# 3

GLP10-01-02 Interim Report 21: Analysis for PFOS, P FHS and PFBS in Decatur, AL Soils Collected from Well Location 610 in August, 2011


## Study Title 3M Environmental Laboratory Analytical Protocol GLP 10-01-01: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur P hase 3 Site-Related Monitoring Program 

## Data Requirement
Data Requirement EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792



## Study Director Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 

### Phone: 610-701-3761 

## Principal Analytical Investigator

Cleston C. Lange, Ph.D. 3M Environmental Laboratory 

## Interim Report Completion Date

Upon Signing 

## Performing Laboratory 3M Environmental Health and Safety Operations

Environmental Laboratory 3M Center, Bldg 260-05-N-17 St. Paul, MN 55144 

## Project Identification GLP10-01-02-21
Total Number of Pages

23Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 2 of 23 This page has been reserved for specific country re quirements.study : GLP10-01-02 , Interi m Repor t 2 1 Analysi s fo r PFOS , PFH S & PFB S i n Decatur , A L Soil s Collecte d fro m Wel l Locatio n 61 0



### GL P COMPLIANC E STATEMEN T

Repor t Title : GLP10-01-0 2 Interi m Repor t 21 : Analysi s fo r PFOS , PFH S an d PFB S i n Soil s Collecte d fro m Wel l Locatio n 61 0 i n Augus t 2011

. 3 M Environmenta l Laborator y Analytica l Protoco l GLP-10-01-02 : Analysi s o f Perfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo r th e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program

. Thi s analytica l phas e wa s conducte d i n complianc e wit h Toxi c Substance s Contro l Ac t (TSCA ) Goo d Laborator y Practic e (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

Exception s t o GL P compliance :

• Th e referenc e substance s wer e no t al l characterize d unde r GLPs

.

• Becaus e thes e ar e environmenta l sample s an d th e stud y analytica l i n natur e only , ther e wa s n o specifi c tes t substanc e o r contro l substanc e fo r thi s study

.

Gar y Hohenstein , Sponso r Representativ e Dat e

Jaisimh a Kesari , P.E. , DEE , Stud y Directo r

Pag e 3 o f 2 3study : GLP10-01-02 , Interi m Repor t 2 1 Analysi s fo r PFOS , PFH S & PFB S i n Decatur , A L Soil s Collecte d fro m Wel l Locatio n 61 0



### QUALIT Y ASSURANC E STATEMEN T

Repor t Title : GLP10-01-0 2 Interi m Repor t 21 : Analysi s fo r PFOS , PFH S an d PFB S i n Soil s Collecte d fro m Wel l Locatio n 61 0 i n Augus t 2011

. 3 M Environmenta l Laborator y Analytica l Protoco l GLP-10-01-02 : Analysi s o f Perfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo r th e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program

.
Thi s interi m analytica l repor t an d th e accompanyin g dat a wer e audite d b y th e 3 M Environmenta l Laborator

y Qualit y Assuranc e Uni t (QAU) , a s indicate d below

. Th e finding s wer e reporte d t o th e principa l investigato r (P.I.) , laborator y managemen t an d stud y director

.

stud y Inspectio n Date s Phas e Dat e Reporte d t o stud y Inspectio n Date s Phas e P.I

. Stud y Directo r Managemen t Stud y Directo r

Nov

. 14-15 , 201 1 Interi m Repor t an d Dat a 11/25/201 1 1/13/201 2 1/13/201 2

QA U Represerjfativ e Dat e

Pag e 4 o f 2 3Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 5 of 23 

## T ABLE OF 

## C ONTENTS GLP Compliance Statement ..........................

................................................... ......................................... 3 Quality Assurance Statement .......................

................................................... .......................................... 4
Table of Contents .................................

................................................... ................................................... 5
List of Tables ....................................

................................................... ................................................... ..... 6
1 Study Information .................................

................................................... ............................................ 7
2 Summary ...........................................

................................................... ............................................... 8
3 Introduction ......................................

................................................... ................................................. 9
4 Test, Control and Reference Substances ............

................................................... ........................... 9
5 Test System .......................................

................................................... ............................................. 11
6 Method Summary ....................................

................................................... ....................................... 11
6.1 Methods ...........................................

................................................... .................................. 11
6.2 Sample Receipt ....................................

................................................... ............................. 11
6.3 Sample Preparation ................................

................................................... ........................... 11
6.4 Percent Soil Moisture Determination ...............

................................................... ................. 12
6.5 LC/MS/MS Analysis .................................

................................................... .......................... 12

7 Analytical Results ................................

................................................... ........................................... 14
7.1 Calibration .......................................

................................................... ................................... 14
7.2 Limits of Quantitation (LOQs) .....................

................................................... ...................... 15
7.3 Continuing Calibration ............................

................................................... ........................... 15
7.4 Blanks ............................................

................................................... ..................................... 15
7.5 Laboratory Control Spikes (LCSs) ..................

................................................... .................. 16
7.6 Laboratory Matrix Spikes (LMSs) ...................

................................................... .................. 17

7.7 Percent Moisture Determinations ...................

................................................... .................. 18
7.8 Individual Sample Results .........................

................................................... ........................ 18Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 6 of 23 8 Conclusion ........................................

................................................... .............................................. 21
9 Data/Sample Retention .............................

................................................... ..................................... 22
10 List of Attachments ...............................

................................................... .......................................... 22
11 Signatures ........................................

................................................... ............................................... 22 

## L IST OF 

## T

ABLES
Table 1. Results for Decatur, AL Soils from Well L ocation 610 ....................................... ....................... 8 Table 2. LMS Recovery for Decatur, AL Soils from W ell Location 610 .................................. ................ 8
Table 4. Instrument Information ..................

................................................... ......................................... 13 Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053)....................................... .............. 13
Table 6. Mass Transitions ........................

