3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 1 OF 16 

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.com 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 2 OF 16 

3M Environmental Laboratory, Analytical Study E12-0849 

3M Environmental Laboratory Manager: William K. Reagen, Ph.D. 

3M Principal Analytical Investigator: Cleston Lange, Ph.D. 

1 Introduction / Summary 

The 3M Environmental Laboratory received six (6) Decatur, AL soil samples on December 20, 2012. 

The objective of this project was to analyze the collected soil samples for perfluorooctanoic acid 

(PFOA), perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHS) and perfluorooctane 

sulfonate (PFOS). 

Samples were analyzed following 3M Environmental Laboratory method ETS-8-053.0 “Solvent 

Extraction and LC/MS/MS Analysis of Soils for C6-C12 Perfluorinated Carboxylic Acids, and 

Perfluorobutane Sulfonate, Perfluorohexane Sulfonate, 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 and PFOA results within the range of the calibration

curve. Results from the analysis of the soil samples and trip blank are summarized in Table 1. 

Concentrations of PFOS were the highest in the Decatur 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 that 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 the added 

stable isotope labeled surrogate recovery standards (SRSs) was a measure of the analytical method 

precision and was determined at 11% for 13C4-PFOA and 9.9% for 13C4-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 NR 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 reported (NR) because it was not 2-times the measured trip blank concentration for that analyte
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 3 OF 16 

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 

[1,2,3,4-13C4]-Perfluorooctane-1-

sulfonate sodium salt 

Chemical Formula n-C8F17SO3 K+ C8F17SO3K+ 13C4

12C4F17SO3 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 [

13C8]-Perfluorooctane-1-

sulfonate sodium salt 

Perfluoro-n-octanoic acid Ammonium perfluorooctanoate 

Chemical Formula 13C8F17SO3 Na+ n-C7F15CO2H C7F15CO2 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 [1,2,3,4-13C4]-Perfluoro-noctanoic acid 

13C8-Perfluorooctanoic acid Perfluorobutane sulfonate 

Potassium salt 

Chemical Formula 13C4

12C3F15CO2H 13C8F15O2H C4F9SO3 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 

PAGE 4 OF 16 

Table 2. Reference Substances 

Reference ID 18O2-PFBS PFHS (linear) ECF-PFHS 

(linear + branched) 

Chemical Name [

18O]-Perfluorobutane 

sulfonate Ammonium salt 

Perfluoro-1-hexanesulfonate 

sodium salt 

Perfluoro-1-hexanesulfonate 

Potassium salt 

Chemical Formula C4F9S[18O2] ONH4

+

n-C6F13SO3 Na+ C6F13SO3 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 [1,2,3-13C4]-Perfluoro-1-

hexanesulfonate sodium salt 

 

Chemical Formula 13C3

12C3F13SO3 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 trip blank were prepared and sent to Decatur, 

AL on December 10, 2012 to Weston Solutions, Inc. personnel. 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 defined in method ETS-8-053.0. In summary, 

preparation involves removal of a 1 cubic centimeter (1 cc) soil sample aliquot (typically ~ 1 gram) from 

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 generally larger than 5 mm were typically removed 

during weighing to ensure better sample homogeneity. 

Prior to extraction, each weighed sample aliquot was fortified with a fixed quantity of stable isotope

labeled internal standards (IS) and surrogate recovery standards (SRS) as defined in Table 2. 

Following the addition of IS and SRS compounds, each 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 transferred to an autovial for LC/MS/MS analysis. 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 5 OF 16 

Soil matrix blanks and calibration standards are prepared similar to samples using a control soil 

TCR-455. A 1 cc aliquot of soil TCR-455 weighed nominal 1.0 gram (dry weight). Because 

environmental soil and sediment samples can vary significantly 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 extraction. Calibration standards were fortified from the range of 

0.200 ng to 500 ng for each analyte; nominal calibrated range was 0.200 ng/g to 500 ng/g in control soil 

TCR-455. Percent moistures used for calculating soil 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 s130102b and s130103a. Results of the screening 

analysis were not used for reporting. Data for definitive 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 s130117a (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 described 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-8-053.0

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 1.6.1 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 6 OF 16 

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 

13C4-PFOA (SRS) 417>372 

13C8-PFOA (IS) 421>376 

PFOS 499>130, 499>99, 499>80 

13C8-PFOS (IS) 507>80 

PFHS 399>99, 399>80 

13C3-PFHS (IS) 402>80 

PFBS 299>99, 299>80 

18O2-PFBS (IS) 303>84 

13C4-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 used for calibration. Each soil calibration standard

received nominal 3 ng of each IS and 3 ng of each SRS. A total of twelve spiked standards ranging 

from nominal 0.200 ng to 500 ng of each target analyte were prepared and analyzed. To meet 

linearity and accuracy criteria, the high calibration standard (500 ng) was disabled for PFBA. The 

plot of the analyte/IS ratio for each standard versus known standard analyte fortification amount was 

fitted using a quadratic, 1/x weighted linear regression. The data were not forced through zero during 

the fitting process. Back-calculating the standard concentrations using the peak area ratios and the 

resultant calibration curve confirmed accuracy of each curve point at within 100 + 30% (+ 35% at 

LLOQ). The correlation coefficient (r) was greater than 0.995 for each analyte fitted calibration curve. 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 7 OF 16 

3.2 Limits of Quantitation 

The lower limit of quantitation (LLOQ) for each analyte was the lowest non-zero calibration standard in 

the curve that met linearity and accuracy requirements and for which the peak area ratio was at least 

two times the average peak area response of the method 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 calibration 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 achieve results within the range of the calibration. 

