## 3M

Company St. Paul, Minnesota 

# 3~G5~- p. 1



# Perfluoroodanoic Acid (PFOA) Site Related Environmental Assessment Program 3M and Dyneon LLC Decatur, Alabama

Quarterly Status Report November 19, 2009to March 21, 2010

O8P-1106-v6 

## CONTAINS NOC131

## Perfluorooctanoic Acid (PFOA) Site Related Environmental Assessment Program 3MDecatur, Alabama Site Quarterly Status Report November 19, 2009 to March 31, 2010

Prepared for 

### 3M Company and Dyneon LLC 

## By WESTONSOLUTIONS, INC . West Chester, Pennsylvania 19380 W .O. No. 02181 .129.108.0001

## TABLE OF CONTENTS

Section Page 1 . BACKGROUND. . .... ... .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-1 2 . SUMMARY OF ACTIVITIES. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82-1



### ATTACHMENTS Attachment Title 1 SOIL SAMPLING TECHNICAL PROGRESS REPORT 2 GLP10-O1-01 STUDY PROTOCOL

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.0-9\3M-DECA7\Phase 3 Work PIan1101o Status Raport11010Status Raport .doc 1

## 1 . BACKGROUND

In accordance with the Phase 3 Work Plan for Sampling Environmental Media (WESTON, 2009) and the Memorandum of Understanding (MOU; 3M, 2004) with USEPA, 3M

and Dyneon LLC are undertaking a Perfluorooctanoic Acid (PFOA) SiteRelated Environmental Monitoring and Assessment Programat their Decatur, Alabama plant. Per the agreement between USEPAand 3M, this report represents the status report of this effort as required by the MOU for the November 19, 2009 through March 31 ., 2010 time period. For brevity, and following previous convention, this report will be referred to as the March 31, 2010 Quarterly Status Report.

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.0-913M-DECAIIPhase 3 Work Plan\1010Status Report\7010Status Report .doc 1-1p. 5



## 2 . SUMMARY OFACTIVITIES 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 quarterly status report that covers the January 1, 2010 to March 31, 2010 timeframe and includes a description of activities completed under the Phase 3 Work Plan. By agreement with agency personnel, the time period fromNovember 19, 2009 through December 31, 2009 is also addressed by this report. Details are as follows: Groundwater Technical Pro ess: Access agreements have been finalized with some off-site landowners for the installation of monitoring well clusters and sampling of groundwater. It is anticipated that the remaining access agreements will be in place by the end of June 2010 and that monitoring well installation, development and sampling will be performed in July 2010 . In addition, file reviews have been performed for the Morgan County Landfill and BFI Morris FarmLandfill and candidate monitoring well locations have been identified for sampling and analysis of PFOA. 

### " Soil and Sediment Technical Progress, : o Off-site Soil - Soil sampling will be performed during the installation of the residuumwell boreholes at the off-site monitoring locations described above after access agreements are in place. Sampling of surface soils fromthe 0- 12 inch depth interval at locations within approximately 2 miles of the 3M Decatur facility is expected to commence sometime in May 2010 . Upon completion of analyses, data on surface soil PFOA concentrations will be provided in subsequent quarterly status reports and a technical consultation will be held with EPA to reviewthe findings and to establish the range of soil concentrations to be evaluated in the vegetative uptake study and other design details.

N :\FOLDERS.O-9\3M-DECATPhase 3 Work Plan\7010Status Report\1Q10 Status Report.doc 2-1p. 6

o Off-site Sediment - It is anticipated that an access agreement will be finalized with the Wetlands Edge Environmental Center (WEEC) swamp property owner (BP) with sediment sampling expected to commence sometime in May 2010 . o On-site Soil - Sampling ofon-site surface (0 - 6 inch depth) and subsurface (1 to 1 .5 foot depth) soils in former sludge incorporation area fields 5, 8C and 11 was performed on March 30 - 31, 2010 to provide additional characterization of PFOA for the engineering design and construction of the multilayer cap currently being installed on the former sludge incorporation area under the NPDES Remedial Action Agreement between 3M and the Alabama Department of Environmental Management (ADEM) . Although this sampling is not a MOU-specified activity, analyses are being performed under the GLP 10-01-01 protocol and sampling procedures, locations, and analytical results will be summarized in a future Quarterly Status Report. Additional information on the soil sampling activity is provided in the Soil Sampling Technical Progress Report (Attachment 1) . o Vegetative Uptake Study Technical Progress: Aresidential garden crop survey to identify the vegetables most commonly grown by residential gardeners in the Decatur area is in progress. The information obtained frominterviews of retail suppliers of seed and plant starts will be used to establish the type of leafy, root and fruiting vegetable crops to be evaluated in the vegetative uptake study. Other planning activities for the vegetative uptake study that are underway include the evaluation of a potential borrowarea for the off-site reference soil for soil blending / dilution, study siting and facility requirements and analytical method development for the analysis of PFOA in vegetable samples. In conjunction with the surface soil sampling activities described above, sampling will be performed at the off-site reference soil borrowarea and at on-site locations within the Former Sludge Incorporation Area Field 14 for range-finding analyses. These data are intended to determine source areas

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.0-913M-DECATPhase 3 Work Planli010

