORT 11 The full data package, including rawdata, is provided in the RawData Appendix.

1:\FOLDERSC-9-3M-DECA91Phase 3 H4,rk Plau\IQI I Stalus Rcpcxi\IQI I St-, Repom FINAL d« 4/27/201 1GLP10-01-01 . Interim Report 11. " Analysis of PFOA In Groundwater Samples Collected at the Former Sludae incorDoration Area (FSIA) located in Decatur. AL in Novem ber 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 EPATSCA Good Laboratory Practice Standards 40CFR Part 792 Study Director Jaisimha Kesari P

.E., DEE Weston Solutions, Inc

. 1400Weston Way West Chester, PA 19380 Phone: 610-701-3761 Author Susan Wolf 3MEnvironmental Laboratory InterimReport 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 ISO9001 :2000

. Certificate #2052.01

### p. 23 GLP10-01-01 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - November 2010

This page has been reserved for specific country requirements.

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### p. 24 GLP10-01-01 ; IntenmReport 11 Analysis of PFOAin Groundwater Former Sludge Incorporation Area - November 2010



### GLP COMPLIANCE STATEMENT Report Title: GLP10-01-01, InterimReport 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, 40CFR 792, with theexceptions listed below : 

### " These are environmental samples where there is no specific test substance, no specific test system and nodosing of a test system . " The reference substances have not been characterized under theGI-Ps and thestability under storage conditions at thetest site have not been determined under GI-Ps.

Date 

# ~dzlbl Jaisimha Kesari, P

.E., DEE, Study Director Date

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### p. 25 GLP10-01-01 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - November 2010



### QUALITYASSURANCE STATEMENT Report Titie

: GLP10-01-01, InterimReport 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 3MEnvironmental Laboratory Quality Assurance Unit (QAU), as indicated below . The findings were reported to the principal investigator (P.I .), laboratory management and studydirector. 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

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### p. 26 GLP10-01-01 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - November 2010



### TABLE OF CONTENTS GLPCompliance 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 SystemSuitability . .. .. ... .. ... . .. ... ... . .. . ... .. . .. . ... ... . .. . .. ... .. . ... . .. ... .. . .. . .. .. ... .... .. ... . .. ... . .. .. ... . .. .... .14 8.3 Limit of Gluantitation (LOQ) .. .. . ... ... ... ... .. ... .. . ... .. ... ... .. . .. . .. ... .. . ... ... . .. ... .. .:. . .. ... . .. .. . ... . .. . .. .14 8 .4 Continuing CalilJraGon .. ... ... .. . .. ... . .. ... .... ... .. . ... ... .. ... . . ... .. . .. .... . ... . . .. .. ... ... ., . . . ..... .. .... .. . .. . .. .14 8 .5 Blanks ... .. . .. . .. ... .. .. .. ... ... .. . .. ... .. ... ... . .. ... ... ... ... ... ... .. ... . . ... ... .. . ... .. .... ... .. ... ... ... ... .... .. ... .. . ... .. .14 8 .6 LabControl Spikes (LCSs) .. . ... ._. ... . ... .. ... ... . .. . ... .. . ._.. ... ... . ... ... ... .. .... ... .. ... .. . ... ... ... . . .14 8 .7 Analytical Method Uncertainty . . ... ... .. . .... ... ... .. . .. . .. . .. ... .. . .. ... .. ... .. . .. .... .. ... ... . .. ... .... .. . ... ... . .16 8 .8 Field Matrix Spikes (FMS) .. . .. ... . .. ... .. .. ... ... ... . ... .. . .. . .. ... ... ... ... .. ... ... .. . .. . .. ... .. . ... .. .... .. . ... ... . .16

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### p. 27 GLP10-01-01 : InterimReport 11 Analysis of PFOA in Groundwater 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

Page 6of 53

### p. 28 GLP10-01-01 ; InterimReport 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

Page 7 of 53

### p. 29 GLP10-01-01 ; InterimReport 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 3MEHS Operations 3MEnvironmental Laboratory Building 260-5N-17 Maplewood, MN 55106 Study Personnel 

