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, 2009 to March 21, 2010 

O8P-1106-v6 CONTAINS NO C131 
Perfluorooctanoic Acid (PFOA) Site Related 

Environmental Assessment Program 

3M Decatur, Alabama Site 

Quarterly Status Report 

November 19, 2009 to March 31, 2010 

Prepared for 

3M Company and Dyneon LLC 

By 

WESTON SOLUTIONS, 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 

N1FOLDERS.0-9\3M-DECA7\Phase 3 Work PIan1101o Status Raport11010 Status 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 Program at their Decatur, Alabama 

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

of this effort as required by the MOU for the November 19, 2009 through March 3 1 ., 

2010 time period . For brevity, and following previous convention, this report will be 

referred to as the March 31, 2010 Quarterly Status Report. 

NIFOLDERS.0-913M-DECAIIPhase 3 Work Plan\1010 Status Report\7010 Status Report .doc 

1-1 
p. 5 

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 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 from November 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 

Farm Landfill 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 

residuum well boreholes at the off-site monitoring locations described above 

after access agreements are in place. Sampling of surface soils from the 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 review the 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\7010 Status Report\1Q10 Status Report.doc 

2-1 
p. 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 of on-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: A residential garden crop survey 

to identify the vegetables most commonly grown by residential gardeners in 

the Decatur area is in progress . The information obtained from interviews 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 borrow area 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 borrow area 

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 

N:\FOLDERS.0-913M-DECATPhase 3 Work Planli010 Status Report11010 Status Raport .doc 

2-2 
p. 7 

for the bulk soils, establish soil concentrations at the borrow area (expected to 

be below the limit of quantitation), characterize heterogeneity and allow the 

assessment of the effectiveness of soil 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 for the 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 GLP Protocol P0003267 that was developed for analyses performed 

after completion of Phase 2 is being closed out and a Final Report is in 

preparation. A copy 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. 

N:\FOLDERS.0-9\3M-DECAT\Phese 3 Work Plan\1Q70 Status Report\1Q70 Status Report.doc 

2-3 
ATTACHMENT 1 

SOIL SAMPLING 

TECHNICAL PROGRESS REPORT 

JANUARY 1, 2010 - MARCH 31, 2010 

N:\FOLDERS.0-9\3M-DECA71Phase 3 Work Plan\1 QI O Status Report\IQIO Status Report.dre 
p. 9 

SOIL SAMPLING 

TECHNICAL PROGRESS REPORT 

3M AND DYNEON DECATUR, ALABAMA 

Sampling of 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. 

A total of 13 sample locations were established to supplement previous sampling data 

associated with fields 5, 8C, and 11 generated from the 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 from the 0 to 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 

of the 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. 

N:\FOLDERS.0-914M-DECATPhase 3 Work P1=\ 1Q10 Stams Repon\IQI O Status Report .doo 
p. 10 

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Figure 1 

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- 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, ricksc 
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Table 2. Summary of 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. Datum Reference : WGS 84 
p. 13 

ATTACHMENT 2 

GLP10-01-01 STUDY PROTOCOL 

ANALYSIS OF PERFLUOROOCTANOIC ACID (PFOA) IN 

GROUNDWATER, SOIL AND SEDIMENT FOR THE 3M DECATUR 

PHASE 3 SITE-RELATED MONITORING PROGRAM 

N:1FOI-DERS .0-MM-DECA7\Phase 3 Work Plan\IQIO Slams Repcrt\1Q10 Slams Report.doc 
STUDY PROTOCOL 

STUDY TITLE 

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

Decatur Phase 3 Site-Related Monitoring Program 

DATA REQUIREMENTS 

TSCA Good Laboratory Practices 40 CFR part 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 #: GLP10-01-01 
p. 15 
p. 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 from the 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 shallow sample. Table 1 presents a summary of the 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. 

N:\FOLDERS.0-9\3M-DECA'Mhase 3 Wark Plen\IQ10 Smms Report\IQIO Stams Reput.dce 
Laboratory Project Number GLP10-01-01 

Protocol Signatures 

Jai Kesari, P.E., DEE Date : 

Weston Solutions, Inc. 

Sponsor Representative: 

Gary Hohenstein Date: 

3M Environmental Health and Safety Operations 

Principal Analytical Investigator. 