Status Report11010 Status Raport .doc

2-2p. 7

for the bulk soils, establish soil concentrations at the borrowarea (expected to be belowthe limit of quantitation), characterize heterogeneity and allowthe assessment of the effectiveness ofsoil blending procedures . The range-finding results will be included in the evaluation of the range of test concentrations during a technical consultation with EPA . " Phase 3 Analytical Methodology :

. A new Good Laboratory Practice (GLP ) Protocol GLP10-O1-01 has been developed forthe analysis of PFOA in water, soil and sediment samples that will be collected during Phase 3. A separate GLP Protocol is under development for the analysis of the vegetation, soil and water samples associated with the vegetative uptake study component of the Phase 3 program . The GLPProtocol P0003267 that was developed for analyses performed after completion of Phase 2 is being closed out and a Final Report is in preparation. Acopy of GLP10-O1-01 Study Protocol is provided in Attachment 2 . 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 SOIL SAMPLING TECHNICAL PROGRESS REPORT JANUARY 1, 2010 - MARCH 31, 2010

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.0-9\3M-DECA71Phase 3Work Plan\1 QI OStatus Report\IQIO Status Report.drep. 9

SOIL SAMPLING TECHNICAL PROGRESS REPORT 3M ANDDYNEON DECATUR, ALABAMA Sampling ofsurface (0 - 6inch depth) and subsurface (1 to 1 .5 foot depth) soils in former sludge incorporation area fields 5, 8C and 11 was performed on March 30 - 31, 2010 to provide additional characterization of PFOA for the engineering design and construction of the multilayer cap currently being installed on the former sludge incorporation area under the NPDES Remedial Action Agreement between 3M and the Alabama Department of Environmental Management (ADEM) . Although this sampling is not a MOU-specified activity, analyses are being performed under the GLP 10-01-01 protocol and sampling procedures, locations, and analytical results will be summarized in a future Quarterly Status Report. Atotal of 13 sample locations were established to supplement previous sampling data associated with fields 5, 8C, and 11 generated fromthe Phase 2 program . The sample locations are presented in Figure l . Fields 5 and 11 have undergone previous investigation. Field 8C is believed to have served as a area with no known history of sludge incorporation. Prior to sampling, locations were cleared of vegetation and humus, exposing the underlying soil . Soil fromthe 0to 6-inch depth interval was collected via a stainless steel hand auger and placed into a disposable plastic tray. When the interval was collected, the soil was described, noting the color, moisture content, texture, organic content, and any visual evidence to suggest sludge may have been applied at the location. The soil was then blended removing as much of the root debris as possible, and an appropriate volume ofthe material was placed into a laboratory-prepared container, avoiding soil with visible root debris. The container was sealed, labeled with the date, time, and a unique sample number, and placed into an ice chest pending transfer to the laboratory. The sample information was also recorded onto a Chain-of-Custody (COC) which accompanied the samples to the laboratory.

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" . . , DAL-DF11-'-SS-SS07 ~ .-~ .

Field 8a DAL-DF11-SS-SS06

Field 11 IL DAL-DF11-SS-SS05 iD

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Soil sampling locations 350 175 0 Feet Figure 1 Field boundaries are conceptual Soil sampling locations - and indistinct . Sample designations a'1~T~} E March 30-31 2010 based on soil characteristics. , s Decatur, AL File: \lfsfed0l\fig\3MDec\MXD\Soil samps 3302010 .mxd, 23-Apr-10 16:25, rickscp. 11

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### Table 2 . Summaryof Sample Station Location Data Field Sample No. Station NORTHING EASTING ' 5 SS06 34° 37' 13.14" N 87° 2' 25.92" W 5 SS07 34° 37' 15.72" N 87° 2' 32.22" W 5 SS08 34° 37' 17.46" N 87° 2' 26.04" W 5 SS09 34° 37' 22.44" N ~: 87° 2' 22.92" W 5 5510 34° 37' 25.50" N 87° 2' 25.74" W 8C SS01 34° 37' 21 .54" N : 87° 2' 49.74" W 8C SS02 34° 37' 19.56" N '' 87° 2' 44.34" W 8C SS03 34° 37' 15.36" N _- 87° 2' 41 .64" W 8C SS04 34° 37' 17.58" N 87° 2' 38.52" W 8C SS05 34° 37' 13.80" N : 87° 2' 37.62" W 11 SS05 34° 37' 29.22" N 87° 2' 25.68" W 11 SS06 34° 37' 33.06" N ' 87° 2' 23.76" W 11 SS07 34° 37' 34.86" N ; ; . 87° 2' 32.88" W Coordinates obtained using a hand-held GPS. DatumReference: WGS 84p. 13



## ATTACHMENT 2 GLP10-01-01 STUDY PROTOCOL ANALYSIS OF PERFLUOROOCTANOICACID (PFOA) IN GROUNDWATER, SOIL AND SEDIMENT FORTHE 3MDECATUR PHASE 3 SITE-RELATED MONITORING PROGRAM