................................................... ............................................ 13 Table 7. PFOS Calibration Summary ................

................................................... .................................. 14 Table 8. PFHS Calibration Summary ................

................................................... .................................. 15 Table 9. PFBS Calibration Summary ................

................................................... .................................. 15 Table 10. LCS Results (PFOS, linear + branched iso mer) .............................................. ..................... 16 Table 11. LCS Results (PFHS, linear + branched iso mer) .............................................. ..................... 16 Table 12. LCS Results (PFBS) .....................

................................................... ....................................... 17 Table 13. Analytical Method Uncertainties ........

................................................... .................................. 17 Table 14. Percent Moistures for Decatur, AL Soils from Well Location 610 ............................ ............ 18 Table 15. Individual PFOS Results for Decatur, AL Soils from Well Location 610 ...................... ........ 18 Table 16. Individual PFHS Results for Decatur, AL Soils from Well Location 610 ...................... ........ 19 Table 17. Individual PFBS Results for Decatur, AL Soils from Well Location 610 ...................... ........ 20Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 7 of 23 

### 1 Study Information

Sponsor 3M Company
Sponsor Representative Gary A. Hohenstein Environmental Manager Special Projects, EHS Operations Bldg 224-5W-03 St. Paul, MN 55144 Phone: (651) 737-3570 gahohenstein@mmm.com
Study Director Jaisimha Kesari, P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380
Study Analytical Testing Facility 3M EHS Operations Environmental Laboratory Building 260-5N-17 St. Paul, MN 55144
Study Personnel (3M Environmental Laboratory) Cleston C. Lange, Ph.D., Principal Analytical Inves tigator William K. Reagen, Ph.D., Laboratory Manager Patrick Kenney, Laboratory Technician (Pace Analyti cal, Professional Services) Marlene Heying, Laboratory Technician (Pace Analyti cal, Professional Services)
Study Dates Study Initiation: March 08, 2010 Interim Analytical Initiation: September 12, 2011 Interim Analytical Completion: October 19, 2011 Interim Report Completion: Upon final Signatures

Location of Archives All original raw data and analytical reports have b een archived at the 3M Environmental Laboratory according to 40 CFR Part 792. The analy tical reference standard reserve samples are archived at the 3M Environmental Labora tory according to 40 CFR Part 79Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 8 of 23 

### 2 Summary
This interim report provides the PFOS, PFHS and PFB S concentration results for the four soils collecte d in August 2011 near well location 610, located near the 3M facility at Decatur, AL. One travel blank (trip blank), containing approximately 16 grams of contro l soil in a sample bottle, accompanied the sample bottles to and from the site and was also analyzed. Samples were logged into the 3M Environmental Laboratory information management system (LIMS) und er project GLP10-01-01-21. Four aliquots of soil were removed from each sample bottle and accurately weighed for extraction. The first and second aliquot served as sample and duplicate sample. The third and fourth replicates were fortified with no minal 5.00 and 50.0 ng of PFOS (linear isomer), PFHS (lin ear isomer) and PFBS as a low and high laboratory matrix spike (LMS), respectively. A single LMS for the trip blank was fortified with nominal 1.00 ng of PFOS (linear isomer), PFHS (linear isomer) and PFBS . Sample were extracted and analyzed per method ETS-8-053 which employs analysis by liquid chromato graphy with triple quadrapole mass spectrometric detection (LC/MS/MS). The LMS recovery results pro vided a measure of data accuracy. The relative percent difference (RPD) of the duplicate sample re sults was used to assess the analytical precision o f the sample results. The percent moisture of each s oil was also determined as part of the study. The PFOS, PFHS and PFBS concentrations are summarized i n Table 1 . The PFOS, PFHS and PFBS recoveries from the LMS samples are summarized in Table 2

.
Table 1. Results for Decatur, AL Soils from Well L ocation 610



### 3M LIMS ID [d] 

### Sample ID Analyte Concentration (ng/g; dry) PFOS PFHS PFBS GLP10-01-01-21-001 DAL-SB-610S-0-0000 36.1 0.586 0.991 GLP10-01-01-21-002 DAL-SB-610S-0-0010 19.5 0.690 0.439 GLP10-01-01-21-003 DAL-SB-610S-0-0040 3.00 1.11 0.572 GLP10-01-01-21-004 DAL-SB-610S-0-0150 BLQ BLQ BLQ GLP10-01-01-21-005 TRIP BLANK-1 BLQ BLQ BLQ LMS results were within acceptance criteria of 100 + 30% Concentration values are shown at 3 significant fig ures, but more precise data was used for data calcu lations. RPD values were less than 50% for all duplicate sam ple results unless otherwise indicated BLQ; analyte response was lower than the analyte re sponse of the LLOQ which was nominal 0.200 ng/g low standard

Table 2. LMS Recovery for Decatur, AL Soils from W ell Location 610


### 3M LIMS ID [b] 

### Sample ID LMS Recovery (%) PFOS PFHS PFBS GLP10-01-01-21-001 Low DAL-SB-610S-0-0000 Lab Matrix Spike Low [a] 91.3% 93.8% GLP10-01-01-21-001 High DAL-SB-610S-0-0000 Lab Matrix Spike High 97.8% 102% 109% GLP10-01-01-21-002 Low DAL-SB-610S-0-0010 Lab Matrix Spike Low [a] 103% 110% GLP10-01-01-21-002 High DAL-SB-610S-0-0010 Lab Matrix Spike High 93.0% 95.0% 101% GLP10-01-01-21-003 Low DAL-SB-610S-0-0040 Lab Matrix Spike Low 112% 103% 112% GLP10-01-01-21-003 High DAL-SB-610S-0-0040 Lab Matrix Spike High 111% 97.6% 109% GLP10-01-01-21-004 Low DAL-SB-610S-0-0150 Lab Matrix Spike Low 98.1% 92.3% 91.5% GLP10-01-01-21-004 High DAL-SB-610S-0-0150 Lab Matrix Spike High 87.4% 91.6% 100% GLP10-01-01-21-005 LMS Trip Blank-1 Lab Matrix Spike Low 97.4% 102% 115% LMSs were fortified with PFOS, PFHS and PFBS (linea r isomers only) at nominal 5.0 ng (low) and 50.0 ng (high). The LMS for the trip blank was fortified at nominal 1.0 ng each of PFOS, PFHS and PFBS Concentration values are shown at 3 significant fig ures, but more precise data was used for data calcu lations. [a] LMS fortification level was too low relative to the endogenous analyte level to make an accurate d etermination of recovery.Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 9 of 23 