Cleston Lange, Ph.D. 

3M Environmental Laboratory 

Laboratory Management: 

Date: 

~.- 

~ ~~ ~.~L~ f f - ..2c,1 0 

William Reagen, Ph.D. Date : 

3M Environmental Laboratory 

Laboratory Technical Review 

Cliffton .lacoby; Ph .D. / Date: 

3M Environmental Laboratory 

Quality Assurance 

rel 2C /0 

Quality 4surance Representative Date : 

Quality Associates, Inc. 

Page 2of15 
Laboratory Project Number GLP10-09-01 

Protocol Signatures 

Study Director: 

Jai Kesari, P.E., DEE Date: 

Weston Solutions, Inc. 

Sponsor Representative: 

, 

henstein 

ironmental Health and Safety Operations 

Principal Analytical Investigator: 

Date: 

Cleston Lange, Ph.D. Date: 

3M Environmental Laboratory 

Laboratory Management: 

William Reagen, Ph.D. Date: 

3M Environmental Laboratory 

Laboratory Technical Review 

Cliffton Jacoby, Ph .D. Date: 

3M Environmental Laboratory 

Quality Assurance 

Quality Assurance Representative Date: 

Quality Associates, Inc. 

Page 2 of 15 
P. 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, MN 55144 

651-737-3570 

Cleston Lange, Ph.D. 

3M Environmental Laboratory 

3M Center, Building 0260-05-N-17 

St. Paul, MN 55144 

651-733-9860 

3M Environmental Laboratory 

3M Center, Building 0260-OS-N-17 

St. Paul, MN 55144 

Study Initiation Upon Protocol Signature 

Experimental Start Date March 5, 2010 

Experimental Terrnination Date December 01, 2011 

Study Completion December 31, 2011 

Page 3 of 15 
p. 20 

Laboratory Praject Number GLP10-01-!)1 

1 . INTRODUCTION AND OBJECTIVE 

This study is being conducted as part of the Memorandum of Understanding (MOU) between 3M 

Company, Dyneon and the United States Environmental Protection Agency, effective October 

25, 2004. As part of the MOU, 3M is to conduct a perfluorooctanoic Acid (PFOA) site-related 

environmental monitoring and assessment program for the 3M Decatur, Alabama facility. 

The objective of this study is to aid in the characterization of PFOA concentrations in various 

environmental media (groundwater, soil and sediments) associated with and near the Decatur 

facility. 

2. REGULATORY COMPLIANCE 

This study will be conducted in accordance with the Toxic Substances Control Act (TSCA) 

Good Laboratory Practices Standard, 40 CFR part 792 . This study is for the analysis of 

environmental samples and only the analytical portion, as described herein, will be conducted 

under the GLP standard at the 3M Environmental Laboratory. 

3. SCOPE OF INVESTIGATION 

This study will help to detennine the presence and concentration of perfluorooctanoic acid in 

groundwater, soil and sediment samples collected in the vicinity of the 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, TCR number, physical description, and 

purity of the test substance being monitored in the test system is not known as it would be 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 

CF Z\0 

/ 

3 CF 2 CF 2 CH 

C$F15O2H 

414.07 

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Laboratory Project Number GLP10-01-09 

5. REFERENCE SUBSTANCE 

5. 9 The 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 Sealed Ampule) 

5.2 Reserve Samples: A reserve sample of each 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, if any, of the reference substances . 

5.4 Safety Precautions: All laboratory safety precautions will be followed. A current 

MSDS will be maintained for each of the reference substances . 

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Laboratory Project Number GLP10-01-01 

5.5 Stability: The stability of the test substance will be documented during the study. 

Stability is demonstrated by successful calibration verification standards bracketing the 

samples within an analytical run, comparison of standard curves from different runs 

performed on different days, and precision requirements for replicate samples. 

6. TEST SYSTEM 

6.1 Description of the Test System. The test systems for this study will be a variety 

of groundwater, soil and sediment samples collected in the vicinity of the 3M Decatur, 

Alabama facility and landfills which received waste from the 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 of samples is unknown 

since the sampling and analysis will be of an iterative nature that is dependent on 

results. Samples anticipated for each sampling event will be defined apriori by a 

protocol amendment which is written in the form of a 3M Environmental Laboratory 

general project outline (GPO) describing the number and types of samples anticipated. 

