3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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# Final Report-Revision 1

Analysis of PFOS, PFHS, PFBS and PFOA in Soils from Decatur, AL in December 2012

Laboratory Request Number: E12-0849
Method Requirement: 3M Method ETS-8-053.0
Regulatory Requirement: Non-GLP

Report Date – Date of Final Signature



## Testing Laboratory 3M EHS Operations 3M Environmental Laboratory Building 260-5N-17 Maplewood, MN 55144-1000

Requester Gary Hohenstein Manager, Environ/Regulatory Affairs 3M, Environmental Health and Safety Operations

3M Center, Bldg 224-5W-03 Saint Paul, MN 55144-1000 Phone: (651) 737-3395 gahohenstein@mmm.com3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### 3M Environmental Laboratory, Analytical Study E12-084 9
3M Environmental Laboratory Manager: William K. Re agen, Ph.D. 3M Principal Analytical Investigator: Cleston Lange , Ph.D.



# 1 Introduction / Summary

The 3M Environmental Laboratory received six (6) De catur, AL soil samples on December 20, 2012. The objective of this project was to analyze the co llected soil samples for perfluorooctanoic acid (PFOA), perfluorobutane sulfonate (PFBS), perfluoro hexane sulfonate (PFHS) and perfluorooctane sulfonate (PFOS).
Samples were analyzed following 3M Environmental La boratory method ETS-8-053.0 “Solvent Extraction and LC/MS/MS Analysis of Soils for C6-C1 2 Perfluorinated Carboxylic Acids, and Perfluorobutane Sulfonate, Perfluorohexane Sulfonat e, Perfluorooctane Sulfonate and Perfluorooctane Sulfonamide (FOSA): Quantification Using Stable Isotope Labeled Internal Standards”. One soil trip blank, included with the shipments to the field and back to the laboratory, was also analyzed with the samples.
Several samples required dilutions to attain PFOS a nd PFOA results within the range of the calibration curve. Results from the analysis of the soil sampl es and trip blank are summarized in Table 1

. Concentrations of PFOS were the highest in the Deca tur soil samples, followed generally by PFOA, PFHS and then PFBS. Laboratory matrix spike (LMS) recoveries were within 100 + 30% for all analytes in all samples, except for one PFOA result with LMS recovery of 59.1%, one PFBS result with a LMS recovery of 63.9% and PFBS in one sample for which a reliable LMS recovery could not be achieved and a PFBS result not reported (NR) for th at sample. Results for laboratory control samples (LCSs) were used to determine the analytical method uncertainty (95%CI) for PFOS at + 12%, PFHS at + 30%, PFBS at + 7.9% and PFOA at + 25%. The relative standard deviation (RSD) for th e added stable isotope labeled surrogate recovery standards (SRSs) was a measure of the analytical method precision and was determined at 11% for 13 

### C 4 

### -PFOA and 9.9% for 13 

### C 4 

### -PFOS (representing the three sulfonates).

Table 1. Results for Decatur Soils Analysis

LIMS ID Sample ID Average Concentration (ng/g; dry weight) PFOS PFHS PFBS PFOA E12-0849-001 DAL SB DF601 0 0000 121213 3890 33.3 N R 158 E12-0849-002 DAL SB DF601 0 0050 121213 229 5.04 1. 67 [a, c] 

### 38.0 E12-0849-003 DAL SB DF602 0 0000 121213 851 3.56 0. 373 17.0 E12-0849-004 DAL SB DF602 0 0050 121213 1730 270 64 .8 1410 [c]


### E12-0849-005 DAL SB DF603 0 0000 121213 112 NR [d] 

### 0.423 23.5 E12-0849-006 DAL SB DF603 0 0050 121213 3.86 6.58 2 .43 35.0 E12-0849-007 Trip Blank 1 BLOQ 0.910 [b] 

### BLOQ BLOQ [a] RPD > 50% [b] Trip blank result indicated possible low level contamination of PFHS at ~ 1 ng/g (dry wt.) [c] LMS recovery result was outside of 100+ 30%, but within 100 + 50% [d] Value was not rep o rted (NR) because it was not 2-times the measured t rip blank concentration for that analyte3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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# 2 Methods- Analytical and Preparatory

1.1 Methods
Analyses were performed following 3M Environmental Laboratory Method ETS-8-053.0. The analytical reference substances listed in Table 2 were used during this study.