### 3 Introduction
The soil analyses results reported herein were cond ucted as part of the Phase 3 Environmental Monitoring and Assessment Program for the 3M facili ty located in Decatur, Alabama. The objective of the overall program is to gain information regar ding concentrations of perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) and perflu orobutane sulfonate (PFBS) in various environmental media such as groundwater, soils and sediments that are associated with and near the Decatur facility. Reported herein are the resu lts from analysis of soils from near well location 610, located near the 3M facility in Decatur, AL. The samples were collected by Weston Solutions, Inc. personnel in August 2011 and shipped to the 3M Environmental Laboratory for quantitative analysis of PFOS, PFHS and PFBS. One soil travel b lank (trip blank) was also analyzed. This report describes the sample shipment, receipt, extraction and quantitative LC/MS/MS analysis procedures conducted for determination of PFOS, PFH S and PFBS in the soil samples received. Additionally included in this report are the assess ment of the analytical precision and accuracy for t he reported PFOS, PFHS and PFBS concentration results.



### 4 Test, Control and Reference Substances
This study does not have a test substance in the cl assic sense of a GLP study because this study was purely analytical in nature. The reference and control substances are listed in Table 3

.

Table 3. Reference Substances

Reference ID PFOS (linear) PFOS (linear + branched) PFHS (linear)

Chemical Name n-Perfluorooctane-1- Sulfonate Potassium Salt Perfluorooctane Sulfonate Potassium Salt n-Perfluorohexane-1-sulfonate Sodium Salt
Chemical Formula n-C 8 F 17 SO 3 K C 8 F 17 SO 3 K n-C 6 F 13 SO 3 Na

Use Reference Standard for Calibration and LMSs Reference Standard for LCSs Reference Standard for Calibration and LMSs
Source Wellington Laboratories 3M Wellington Laboratories
Expiration Date 10/18/18 12/14/16 3/25/18
Storage Conditions -20 ̊C -20 ̊C -20 ̊C

Chemical Lot Number LPFOSKBM06 171 LPFHxSAM08

TCR Number TCR08-0001-1/1 TCR-696 TCR08-0018-1/1
Physical Description Crystalline White Powder Crystalline
Purity 98% 86.4% >98%Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 10 of 23 Table 3. Reference Substances

Reference ID PFHS (linear + branched) PFBS (predominantly linear) 13 C 4 -PFOS

Chemical Name n-Perfluorohexane-1- sulfonate Potassium Salt Perfluorobutane-1-sulfonate Potassium Salt [1,2,3,4- 13 C 4 ]-Perfluorooctane1-Sulfonate Sodium Salt
Chemical Formula n-C 6 F 13 SO 3 K n-C 4 F 9 SO 3 K 13 C 4 12 C 4 F 17 SO 3 Na

Use Reference Standard for LCSs Reference Standard for All PFBS Surrogate

Source 3M 3M Wellington Laboratories
Expiration Date 2/12/17 1/10/17 9/8/2013
Storage Conditions -20 ̊C -20 ̊C -20 ̊C

Chemical Lot Number NB 120067-69 101 MPFOS0910

TCR Number TCR-083 TCR-121 TCR10-0044-2/9
Physical Description White Powder White Powder Methanol solution, sealed ampoule Purity 98.6% 96.7% >98% [a]

Reference ID 13 C 8 -PFOS 13 C 3 -PFHS 18 O 2 -PFBS

Chemical Name [ 13 C 8 ]-Perfluorooctane-1- Sulfonate Sodium Salt [ 13 C 3 ]-Perfluorohexane-1- Sulfonate Sodium Salt [ 18 O 2 ]-Perfluorobutane-1- Sulfonate Ammonium Salt
Chemical Formula 13 C 8 F 17 SO 3 Na 13 C 3 12 C 3 F 13 SO 3 Na C 4 F 9 S 18 O 2 16 O NH 4
Use Internal Standard for PFOS Internal Standard for PFHS Internal Standard for PFBS

Source Wellington Laboratories Wellington Laboratories RTI International
Expiration Date 9/28/2013 9/28/2013 3/9/15
Storage Conditions -20 ̊C -20 ̊C -20 ̊C

Chemical Lot Number 092310 092310 11546-107-2

TCR Number TCR10-0048-3/16, 4/16 TCR10-0048-3/16, 4/16 TCR-1042
Physical Description Mixed IS methanol solution in sealed ampoule Mixed IS methanol solution in sealed ampoule Methanol solution, sealed ampoule Purity >98% [a] >98% [a] >99% [a] [a] The commercially provided material was a methan ol solutions and labeled with a weight/volume conce ntration purity value. However, the concentration of furthe r dilutions was based on the certified concentratio n of the stock material.Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 11 of 23 

### 5 Test System
There was not a test system for this study in the c lassic sense of a GLP study. This study was conducted for analysis of off-site soils collected near well location 610, near the 3M facility in Decatur, AL. Samples for this study are “real worl d” environmental samples. 