The total number of samples analyzed will be amended quarterly to this protocol and a 

final tallied number amended prior to the completion of the 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 of the samples(sample, trip blank, field matrix spike, etc.) . This 

information will be provided on the labels by Weston Solutions, Inc. field personnel. 

Once received at the 3M Environmental Laboratory with a proper chain of custody, the 

samples will be additionally labeled with a laboratory information management system 

(LIMS) generated sample ID number for internal tracking purposes. 

7. SPECIMEN RECEIPT AND STORAGE 

Samples received are logged and tracked according to the 3M Environmental Laboratory 

standard operating procedures (SOP's). Once received at the 3M Environmental Laboratory 

with a proper chain of custody, the samples are logged into the LIMS system and then stored 

refrigerated. 

8. ANALYTICAL METHODS 

Analysis of the study samples will be conducted at the 3M Environmental Laboratory. The 

analysis will be carried out utilizing liquid chromatography with tandem mass spectrometry 

detection (LGMSIMS). The anticipated method to be used for the analysis of each 

environmental matrix is given in Table 2, along with the target lower limits of quantitation 

(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 LLOQ is not attainable, this will be discussed in the final report. The instrumental 

conditions used will be documented in detail in the raw data. 

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Laboratory Project Number GLP90-01'-01 

All concentrations of PFOA will be reported as the anion form, [C7F1SCOO]" . 

TABLE 2. LIST OF MATRICES, METHODS AND TARGET LLOQS 

Matrix Method Number and Name Target LLOQ 

Groundwater Method ETS-8-044 "Method of Analysis 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 of stable isotope-labeled internal standard 

calibration, and a stable isotope-labeled surrogate analyte to aid in future evaluations of analyte 

recovery in lieu of laboratory matrix spike (LMS) or field matrix spike (FMS) samples (i .e . data 

will be used to show that recovery of surrogates 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 PFOA will be used for calibration 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 important to assess the quantitative accuracy of the methods for linear + branched 

PFOA using a linear PFOA calibration . Triplicate laboratory control spikes (LCSs) will be 

fortified with reference materials that consist of a mixture of linear + branched isomers (typical 

of the normal distribution from electrochemical fluorination synthesis) and fortified at a 

concentration near the mid-level of the calibration range. Quantitation of these LCSs will be 

performed using the calibration curve constructed from the analysis of linear isomer calibration 

standards. Results of LCSs will offer some level of accuracy assessment, however final results 

will not be adjusted for the level of accuracy determined since the absolute source and isomer 

distribution in the environment for these analytes is not assumed. 

A stable 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 surrogate recovery data is 

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Laboratory Project Number GLPl D-©1-01 

being obtained to build a data set using real environmental samples to better evaluate their 

potential future use in lieu of the more difficult to prepare and more costly and time consuming 

FMSs and LMSs. However, the surrogate recoveries will not be used to assess reportability of 

data in this study. 

A stable 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 PFOA and 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 two phases. A first 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 of three fresh aliquots of each bulk 

sample. The first two aliquots will be identified as sample and sample duplicate. The 

third aliquot will be fortified with linear PFOA as a LMS sample; fortified at an 

appropriate level based on the results of the screening determination or other information. 

The percent moisture of each soil sample will be determined and all final results reported 

on a dry weight basis after adjusting for the percent moisture. 

9. DATA QUALITY OBJECTIVES 

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 of groundwater samples, a procedural (method) blank 

consisting of an aliquot of Milli-Q or 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 of soil and sediment samples, a procedural (method) blank 

consisting of a control 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 devoid of target 

analyte. 

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Laboratory Project Number GLP90-01-09 

The area counts for each analyte in a procedural blank must be < 50°/© of the area 

counts of the LLOQ standard . If not, then the LLOQ must be raised to the lowest 

concentration standard that meets that criterion. An analytical batch may contain 

more than one procedural blank. The analytical results from analysis of multiple 

procedural blanks in an analytical run will be averaged in the evaluation of the 

LLOQ. The procedural blanks should be prepared with the same matrix used to 

prepare the calibration standards in the extraction batch 

9.1.2 Trip Blanks 

For groundwater samples, a trip blank of Milli-Q or 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 of the study results . 