Table 2. Reference Substances

Reference ID PFOS (linear) Technical

- PFOS (linear + branched) M4-PFOS

Chemical Name Pefluoro-n-octane-1- sulfonate potassium salt Perfluorooctane-1-sulfonate potassium salt [1,2,3,4- 13 C 4 ]-Perfluorooctane-1- sulfonate sodium salt Chemical Formula n-C 8 F 17 SO 3 K+ C 8 F 17 SO 3 K+ 13 C 4 12 C 4 F 17 SO 3 Na+
Use Reference Standard for Calibration and LMSs Reference standard for LCSs PFOS Surrogate Recovery Standard Source 

### Sigma-Aldrich Wellington Wellington Expiration Date February 4, 2014 December 14, 2014 December 21, 2014 Storage Conditions Frozen Frozen Frozen Chemical Lot Number 1424328V Br-PFOSK1111 MPFOS1211 TCR Number TCR11-0028-1/1 TCR12-0026-1/20 TCR12-0003-4/14 Physical Description Powder 

### Liquid Liquid Purity 99.7% ≥ 98% >98%

Reference ID M8-PFOS PFOA (linear) Technical PFOA (linear + branched) Chemical Name [ 13 C 8 ]-Perfluorooctane-1- sulfonate sodium salt Perfluoro-n-octanoic acid Ammonium perfluorooctanoate

Chemical Formula 13 C 8 F 17 SO 3 Na+ n-C 7 F 15 CO 2 H C 7 F 15 CO 2 H
Use Internal standard for PFOS Reference Standard for Calibration and LMSs Reference standard for LCSs

Source Wellington Sigma-Aldrich Wellington Expiration Date October 3, 2015 July 27, 2016 March 17, 2014 Storage Conditions Frozen Frozen Frozen Chemical Lot Number 100212 MKBD4574V TPFOA0311 TCR Number TCR12-0038-1/16, -2/16, -3/16, -4/16 TCR11-0029-1/1 TCR11-0042-15/20

Physical Description Liquid Powder Liquid Purity 98% 96.8% >97%

Reference ID M4-PFOA M8-PFOA PFBS
Chemical Name [1,2,3,4- 13 C 4 ]-Perfluoro-noctanoic acid 13 C 8 -Perfluorooctanoic acid Perfluorobutane sulfonate Potassium salt Chemical Formula 13 C 4 12 C 3 F 15 CO 2 H 13 C 8 F 15 O 2 H C 4 F 9 SO 3 K +
Use PFOA Surrogate Recovery Standard Internal standard for PFOA Reference Standard for Calibration, LMSs and LCSs Source Wellington Wellington 3M Expiration Date December 7, 2013 October 3, 2015 January 10, 2017 Storage Conditions Frozen Frozen Frozen Chemical Lot Number MPFOA1210 100212 101 TCR Number TCR11-0001-5/14 TCR12-0038-1/16, -2/16, -3/16, -4/16 TCR-121

Physical Description Liquid Liquid White Powder Purity >98% 98% 96.7%3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### Table 2. Reference Substances

Reference ID 18O2-PFBS PFHS (linear) ECF-PFHS (linear + branched) Chemical Name [ 18 O]-Perfluorobutane sulfonate Ammonium salt Perfluoro-1-hexanesulfonate sodium salt Perfluoro-1-hexanesulfonate Potassium salt Chemical Formula C 4 F 9 S[ 18 O 2 ] O NH 4 + n-C 6 F 13 SO 3 Na+ C 6 F 13 SO 3 K+ Use Internal standard for PFBS Reference Standard for Calibration and LMSs Reference standard for LCSs

Source 3M Wellington 3M Expiration Date March 9, 2015 March 25, 2015 February 12, 2017 Storage Conditions Frozen Frozen Frozen Chemical Lot Number 11546-107-2 LPFHxSAM08 NB 120067-69 TCR Number TCR-964 & TCR-965 TCR12-0021-1/1 TCR-083 Physical Description Liquid Powder White Powder Purity N/A >98% 98.6%
Reference ID M3-PFHS
Chemical Name [1,2,3- 13 C 4 ]-Perfluoro-1- hexanesulfonate sodium salt Chemical Formula 13 C 3 12 C 3 F 13 SO 3 Na Use Internal standard for PFHS Source Wellington Expiration Date October 3, 2015 Storage Conditions Frozen Chemical Lot Number 100212 TCR Number TCR12-0038-1/16, -2/16, -3/16, -4/16 Physical Description Liquid Purity 98%



## 1.2 Sample Collection

Ten empty 250-mL HDPE sample bottles and one soil t rip blank were prepared and sent to Decatur, AL on December 10, 2012 to Weston Solutions, Inc. p ersonnel. Six soil samples were collected from soil borings by Weston Solutions, Inc. personnel on December 13, 2012 near Field 6 and the railroad tracks located on the 3M Decatur Property. Samples were then shipped to 3M on December 19, 2012 and received at the 3M Environmental Laboratory on December 20, 2012 and logged into LIMS under project E12-0849. 