### WilliamK . Reagen, Ph.D., 3MLaboratory Manager Cleston Lange, Ph.O

., Principal Analytical Investigator. (clanueOmmm .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 InterimReport Signing Location of Archives All original raw

data and the analytical report have been archived at the 3MEnvironmental Laboratory according to 40 CFR Part 792 . The test substance and analytical reference standard reserve samples are archived at the 3MEnvironmental Laboratory according to 40 CFR Part 792

Page 8 of 53

### p. 30 GLP10-01-01 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporahon Area - November 2010

The 3M Environmental Laboratory received groundwater samples fromwells 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 fromeach sampling location. Samples also included at least twofield 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 fromGLP10-01-01-12 was analyzed. The equipment rinseate blanks did not have FMSsamples prepared for determination of PFOA recovery. Thegroundwater samples, trip blanks and twoequipment rinseate blanks associated with GLP10-01- 01-10were received fromWeston personnel on November 18, 2010 . Theequipment rinseate blank associated with GLP10-01-01-12 was received from Weston personnel on October 15, 2010. All ofthe sampleswere prepared and analyzed for PFOAfollowing 3M Environmental Laboratory Method ETS8-044.0 under 3M

project GLP-10-01-01-11 . Many of thegroundwater samples required dilution to attain PFOAconcentrations within the rangeof thecurve, in some instances up to 100-fold dilution were required. The average measured PFOAconcentrations are summarized in Table 1 . The equipment rinseates and thetrip 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 PFOAconcentration results for all groundwaters ranged over fourorders of magnitude from 0 .271 ng/mL to 2910 ng/mL

. The analytical uncertainty was estimatedat 100+ 23% .

Page 9of 53

### p. 31 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 R101103 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% Tri p 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 PFOAwasestimated at 100 + 23%
. (aj Sampling location did not have an appropriate FMS spike level to sufficiently evaluate PFOArecovery. b The anal ytical uncertain 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 forthe 3M

facility located in Decatur, Alabama. Theobjective 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 ; InterimReoort 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - Novernber 2010

such as groundwater, soils and sediments that areassociated with and near the Decaturfacility. This analytical study was conducted to analyze ground water samples collected fromvarious wells located at the Former Sludge incorporation Area (FSAI) in Decatur, AL for PFOAin an effort to characterize regional groundwater conditions
. The 3MEnvironmental 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 producea final sample volume of 200 mL. Containers designated for field matrix sampleswere fortified with an appropriate matrix spike solution containing PFOAprior to beingsent to the field for sample collection. See section 8 .8of the report for field matrix spike levels. Samples were prepared. and analyzed according to the procedure defined in 3MEnvironmental 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 andanalyzed with thesamples are reported anddiscussed elsewherein this report. 

### 4 Test 8 Control Substances There was not a test substance or control substances in the classic sense of a GLPstudy. This study was purely analytical in nature. 

### 5 Reference Substances Theanalytical referencesubstances 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 AmmoniumSalt 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 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - November 2010

There was not a test systemfor 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 forthis study are "real world" environmental samples
. Sample Description Key Code. Stri ng Number S fty Descri ptor Exam pl e Example DAL 132R0101102 1 Sample Locaaton DAL= Decear, Alabama 

### wen to Eranple:1sz Well Level R - Rasld+anshallow water-beadngzone L = Bedrockwater-bearing zkre S =Epikarst mirkBewater-beadingzone 

### s Sampling Daft 101102- n+owamlm z 2010 Sample Type O--Pdmaiysample 1=dupllcate sample LS alow Spike US midspike I HS = high spi ke



## 7.1 Methods Analysis for all analytes wascompleted 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 250mL 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 . Theequipment 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 . Aset of laboratory prepared Trip BlankandTrip 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-Qwater (dilution 1 :10) . Some sampling locationswere diluted 1 :100 by diluting the 1 :10 and additonal with Mil6- Q water. 