For soil/sediment samples, a trip blank of approximately 5 grams of standard control 

soil is prepared in a sample container in the laboratory and 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 of the 

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% of the lowest calibration standard. 

9.'!.4 Rinseate Samples 

A number of rinseate samples may be collected as part of the soil and sediment 

sample collection process for evaluating the effectiveness of decontamination of 

sample collection equipment. Such samples will be provided 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 from these samples will be considered in the evaluation 

of the final study results . 

9.2 Calibration and Lower Limit of Quantitation (LLOQ): 

9.2.9 Calibration 

The reference material for the target analyte is the linear isomer of PFOA and will be 

used for calibration standard preparations and LMS fortifications . A stable 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. A stable isotope-labeled surrogate [(1,2,3,4-I3C4)-PFOA] 

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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 calibration standards, and quantified to determine 

surrogate recoveries. 

The linear PFOA, surrogate and internal standard (IS) will be spiked as appropriate to 

the matrix aliquots prior to extraction. Calibration points 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 LLOQ for water 

calibration, and 100 +_ 30% L 35°lo at LLOQ) for soil calibration. A minimum 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 

calibration verification (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/MS transitions to be used for the target analyte, surrogate and IS are 

provided in Table 3 . 

TABLE 3. THE MS/MS TRANSITIONS FOR THE TARGET ANALYTE(S), 

INTERNAL STANDARD AND SURROGATE. 

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 of Quantitation (LLOQ) 

The LLOQ is the lowest non-zero active standard in the calibration curve. The peak 

area counts of the LLOQ must be greater than two times the peak area counts of the 

procedural blanks . By definition, the measured value of the LLOQ must be within ± 

30% of the theoretical value for water calibrations, and ± 35% for soil calibrations . 

The target LLOQ for water analysis is 0 .025 nglmL (0.025 ppb, 25 ppt) and 0.200 

nglg (0.200 ppb, 200 ppt; wet weight basis) for soil/sediment analyses . 

9.3 Laboratory Control Spike (LCS) 

Laboratory control spike samples (LCSs) for groundwater samples consist of an aliquot 

of Milli-Q or equivalent water, or a standard control soil or sediment, to which known. 

quantities of PFOA, surrogate and IS are added in the laboratory. The linear + branched 

mixed isomer form of PFOA will be used for LCS preparations, 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) from LCSs must be within 100 _+ 20°lo for water 

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%. 

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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 from the 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 RPD of duplicate 

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 such when reported. 

9.6 Field Matrix Spikes and Lab Matrix Spikes 

The addition of known quantities of target analyte to samples for determining the 

efficiency of analyte recovery for the sample is commonly used for evaluating data 

quality and criteria for reporting of results . In general, the highest level of confidence is 

acquired from FMS recovery results in water samples, and FMS results will be treated as 

the primary (highest) quality control parameter for reporting those sample results. 

However, in some instances FMS recoveries may not be at appropriate levels relative to 

endogenous sample analyte levels for proper recovery determinations . In those 

instances, the preparation of LMSs and evaluation of LMS recovery results will dictate 

the reportability of results. The recovery of the mass-labeled surrogate will not be 

considered in the reporting of results, and is included herein to collect data for surrogate 

recovery in real world samples, and results of the surrogates will be correlated to LMS 

and FMS recoveries in a separate data analysis. Failure to meet reporting criteria from 

FMS or LMS results 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 study director and sponsor. 

9.6.1 Field Matrix Spikes (FMS) - Groundwater Samples 

An FMS is a sample to which known quantities of the 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. A low 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 10 times the measured sample 