### 6 Method Summary

6.1 Methods
Soil extractions and quantitative LC/MS/MS analysis were performed following validated method ETS-8-053.0. The analysis conducted for reporting results was performed on October 7, 2011 as analytical run s111007a. 

### 6.2 Sample Receipt
On August 23, 2011 four (4) empty 250-mL HDPE Nalg eneTM sample bottles, and one travel blank (trip blank) containing approximately 16 gram s of a control soil TCR-842, were sent from the 3M Environmental Laboratory to Weston Solutions, In c. field personnel for collection of soils from well location 610. Following the soil sample col lections by Weston Solutions, Inc. personnel, 4 soil-filled sample bottles and the trip blank were sent to the laboratory for analysis. The samples were received with sample chains of custody numbers 16926 on September 12, 2011. A discrepancy between the date of bottle order sent t o Decatur (8/23/2011) and the listed date of collection of the soils (8/19/2011) indicated sampl es were collected prior to receiving the bottles and trip blank. Charles Young of Weston, Inc. wh o oversaw the soil collections at Decatur was notified and indicated that the trip blank likely d id not accompany the samples during collection in Decatur since other bottles apparently were used th an those sent on 8/23/2011. However, the trip blank did accompany the samples when shipped back t o 3M. A protocol deviation regarding this was written and is maintained in the study folder f or project GLP10-01-01-21. Soil samples from Decatur, AL are regulated and wer e appropriately shipped in accordance with USDA/APHIS soil permit number P330-09-00125. Sample nomenclature follows the form DAL-SB-610x-xx -xxxx where the first string defines the Decatur Alabama (DAL) project area, the second string defin es the sample media (i.e., SB= soil boring), the th ird string defines the specific well identity (well 610 ). The fourth string defines the sample type (0 = primary sample, DB = field duplicate, RB = equipment rinsea te blank). The fifth string indicates the sampling depth range (0040 indicates 4.0 ft to 4.5 ft interv al soil sample).


### 6.3 Sample Preparation
Sample preparation was conducted as a single batch on October 4-5, 2011. Each soil extraction involved removal of a 1 cubic centimeter (1 cc; 1 mL) soil aliquot (typically ~ 1 gram) from each sample bottle using a fixed volume 1 cc s poon, transferring it to a 15 mL conical centrifuge tube, followed by accurate weight determination of the aliquot on a 5-place balance. Then, nominal 3. 0 ng of each stable isotope labeled internal standard (IS) was added to each soil aliquot. Internal standards 13 C 4 -PFOS, 13 C 3 -PFHS and 18 O 2 -PFBS are described in Table 3 . Each soil aliquot was extracted by addition of 8 mL of a 4:1 acetonitrile :water solution followed by sonication for 1 to 2 h ours and then centrifugation to remove solids. The supe rnatant from each was then transferred to an autovi alStudy: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 12 of 23 for analysis. An accurately measured volume of eac h supernatant was analyzed by LC/MS/MS. For a few samples, the 1cc aliquot resulted in only ~0.65 gram of soil, therefore, extra soil was used in those extractions in order to be closer to 1 gram o f sample. In those few instances the inclusion of extra sample ensured adequate sensitivity for target ana lytes was achieved for the final extract. During preparation, each sample received nominal 3. 0 ng of a stable isotope labeled surrogate recovery standard (SRS) as 13 C 4 -PFOS. Although not included as part of the data accuracy assessment for this study, SRS recovery determinations were included as part of an ongoing method validation aspect for SRS behavior in environmental soil samples for pote ntial future applications. The SRS was quantified from a SRS calibration curve constructed from analy sis of calibration standards prepared from the SRS in calibration standards. The SRS recovery was det ermined based on the calculated concentration of SRS from the analysis and recovery of SRS from each sample is included in Table 15, Table 16 and Table 17 , but was not used for evaluation of data accuracy for this study and is otherwise excluded from the discussions in the report. Each analytical sample was prepared in duplicate fo r analysis of PFOS, PFHS and PFBS in the soil sample. Additionally, a third and fourth replicat e was weighed out and used to prepare a low- LMS an d high-LMS, fortified with PFOS (linear), PFHS (line ar) and PFBS at nominal 5.0 ng and 50.0 ng each, respectively. LMS results were used for determinat ion of data accuracy. RPD of duplicate samples results was used for determination of data precisio n. Calibration standards were prepared by spiking know n quantities of PFOS (linear isomer), PFHS (linear isomer) and PFBS into 1-cubic centimeter (1 cc, 1 m L) aliquots of 3M Environmental Laboratory control soil TCR-842. The nominal mass of 1 cc of control soil TCR-842 is 1.0 gram (dry). The nominal calibration standard range prepared and analyzed wa s 0.200 ng/g to 500 ng/g. Laboratory control spike (LCS) samples were prepare d with each sample preparation batch; prepared at three levels (nominal 3.0 ng/g, 30.0 ng/g and 300 n g/g) and each level in triplicate. The LCSs were prepared using control soil TCR-842, same as calibr ation standards, and were fortified with technical PFOS (mixed linear and branched isomer), technical PFHS (mixed linear and branched isomers) and PFBS. The LCS results were used to estimate the a nalytical method uncertainty.



### 6.4 Percent Soil Moisture Determination
The percent moisture of soils was used to calculate the dry weight of the wet soils weighed during sample preparations for PFOS, PFHS and PFBS analysi s, and was determined by gravimetric analysis. Dry weights were determined for separate weighings than the weighings used for extractions. To determine the percent moisture, duplicate aliquots of each soil sample were removed and the accurate “wet” weight determined for each. All aliquots wer e dried at > 100°C until no further mass loss occurred from water evaporation, at which time the accurate dried weights were determined. The difference in mass, attributed to water evaporation, was used to calculate the percent moisture of the original soil

. The averaged percent moisture result for each was t hen used to calculate the soil PFOS, PFHS and PFBS concentration on a dry weight basis. 

