Document Gz4J7xGZe93radK7E9wBnm97
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3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
AR _ 3^ 7 /
Final Report
Analysis of PFBA, NFPA, PFHA, PFOA, PFBS, PFHS, and P FO S in Aqueous Samples
From Oakdale, Minnesota Municipal Wells
Laboratory Request Number E06-0294
Method Requirement: 3M Methods ETS-8-11.0 and ETS-8-154.1 (modified)
Report- Revision 1,07/18/06 (supersedes report 06/09/06)
Testing Laboratory 3M EHS Operations 3M Environmental Laboratory
Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106
Requester
Gary Hohenstein 3M Building 42-02-E-27
PO Box 3331 Saint Paul, MN 55133-3331
Phone:(651)778-5150 Fax:(651)778-7203
lACCBtPjTEp)
The testin g reported herein m eet th e requirem ents o f IS O /IE C 17025-1999 "G eneral
R equirem ents fo r th e C om petence o f Testing and C alibration Laboratories'', in accordance w ith the A 2LA C ertificate #2052-01. Testing th at com plies w ith this International Standard also operate in accordance w ith ISO 9001/IS O 9002 (1994).
Certificate #2052-01
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3M ENVIRONMENTAL LABORATORY REPORT NO. ED6-0294
Reason for Report Revision
This report was revised in order to achieve analytical data of the highest quality for all target compounds. T h e PFB A data reported here w ere generated using method E T S -8 -1 1.0 and was not changed from the original report. All other target analytes w ere requantitated using method E T S -8 -1 5 4 .1 . PFO S and P FO A data generated by E T S -8 -1 1.0 did not consistently m eet m ethod acceptance criteria requirem ents. Im proved P FO S and PFO A data accuracy was obtained using E T S -8 -1 5 4 .1 , a m ethod validated for PFO S and PFO A . D ata for the rem aining target compounds w ere consistent betw een the m ethods. Only data from E TS -8-154.1 was reported for those a n a ly te s .
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3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
3M Environmental Laboratory
3M Environmental Laboratory Technical Manager: William K. Reagen, Ph D. 3M Technical Leads: Mark E. Ellefson, Kent R. Lindstrom Report Author: Susan W olf
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Analytical Report E06+0294, Revision 1 o;
Oakdale Municipal W ell Samples: Minnesota Department of Health Co-Sam pling M a y 1 1 ,2 0 0 6
Report Date; July 1 8 ,2 0 0 6 Supersedes report dated June 9 ,2 0 0 6
The 3M Environmental Laboratory prepared and analyzed municipal water samples collected by Pace Analytical Field Services personnel on M ay 1 1 ,2 0 0 6 , from Oakdale municipal wells 1 ,2 ,3 , 5 ,7 ,8 , and 9 in conjunction with the monthly Minnesota Department of Health sampling. Samples w ere returned to the 3M Environmental Laboratory for analysis of perfluorobutanoic acid (PFBA), nonafluoropentanoic acid (NFPA), perfluorohexanoic acid (PFH A ), perfluorooctanoic add (PFOA), perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFH S) and perfluorooctane sulfonate (P FO S ) under laboratory project num ber E 06-0294. Analysis was completed following 3M Environmental Laboratory method ETS 8-11.0 "Determination of C 4 - C 8 Highly Fluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by High Perform ance Liquid Chromatography/Mass Spectrom etry' and ETS-8-154.1 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extraction and High Perform ance Liquid Chromatography/Mass Spectrom etry.
The 3M Environmental Laboratory prepared sets of sample containers for seven sampling locations. Each sam ple set consisted of a field sample, field sample duplicate, low field spike, and high field spike. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 450 mL. Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution containing ali analytes prior to being sent to the field for sample collection.
Table 1 summarizes the sample results using both analytical methods identified above. All results for quality control samples prepared and analyzed with the samples w il be reported and discussed elsewhere in this report.
Certificate #2052-01
The testing reported herein meet the requirements of ISO/IEC 17025-1999 `General Requirements for the Competence o f Testing and Cstfbration Laboratories', in accordance with the A2LA Certificate
#2052-01. Tesfng ttial complies with this International Standard also operate In accordance with ISO 9C01/ISO 9002 (1994).