N :1FOI-DERS .0-MM-DECA7\Phase3 Work Plan\IQIOSlamsRepcrt\1Q10Slams Report.doc

## STUDY PROTOCOL STUDYTITLE Analysis ofPerfluorooctanoic Acid (PFOA) in Groundwater, Soil and Sediment forthe 3M

Decatur Phase 3 Site-Related Monitoring Program



### DATA REQUIREMENTS TSCAGood Laboratory Practices 40CFRpart 792

DATE March 2, 2010 PERFORMING LABORATORY 3M Environmental Health and Safety Operations 3M Environmental Laboratory 3M Center, Building 0260-05-N St. Paul, MN 55144 LABORATORY PROJECT IDENTIFICATION

Project# : GLP10-01-01p. 15p. 16

After completing the sampling of the 0 to 6-inch interval, the boring was extended to 1 .0 feet in depth and cleaned of any loose soil debris. Using a clean stainless steel auger, additional soil was collected fromthe 1 .0 to 1 .5-foot depth interval and placed into a new disposable plastic tray. The material was described, blended, and sampled in the same manner as the shallowsample. Table 1 presents a summary ofthe soil data collected for each sample. Following sampling, the boring was backfilled with the remaining soil . The location was staked and the location was documented using a hand-held global positioning system(GPS) . The sample location coordinates are presented in Table 2. In addition to the 26 media samples, WESTON collected three duplicate samples and two rinseate blanks as part of the sampling QA/QC program . Duplicate samples were collected at the same time as the media samples from the blended soil at randomlyselected locations. The rinseate was collected by pouring laboratory-grade water onto a cleaned stainless steel auger bucket, collecting the discharge for laboratory testing. Each rinseate sample was identified with the location where the auger was used prior to cleaning. Samples were shipped to the 3M Environmental Laboratory in St. Paul, MN for PFOA analyses under the GLP Protocol GLP10-O1-01 . When available, final analytical data will be provided in a future Quarterly Status Report.

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.0-9\3M-DECA'Mhase 3 Wark Plen\IQ10Smms Report\IQIOStams Reput.dceLaboratory Project Number GLP10-01-01 

### Protocol Signatures

Jai Kesari, P.E., DEE Date: Weston Solutions, Inc. SponsorRepresentative: Gary Hohenstein Date: 3M Environmental Health and Safety Operations PrincipalAnalytical Investigator. 

### Cleston Lange, Ph.D. 3M Environmental Laboratory Laboratory Management: Date:

~ .- ~ ~~ ~ .~L~f f - ..2c,1 0 WilliamReagen, Ph.D. Date: 3M Environmental Laboratory Laboratory Technical Review Cliffton .lacoby

; Ph.D. / Date: 3M Environmental Laboratory QualityAssurance 

### rel 2C/0 Quality 4surance Representative Date: Quality Associates, Inc.



### Page 2of15Laboratory Project Number GLP10-09-01 

### Protocol Signatures StudyDirector: Jai Kesari, P

.E., DEE Date: Weston Solutions, Inc

. Sponsor Representative:

, henstein ironmental Health and Safety Operations PrincipalAnalytical Investigator: Date:

Cleston Lange, Ph.D

. Date: 3M Environmental Laboratory Laboratory Management: WilliamReagen, Ph.D. Date: 3M Environmental Laboratory Laboratory Technical Review Cliffton Jacoby, Ph .D. Date: 3M Environmental Laboratory QualityAssurance Quality Assurance Representative Date: Quality Associates, Inc.



### Page 2 of 15P. 19 Laboratory Project Number GLP90-01-09 

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

Decatur Phase 3 Site-Related Monitoring Program 

### Test Material Study Director Pertluorooctanoic Acid CAS# 335-67-1 Jai Kesari, P.E., DEE Weston Solutions, Inc. West Chester, PA 19380 601-701-3761 

### Sponsor Representative Principle Analytical Investigator

Testing Facility Proposed Study Timetable Gary Hohenstein 3M Center, Building 0224-05-W-03 St. Paul, MN55144 

### 651-737-3570 Cleston Lange, Ph.D

. 3M Environmental Laboratory 

### 3M Center, Building 0260-05-N-17 St. Paul, MN55144 651-733-9860 3M Environmental Laboratory 3M Center, Building 0260-OS-N-17 St. Paul, MN 55144 Study Initiation Upon Protocol Signature ExperimentalStart Date March 5, 2010 Experimental Terrnination Date December 01, 2011 Study Completion December 31, 2011



### Page 3 of 15p. 20 Laboratory Praject Number GLP10-01-!)1 1 . INTRODUCTIONAND OBJECTIVE This study is being conducted as part ofthe Memorandum of Understanding (MOU) between 3M Company, Dyneon and the United States Environmental Protection Agency, effective October 25, 2004. As part ofthe MOU, 3M is to conduct a perfluorooctanoic Acid (PFOA) site-related environmental monitoring and assessment program for the 3M

Decatur, Alabama facility. 