### 7.4 Analysis All study samples and quality control sampleswere analyzed for PFOAusing high performance liquid chromatography/ tandemmass spectrometry (HPLC/MSIMS)

. Detailed instrument parameters, the

Page 12 of 53

### p. 34 GLP10-01-01 ; InterimReport 11 Analysis of PFOAin Groundwater Former Sludge Incorporation Area - November 2010
liquid chromatography gradient program, and the specific mass transitions analyzed aredescribed 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 Liquid Chrom ra lent 1100 Guard column PrismRP 2 .1 mm X 50 mm 5 An I column Betasi C18 2 .1 mm X 100 mm

), 51, I ection Volume 2or 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 thetarget anatytes into a laboratory- Mi11i Q water. Atotal offifteen spiked standards ranging from0 .025 ng/ml to 100 ng/mL (nominal)were

Page 13 of 53

### p. 35 G1 .P10-01-01 ; InterimReport 11 Analysis of PFOAin Groundwater Former Sludge Incorporation Area - November 2010 prepared. Thetwo highest curve points were disabled to meet linearity criteria. Aquadratic, 1/x weighted, calibration curve ofthe peak area counts was used to fit thedata for PFOA . The data were not forced through zero during thefitting process. Calculating the standard concentrations using the peak area confirmed accuracy of each curve point. Each curve point wasquantitated using theoverall calibration curveand reviewed foraccuracy. Method calibration accuracy requirements of 100t25%(100t30%for the lowest curve point) were met for all analytes
. Thecorrelation coefficient (r) was greater than 0 .995for PFOA 

### 8 .2 SystemSuitability Acalibration 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%RSDwas met for PFOA

. 

### 8 .3 Limit of Quantitation (LOQ) The LOQfor 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 thoseof the appropriate blanks. Thenominal 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 thecourse of each analytical sequence, continuing calibration verification samples (CCVs) were analyzed to confirmthat 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 performanceto determinethe LOQfor PFOA . Trip blanks reflect the shipping and sample collection conditons the sample bottles and samples experience
. Equipment rinseate blanks are aqueous samples that reflect theefficiency of equipment cleaning in the field between different sample coilections and are proofof no cross contamination of samples fromthe 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 theanalyte into 40 mL of laboratory Milli Q water, to produce the desired concentration
. The spiked water samples were then analyzed in thesame manner as the samples. The method acceptance criteria, average of LCS at each level should be within 100%120% with an RSD 52Qio, were metfor the linear PFOA LCS samples. As the reference materials used for quantitation of PFOA is predominantly linear, and the PFOA present in thewater samples arecomprised of linear and branched isomers, additional LCSsamples of linear and branched PFOAwere 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 sampleswere used in the determination of method uncertainty in section 8 .7. Page 14of 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 6for laboratory control spikes: LGSPercent 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 LabID (0

9~ 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 A verag e 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 got%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%t1 .5'1e (1) Laboratory control sample average recoverydid not meet method acceptance criteria of 100%t 20% .

Page 15 of 53

### p. 37 GtP10-01-01 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - November 2010



## 8.7 ~ Analytical Method Uncertainty Analytical uncertainty is based on historical QCdata 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 QCsamples. The expanded uncertainty is calculated by multiplying the standard deviation by afactor of2, which corresponds to aconfidence level of 95% . 

### Table 7 . Analytical Method Uncertainty. Analyte Method Standard Deviatfon Method Uncertainty PFOA E78-8-044 .0 11 .3 t 23% 

### 8 .8 Field Matrix Spikes (FMS) Aminium

of two field matrix spikes were collected at each sampling point to verify that theanalytical method is applicable to thecollected matrix. Field matrix spikes were generated by adding a measured volume of field sample to acontainer 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 interferewith theextraction and analysis of theanalytes of interest. Field matrix spike concentrations must be 50°!0of thesample concentration to be considered an appropriate field spike. Field matrix spikes are presented in section 9of 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 Hi gh 9.91 Low 0 .991 13oL, 131 L, 131 S, 1331R, 134S, 135S, 136S Mid 9.91 Hi gh 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 H igh 991 134R R 35R 3 Low 99.1 1 , , 1 1 Hi gh 991 Low 0 .991 ' T i Bl k Mid 9 .91 rp an Mid-Hi 99.1 I High ~ - 991 FMS Recovery = (Sample Concentration of FMS--Average Concentration : Field Sample&Field Sample Dup.) 100% Spike Concentraton