### 6.5 LC/MS/MS Analysis
The analysis of soil extracts for PFOS, PFHS and PF BS was performed by LC/MS/MS as described in method ETS-8-053.0. The relative perc ent difference (RPD) of duplicate prepared sample results was used as a measure of the analyti cal precision. The determined recovery of fortified PFOS, PFHS and PFBS from LMS samples was used as a measure of analytical accuracy. Surrogate recoveries are reported in Tab le 10, but were not used for evaluating analyte recovery for this study. The surrogate data was co llected as part of an on-going evaluation of surrogate recovery from environmental field samples for supporting a method validation of ETS-8- 053.Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 13 of 23 Details of the specific instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are detailed in the raw data, and are briefly described below in Table 4 , Table 5 and Table 6

.

Table 4. Instrument Information

Instrument Name ETS-Stan Analytical Method ID ETS-8-053.0 Liquid Chromatograph Agilent 1100 with Binary Pump Guard column Pre-Autosampler; Prism RP (2.1 x 50 mm, 5 μ m) Extraction column Oasis HLB (3 x 20 mm, 25 μ ); 30°C Analytical column Betasil C18 (2.1 x 100 mm, 5 μ ) Injection Volume 25 μ L Mass Spectrometer API 4000 Ion Source TurboIon Spray Polarity Negative Software Analyst 1.4.2
Table 5. Gradient Liquid Chromatography Conditions (ETS-8-053)
Step Number Total Time

[min] Flow Rate

[mL/min] Percent A

[2 mm Aqueous Ammonium Acetate] Percent B [ Acetonitrile]

1 0.0 0.400 97.0 3.0 2 3.0 0.400 97.0 3.0 3 3.5 0.400 70.0 30.0 4 17.0 0.400 40.0 60.0 5 17.5 0.400 10.0 90.0 6 19.5 0.400 10.0 90.0 7 20.0 0.400 97.0 3.0 8 23.0 0.400 97.0 3.0

Table 6. Mass Transitions

Analyte Mass Transitions Monitored PFBS 299>99, 299>80 18 O 2 -PFBS (IS) 303>84 PFHS 399>99, 399>80 13 C 3 -PFHS (IS) 402>80 PFOS 499>130, 499>99, 499>80 13 C 8 -PFOS (IS) 507>80 13 C 4 -PFOS (Surrogate) 503>80 Note: Multiple mass transitions are summed to give the instrument response for that analyte.Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 14 of 23 

### 7 Analytical Results
Concentration results are rounded to three signific ant figures according to EPA rounding rules. Because of rounding some calculated values may vary slightly from those found in the raw data. Samples with RPDs for duplicate results of less tha n 50% and associated LMS results meeting the method acceptance criteria of 100 ± 30% demonstrate d that the method was appropriate for those samples and were reported without footnotes in resu lts tables. The nominal 5.00 ng and 50.0 ng fortified quantities of PFOS, PFHS and PFBS into LM Ss for field samples were at an appropriate level for evaluating sample-specific analyte recoveries, with respect to the endogenous levels measured in the samples.



### 7.1 Calibration
A set of calibration standards were prepared by spi king varying known quantities of PFOS (linear), PFH S (linear), PFBS and surrogate ( 13 C 4 -PFOS), and a fixed quantity of stable isotope labe led internal standards, into one cubic centimeter (1 cc, 1 mL) a liquots of 3M Environmental Laboratory control soil TCR-842 (nominal soil mass of 1.0 g/mL). A total o f twelve (12) calibration standards were prepared a s a set. The prepared standards were fortified from nominal 0.200 ng to 500 ng in 1 cubic centimeter of control soil TCR-842; equivalent to nominal 0.200 n g/g to 500 ng/g in soilTCR-842. Following analysis of the calibration standards, the concentration of eac h standard was plotted against the measured analyte /IS peak area ratio. A quadratic equation with 1/x weighting was used to fit the data for each analyt e. Calibration curves were not forced through zero. D etermining the standard concentration using the resultant calibration curve and comparing to the kn own concentration confirmed accuracy of each curve point at within 100 ± 30% (+ 35% at the LLOQ). The correlation coefficient (r) was greater than 0.999 for all calibration curves, and the coefficient of dete rmination (r 2 ) was greater than 0.990. Calibration results for PFOS, PFHS and PFBS are summarized in Table 7 , Table 8 and Table 9 , respectively. Because soil weights can vary significantly for a 1 cc (1 mL) field sample, depending on soil type and moisture content, the instrument response was calib rated for the known concentrations of target analytes based on the mass quantity of reference s ubstance added to a 1 cc soil (1 mL) calibration standard prior to extraction ( e.g. calibrated in this study for a range of 0.200 ng/m L to 500 ng/mL PFOS, PFHS and PFBS). Because a 1cc aliquot of control s oil TCR-842 weighs nominally 1.0 gram (dry weight) and has less than 5% moisture content, the nominal concentration range of the calibration was essentially 0.200 ng/g to 500 ng/g. However, becau se the sample soil aliquots typically weigh more th an 1.0 gram and contain significant moisture, the dete rmined concentrations during the analysis on an ng/mL basis from the calibration curve were adjuste d for the accurate determined weight and percent moisture so they could be reported on a ng/g (dry w eight) basis.