## 1.3 Sample Preparation
Samples were prepared by the extraction procedure d efined in method ETS-8-053.0. In summary, preparation involves removal of a 1 cubic centimete r (1 cc) soil sample aliquot (typically ~ 1 gram) f rom each sample bottle using a fixed volume 1 cc spoon, followed by accurate weight determination of the aliquot on a 5-place balance. Stones and debris ge nerally larger than 5 mm were typically removed during weighing to ensure better sample homogeneity

. Prior to extraction, each weighed sample aliquot wa s fortified with a fixed quantity of stable isotope labeled internal standards (IS) and surrogate recov ery standards (SRS) as defined in Table 2

. Following the addition of IS and SRS compounds, eac h was extracted by adding 8 mL of a 4:1 acetonitrile:water solution followed by sonication for 1-2 hours, then centrifugation to separate out the solids. An aliquot of the clear supernatant was tr ansferred to an autovial for LC/MS/MS analysis.3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### Soil matrix blanks and calibration standards are pr epared similar to samples using a control soil TCR-455. A 1 cc aliquot of soil TCR-455 weighed no minal 1.0 gram (dry weight). Because environmental soil and sediment samples can vary si gnificantly by dry weight for a 1 cc sample, the instrument response is calibrated for each analyte based on the mass of target analyte added to the standard calibration soil matrix prior to extractio n. Calibration standards were fortified from the r ange of 0.200 ng to 500 ng for each analyte; nominal calibr ated range was 0.200 ng/g to 500 ng/g in control so il TCR-455. Percent moistures used for calculating so il dry weights for the environmental samples were determined from separate weighings of sample. 

## 1.4 LC/MS/MS Analysis
Each extract was analyzed for PFOS, PFHS, PFBS and PFOA by LC/MS/MS as described in method ETS-8-053.0. Sample analyte concentrations for LMS preparations were estimated from a range finding (screening) analyses as analytical runs s13 0102b and s130103a. Results of the screening analysis were not used for reporting. Data for de finitive reporting of results were obtained from analysis of analytical batch s130109a and s130111a. Samples with QC failure in run s130109a or s130111a were reassayed in analytical batch s130117 a (PFOS, PFOA and PFBS only).
Details of the specific instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the raw data which are provided as hard copies in the final study data packet, and are briefly descri bed below in Tables 3, 4 and 5 . All data used for reporting these results were from analytical runs

Table 3. Instrument Information
Definitive Analysis Instrument Name (s) ETS-Stan Analytical Method ID 

### ETS

- 8

- 0 53 .0 Liquid Chromatograph 

### Agilent/HP 1100 HPLC
Guard Column 

### Prism RP Analytical column 1 

### Oasis HLP Analytical column 2 

### C18 Betasil Injection Volume 

### 25 μL Mass Spectrometer 

### API 4000
Ion Source 

### Turbo Ion Spray Polarity 

### Negative Ion
Software 

### Analyst 1.6.13M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### Table 4. Isocratic 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 0.4 97 3 2 3.0 0.4 97 3 3 3.5 0.4 70 30 4 17.0 0.4 40 60 5 17.5 0.4 10 90 6 19.5 0.4 10 90 7 20.0 0.4 97 3 8 23.0 0.4 97 3

Table 5. Mass Transitions
Analyte Mass Transitions Monitored PFOA 413>169, 413>219, 413>369

13 C 4 -PFOA (SRS) 417>372

13 C 8 -PFOA (IS) 421>376 PFOS 499>130, 499>99, 499>80
13 C 8 -PFOS (IS) 507>80 PFHS 399>99, 399>80
13 C 3 -PFHS (IS) 402>80 PFBS 299>99, 299>80
18 O 2 -PFBS (IS) 303>84
13 C 4 -PFOS (SRS) 503>80 Note: Multiple mass transitions are summed to give the instrument response for that analyte.



# 3 Results

3.1 Calibration
Internal Standard Calibration: All samples were analyzed against a matrix-matched stable isotope IS calibration curve. Calibration standards were prepared by spiking known amounts of target analytes into 1cc aliquots of control soil TCR-455. Linear isomers of target analytes were us ed for calibration. Each soil calibration standard received nominal 3 ng of each IS and 3 ng of each S RS. A total of twelve spiked standards ranging from nominal 0.200 ng to 500 ng of each target anal yte were prepared and analyzed. To meet linearity and accuracy criteria, the high calibrati on standard (500 ng) was disabled for PFBA. The plot of the analyte/IS ratio for each standard vers us known standard analyte fortification amount was fitted using a quadratic, 1/x weighted linear regre ssion. The data were not forced through zero duri ng the fitting process. Back-calculating the standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of e ach curve point at within 100 + 30% (+ 35% at LLOQ). The correlation coefficient (r) was greater than 0.995 for each analyte fitted calibration cur ve.3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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## 3.2 Limits of Quantitation The lower limit of quantitation (LLOQ) for each ana lyte was the lowest non-zero calibration standard i n the curve that met linearity and accuracy requireme nts and for which the peak area ratio was at least two times the average peak area response of the met hod blanks. The LLOQs for this analysis were the nominal 0.200 ng calibration standard (nominal 0.2 00 ng/cc soil) for all analytes. The reportable LLOQ for PFHS was adjusted up to 1.8 ng/g based on the trip blank result. The ULOQ was the highest standard in the curve, and was the 500 ng calibrati on for all analyses.
Values above the ULOQ were appropriately diluted to achieve results within the range of the curve. In some instances, samples were diluted 100-fold to ac hieve results within the range of the calibration.