3.3 Continuing Calibration 

Reinjection of calibration standards during analytical runs were conducted to verify the analytical run 

was maintained in control throughout the analysis. During the course of the analytical sequence, 

several mid-level continuing calibration verification samples (CCVs) were analyzed to confirm that the

instrument response and the initial calibration curve were still in control. The method acceptance 

criterion of 100% ± 30% for CCVs was met for all analytes 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 instrument blanks (zero volume injections). Method blank 

results were reviewed and used to evaluate method performance 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 carboxylate (13C4-PFOA for PFOA) and the other 

representing the perfluorinated sulfonates (13C4-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 13C4-PFOA (n = 58) and 97.7% + 9.6% for 13C4-PFOS (n = 58). The analytical 

method precision was indicated by the RSDs and was 11% 13C4-PFOA and 9.9 % for 13C4-PFOS. 

Overall, the SRSs results demonstrate excellent analytical 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 was at 138%. The analytical method 

uncertainties (95%CI) determined from LCS results were + 12% for PFOS, + 30% for PFHS, + 7.9% for 

PFBS and + 25% for PFOA. 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 8 OF 16 

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 

PAGE 9 OF 16 

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 

PAGE 10 OF 16 

3.7 Laboratory Matrix Spikes (LMS) 

Laboratory matrix spikes (LMSs) were prepared for each sample at a level that was appropriate relative

to the endogenous target analyte level. All LMS recoveries were within method acceptance criteria of 

100 ± 30%, except for the PFBA result of the Trip Blank which was 143%. Overall, the LMS results 

confirmed that “unknown” components in the sample matrix did not significantly interfere with the 

extraction and analysis of the analytes of interest for most samples. The reference materials used for 

fortification of LMS was comprised of primarily linear 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%

Spike Concentration

(Determine d Concentration of LMS Determined Concentration of Field Sample) LMS Recovery −

=

3.8 Percent Moisture Determination 

The percent moisture was determined in duplicate for 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 evaporation), and then the dry weight is accurately 

determined. The average percent moisture and RPD of the duplicate determinations for each is 

reported in Table 10. The percent moisture was calculated by the following equation: 

*100%

Original Soil Wet Mass

(Original Soil Wet Mass Dried Soil Mass) Percent Moisture −

= 

Table 10. Percent Moistures for Decatur Soils (December 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 samples of soil taken from each sample bottle, RPD is the relative percent difference of 

the duplicate determined values. 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 11 OF 16 

3.9 Sample Results 

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

Sample Description 

Surrogate 

(

13C4

-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 figures, statistical results rounded to 2 significant 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 that 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 standard 

NA; Not applicable 

NR; Not Reported because LMS fortification level was not appropriate relative to the determined level of analyte in the sample 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 12 OF 16 

Table 12. Individual PFHS Results for Decatur Soils (December 2012) 

Sample Description 

Surrogate 

(

13C4

-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 figures, statistical results rounded to 2 significant 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 that 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 standard 

NA; Not applicable 

NR; Not Reported because LMS fortification level was not appropriate relative to the determined level of analyte in the sample 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 13 OF 16 

Table 13. Individual PFBS Results for Decatur Soils (December 2012) 

Sample Description 

Surrogate 

(

13C8

-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 figures, statistical results rounded to 2 significant 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 that 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 standard 

NA; Not applicable 

NR; Not Reported because LMS fortification level was not appropriate relative to the determined level of analyte in the sample 

NR*; Not reported because of QC failure 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 14 OF 16 

Table 14. Individual PFOA Results for Decatur Soils (December 2012) 

Sample Description 

Surrogate 

(

13C4

-

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 figures, statistical results rounded to 2 significant 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 that 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 standard 

NA; Not applicable 

NR; Not Reported because LMS fortification level was not appropriate relative to the determined level of analyte in the sample 
3M ENVIRONMENTAL LABORATORY 

STUDY NO. E12-0849, REVISED REPORT 

PAGE 15 OF 16 

4 Data/Sample Retention 

All remaining sample and associated project data (hardcopy and electronic) will be archived according 

to 3M Environmental Laboratory standard operating procedures. 

5 Conclusion 

The quantitative analysis of the Decatur soils collected from near Field 6 and near the railroad tracks at 

the 3M Decatur facility was complete. The levels of PFOS were generally the highest concentrations, 

followed by PFOA, PFHS and then PFBS. PFOS concentrations ranged from 3.86 ng/g (dry wt) to 

3890 ng/g (dry wt.) ;PFOA ranged from 23.5 ng/g (dry 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 quality control failure. 

Laboratory matrix spike recoveries were used to determine the sample specific accuracy and showed 

good recoveries within 100 + 30% for all analytes reported in samples, except one PFBS result which 

could not be reported because of poor LMS recovery. The relative percent difference (RPDs) between 

duplicate analytical sample results was typically less than 20%, and less than 50% for all samples 

except for one PFBS result with a RPD of 104% and one PFOS result with a RPD of 87%. 

 The analytical data accuracy determined from SRS recoveries showed acceptable recovery at within 

100 + 30% and the RSD (data precision) was less than 10%. 

The analytical method uncertainties (95%CI) determined from LCS results were + 12% for PFOS, +

30% for PFHS, + 7.9% for PFBS and + 25% for PFOA. 

6 Attachments 

None