Page 16 of 53

### p. 38 GLP10-01-01 ; InterimReport 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 andfield matrix spike recoveries for thesampling locations aswell as theTrip Blanks and rinseate blanks. Results and averagevalues are rounded to three significant figures according to EPA rounding rules. Because of rounding, values may vary slightly from thoselisted in the raw

data. Field matrix spike recoveries meetingthe method acceptance criteria of t 30%, demonstratethat the method was appropriate for thegiven matrix and their respective quantitative ranges. DAL GW

134R 101104 -The high-level FMS did meet method acceptance criteriawith a recovery of 69.1 % . The low-level FMS was not appropriate as compared to thesample concentration. The analytical uncertainty has been adjusted for PFOA to t 31 % . DAL GW

131 R101103 - Dueto the high concentration of PFOAdetected 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 PFOAdetected in the sample, this sampling location did not have an appropriate FMS spike level tosufficiently evaluate PFOA recovery.

Page 17 of 53

### p. 39 GLP10-01-01 ; InterimReport 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 130R0 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 :tQ88% 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 AverageConcentfadon (nWmL) t %RPD T 1 74 ng/mt t0 .58'rd NA = Not Applicable NC = Not Calculated; Endogenous sample concentrationgreaterthan 2xspike 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 DA L GW 130L HS 101105 162 92.8 AverageConcentradon (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 18 of :53

### p. 40 GLP10-01-01 ; InterimReport 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 AverageConcentration (nglrnL) tV .RPD 2500nghrrL t 1.6% n~ NA = Not Applicable NC= Not Calculated; Endogenou s sample concentratfon greater than 2x spike level . (1) Sampling location did not have an appropriate spice level toevaluate PFOArecovery. 

### 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 GLP10-01-01-11-025 DAL GW 131S HS 101103 127 103 AverageConcentradon (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 IRecove 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 G LP10-01-01-11-030 DAL GW 131L HS 101103 179 89.2 AverageConcentrafton (ng/rnL) t %RPD 90 .7 ng/mL t 5

.2 " / NA = Not Applicable NCa Not Calculated; Endogenous sample coricentradon greater than 2x spike level .

### p. 41 G1F10-01-01 ; InterimReport 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 AverageConcentmtion (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 GLP10 -01-01-11-040 DAL GW 132S HS 101102 1810 85.6 _ _ Average Concerrbatforr (ng4nL) t %RPD 962ngftL t Q 5Y .6 NA = Not Applicable NC= Not Calculated; Endogenous sample concentrationgreaterthan 2x spike level . 

### Table 17. DAL GIN1321-101103 PFOA Concentraffon 3M UMS1D Descri p tion 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 greaterthan 2x spike level .

Page 20 of 53

### p. 42 GLP10-01-01 ; Interim Report 11 Analysis of PFOAin 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 AverageConcentraUon (nglmL) t % .RPD 102nallmL t 9 .5% NA = NotApplicable NC = Not Calculated; Endogenous sample concentration greater than 2x spikelevel . Table 19

. DAL GW

133S 101103 PFOA Concentration 3M UMS!D Desc ' on n ML oReco GLP10-01-01-11-051 DAL GW 13330101103 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 385ng/mL t 4 .2'/ NA = Not Applicable NC= Not Calculated: Endogenous sample concentration greater than 2xspikelevel . 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 IRPD 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 AverageCorncentraLion (ng/mL) t %RPD 1570ng(mL 19 .6% NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greaterthan 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 UMSfD 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 .49ng/mL t 5 5% NA = NotApplicable NC = Not Calculated

;

Endogenous sample concentration greater than 2xspike level . Table 23. DALGW

134L 101105 PFOA ' ConcentYatYon 3M LfMS ID Descd tlon n mL %Recove GLP10-01-01-11-070 DAL GW 134L0101105 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 AverageConcentyatlort (no/mL) 3 %RPD ~ _ 520ncymL t 13% I NA = Not Applicable NC= Not Calculated; Endogenaus sample concentration greater than2x spike level .