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3M ENVIRONMENTAL LABORATORY REPORT NO E06-0294
T a b le 1. S a m p le R esu lts S um m ary l1>
3M L1MS ID EQ6-0294-001 E 0 6 -0 2 9 4 -0 0 2
E 0 6 -0 2 9 4 -0 0 5 E<n>n294~n06
E 0 6 -0 2 9 4 -0 0 9 E 0 6 -0 2 9 4 -0 1 0
E 06-C 2 94-013 E 06-G 294-014
EOO-0294-O2O E06-02S4-021
E 0 6 -0 2 9 4 -0 2 4 E 0 6 -0 2 9 4 -0 2 5
E 06-0294 -D 28 E 0 6 -0 2 9 4 -0 2 9
Sam ple Description
PFBA C o n c e n tra tio n
(n a to li.)
3ottte 1, W ell 5, Sample Bottle 2. W ell 5. Sample Duplicate
A verage W ell 5 % RPD Sam Dle/Sam Dle Du d W ell 5
Bottle 5, Well 7, Sam ple
;
Bottle 6 W ell 7. Sam ple Duplicate
A verage W ell 7
% RPD Sam ple/Sam ple Dup W eil 7
Bottle 9, WeH 8, Sample Botile 10. W ell 8. Sample Duplicate
A verage W ell 8
% RPD Sam ple/Sam ple D up W ell E
Botile 13, W ell 9, Sample Botile 14. W ell 9. Sample Duplicate
A verage W ell S % RPD Sam ple/Sam ple D up W ell 9
Bottle 20, W e l 1, Sample Bottle 21. W ell 1. Sample Duplicate
Average W ell 1
/RPD Sam ple/Sam ple Dup W ell 1
Bottle 24, W ell 2, Sample
Bottle 25. W ell 2. Sample Duplicate A verage W all 5
% r p d S am nie/Sam plc D up WeH
Botile 28. W ell 3, Sample
Bottle 29. W ell 3, Sample Duplicate A verage W ell
% RPD Sam ple/Sam ple D up W ell
1.74 1.75 1.75 1 .0 0.824 0.828 0.826 0 .5 6 1.28 1.28 1.28 0.078 2.04 2.02 2 .0 3 0.79 0295 0.207 0.291
3 .0 0.381 0.373 0.377
2 .0 0.0949 0.0855 0.0902
10
nfpa" C oncentration
(ng/m L)
0.0765 0.0781 0.0773
2.1 0 .0 3 0 6 0 .0 2 6 9 0 .0 2 8 8
13 0 .0 4 6 8 0.0491 0.0460
4.8 0.0895 0.0914 0 .0 9 0 4
2.1 0 .0 2 4 8 0 .0 2 4 0 0 .0 2 4 6
NA 0 .0 2 4 8 0 .0 2 4 8 0 .0 2 4 8
NA 0 .0 2 4 8 0 .0 2 4 8 0 .0 2 4 8
NA
PFHA" C oncentration
(ng/m L)
0 .2 0 8 0 .1 9 8 0 .2 0 3
4 .9 00793 0.0727 0.0760
8 .7 0-112 0.131 0.122 16" 0 .2 2 5 0-235 0-230
4 .3 < 0 .0 2 5 2 0 .0 2 5 2 <0.0252
NA 0 .0 3 7 6 0.0364 0 .0 3 7 0
3.2 <0.0252 <0.0252 < 0 .0 2 5 2
NA
PFOA" C oncentration
(ng/m L)
0732 0.722 0,727
1.4 0255 0 .2 3 6 0 .2 4 6
7.7 0.431 0.437 0 .4 3 4
1 .4 0.726 0 .6 5 2 0.689
11 0.0781 0.0601 0.0791
2.5 0.0931 0 .0 9 1 5 0 .0 9 2 3
1.7 < 0 .0 2 5 4 < 0 .0 2 5 4 < 0 .0 2 5 4
NA
PFBS" C o n c e n tra tio n
(ng/m L)
0.0426 0 .0 3 8 5 0.0406
10 <0.0250 <0.0250 < 0 .0 2 5 0
NA 0.0251 < 0 .0 2 5 0 " 0 .0 2 5 1
NA 0.0521 0 .0 4 9 2 0 .0 5 0 6
5 .7 <0.0250 <0.0250 < 0 .0 2 5 0
NA <0.0250 <0.0250
<0.0250
NA < 0 .0 2 5 0 < 0 .0 2 5 0 < 0 .0 2 5 0
NA
PFHS" C oncentration
(ng/m L)
00858 0 .0 8 1 7 0.0B3S
4 .9 0 .0 3 4 3 0 .0 3 1 5 0 .0 3 2 9
8.5 0 .0 5 1 8 0 .0 5 0 8 0 .0 5 1 3
1 .9 0.106 0 .1 0 3 0 .1 0 4
2 .9 < 0 .0 2 5 2 0 .0 2 5 2 < 0 .0 2 5 2