Table 7. PFOS Calibration Summary

Analytical Run PFOS (ng) r

STD 1 STD 2 STD 3 STD 4 STD 5 STD 6 STD 7 STD 8 STD 9 STD 10 STD 11 STD 12
Actual 0.200 0.500 0.750 1.00 2.50 5.00 10.0 25.0 50.0 100 200 500 N/A

s111007a 0.202 0.482 0.725 1.09 2.45 4.91 9.56 24.7 53.8 101 195 502 0.9997
Recovery 101% 96.4% 96.6% 109% 98.2% 98.2% 95.6% 98.8% 108% 101% 97.5% 100% N/AStudy: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 15 of 23 Table 8. PFHS Calibration Summary

Analytical Run PFHS (ng) r

STD 1 STD 2 STD 3 STD 4 STD 5 STD 6 STD 7 STD 8 ST D 9 STD 10 STD 11 STD 12
Actual 0.200 0.500 0.750 1.00 2.50 5.00 10.0 25.0 50.0 100 200 500 N/A

s111007a 0.234 0.491 0.746 0.96 2.37 4.84 9.9 24.6 49.8 99.9 202 499 1.000
Recovery 117% 98.2% 99.4% 96.0% 95.0% 96.8% 99.0% 98.3% 99.6 % 99.9% 101% 99.8% N/A

Table 9. PFBS Calibration Summary

Analytical Run PFBS (ng) r

STD 1 STD 2 STD 3 STD 4 STD 5 STD 6 STD 7 STD 8 STD 9 STD 10 STD 11 STD 12
Actual 0.200 0.500 0.750 1.00 2.50 5.00 10.0 25.0 50.0 100 200 500 N/A

s111007a 0.199 0.47 0.802 0.989 2.41 5.00 9.96 26.1 50.3 102 195 502 0.9999
Recovery 99.3% 94.1% 107% 98.9% 96.3% 99.9% 99.6% 105% 101% 102% 97.4% 100% N/A



### 7.2 Limits of Quantitation (LOQs)
The lower limit of quantitation (LLOQ) was the low est non-zero calibration standard in the curve that met the linearity and accuracy requirement for a low st andard (100 + 35%) and for which the area counts were at least 2X that of the average response deter mined for the method blank injected just prior to t he calibration standards . The LLOQ for this study wa s the nominal 0.200 ng calibration standard (nomina l 0.200 ng/g in soil TCR-842), and was the lowest pre pared calibration standard. All sample analyte responses less than the response of the 0.200 ng ca libration standard were reported as BLQ (below the limits of quantitation). The upper limit of quanti tation (ULOQ) was the nominal 500 ng calibration standard. 

### 7.3 Continuing Calibration
During the course of each analysis, continuing cali bration verifications (CCVs) were performed by regu lar injection of a mid-level calibration standard after approximately every 15th sample injected in the analytical run. The back calculated concentration results were used to confirm that the instrument response and the initial calibration curve were sti ll in control. All CCVs flanking reported data met the method criteria of 100% ± 30% accuracy.



### 7.4 Blanks
Three types of blanks were analyzed during this ana lysis: method blanks were prepared with blank matrix soil TCR-842 and were spiked with IS and sur rogate; travel blanks (trip blanks) prepared from aliquots of soil TCR-842 sealed in s ample bottle t hat accompanied the bottle order to and from the sampling site; and solvent blanks containing extrac tion solvent. The different blank results were reviewed to evaluate potential contamination during shipment, and to evaluate method performance parameters such as injector carry over and to estab lish the LLOQ. All blanks were below the LLOQ (BLQ)Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 16 of 23 

### 7.5 Laboratory Control Spikes (LCSs)
Laboratory control spikes were prepared by spiking know quantities of PFOS (linear + branched) and PFHS (linear + branched) into 1 cc aliquots of soil TCR-842, fortified with nominal 3.0 ng and 30 ng levels, with each level prepared in triplicate. Th e results of the LCS analyses and calculation of an alyte measurement accuracies (percent recovery) for PFOS and PFHS are shown in Table 10, Table 11 and Table 12 respectively. The analytical method uncertainty determined from LCS results is shown in Table 13

.



### 100% * ion Concentrat Spike LCS)

of ion Concentrat d (Determine Recovery LCS =

Table 10. LCS Results (PFOS, linear + branched iso mer)

Sample ID PFOS Recovery 3.01 LCS 30.1 LCS 301 LCS LCSs (S111007a) 126% 130% 128% 125% 127% 134% [a ] 139% [a] 118% 119% Average Recovery 

### 130% 125% 127% Std Dev. 

### 7.7% 6.4% 6.6% RSD 

### 5.9% 5.1% 5.2% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/ g and 300 ng/g of PFOS (linear + branched isomers), each prepared and analyzed in triplicate. [a] LCS result was outside of 100 + 30%, but included in statistical calculations

Table 11. LCS Results (PFHS, linear + branched iso mer)

Sample ID PFHS Recovery 3.00 LCS 30.0 LCS 300 LCS LCSs (S111007a) 110% 103% 100% 108% 106% 112% 107% 104% 108% Average Recovery 

### 108% 104% 107% Std Dev. 

### 1.3% 1.3% 6.1% RSD 

### 1.2% 1.3% 5.8% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/ g and 300 ng/g of PFHS (linear + branched isomers), each prepared and analyzed in triplicate.Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 17 of 23 Table 12. LCS Results (PFBS)

Sample ID PFBS Recovery 3.01LCS 30.1 LCS 301 LCS LCSs (S111007a) 101% 97.3% 88.4% 105% 102% 96.3% 105% 96.0% 92.7% Average Recovery 

### 103% 98.6% 92.5% Std Dev. 

### 2.1% 3.3% 4.0% RSD 

### 2.0% 3.4% 4.3% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/ g and 300 ng/g of PFBS, each prepared and analyzed in triplicate.
Table 13. Analytical Method Uncertainties

Sample ID LCS Results PFOS PFHS PFBS

3.00 LCSs 126% 110% 101% 125% 108% 105% 139% 107% 105%
30.0 LCSs 130% 103% 97.3% 127% 106% 102% 118% 104% 96.0%
300 LCSs 128% 100% 88.4% 134% 112% 96.3% 119% 108% 92.7% Average Recovery 127% 106% 98.2% Std Dev. 6.6% 3.6% 5.5% RSD 5.2% 3.4% 5.6% Method Uncertainty (2 x Std. Dev.); 95% CI 13% 7.3% 11% Nominal LCS concentrations were 3.00 ng/g. 30.0 ng/ g and 300 ng/g of PFOS (linear + branched isomers), PFHS (linear + branched isomers) and PFBS; each LCS level was prep ared and analyzed in triplicate. 