## 3.3 Continuing Calibration Reinjection of calibration standards during analyti cal runs were conducted to verify the analytical ru n was maintained in control throughout the analysis. During the course of the analytical sequence, several mid-level continuing calibration verificati on samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration cur ve were still in control. The method acceptance criterion of 100% ± 30% for CCVs was met for all an alytes in the analytical runs used for reporting results.



## 3.4 Blanks Two types of blanks were prepared and analyzed with the samples: method blanks (procedural blanks) consisting of extracted control soil matrix and ins trument blanks (zero volume injections). Method bl ank results were reviewed and used to evaluate method p erformance to determine the LLOQ for each analyte. Instrument blanks provided the ability to monitor for potential instrument carry over from injection to injection. Significant carry over was not observed.



## 3.5 Surrogate Recovery Standards (SRSs) Two stable isotope-labeled SRSs were added to each soil sample aliquot during preparation and extraction, one representing perfluorinated carboxy late ( 13 

### C 4 

### -PFOA for PFOA) and the other representing the perfluorinated sulfonates ( 13 

### C 4 

### -PFOS for PFOS, PFHS and PFBS). The SRS recovery results for the Decatur soils were used to evaluate the analytical method precision overall. The average SRS recoveries and standard deviations for the Decatur soil samples was determined at 97.7% + 10% for 13 

### C 4 

### -PFOA (n = 58) and 97.7% + 9.6% for 13 

### C 4 

### -PFOS (n = 58). The analytical method precision was indicated by the RSDs and was 11% 13 

### C 4 

### -PFOA and 9.9 % for 13 

### C 4 

### -PFOS. Overall, the SRSs results demonstrate excellent ana lytical method precision.



## 3.6 Lab Control Spikes (LCSs) Laboratory control samples were prepared with each analytical batch and were prepared by fortifying target analytes into 1 cc aliquots of control soil TCR-455 at three levels of nominal 3.00 ng, 30.0 ng and 300 ng, with each LCS level prepared in triplicate. In analytical runs containing diluted samples, 10 -fold diluted (DF10) and 100-fold (DF100) LCSs were also included. The LCSs for PFOS, PFHS, PFBS and PFOA were all within acceptance criteria of 100 + 30% as shown in Table 6
, Table 7
, Table 8 and Table 9 , respectively, except for one LCS for PFOA which w as at 138%. The analytical method uncertainties (95%CI) determined from LCS results w ere + 12% for PFOS, + 30% for PFHS, + 7.9% for PFBS and + 25% for PFOA.3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### Table 6. LCS Results (PFOS)

**Sample ID PFOS Recovery** 
**3.0 ng LCS 30 ng LCS**  **300 ng LCS 300 ng LCS**  **(DF 10) 300 ng LCS** 

**(DF 100)**

LCSs (s130109a) 110% 115% 110% NA NA 107% 116% 111% NA NA 108% 123% 110% NA NA

LCSs (s130111a) 107% 112% 103% 106% 104% 106% 111% 101% 104% 109% 110% 127% 103% 104% 105%

LCSs (s130117a) 117% 105% 108% 105% 98.0% 110% 97.3% 107% 103% 109% 102% 103% 101% 107% 110% Average Recovery 108% 112% 106% 105% 106% Std. Dev. 4.1% 9.5% 4.0% 1.4% 4.7% RSD 3.8% 8.4% 3.8% 1.4% 4.4% **Overall Average 108%**  **Overall Std. Dev. 6.0%**  **Overall RSD 5.6%**  **PFOS Method Uncertainty (2 x Std. Deviation, 95% CI)**  **+ 12%** 

Table 7. LCS Results (PFHS)

**Sample ID PFHS Recovery** 
**3.0 ng LCS 30 ng LCS**  **300 ng LCS 300 ng LCS**  **(DF 10) 300 ng LCS** 

**(DF 100)**

LCSs (s130109a) 130% 97.3% 93.3% NA NA 125% 97.3% 96.0% NA NA 124% 111% 95.7% NA NA

LCSs (s130111a) 124% 101% 91.3% 96.7% 125% 130% 93.3% 93.3% 92.7% 121% 121% 103% 87.0% 93.7% 119%

LCSs (s130117a) NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Average Recovery 126% 100% 92.8% 94.3% 122% Std. Dev. 3.7% 6.0% 3.3% 2.1% 3.4% RSD 3.0% 6.0% 3.6% 2.2% 2.8% **Overall Average** 107% **Overall Std. Dev.** 15% **Overall RSD** 14% **PFHS Method Uncertainty (2 x Std. Deviation, 95% CI)**  + 30%3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### Table 8. LCS Results (PFBS)