Page 22 of 53

### p. 44 GLP10-01-01 ; InterimReport 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 135R0101105 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 2910ngumL 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 levelto 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 .7n mL t 3

.T/ NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greaterthan 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 ; InterimReport 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 sampleConoentration greaterthan 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 AverageConcentraldon (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 LJMSID 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 NCmNot Calculated; Endogenous sample concentration greater than 2x spike level .

### p. 46 GLP10-01-01 ; InterimReport 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 AverageConcentxadan (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 AverageConcentration (ng/mL) t %RPD 147 n9mL t 3 .4% NA = Not Appucable NC= Not Caiadated; Endogenous serrVe concentration greaterthan 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 = NotApplicable NC = Not Calculated; Endogenous sample concentration greaterthan 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 CW26R0101110 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 CW26RHS 101110 1290 91 .3 AverageConcentraHon (ng/mL) t %RPD 386 mL 11. 8 % NA = Not Applicable NC = NotCalculated; Endogenous sample concentration greater than 2x spike tevel . Table 34. DAL GW

CW26L 101110 PFOA I Concentranfon 3M L1MSID 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- NotApplicable NC = NotCalculated; Endogenous sample concentration greater than 2x spike level . 

### Table 35. DAL GW

140R 101104 

## Pr-OA Concentratfon 3M LIMS!D Descn' 8on rnL IRecove 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 t0 .83 % NA = NotApplicable NC m Not Calculated; Endogenous sample concentration greater than 2x spike level .

Page 26of 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 R0101110 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 1.84n mL t 10% NAa Not Applicable NC" Not Calculated; Endogenan sample concentrationgreaterthan 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 AverageConcentradon (na/mL) t %RPD ~ 47 . 6ncymL 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 144R0 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 Averag eConcenbaLlon n m t %RPD 57.3 n mL t 0 .17 % NA = Not Applicable NC = NotCalculated; 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 UMSID 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 BLANK1 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 RIPBLANK20 <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 TR IP BLANK 2 HS 1020 103 NA= Not Applicable 

### Table 41 . Trip Blank 3 PFOA Concenfradon 3M LIMS f0 Descri don n mL ecove % R GLP10-01-01-11-160 TRIP BLANK 3 0 <0.0250 NA GLP10-01-01-11-161 TRIP BLANK3 LS 1 .07 108 GLP10-01-01-11-162 TRIP BLANK 3MS 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 ; InterimReport 11 Analysis of PFOA in Groundwater Former Sludge Incorporation Area - November 2010

Table 42

. Trip Blank 4 ' PFOA i ~ ConcentraUon 3M LOSID Descal tlon ~ n mf . I

Recov GLP10-01-01-11-165 TRIP BLANK 4 0 <0.0250 NA GLP10-01-01-11-166 TRIP BLANK4 LS 1 .06 107 GLP10-01-01-11-167 TRIP BLANK 4 MS 10 .4 105 GLP10-01-01-11-168 TRIP BLANK4MHS 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 RB0040 <0.0250 NA NA = NotAppIicable

Page 29of 53

### p. 51 GLP10-01-01 ; InterimReport 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 todetermine 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 ; InterimReport 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// WilliamK

. Reagen, Ph.D., 3M

Environmental Laboratory Manager Date 

## 4UW7yfZ//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 ANDSEDIMENT 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 AArea 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), shallowsubsurface 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 l . The Avenue A assessment is intended to obtain additional data for the Remedial Action Agreement Programbeing undertaken by 3M under the ADEM

NPDES programand 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