### 7.6 Laboratory Matrix Spikes (LMSs)
Laboratory matrix spikes (LMSs) were generated by a dding a known quantity of PFOS (linear), PFHS (linear) and PFBS to an aliquot of soil sample, and then preparing the sample the same as non-spiked samples. Spikes for this study, LMSs were spiked a t levels that were appropriate for the endogenous analyte levels in the soils, determined from screen ing analysis and fortified with the target analytes from 0.5-times to 10-times the endogenous analyte levels determined in the soil/sediment samples during the range finding analysis. The LMS method acceptance criterion of within 100 ± 30% were met for all LMS recoveries. The LMS recovery results are summarize d in Table 2 . The PFOS, PFHS and PFBS recovery calculations for LMSs used the following e quation:

100% * ion Concentrat Spike Sample) Field of ion Concentrat Determined LMS of ion Concentrat d (Determine Recovery LMS −

=Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 18 of 23 

### 7.7 Percent Moisture Determinations
The percent moisture was determined for each soil s ample. Duplicate aliquots of each were taken and accurately weighed to determine the “wet” weight. Then each aliquot was dried at > 100°C until no further loss in mass occurred due to water evaporat ion, after which the dry weight was accurately determined. The average percent moisture and RPD o f the duplicate determinations for each soil are reported in Table 14 . The percent moisture was calculated by the follo wing equation:



### 100% * Mass Wet Soil Original Mass)

Soil Dried Mass Wet Soil (Original Moisture Percent −

=

Table 14. Percent Moistures for Decatur, AL Soils from Well Location 610
LIMS ID Sample ID Average Percent Moisture (w/w) [a] Relative Percent Difference [a]
GLP10-01-01-21-001 DAL-SB-610S-0-0000 13.0% 2.1% GLP10-01-01-21-002 DAL-SB-610S-0-0010 9.46% 0.53% GLP10-01-01-21-003 DAL-SB-610S-0-0040 12.8% 14% GLP10-01-01-21-004 DAL-SB-610S-0-0150 19.4% 0.32% GLP10-01-01-21-005 TRIP BLANK-1 1.97% 16% [a] Percent moisture determined for duplicate sampl es of soil taken from each sample bottle



### 7.8 Individual Sample Results
The individual sample results for PFOS, PFHS and PF BS are shown in Table 15 , Table 16 and Table 17, respectively

.

Table 15. Individual PFOS Results for Decatur, AL Soils from Well Location 610

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery LMS Spike

Concentration (ng/g; dry weight) Measured PFOS

Concentration (ng/g; dry weight) LMS

Recovery Average PFOS

Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-21-001 108% N/A 29.8 N/A 36.1 GLP10-01-01-21-001 Dup 105% 42.5
GLP10-01-01-21-001 Low LMS 110% 5.58 43.7 137% [a] 35% GLP10-01-01-21-001 High LMS 102% 57.5 92.4 97.8%
GLP10-01-01-21-002 114% N/A 21.1 N/A 19.5 GLP10-01-01-21-002 Dup 106% 17.9Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 19 of 23 Table 15. Individual PFOS Results for Decatur, AL Soils from Well Location 610

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery LMS Spike

Concentration (ng/g; dry weight) Measured PFOS

Concentration (ng/g; dry weight) LMS

Recovery Average PFOS

Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-21-002 Low LMS 103% 5.06 30.9 226% [a] 17% GLP10-01-01-21-002 High LMS 101% 48.5 64.6 93.0%
GLP10-01-01-21-003 100% N/A 2.94 N/A 3.00 GLP10-01-01-21-003 Dup 102% 3.05
GLP10-01-01-21-003 Low LMS 108% 5.07 8.66 112% 3.7% GLP10-01-01-21-003 High LMS 120% 55.2 64.1 111%
GLP10-01-01-21-004 107% N/A BLQ N/A BLQ GLP10-01-01-21-004 Dup 116% BLQ
GLP10-01-01-21-004 Low LMS 118% 4.66 4.58 98.1% N/A GLP10-01-01-21-004 High LMS 94% 59.7 52.2 87.4%
GLP10-01-01-21-005 108% N/A BLQ N/A BLQ GLP10-01-01-21-005 Dup 107% BLQ GLP10-01-01-21-005 LMS 105% 0.990 0.965 97.4% N/A N/A; not applicable BLQ; analyte response was lower than the analyte re sponse of the LLOQ which was nominal 0.200 ng/g low standard. [a] LMS fortification level was too low relative to the endogenous analyte level to make an accurate d etermination of recovery.

Table 16. Individual PFHS Results for Decatur, AL Soils from Well Location 610

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery LMS Spike

Concentration (ng/g; dry weight) Measured PFHS

Concentration (ng/g; dry weight) LMS

Recovery Average PFHS

Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-21-001 108% N/A 0.449 N/A 0.586 GLP10-01-01-21-001 Dup 105% 0.723 GLP10-01-01-21-001 Low LMS 110% 5.58 5.68 91.3% 47% GLP10-01-01-21-001 High LMS 102% 57.5 59.3 102%
GLP10-01-01-21-002 114% N/A 0.720 N/A 0.690 GLP10-01-01-21-002 Dup 106% 0.660 GLP10-01-01-21-002 Low LMS 103% 5.06 5.87 103% 8.7% GLP10-01-01-21-002 High LMS 101% 48.5 46.8 95.0%Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 20 of 23 Table 16. Individual PFHS Results for Decatur, AL Soils from Well Location 610