**Sample ID PFBS Recovery** 
**2.99 ng LCS 29.9 ng LCS**  **299 ng LCS 299 ng LCS**  **(DF 10) 299 ng LCS** 

**(DF 100)**

LCSs (s130109a) 93.6% 98.7% 91.6% NA NA 97.3% 95.0% 92.3% NA NA 94.6% 97.0% 90.6% NA NA

LCSs (s130111a) 97.7% 98.3% 100% 102% 96.0% 99.0% 99.0% 99.0% 91.0% 95.0% 99.7% 107% 95.7% 97.7% 91.3%

LCSs (s130117a) 104% 88.0 % 97.7% 93.0% 89.0% 95.3% 91.0 % 98.7% 96.7% 99.3% 97.0% 94.3% 94.3% 96.0% 97.3% Average Recovery 97.6% 96.4% 95.6% 96.0% 94.6%
Std. Dev. 3.2% 5.3% 3.5% 3.7% 3.9%
RSD 3.3% 5.5% 3.7% 3.9% 4.1% **Overall Average** 96.2% **Overall Std. Dev.** 3.9% **Overall RSD** 4.1% **PFBS Method Uncertainty (2 x Std. Deviation, 95% CI)**  + 7.9%

Table 9. LCS Results (PFOA)

**Sample ID PFOA Recovery** 
**3.0 ng LCS 30 ng LCS**  **300 ng LCS 300 ng LCS**  **(DF 10) 300 ng LCS** 

**(DF 100)**

LCSs (s130109a) 85.6% 108% 107% NA NA 102% 115% 112% NA NA 111% 121% 101% NA NA

LCSs (s130111a) 89.6% 82.3% 119% 100% 87.0% 92.3% 93.3% 138% [a] 

### 93.6% 75.3% 85.6% 101% 102% 87.0% 102%

LCSs (s130117a) 95.3% 104% 123% 100% 95.3% 89.6% 94.3% 96.0% 96.0% 115% 96.3% 83.3% 105% 101% 101% Average Recovery 94.1% 100% 111% 96.3% 96.0%
Std. Dev. 8.2% 13% 13% 5.4% 14%
RSD 8.7% 13% 12% 5.6% 14% **Overall Average** 100% **Overall Std. Dev.** 13% **Overall RSD** 13% **PFOA Method Uncertainty (2 x Std. Deviation, 95% CI)**  + 25% [a] Result was outside of 100 + 30%3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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## 3.7 Laboratory Matrix Spikes (LMS) Laboratory matrix spikes (LMSs) were prepared for e ach sample at a level that was appropriate relative to the endogenous target analyte level. All LMS re coveries were within method acceptance criteria of 100 ± 30%, except for the PFBA result of the Trip B lank which was 143%. Overall, the LMS results confirmed that “unknown” components in the sample m atrix did not significantly interfere with the extraction and analysis of the analytes of interest for most samples. The reference materials used fo r fortification of LMS was comprised of primarily lin ear isomers for PFOA and PFOS. The LMS recovery results are shown with sample results in Table 11
, Table 12
, Table 13 and Table 14 for PFOS, PFHS, PFBS and PFOA, respectively.



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

=



## 3.8 Percent Moisture Determination

The percent moisture was determined in duplicate fo r each soil sample. For each replicate, a sample aliquot is accurately weighed to determine the “wet ” weight. Then the aliquot is dried at > 105°C unt il no further loss in mass occurs (due to water evapor ation), and then the dry weight is accurately determined. The average percent moisture and RPD o f the duplicate determinations for each is reported in Table 10 . 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 10. Percent Moistures for Decatur Soils (Dec ember 2012)

LIMS ID Sample ID Average Percent Moisture (w/w) [a] 

### Relative Percent Difference [a]


### E12-0849-001 DAL SB DF601 0 0000 121213 13.6% 3.8% E12-0849-002 DAL SB DF601 0 0050 121213 20.2% 11% E12-0849-003 DAL SB DF602 0 0000 121213 16.0% 0.92% E12-0849-004 DAL SB DF602 0 0050 121213 17.4% 6.8% E12-0849-005 DAL SB DF603 0 0000 121213 13.3% 0.86% E12-0849-006 DAL SB DF603 0 0050 121213 15.1% 1.1% E12-0849-007 Trip Blank 1 2.23% 8.9% [a] Percent moisture determined for duplicate samp les of soil taken from each sample bottle, RPD is t he relative percent difference of the duplicate determined values.3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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## 3.9 Sample Results

Table 11. Individual PFOS Results for Decatur Soil s (December 2012)

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery [a] LMS Spike Concentration (ng/g; dry weight) Measured PFOS