### The objective ofthis study is to aid in the characterizationofPFOAconcentrations in various environmental media (groundwater, soil and sediments) associated with and nearthe Decatur facility. 2. REGULATORYCOMPLIANCE This studywill be conducted in accordance with the Toxic Substances ControlAct (TSCA) Good Laboratory Practices Standard, 40 CFRpart 792. This study is for the analysis of environmental samples and only the analytical portion, as described herein, will be conducted under the GLPstandard at the 3M Environmental Laboratory. 3. SCOPE OF INVESTIGATION 

### This study will help to detennine thepresence and concentration ofperfluorooctanoic acid in groundwater, soil andsediment samples collected inthe vicinity ofthe 3M Decatur, Alabama facility and from

landfills that received waste from the Decatur facility. 4. TEST SUBSTANCE 

### The test substance for this study is not a test substance in the classic sense. The known source, expiration date, storage conditions, chemical lot number, TCRnumber, physical description, and purity ofthe test substance being monitored in the test systemis not known as it wouldbe known for the reference substances. Name: perfluorooctanoic acid CAS# : 335-67-1 Molecular Fonnula: C7F15COOH Molecular Weight: 414.07 Appearance: White Solid Figure 1 . Chemical Structure of Perfluoro-n-octanoic Acid, PFOA (linear) 

## O CFZ CF? CF2 Z

\0 CF / CF CF CH 3 2 2



### C$F15O2H 414.07 Page 4 of 15p. 21 Laboratory Project Number GLP10-01-09 5 . REFERENCESUBSTANCE 

### 5 .9The reference substances in Table 1, or equivalent, will be used for quantitative analytical determinations.

FFOA ~BRA~JCHED+ LINEAR~



## TcRas-0042 Liquid, Solution in Methanol I Liquid, Solution in Methanol (49 t 2 .5 pg/mL, Sealed Ampule) (50i 2.5 pg/mL in SealedAmpule)

5 .2 Reserve Samples: Areserve sample ofeach reference material will be retained and archived by the 3M

Environmental Laboratory in St. Paul, MN . 5 .3 Disposition: Records will be maintained by the 3M Environmental Laboratory documenting the use, transfer and disposal, ifany, ofthe reference substances. 5 .4 Safety Precautions: All laboratory safety precautions will be followed. Acurrent MSDS will be maintained for each ofthe reference substances. 

### Page 5 of 15p. 22 Laboratory Project Number GLP10-01-01 

### 5 .5 Stability: The stability ofthe test substance will be documented during the study. Stability is demonstrated by successful calibration verification standards bracketing the samples within an analytical run, comparison ofstandard curves fromdifferent runs performed on different days, andprecision requirements for replicate samples. 6 . TEST SYSTEM 6 .1 Description of the Test System . The test systems for this study will be a variety ofgroundwater, soil and sediment samples collected in the vicinity ofthe 3M Decatur, Alabama facility and landfills which receivedwaste fromthe Decatur facility. The study sampling plan and collection will be completed by Weston Solutions, Inc . All study samples will be provided to the 3M Environmental Laboratory by Weston Solutions, Inc

. (or designated contractor) . The exact number ofsamples is unknown since the sampling and analysis will be ofan iterative nature that is dependent on results. Samples anticipated for each sampling event will be defined apriori by a protocol amendmentwhich is written in the formof a 3M Environmental Laboratory general project outline (GPO) describing the number and types ofsamples anticipated. The total number ofsamples analyzed will be amended quarterly to this protocol and a final tallied number amended prior to the completion ofthe study. 

### 6 .2 Identification of Test System . Each sample will be identified by study number, unique sample identification number, sample collection date, test system(soil, water or sediment) and nature ofthe samples(sample, trip blank, field matrix spike, etc.). This informationwill be provided on the labels by Weston Solutions, Inc. fieldpersonnel . Once received at the 3M Environmental Laboratory with a proper chain ofcustody, the samples will be additionally labeled with a laboratory information management system (LIMS) generated sample IDnumber for internal trackingpurposes. 7. SPECIMEN RECEIPTANDSTORAGE 

### Samples received are logged and tracked according to the 3M Environmental Laboratory standard operatingprocedures (SOP's) . Once received at the 3M Environmental Laboratory with a proper chainofcustody, the samples are logged into the LIMS systemand then stored refrigerated. 8. ANALYTICAL METHODS 

### Analysis ofthe study samples will be conducted at the 3M Environmental Laboratory. The analysis will be carried oututilizing liquid chromatography with tandemmass spectrometry detection (LGMSIMS) . The anticipated method to be used for the analysis ofeach environmental matrix is given in Table 2, alongwith the target lower limits ofquantitation (LLOQs) . An alternative method is also listed,which may offer better recovery or statistical results in some instances, particularly when samples exhibit significant matrix interferences. If the target LLOQis not attainable, this will be discussed inthe final report. The instrumental conditions used will be documented in detail inthe raw data. 