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Laboratory Project Number GLP10-01-01 

concentration. FMS acceptance criteria are recoveries within 100 ± 30% of the 

expected value . Sample data with FMS recovery outside of 100 ± 30%, but within 

±50°l0, of the expected value are flagged and reported as outside of QC acceptance 

criteria . Data with FMS recovery outside of f50% of the expected value are reported 

as NR, where NR is defined as "Not Reportable" data outside of QC acceptance 

criteria . If FMS recovery 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 

Because the 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 spiking of a pre-measured volume of soil or sediment with known 

quantities of the target analyte, surrogate and IS. As the density of soil and sediment 

samples will vary from one sample to the next, the true spiked concentrations will be 

corrected for the accurate mass of each sample. The recovery of each target analyte 

will be used to evaluate the ability to quantitatively recover the same endogenous 

analytes from a specific study sample. The ratio of endogenous analyte to lab spike 

concentration that is appropriate to assess accuracy is defined as approximately 0.5 to 

10-times the measured sample concentration. LMS method acceptance criteria are 

recoveries within 100% + 30% of the expected value. Sample data with LMS 

recovery outside of-±30% but within t50% of the expected value are flagged and 

reported as outside of QC acceptance criteria. Data with LMS recovery outside of 

100% f 50% of the expected value are reported as NR, where NR is defined as "Not 

Reportable" data outside of QC acceptance criteria. 

9.7 Surrogates 

Mass-labeled PFOA (Table 1) will be used as a surrogate target analyte to aid in the 

future evaluation of analyte recovery and method precision and accuracy by this 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 

of within 100 +_ 30°Jo is expected, and recovery results will be correlated to LMS and/or 

FMS recoveries determined for those saine environmental samples to determine how well 

the surrogate tracks the FMS/LMS analyte recoveries. Surrogate recoveries will not be 

Page 12 of 15 
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Laboratory Project Number GLP9D-01-0a 

used to assess reportability of results, however a summary of surrogate recoveries will be 

provided in a separate table in each interim report . 

9.8 Demonstration of specificity 

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 of each 

study sample will have their accurate wet weight determined on a four decimal place 

analytical balance and recorded, and then the aliquot will be dried in an oven at greater 

than 102°C until a stable weight 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 

of the sample. The average percent moisture 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 location will include the average of the 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 two significant 

digits. 

11 . REPORT 

To accommodate quarterly reporting of the overall study progress to EPA, the issuance of 

interim analytical 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 . A targeted tum-around time for interiuu analytical reports is eight (8) 

weeks from the date of sample receipt at the laboratory, however, circumstances may facilitated 

the need for shorter or longer turn-around times. Each interim report will include, but not be 

limited to, the following when applicable: 

11.1 Name and address of the facility performing the study, 

1 1 .2 Dates upon which the study was initiated and completed. 

19.3 A statement of compliance 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. 

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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 of the test substances under the conditions of administration, if provided by 

the Sponsor. 

11.7 A description of the methods used to conduct the test(s). 

11.8 A description of the test system. 

11.9 A description of any circumstances that may have affected the quality or the integrity 

of the data. 

11. '1 D The name of the Study Director and the names of other scientists, professionals, and 

supervisory personnel involved in the study. 

11. '! 1 A description of the transformations, calculations, or operations performed on the 

analytical data, a summary and analysis of the 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, if applicable. 

11.13 The signed and dated reports of each of the individual scientists or other professionals 

involved in the study, if applicable. 

11.14 The location where raw data and the final report are to be stored. 

11.15 A statement prepared by the Quality assurance unit listing the dates that study 

inspections and audits were made and the dates of any findings reported to the Study 

Director and Management. 

11.16 If it is necessary to make corrections or additions to a final report after it has been 

accepted, the changes will be made in the form of an amendment issued by the Study 

Director. The amendment will clearly identify the part of the final report that is being 

amended, the reasons for the amendment, and will be signed by the Study Director. 

12. LOCATION OF RAW DATA, RECORDS, AND F1NAL 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 of the 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 10 years 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 

12.1.2 Study correspondence 

12.1 .3 Shipping records 

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Laboratory Project Number GLP10-01-01 

12.1.4 Raw data 

12.1.v Approved final report (original signed copy) 

12.1 .6 Electronic copies of data 

92.2 The following supporting records will be retained separately from the study folder in 

the archives according to 3M Environmental Laboratory Standard Operating 

Procedures: 

12.2.1 Training records 

12.2.2 Calibration records 

12.2.3 Instrument maintenance logs 

72.2.4 Standard 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 of a laboratory GPO, which will 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 of the protocol and will be attached to the final 

protocol . Any other changes will be in the form of written 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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