NA 0 .0 2 5 2 0 .0 2 5 2 0 .0 2 5 2
NA 0 .0 2 5 2 < 0 .0 2 5 2 <0.0252
NA
PFOS" C oncentration
(ng/m L)
1.02 0.905 0.962
12 0 .2 0 4 0 .1 9 8 0201
3-0 0 .5 9 6 0 .6 4 7 0.622
82 0.567 0.544 0.556
4.1 0.0415 0-0381 0 .0 3 9 8
8 .5 0.0387 0.0324 0.0356
"18 <0.0252 <0.0252 ! <0.0252 | NA
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3M ENVIRONMENTAL LABORATORY REPORT NO E06-0294
N/A = No* Applicable
(1) The analytical method uncertainties are as follows: PFBA is 100% 8.0% , NFPA is 100% 8.4% , PFHA is 100% 20%
PFOA is 100% 1 8 9 % , PFBS is 100% 4.6% . PFHS is 100% 3.3% , PFOS is 100% 5.5% Refer to Sections 3 and 4 for
data acceptance criteria and discussion. (2) Sample results for PFBA were determined folkxMng method E TS -8-11.0.
(3) Sam ple results for NFPA, PFHA, PFOA, PFBS, PFHS, and PFOS were determined tallowing method ETS-8-154.1 (4) The Relative Percent Difference between the Sam ple/Sample Duplicate exceeds 15%.
(5) Average and % RPD were not calculated due to one sample being <LOQ. Reported the higher of the two values.
:&*vyq)tir
I
2.1 Methods
Analysis was completed following 3M Environmental Laboratory method ETS 8 -1 1 .0 "Determination of c < - c 8 Highly Fluorinated A dds, Alcohols, Amides, and Sulfonates in W ater by High Performance Liquid Chromatography/Mass Spectrometry' and E TS -8-154.1 "Determination o f Perfluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extraction and High Performance Liquid ' Chromatography/Mass Spectrom etry. E TS -8-154.1 is currently on the laboratorys scope of accreditation to ISO /IEC 17025:1999. E TS -8-11.0 is not currently on the laboratorys scope of accreditation.
2.2 Sample Collection
Samples w ere collected in NalgeneTM (low-density polyethylene) bottles prepared at the 3M
Environmental Laboratory. Prior to sam ple collection, bottles designated for field matrix spikes were
spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing the
analytes of interest. Collected sample bottles w ere returned to the iaboratory at ambient conditions on
May 12,2006.
..
2.3 Sample Preparation
PFBA Analysis:
AH samples, calibration standards, and associated quality control samples were prepared using method ETS 8-11.0 "Determination of C4- C BHighly Fluorinated Adds, Alcohols, Amides, and Sulfonates in W ater by High Perform ance Liquid Chromatography/Mass Spectrometry*. Briefly, aqueous samples and calibrations standards were prepared for analysis by diluting the samples 1:1 using a 10-mM ammonium hydroxide in methanol solution. This method is currently not on the laboratory's scope of accred itation to ISO/! EC 17025:1999.