### Page 6 of 15p. 23 Laboratory Project Number GLP90-01'-01 

### Allconcentrations of PFOAwill be reported as the anion form, [C7F1SCOO]" .

TABLE 2. LIST OF MATRICES, METHODSANDTARGET LLOQS 

### Matrix Method Number and Name Target LLOQ Groundwater Method ETS-8-044 "Method ofAnalysis for the 0.025 nglmL (0.025 ppb,

Determination of Perl9uorinated Compounds in Water by 25 ppt) LC/MS/MS; Direct Injection Analysis" . Groundwater Method ETS-8-154 "Determination of Perfluorinated Acids, 0.025 nglmL (0.025 ppb, (alternative Alcohols, Amides, and Sulfonates in Water by Solid Phase 25 ppt) method) Extraction and High Performance Liquid

Chromatography/Mass Spectrometry" . Soil and ETS-8-053 "LC/MS/MS Analysis of Soils for C4-C12 0.2 nglg (0.200 ppb, 200 Sediment Perfluorinated Carboxylic Acids and Perfluorobutane ppt)

Sulfonate, Perfluorohexane Sulfonate and Perfluorooctane Sulfonate Using Stable Isotope-labeled Internal Standards" Soil and ETS-8-042 "Solvent Extraction and Isocratic LC/MS/MS 0.2 nglg (0.200 ppb, 200 Sediment Analysis of Soils for C4-C12 Perfluorinated Carboxylic ppt) (altemative Acids and Perfluorobutane Sulfonate, Perfluorohexane method Sulfonate and Perfluorooctane Sulfonate" The methods identified above will include the use ofstable isotope-labeled internal standard calibration, and a stable isotope-labeledsurrogate analyte to aid infuture evaluations ofanalyte recovery in lieu of laboratory matrix spike (LMS) or field matrix spike (FMS) samples (i .e. data will be used to show

that recovery ofsurrogates mimic, or doesn't mimic, the recoveries measured in LMSs and FMSs for environmental samples) . 

### The reference material for the target analyte in study samples is the linear isomer of PFOA . Linear PFOAwill be used forcalibration standard preparations and also for LMS and FMS sample fortifications. Because environmental samples may contain a mixture of both linear and branched isomers of PFOA, it is importantto assess the quantitative accuracy ofthe methods for linear + branched PFOAusing a linear PFOA calibration. Triplicate laboratorycontrol spikes (LCSs) will be fortified with reference materials that consist ofa mixture oflinear + branched isomers (typical ofthe normal distribution from electrochemical fluorination synthesis) and fortified at a concentration near the mid-level ofthe calibration range. Quantitation ofthese LCSs will be performed using the calibration curve constructed from the analysis oflinear isomer calibration standards. Results of LCSs will offer some level ofaccuracy assessment, however finalresults will not be adjusted for the level ofaccuracy determined since the absolute source and isomer distribution in the environment for these analytes is not assumed. Astable isotope-labeled surrogate [(1,2,3,4 -13C4)-PFOA] will be added at a fixed level to each sample, LMSIFMS, LCS, procedural blank . The surrogate will be added at an equivalent concentrations to calibration standards as is the linear PFOA . The surrogaterecovery data is



### Page 7 of 15p. 24 Laboratory Project Number GLPlD-©1-01 being obtained to build a data setusing real environmental samples to better evaluate their potential future use in lieu of themore difficultto prepare and more costly and time consuming FMSs and LMSs. However, the surrogate recoveries will not be usedto assess reportability of data in this study. 

### Astable isotope-labeled internal standard (IS), [(1,2,3,4,5,b,7,8 -13C8)-PFOA], will be added at a fixed concentration to each sample, LMS, FMS, LCS, procedural blank and calibration standard and used to aid in the quantitation of both PFOAand the surrogate. 8 .1 Groundwater Sample Analysis All groundwater samples will be analyzed as described in the above water method(s) . For each sampling location, the analyses will include: sample, sample duplicate, lowlevel field matrix spike and high-level field matrix spike. 8 .2 Soil and Sediment Sample Analysis All soil and sediment samples will be analyzed as described in the above soil/sediment method(s) . However, the analysis may occur in twophases. Afirst phase may be performed for screening purposes to aid in the rough determination of PFOA concentrations. The screening data will be used to determine appropriate fortifications (spiking) level for laboratory matrix spike (LMS) samples during the definitive second analysis. Only the results of the definitive analysis will be reported, but the screening level analysis data will be included in the final data package with the study report. 

### The definitive analysis will include the preparation ofthree fresh aliquots ofeach bulk sample. The first two aliquots will be identified as sample and sample duplicate. The third aliquot will be fortifiedwith linear PFOAas a LMS sample; fortified at an appropriate level based on the results ofthe screening determination orother information. The percent moisture ofeach soil sample will be determined and all final results reported on a dryweight basis after adjusting for the percent moisture. 9 . DATA QUALITYOBJECTIVES 

### The analytical quality control objectives and data acceptance criteria are listed below . 9 .1 Procedural, Solvent, Trip and Rinseate Blanks 9 .'1.9 Procedural Blanks For each analytical batch ofgroundwater samples, aprocedural (method) blank consisting ofan aliquotofMilli-Qor equivalent laboratory water will be prepared and analyzed in the same manner as the samples and will be run in each extraction batch. For each extraction batch ofsoil and sediment samples, a procedural (method) blank consisting of acontrol soil or sediment will be extracted in the same manner as the samples and analyzed in each analytical run. The standard control soil will be TCR-842, or other standard soil demonstrated to be sufficiently devoidoftarget analyte. 