Concentration (ng/g; dry weight) LMS recovery

(Data Accuracy) Average PFOS

Concentration (ng/g; dry wt.) and RPD (Data Precision)
DAL SB DF601 0 0000 121213 92.4% NA 3420 NA 3890 DAL SB DF601 0 0000 121213 Duplicate 90.7% 4350
DAL SB DF601 0 0000 121213 LMS 96.2% 9220 14800 118% 24%
DAL SB DF601 0 0050 121213 94.1% NA 251 NA 229 DAL SB DF601 0 0050 121213 Duplicate 90.7% 207
DAL SB DF601 0 0050 121213 Low LMS 87.9% 450 665 96.8% 19% DAL SB DF601 0 0050 121213 High LMS NR NR 1660 NR

DAL SB DF602 0 0000 121213 93.4% NA 846 NA 851 DAL SB DF602 0 0000 121213 Duplicate 92.7% 856
DAL SB DF602 0 0000 121213 Low LMS 96.6% 432 1280 99.0% 1.2% DAL SB DF602 0 0000 121213 High LMS NR NR 1620 NR

DAL SB DF602 0 0050 121213 98.0% NA 1420 NA 1730 DAL SB DF602 0 0050 121213 Duplicate 98.0% 2040
DAL SB DF602 0 0050 121213 Low LMS NR NR 3520 NR 36% DAL SB DF602 0 0050 121213 High LMS 94.8% 1360 3000 93.5%
DAL SB DF603 0 0000 121213 95.5% NA 115 NA 112 DAL SB DF603 0 0000 121213 Duplicate 95.2% 109
DAL SB DF603 0 0000 121213 Low LMS 94.8% 428 534 98.5% 4.8% DAL SB DF603 0 0000 121213 High LMS NR NR 1980 NR

DAL SB DF603 0 0050 121213 85.4% NA 4.02 NA 3.86 DAL SB DF603 0 0050 121213 Duplicate 93.4% 3.69
DAL SB DF603 0 0050 121213 Low LMS 91.4% 4.13 7.74 94.2% 87% [c] DAL SB DF603 0 0050 121213 High LMS NR NR 37.3 NR Trip Blank 1 92.7% NA BLOQ NA BLOQ Trip Blank 1 Duplicate 104% BLOQ Trip Blank 1 Lab Matrix Spike 87.5% 1.01 1.14 113% NA Concentration values are rounded to 3 significant f igures, statistical results rounded to 2 significan t figures, but non-rounded values used for data calculations. [a] SRS recovery only shown from the analytical run used to report the results for that analyte in tha t sample [b] Recovery was outside of 100 + 30% [c] RPD > 20% BLOQ; result was less than the analyte/IS response for the lowest (nominal 0.200 ng) calibration stan dard NA; Not applicable NR; Not Reported because LMS fortification level wa s not appropriate relative to the determined level of analyte in the sample3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

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### Table 12. Individual PFHS Results for Decatur Soil s (December 2012)

Sample Description Surrogate ( 13 C 4 -PFOS) Recovery [a] LMS Spike Concentration (ng/g; dry weight) Measured PFHS

Concentration (ng/g; dry weight) LMS recovery

(Data Accuracy) Average PFHS

Concentration (ng/g; dry wt.) and RPD (Data Precision)
DAL SB DF601 0 0000 121213 