NFPA, PFHA, PFOA, PFBS, PFHS, and PFOS Analysis:
All samples, calibration standards, and associated quality control samples were extracted using a modified procedure of E TS -8-154.1. Briefly, 40 mL of sample were loaded onto a pre-conditioned W aters C18 solid phase extraction (SPE) cartridge (Sep-Pak, 1.0 g, 6 cc) using a vacuum manifold The loaded SPE cartridges were then eluted with 5 mL of methanol. This extraction procedure concentrates the samples by a factor of eight. (Initial volume = 40 mL, final volume = 5 mL). Lab control spikes extracted in the sam e manner cross-validate all the method modifications/deviattons from E TS -8-154.1. See Section 3.6 for additional information.
Modifications from E TS -8-154.1 that were used for this analysis:
Samples were not extracted in duplicate as samples were collected in duplicate in the field. Extraction columns were not rinsed with 40% methanol after sample loading. After loading the sample onto the column, and just prior to eluting the column with methanol,
vacuum was applied for approximately 5 minutes to remove as much sam ple as possible.
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3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
2.4 Analysis
, . .. .
All samples and quality control samples were analyzed for seven target analytes using nigh
performance liquid chromatography/ tandem mass spectrometry (H P LC /M S/M S ). Pertinent instrument
parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed
are described in the tables below.
Table 2. Instrument Parameters.
AnalvH**Al M ethod follow ed i quid chrom atoaranh G uard colum n A nalytical colum n Injection Volum e Mm * Soectrom eter
: Softw are
ETSG inger E T S -8 -1 1 .0 A dlentH O O Prism RP (2 mmJC 50 mm). 5 um
Betasll C 18 (2.1 mm X 100 m m), 5 urn
10 uL Aoolied Biosystems A PI 5000
Turbo Sorav Z-sprav Negative
Analyst 1.4.1
Table 3. Liquid Chromatography Gradient Program.
E TS O Ilie E T S -8-154 .1 Agilent 1100 Betasil C 18 12.1 m m .X i00 mm), 5 um Betasil 0 1 8 (2 .1 mm X 100 mm), 5 urn
5 fiL Aoolied Bioevstems API 4000 Q trap
Turbo Spray Z-spray Negative
Analyst 1.4.1
E T S G in g e r S tep
Numbe r
o 1 2 3 4 5
Total Time (min)
0 2.0 10.0 12.0 12.5 16.0
E T S O lite S tep
Number
o 1 2 3 4
5
Total Time (min)
0 1.0 14.5 15.5 16.5 20.0
Row Rate (fjL/min)
300 300 300 300 300 300
PercentA (2 mM ammonium acetate)
90.0 90.0 10.0 10.0 90.0 90.0
Percent 0 (Methanol)
10.0 10.0 90.0 90.0 10.0 10.0
Row Rate (nL/min)
300 300 300 300 300 300
Percent A (2 mM amirumium acetate)
80.0 80.0 10.0 10.0 00.0 80.0
Percent B (Methanol)
20.0 20.0 90.0 90.0 20.0 20.0
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3M ENVIRONMENTAL LABORATORY REPORT NO E06-0294
Table 4. Mass Transitions
Analyte PFBA PFOA
PFOS
PFHS PFBS PFHA NFPA
Mass Transition Q1/Q3
213/169 413/369 413/219 413/169 499/99 499/80 499/130 399m 399/80 299Mb 29SV99 313H19 263/219
DwaH Tima (msec) Dwell Tima fmsac)
ETSGkiger
ETSOOie
BO
80 100
80 100
80 100
80 -
100
80' `
100
- 80
100
80 100
" 80
' 100
80 " 100
80 100
80 100
80 100
3.1 Calibration
PFBA Analysis: Calibration standards w ere prepared by spiking known amounts of stock solutions containing the target analytes into 2 mL of ASTM type I water. A 750uL aliquot of each water standard was then transferred to an autosampler vial. Subsequently, a 750uL aliquot of a 10mM ammonium hydroxide in methanol solution was added to the vial. Ten spiked standards ranging from 0.025 ng/mL to 10 ng/mL (nominal) were prepared. After dilution, the nominal concentration of each analyte in the vial was 0.0125 ng/mL to 5.0 ng/mL. Quadratic, i/x weighted, calibration curves were used to fit the data for each analyte.