### Page 8 of 15p. 25 Laboratory Project Number GLP90-01-09

The area counts for each analyte in a procedural blank must be <50°/© ofthe area counts ofthe LLOQstandard. If not, then the LLOQmust be raised to the lowest concentration standard that meets that criterion. An analytical batch may contain more than one procedural blank. The analytical results fromanalysis ofmultiple procedural blanks in an analytical runwill be averaged in the evaluation of the LLOQ . The procedural blanks should be prepared with the samematrix used to prepare the calibration standards inthe extraction batch 

### 9 .1 .2 Trip Blanks For groundwater samples, a trip blank of Milli-Qor equivalent water is prepared in a sample container in the laboratory and is then exposed to the same shipping, sampling site conditions, storage, preservation and all analytical procedures as a field sample experiences. There are no acceptance criteria for these samples. However, the results from these samples will be considered in the evaluation ofthe study results. For soil/sediment samples, a trip blank ofapproximately 5 grams of standard control soil is prepared in asample container in the laboratory andexposed to the same shipping, sampling site conditions, storage, preservation and all analytical procedures as a field sample experiences. There are no acceptance criteria for these samples. However, the results fromthese samples will be considered in the evaluation ofthe study results. 

### 9 .' .3 Solvent Blanks Solvent blanks are analyzed in each analytical run to evaluate any possible instrumental contamination or sample injector carryover. Analysis of solvent blanks should produce peak area counts that are <50%ofthe lowest calibration standard. 9.'!.4 Rinseate Samples Anumber ofrinseate samples maybe collected aspartofthe soil and sediment sample collection process for evaluating the effectiveness ofdecontamination of sample collection equipment. Such samples will beprovided at the discretion of Weston Solutions, Inc. field personnel, and will be treated and analyzed as water samples during this study. There are no acceptance criteria for rinseate sample results; however, the results fromthese samples will be considered in the evaluation ofthe final study results. 9.2Calibration and Lower Limit of Quantitation (LLOQ) : 9.2 .9 Calibration The reference material for the target analyte is the linear isomerof PFOAandwill be used for calibration standard preparations and LMS fortifications. Astable isotopelabeled internal standard, [(1,2,3,4,5,6,7,8-13C$)-PFOA] will be added to each sample, LMS, LCS, procedural blank and calibration standard for aiding quantitation of PFOA and the surrogate. Astable isotope-labeled surrogate [(1,2,3,4-I3C4)-PFOA] 

### Page 9 of 15p. 26 Laboratory Project Number GLP10-01-01 will also be added at a fixed level to each sample, LMS, LCS, procedural blank, and at variable known concentrations in calibrationstandards, andquantified to determine surrogate recoveries. The linear PFOA, surrogate and internal standard (IS) will be spiked as appropriate to the matrix aliquots priorto extraction. Calibrationpoints may be rejected due to a bad injection or failing to meet accuracy requirements defined within the individual methods. These criteria will be 100_+ 25% (and + 30%

at LLOQfor water calibration, and 100+_ 30%L 35°lo at LLOQ) for soil calibration. Aminimum of 6 points will be used to construct the calibration curve. The coefficient of determination (r2) value for the calibration curve must be > 0 .990. Continuous calibrationverification (CCV) samples must be within t 25% for water, and_+ 30% for soil, to be considered acceptable. The initial passing calibration and/or passing CCVs must bracket all reportable sample values . The MS/MStransitions to be used for the target analyte, surrogate and IS are provided in Table 3. TABLE 3. THE MS/MS TRANSITIONS FORTHE TARGET ANALYTE(S), INTERNAL STANDARDANDSURROGATE.

TargetAnalyte MS/MS Transitions PFOA (linear) 413>369,413>219,413>169 PFOA (linear/branched) 413>369,413>219,413>169 1,2,3,4,5,6,7,8-'3Cg - PFOA Intemal Standard 421>376 (1,2,3,4-13Cal- PFOA (Surrogate) 417>372 9 .2 .2 Lower Limit ofQuantitation (LLOQ) The LLOQis the lowest non-zero active standard in the calibration curve. The peak area counts ofthe LLOQmust be greater than two times thepeak area counts of the procedural blanks. By definition, the measured value ofthe LLOQmust be within ± 30% of the theoretical value for water calibrations, and ± 35% for soil calibrations. The target LLOQfor water analysis is 0.025 nglmL (0.025 ppb, 25 ppt) and 0 .200 nglg (0.200ppb, 200ppt; wet weight basis) for soil/sediment analyses. 

### 9 .3 Laboratory Control Spike (LCS) Laboratory control spike samples (LCSs) for groundwater samples consist ofan aliquot of Milli-Qorequivalent water, or astandard control soil or sediment, to which known . quantities of PFOA, surrogate and IS are added in the laboratory. The linear + branched mixed isomer formof PFOAwill be used for LCSpreparations, as opposed to strictly linear isomer form

. Minimally, one level of LCS, typically a mid-level, will be prepared in triplicate for each sample batch extracted for analysis. The average recovery of PFOA (linear + branched isomers quantified) fromLCSs must be within 100_+ 20°lo forwater and 100+_ 30%

for soil/sediment. The relative standard deviation (RSD) of the recoveries for the triplicate LCSs must be less than or equal to 20% . 