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery LMS Spike

Concentration (ng/g; dry weight) Measured PFHS

Concentration (ng/g; dry weight) LMS

Recovery Average PFHS

Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-21-003 100% N/A 1.070 N/A 1.11 GLP10-01-01-21-003 Dup 102% 1.152 GLP10-01-01-21-003 Low LMS 108% 5.07 6.33 103% 7.3% GLP10-01-01-21-003 High LMS 120% 55.2 54.9 97.6%
GLP10-01-01-21-004 107% N/A BLQ N/A BLQ GLP10-01-01-21-004 Dup 116% BLQ GLP10-01-01-21-004 Low LMS 118% 4.66 4.31 92.3% N/A GLP10-01-01-21-004 High LMS 94% 59.7 54.7 91.6%
GLP10-01-01-21-005 108% N/A BLQ N/A BLQ GLP10-01-01-21-005 Dup 107% BLQ GLP10-01-01-21-005 LMS 105% 0.990 1.01 102% N/A
N/A; not applicable BLQ; analyte response was lower than the analyte re sponse of the LLOQ which was nominal 0.200 ng/g low standard.

Table 17. Individual PFBS Results for Decatur, AL Soils from Well Location 610

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery LMS Spike

Concentration (ng/g; dry weight) Measured PFBS

Concentration (ng/g; dry weight) LMS

Recovery Average PFBS

Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-21-001 108% N/A 0.804 N/A 0.991 GLP10-01-01-21-001 Dup 105% 1.18
GLP10-01-01-21-001 Low LMS 110% 5.58 6.23 93.8% 38% GLP10-01-01-21-001 High LMS 102% 57.5 63.7 109%
GLP10-01-01-21-002 114% N/A 0.470 N/A 0.439 GLP10-01-01-21-002 Dup 106% 0.408
GLP10-01-01-21-002 Low LMS 103% 5.06 6.02 110% 14% GLP10-01-01-21-002 High LMS 101% 48.5 49.7 101%
GLP10-01-01-21-003 100% N/A 0.609 N/A 0.572 GLP10-01-01-21-003 Dup 102% 0.536
GLP10-01-01-21-003 Low LMS 108% 5.07 6.24 112% 13%Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 21 of 23 Table 17. Individual PFBS Results for Decatur, AL Soils from Well Location 610

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery LMS Spike

Concentration (ng/g; dry weight) Measured PFBS

Concentration (ng/g; dry weight) LMS

Recovery Average PFBS

Concentration (ng/g; dry wt.) and RPD (%) GLP10-01-01-21-003 High LMS 120% 55.2 60.8 109%
GLP10-01-01-21-004 107% N/A BLQ N/A BLQ GLP10-01-01-21-004 Dup 116% BLQ
GLP10-01-01-21-004 Low LMS 118% 4.66 4.27 91.5% N/A GLP10-01-01-21-004 High LMS 94% 59.7 59.5 100%
GLP10-01-01-21-005 108% N/A BLQ N/A BLQ GLP10-01-01-21-005 Dup 107% BLQ GLP10-01-01-21-005 LMS 105% 0.990 1.14 115% N/A N/A; not applicable BLQ; analyte response was lower than the analyte re sponse of the LLOQ which was nominal 0.200 ng/g low standard.



### 8 Conclusion
Soils collected from near groundwater well location 610 in August 2011 were successfully analyzed for PFOS, PFHS and PFBS following 3M Environmental Laboratory method ETS-8-053.0 and conducted as 3M study GLP10-01-02-21. The average PFOS, PFHS and PFBS concentration results for the soil samples are summarized in Table 1 and the LMS recoveries are summarized in Table 2 . The individual analytical sample results are sho wn in Table 15 , Table 16 , and Table 17 for PFOS, PFHS and PFBS, respectively. The soil trip bl ank that accompanied the sample bottles to the site and then accompanied samples back to the labor atory was sufficiently devoid of PFOS, PFHS and PFBS, indicating that no contamination of the s amples occurred during sample shipment to the laboratory. The accuracy of the results based on LMS recoveries were within acceptance criteria of 100 + 30%; when the appropriate level of fortified LMS was eva luated relative the endogenous analyte level measured. The analytical method uncertainties were determined by statistical examination of the LCS results for PFOS, PFHS and PFBS and were determined to be + 13% for PFOS, + 7.3% for PFHS and + 11% for PFBS, respectively; determined at the 95% confi dence interval (CI).Study : GLP10-01-02 , Interi m Repor t 2 1 Analysi s fo r PFOS , PFH S & PFB S i n Decatur , A L Soil s Collecte d fro m Wel l Locatio n 61 0

9 Data/Sampl e Retentio n

Al l soi l sample s an d associate d projec t dat a (hardcop y an d electronic ) wil l b e archive d a s projec t GLP10

- 01-02-2 1 accordin g t o 3 M Environmenta l Laborator y standar d operatin g procedures

.



## 1 0 Lis t o

f Attachment s

Attachmen t A : Preparatio n Forms , Ra w Dat a an d Chromatogram s

i l l Signature s

Repor t Approval :

' Dat e Clesto n C

. Lange , Ph.D. , Principa l Analytica l Investigato r


# /fJi^de//A^
Willia m K

. Reagen , Ph.D. , 3 M Environmenta l Laborator y Managemen t Dat e



# 2

- Gar y A

. Hohenstein , Sponso r Representativ e Dat e

Jaisimh a Kesari , Stud y Directo r Dif e

Pag e 2 2 o f 2 3Study: GLP10-01-02, Interim Report 21 Analysis for PFOS, PFHS & PFBS in Decatur, AL Soils Collected from Well Location 610

Page 23 of 23 

## Attachment A Preparation Forms, Raw Data and Chromatograms