NFPA, P F H A PFOA, PFB S, P FH S , and PFOS Analysis: Calibration standards were prepared by spiking known amounts of stock solutions containing the analytes of interest into 40 mL of ASTM type I water. Each spiked w ater standard was then extracted in the sam e manner as the collected samples. A total of eleven spiked standards ranging from 0.025 ng/mL to 10 ng/mL (nominal) were prepared. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data w ere not forced through zero during the fitting process. Calculating the standard concentration using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point.
Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 10025% (10030% for the lowest curve point) were met. The correlation coefficients (r) were greater than 0.999 for each analyte.
The analytes P FB A N F P A and PFHA w ere initially dissolved in acetonitrile before being further diluted into an intermediate standard solution. This is a deviation for ETS-8-154.1 which specifies that analytes should be dissolved in Methanol. This deviation has no adverse affect on the sample results.
3.2 Limit of Quantitation (LOQ)
The LOQ for this analysis, as defined in methods E TS -8-11.0 and E TS -8-154.1, is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and which the area counts are at least twice those of the appropriate blanks. The nominal LOQ for PFBA was 0.050ng/m L. The nominal LOQ for NFPA, PFHA, PFOA, PFBS, PFHS, and P FO S was 0.025ng/mL..
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3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
3.3 System Suitability
PFBA Analysis: The 5ng/mL calibration standard was analyzed in triplicate at the beginning and end of the analytical sequence to demonstrate overall system suitability. Method acceptance criteria of less than 5% relative standard deviation (R S D ) for peak area and less than 2% R SD for retention time for both opening and closing system suitability injections were met.
NFPA, PFHA, P F O A PFBS, PFHS, and PFO S Analysis: The 1.0 ng/mL extracted-calibration standard was analyzed five times at the beginning and end of the analytical sequence to demonstrate overall system suitability. All compounds met the acceptance criteria of less than 5% relative standard deviation (R S D ) for peak area and less than 2% RSD for retention time for the opening and closing system suitability injections with exception of NFPA and PFOA. The RSD for the area counts for the closing system suitability for NFPA was 6.2% and 6.9% for PFOA. As laboratory control samples and field matrix spikes are used to qualify the samples results, any instrument variability that may have occurred would be accounted for with these samples.
3.4 Continuing Calibration
PFBA Analysis: During the course of the analytical sequence, several continuing calibration verification samples (C CVs) were analyzed to confirm that the instrument response and the initial curve w ere still in control. These CCVs were re-injections of two different concentrations of calibration standards from the first calibration curve (curve not used for quantitation) that were quantitated against the second curve (used for quantitation}. Alt C CVs for PFBA m et method criteria.
NFPA, PFHA, PFOA, PFB S, PFHS, and PFOS Analysis: During the course of the analytical sequence, several continuing calibration verification samples (C C Vs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. O ne C C V level for PFHA analyzed twice during the course of the run had recoveries of 129% and 131 % , which did not m eet method criteria of 10025% . A t other CCVs m et method criteria.
3.5 Blanks
Three types of blanks w ere prepared and analyzed with the samples: method blanks, solvent blanks, and field/trip blanks. Each blank result was reviewed and used to evaluate method performance to determine the LOQ for each analyte-
3.6 Lab Control Spikes (LCSs)
PFBA Analysis: Low and high lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spiking known amounts of the analytes into 2 mL of ASTM Type I water and prepared exactly like the samples and standards. LCS results were be used to determine overall method uncertainty in Section 3.7.
N FP A PFHA, P FO A PFBS, PFH S, and PFOS Analysis: Low and high lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spiking known amounts of the analytes into 40 mL of ASTM Type I water to produce the desired concentration. The spiked water samples were then extracted and analyzed in the sam e m anner as the samples. Analysis of triplicate LCSs at the two specified levels cross-validates the analytical method as used here for any modifications/deviations from ETS 8 -1 5 4 1 . Additionally, LCS results were used to determine overall method uncertainty in Section 3.7. The RSD for the six LCS prepared for PFHA was 19% , which did not m eet method acceptance criteria of <15% .
The following calculations w ere used to generate data in Table 5.