### Page 10 of 15p. 27 Laboratory Project Number GLP90-09-01



### 9 .4 Sample Duplicates Each field sample will be collected as a single sample, with the exception of field duplicates (see section 9.5) . Analytical sample duplicates will be aliquoted fromthe field samples at the time of sample preparation and each aliquot extracted and analyzed individually. The relative percent difference (RPD) of duplicate water sample results should be less than 20%, and duplicate soil/sediment sample RPDs should be less than 50% . Results for duplicate samples not meeting these criteria will be flagged as such when reported. 9 .5 Field Duplicates Field duplicates of bulk samples may be collected at the time of sample collection. All groundwater samples will be collected in duplicate. Duplicate soil/sediment samples will be collected in the field at a frequency of 10%(1 per 10 samples) . The RPDofduplicate field water sample results should be < 20% . The RPD of duplicate field soil/sediment sample results should be _< 50% . Results for field duplicates not meeting these criteria will be flagged as suchwhen reported. 9.6 Field Matrix Spikes and Lab Matrix Spikes The addition of known quantities oftargetanalyte to samples for determining the efficiency ofanalyte recovery for the sample is commonlyused for evaluating data quality and criteria for reporting ofresults. In general, the highest level ofconfidence is acquired fromFMS recovery results inwater samples, and FMS results will be treated as theprimary (highest) quality control parameter for reporting those sample results. However, in some instances FMSrecoveries may not be at appropriate levels relative to endogenous sample analyte levels for proper recovery determinations. Inthose instances, the preparation of LMSs and evaluation of LMS recovery results will dictate the reportability ofresults. The recovery of the mass-labeled surrogate will not be considered in the reporting ofresults, and is included herein to collect data for surrogate recovery in real world samples, and results ofthe surrogates will be correlated to LMS and FMSrecoveries in a separate data analysis. Failure to meet reporting criteria from FMS or LMSresults will result in a Not Reportable (NR) result for that sample, even if surrogate recoveries are acceptable. Exceptions to this can be made with the approval of the studydirector and sponsor. 9 .6 .1 Field Matrix Spikes (FMS) - Groundwater Samples An FMS is a sample to which known quantities ofthe target analyte, surrogate and IS are added to the sample bottle in the field, or in the laboratory before the bottles are sent to the field for sample collection. Alow level and a high level FMS will be prepared for each sampling location. The field spike concentration that is appropriate to assess accuracy is defined as approximately 0 .5 to 10times the measured sample



### Page 11 of 15p. 28 Laboratory Project Number GLP10-01-01 concentration. FMS acceptance criteria are recoveries within 100± 30% of the expectedvalue. Sample data with FMSrecovery outside of 100± 30%, but within ±50°l0, ofthe expectedvalue are flagged and reported as outside of QC acceptance criteria. Datawith FMS recovery outside off50% ofthe expected value arereported as NR, where NRis defined as "Not Reportable" data outside ofQC acceptance criteria. If FMSrecovery can not be assessed because the field spike levels were at an inappropriate level, then Laboratory Matrix Spikes (LMS) may be substituted. If LMS recoveries are within ±30% the data are reportable but flagged as not being at an appropriate field spike level, but because the laboratory spike levels that will be performed in LMSs will be appropriate relative to the endogenous levels and, while less optimal than a field spike, they will be suitable for assessing accuracy. 

### 9.6.2 Lab Matrix Spikes (LMS) - Soil and Sediment Samples Becausethe amount of soil or sediment sample added to the sample collection bottles in the field is not accurately controlled, FMSs are impractical . Therefore LMS samples will be utilized to evaluate the potential for matrix affects and analytical bias in those samples. LMS samples are prepared in the laboratory after receipt of the study samples by the pre-extraction spikingofapre-measured volume ofsoil or sediment with known quantities ofthe target analyte, surrogate and IS. As the density ofsoil and sediment samples will vary fromone sample to the next, the true spiked concentrations will be corrected for the accurate mass ofeach sample. The recovery ofeach target analyte will be used to evaluate the ability to quantitatively recover the same endogenous analytes from

a specific study sample. The ratio ofendogenous analyte to lab spike concentration that is appropriate to assess accuracy is defined as approximately 0 .5 to 10-times the measured sample concentration. LMSmethod acceptance criteria are recoveries within 100%+ 30% of the expected value. Sample data with LMS recovery outside of-±30%but within t50% ofthe expectedvalue are flagged and reported as outside of QC acceptance criteria. Data with LMSrecovery outside of 100% f 50% ofthe expected value arereported as NR, where NRis defined as "Not Reportable" data outside of QC acceptance criteria. 

### 9 .7 Surrogates Mass-labeled PFOA (Table 1) will be usedas a surrogate target analyte to aid in the future evaluation ofanalyte recovery and method precision and accuracy bythis method for "real world" environmental samples. The surrogate target analyte will be spiked at a defined concentration in all standard, QC and study samples at a low to mid level within the curve range. The analytical recovery ofwithin 100+_30°Jo is expected, and recovery results will be correlated to LMS and/or FMSrecoveries determined for those saine environmental samples to determine how well the surrogate tracks the FMS/LMSanalyte recoveries. Surrogate recoveries will not be 

### Page 12 of 15p. 29 Laboratory Project Number GLP9D-01-0a 

### usedto assess reportability ofresults, however a summary ofsurrogate recoveries will be provided ina separate table in each interimreport. 