### 122% NA 27.5 NA 33.3 DAL SB DF601 0 0000 121213 Duplicate 

### 132% [b] 39.0
DAL SB DF601 0 0000 121213 Low LMS 

### 125% NR NR NR 34% DAL SB DF601 0 0000 121213 High LMS 

### 108% 120 152 98.8%
DAL SB DF601 0 0050 121213 

### 94.1% NA 5.60 NA 5.04 DAL SB DF601 0 0050 121213 Duplicate 

### 90.7% 4.49
DAL SB DF601 0 0050 121213 Low LMS 

### 103% 4.50 9.89 108% 22% DAL SB DF601 0 0050 121213 High LMS 

### 101% NR NR NR

DAL SB DF602 0 0000 121213 

### 94.8% NA 3.49 NA 3.56 DAL SB DF602 0 0000 121213 Duplicate 

### 95.9% 3.64
DAL SB DF602 0 0000 121213 Low LMS 

### 97.3% 4.32 8.37 111% 4.2% DAL SB DF602 0 0000 121213 High LMS 

### 102% NR NR NR

DAL SB DF602 0 0050 121213 

### 95.5% NA 256 NA 270 DAL SB DF602 0 0050 121213 Duplicate 

### 99.4% 283
DAL SB DF602 0 0050 121213 Low LMS 

### 95.2% NR NR NR 9.9% DAL SB DF602 0 0050 121213 High LMS 

### 94.8% 340 517 72.8%
DAL SB DF603 0 0000 121213 

### 95.5% NA 0.963 NA NR [c] DAL SB DF603 0 0000 121213 Duplicate 

### 95.2% 1.14
DAL SB DF603 0 0000 121213 Low LMS 

### 97.6% 4.28 5.83 112% 17% DAL SB DF603 0 0000 121213 High LMS 

### 91.0% NR NR NR

DAL SB DF603 0 0050 121213 

### 85.4% NA 6.44 NA 6.58 DAL SB DF603 0 0050 121213 Duplicate 

### 93.4% 6.72
DAL SB DF603 0 0050 121213 Low LMS 

### 91.4% 4.13 10.8 103% 4.3% DAL SB DF603 0 0050 121213 High LMS 

### 92.1% NR NR NR Trip Blank 1 

### 92.7% NA 0.868 NA 0.910 Trip Blank 1 Duplicate 

### 104% 0.952 Trip Blank 1 Lab Matrix Spike 

### 87.5% 1.01 2.17 126% 9.2% Concentration values are rounded to 3 significant f igures, statistical results rounded to 2 significan t figures, but non-rounded values used for data calculations. [a] SRS recovery only shown from the analytical run used to report the results for that analyte in tha t sample [b] Recovery was outside of 100 + 30%, but within 100 + 50% [c] Result was not 2-times the trip blank response and was not reportable (NR) BLOQ; result was less than the analyte/IS response for the lowest (nominal 0.200 ng) calibration stan dard NA; Not applicable NR; Not Reported because LMS fortification level wa s not appropriate relative to the determined level of analyte in the sample3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

PAGE 13 OF 16 

### Table 13. Individual PFBS Results for Decatur Soil s (December 2012)

Sample Description Surrogate ( 13 C 8 -PFOS) Recovery [a] LMS Spike Concentration (ng/g; dry weight) Measured PFBS

Concentration (ng/g; dry weight) LMS recovery

(Data Accuracy) Average PFBS

Concentration (ng/g; dry wt.) and RPD (Data Precision)
DAL SB DF601 0 0000 121213 NR* NR* NR* NR* NR* DAL SB DF601 0 0000 121213 Duplicate NR* NR*
DAL SB DF601 0 0000 121213 LMS NR* NR* NR* NR* NR*

DAL SB DF601 0 0050 121213 

### 100% NA 2.53 NA 1.67 DAL SB DF601 0 0050 121213 Duplicate 

### 103% 0.801
DAL SB DF601 0 0050 121213 LMS 

### 136% [ c ] 1.80 2.82 63.9% [c] 104% [b] DAL SB DF601 0 0050 121213 High LMS 

### NA NR NR NR

DAL SB DF602 0 0000 121213 

### 94.1% NA 0.385 NA 0.373 DAL SB DF602 0 0000 121213 Duplicate 

### 90.7% 0.361
DAL SB DF602 0 0000 121213 Low LMS 

### 87.9% 1.73 2.27 110% 6.5% DAL SB DF602 0 0000 121213 High LMS 

### 96.2% NR NR NR

DAL SB DF602 0 0050 121213 

### 94.8% NA 60.8 NA 64.8 DAL SB DF602 0 0050 121213 Duplicate 

### 95.9% 68.9
DAL SB DF602 0 0050 121213 Low LMS 

### 97.3% NR NR NR 13% DAL SB DF602 0 0050 121213 High LMS 

### 102% 34.0 93.1 83.1%
DAL SB DF603 0 0000 121213 

### 95.5% NA 0.452 NA 0.423 DAL SB DF603 0 0000 121213 Duplicate 

### 99.4% 0.393
DAL SB DF603 0 0000 121213 Low LMS 

### 95.2% 1.71 2.52 122% 14% DAL SB DF603 0 0000 121213 High LMS 

### 107% NR NR NR

DAL SB DF603 0 0050 121213 

### 95.5% NA 2.45 NA 2.43 DAL SB DF603 0 0050 121213 Duplicate 

### 95.2% 2.40
DAL SB DF603 0 0050 121213 Low LMS 

### 97.6% 1.65 3.96 93.1% 2.0% DAL SB DF603 0 0050 121213 High LMS 

### 91.0% NR NR NR Trip Blank 1 

### 85.4% NA BLOQ NA BLOQ Trip Blank 1 Duplicate 

### 93.4% BLOQ Trip Blank 1 Lab Matrix Spike 

### 91.4% 1.01 1.19 118% NA Concentration values are rounded to 3 significant f igures, statistical results rounded to 2 significan t figures, but non-rounded values used for data calculations. [a] SRS recovery only shown from the analytical run used to report the results for that analyte in tha t sample [b] RPD > 50% [c] Recovery was outside of 100 + 30%, but within 100 + 50% BLOQ; result was less than the analyte/IS response for the lowest (nominal 0.200 ng) calibration stan dard NA; Not applicable NR; Not Reported because LMS fortification level wa s not appropriate relative to the determined level of analyte in the sample NR*; Not reported because of QC failure3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