### 9 .8Demonstration ofspecificity Unique retention times in chromatograms and MS/MS transitions, shall be evaluated for each analyte during each analytical run or batch to demonstrate analytical specificity. 9 .9 Soil Percent Moisture Percent moisture will be determined for each bulk sample. In short, two aliquots ofeach study sample will have their accuratewet weight determinedon a four decimalplace analytical balance andrecorded, and then the aliquotwill be dried in anoven at greater than 102°C until a stableweight is achieved (i .e. no fiuther water is lost) . The dried weight will be recorded and percent moisture calculated based on the original wet weight ofthe sample. The averagepercentmoisture values for duplicate determinations will be used in all final result calculations. RPDs for duplicate percent moisture determinations will be < 20%

for reporting. 10 . STATISTICAL ANALYSIS: 

### The result for each sampling locationwill include the average ofthe sample and sample duplicate and the relative percent difference between the duplicate samples. The results of any FMS or LMS analyzed with each sample will also be included. Concentrations will be reported to three significant digits while the RPDs and statistical values will be reported to twosignificant digits. 11 . REPORT To accommodate quarterly reporting ofthe overall study progress to EPA, the issuance of interimanalytical reports will be performed during the study. The sample results to be reported in each interim

report will be determined via correspondence between the study director and PAI as the study progresses. Atargeted tum-around time for interiuu analytical reports is eight (8) weeks fromthe date ofsample receipt at the laboratory, however, circumstances mayfacilitated the need for shorter or longer turn-around times. Each interimreport will include, butnot be limitedto, the following when applicable: 

### 11 .1 Name and address ofthe facility performing the study, 1 1 .2 Dates upon which the study was initiated and completed. 19.3 Astatement ofcompliance by the Study Director addressing any exceptions to Good Laboratory Practice Standards. 

### 99 .4 Objectives and procedures as stated in the approved protocol, including any amendments to the original protocol . Page 13 of 15p. 30 Laboratory Project Number GLP10-01-01 1 1.5 The test substance identification by name, chemical abstracts number or code number, strength, purity, and composition or other appropriate characteristics, if provided by the Sponsor. 

### 11.6 Stability ofthe test substances under the conditions of administration, ifprovided by the Sponsor. 11 .7 Adescription ofthe methods used to conduct the test(s) . 11 .8 Adescription ofthe test system . 11 .9 Adescription ofany circumstances that may have affected the quality or the integrity ofthe data. 11 .'1D The name of the Study Director and the names ofother scientists, professionals, and supervisory personnel involved in the study . 

### 11 .'! 1 Adescription ofthe transformations, calculations, or operations performed on the analytical data, a summary and analysis ofthe analytical results, and a statement of the conclusions drawn regarding the data quality and analytical results. 11 .12 Statistical methods used to evaluate the data, ifapplicable. 11 .13 The signed and dated reports ofeach ofthe individual scientists or other professionals involved in the study, if applicable. 11 .14 The location where rawdata and the final report are to be stored. 11 .15 Astatement prepared bythe Quality assurance unit listing the dates that study inspections and audits were made and the dates ofany findings reported to the Study Director and Management . 

### 11 .16 Ifit is necessary to make corrections or additions to a final report after it has been accepted, the changes will be made in the form ofan amendment issued bythe Study Director. The amendmentwill clearly identify the part ofthe final report that is being amended, the reasons for the amendment, andwill be signed by the Study Director. 12. LOCATION OF RAW DATA, RECORDS, ANDF1NAL REPORT Original data or copies thereof, will be available at 3M Environmental Laboratory to facilitate audits of the study during its progress and before acceptance ofthe final report . Before the final report is completed, all original paper data, including those items listed below will be retained in the archives of 3M

Environmental Laboratory for a period of not less than 10years following signing of the final report . 12 .' The following raw data and records will be retained in the study folder in the archives according to 3M

Environmental Laboratory Standard Operating Procedures. 

### 12 .1 .1 Approved protocol and amendments 12 .1 .2Study correspondence 12 .1 .3Shipping records Page 14 of 15p. 31 Laboratory Project Number GLP10-01-01 

### 12 .1 .4Raw data 12 .1 .v Approved final report (original signed copy) 12 .1 .6 Electronic copies ofdata 92 .2 The following supporting records will be retained separately fromthe study folder in the archives according to 3M Environmental Laboratory Standard Operating 

### Procedures: 12.2 .1 Training records 12 .2 .2Calibrationrecords 12 .2 .3Instrument maintenance logs 72 .2 .4Standard Operating Procedures, Equipment Procedures, and Methods 13. DATA I SAMPLE RETENTION 

### Samples will be maintained in the laboratory indefinitely. 14 . PROTOCOL AMENDMENTS AND DEVIATIONS Planned changes to the protocol will be in the form numbered protocol amendments and consist primarily ofa laboratory GPO, whichwill be attached to the protocol amendment. These amendments will be signed by the PAI, Study Director and the Sponsor's Representative. These GPO/amendments will be considered as part ofthe protocol andwill be attached to the final protocol . Any other changes will be in the formofwritten deviations, signed by the Study Director and filed with the raw data. All changes to the protocol will be indicated in the final report. 15.ATTACHMENTS None



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