PAGE 14 OF 16 

### Table 14. Individual PFOA Results for Decatur Soil s (December 2012)

Sample Description Surrogate ( 13 C 4 - PFOA) Recovery [a] LMS Spike Concentration (ng/g; dry weight) Measured PFOA

Concentration (ng/g; dry weight) LMS recovery

(Data Accuracy) Average PFOA

Concentration (ng/g; dry wt.) and RPD (Data Precision)
DAL SB DF601 0 0000 121213 92.5% NA 145 NA 158 DAL SB DF601 0 0000 121213 Duplicate 97.5% 171
DAL SB DF601 0 0000 121213 LMS 95.5% 307 455 96.6% 16%
DAL SB DF601 0 0050 121213 92.5% NA 39.6 NA 38.0 DAL SB DF601 0 0050 121213 Duplicate 121% 36.3
DAL SB DF601 0 0050 121213 Low LMS 112% 45.0 91.7 120% 8.7% DAL SB DF601 0 0050 121213 High LMS NR NR NR NR

DAL SB DF602 0 0000 121213 111% NA 18.6 NA 17.0 DAL SB DF602 0 0000 121213 Duplicate 93.9% 15.5
DAL SB DF602 0 0000 121213 Low LMS 98.5% 43.2 65.4 112% 18% DAL SB DF602 0 0000 121213 High LMS NR NR NR NR

DAL SB DF602 0 0050 121213 97.9% NA 1396 NA 1410 DAL SB DF602 0 0050 121213 Duplicate 101% 1426
DAL SB DF602 0 0050 121213 LMS 88.8% 1025 2017 59.1% [b] 2.2%
DAL SB DF603 0 0000 121213 95.5% NA 22.9 NA 23.5 DAL SB DF603 0 0000 121213 Duplicate 106% 24.0
DAL SB DF603 0 0000 121213 Low LMS 104% 42.8 79.0 130% 4.7% DAL SB DF603 0 0000 121213 High LMS 83.5% 470 440 88.6%
DAL SB DF603 0 0050 121213 103% NA 30.8 NA 35.0 DAL SB DF603 0 0050 121213 Duplicate 124% 39.2
DAL SB DF603 0 0050 121213 Low LMS 113% 41.3 85.9 123% 24% DAL SB DF603 0 0050 121213 High LMS 98.9% 362 ULOQ ULOQ Trip Blank 1 102% NA BLOQ NA BLOQ Trip Blank 1 Duplicate 99.2% BLOQ Trip Blank 1 Lab Matrix Spike 103% 1.01 1.09 108% NA Concentration values are rounded to 3 significant f igures, statistical results rounded to 2 significan t figures, but non-rounded values used for data calculations. [a] SRS recovery only shown from the analytical run used to report the results for that analyte in tha t sample [b] LMS recover was outside of 100 + 30%, but within 100 + 50% BLOQ; result was less than the analyte/IS response for the lowest (nominal 0.200 ng) calibration stan dard NA; Not applicable NR; Not Reported because LMS fortification level wa s not appropriate relative to the determined level of analyte in the sample3M ENVIRONMENTAL LABORATORY STUDY NO. E12-0849, REVISED REPORT

PAGE 15 OF 16 

# 4 Data/Sample Retention

All remaining sample and associated project data (h ardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating p rocedures.



# 5 Conclusion

The quantitative analysis of the Decatur soils coll ected from near Field 6 and near the railroad track s at the 3M Decatur facility was complete. The levels o f PFOS were generally the highest concentrations, followed by PFOA, PFHS and then PFBS. PFOS concent rations ranged from 3.86 ng/g (dry wt) to 3890 ng/g (dry wt.) ;PFOA ranged from 23.5 ng/g (dr y wt.) to 1410 ng/g (dry wt.); PFHS ranged from 3.56 ng/g (dry wt.) to 270 ng/g (dry wt.) and PFBS ranged from 0.373 ng/g to 64.8 ng/g (dry wt.). One result for PFBS could not be reported (NR) due qual ity control failure.
Laboratory matrix spike recoveries were used to det ermine the sample specific accuracy and showed good recoveries within 100 + 30% for all analytes reported in samples, except o ne PFBS result which could not be reported because of poor LMS recovery. The relative percent difference (RPDs) between duplicate analytical sample results was typically l ess than 20%, and less than 50% for all samples except for one PFBS result with a RPD of 104% and o ne PFOS result with a RPD of 87%.
The analytical data accuracy determined from SRS r ecoveries showed acceptable recovery at within 100 + 30% and the RSD (data precision) was less than 10%

. The analytical method uncertainties (95%CI) determi ned from LCS results were + 12% for PFOS, + 30% for PFHS, + 7.9% for PFBS and + 25% for PFOA. 

# 6 Attachments

None