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C alculated Concentration
100%LCS Percent Recovery Spike Concentration
100standard deviation LCS replicates
LCS%RSD =
%
average LCS recovery
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3M ENVIRONMENTAL LABORATORY REPO RT NO. E06-0294
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3M ENVIRONMENTAL LABORATORY REPO RT NO. E06-0294
Table 5. (1,2)Lab Control Spike Results.
---------------------1
PFBA
NFPA
PFHA
PFOA
Lab ID
Spiked
Calculated
Spiked
Calculated
Spiked
Calculated
Spiked
Calculated
Concentration Concentration
Concentration Concenbation
Concentration Concentration
Concentration Concentration
(no/mL)
(ng/mL) ^R eco very (ng/mL)
(ng/mL) `Recovery (no/mL)
(ng/mL) `Recovery 1ng/mL)
(ng/mU ^R eco very
L C S -060315-1 L C S -060615-2 LCS-O60315-3 LCS-060S15-4 L C S -060615-5 L C S -060615-6
0.494 0.494 0.494 4.94 4 .9 4 4.94
0.457 0.449 0.464 4.92 4.91 4.95
9 2 .5 91.0 94.0 9 9 .7 9 9 .4 100
0 .9 9 0 0 .9 9 0 0 .9 9 0 9.90 9.90 9.90
0.870 0.939 0.969 9.64 9.64 9.98
87.9 54.8 97.9 97.4 97.4 101
1.01 1.01 1.01 10.1 10.1 10.1
1.10 1 21 1.15 7.89 8.18 (5 )
109 120 114 78.1 80.8 NA
1.02 1.02 1.02 10.2 10.2 10.2
0.920 1.03 1.07 (5) (5) (5 )
90.2 101 105 NA NA NA
Average %RSD
96.1% 4 .3%
96.0% 4 ,6 %
100% 19% w
98.7% 7 .7%
Lab ID
PFBS
PFHS
PFOS
Spiked
Calculated
Spiked
Calculated
Spiked
Calculated
Concentration Concentration
Concentration Concentration
C oncentration Concentration
(ng/mL)
(ng/mL) ^R eco very (ng/mL)
(ng/mL) `Recovery (ng/mL)
(ng/mL) ^ R eco very
LCS-060615-1 L C S -060615-2 LC S-060615-3 L C S -060615-4 L C S -0 6061 5-5 iLCS-060615-6
0.999 0.999 0.999 9 .9 9 9 .9 9 9.9900
0.952 0.985 0.S71
(5 ) 981 (6 )
95.3 9 8 .6 9 7 .2 NA 96.2 NA
1.01 1.01 1.01 10.1 10.1 10.1
0 .9 8 6 1.05 1.01 (5 ) 983 (5 )
976 104 100 NA 97.3 NA
1.01 1.01 1.01 10.1 10.1 10.1
0.993 1.03 1.06 9.14 9.97 10.6
98.3 102 105 90.5 98.7 105
IAverage r % RSD
96.8% 1 .5%
99.7% 3 .1%
99.9% 5.4%
NA = Not applicable (1) PFBA was deleimined by method ETS-8-11.0, all other analytes were determined by ETS-8-154.1 (2) All results and average values listed to three significant figures according to EPA rounding rules. % RSD values given to two significant figures. Due to rounding, values m ay vary slightly
from thoseinthe raw data. (3) The LCS descriptions listed above are for the ETS-8-154.1 analysis. The LCS descriptions for PFBA were LCS-060605-1 through LCS-060605-6.
(4) The RSD did not m eet method criteria o f 100% 15%. (5) Sample area counts exceeded the calibration range, recovery could not be determined. While many of the 10 ng/'mL LCS could not be quantitated, the 1 ngrinL LCS w as more in line
with the concentrations detected in the samples.
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3M ENVIRONMENTAL LABORATORY REPO RT NO. E0B-0294
3.7 Analytical Method Uncertainty
Both the accuracy (percent recovery) and precision (% R S D ) of the lab control spikes w ere used to estimate the overall method's analytical uncertainty for a given analyte. For exam ple, if the overall accuracy and precision for PFO S based on LCS results was 99.9% +5.4% . The measured precision (% RSD) is then used to determine the range of the accuracy.
Example: 99.9*(0.054) * 5.4 9 9 .9 + 5 .4 = 1 0 5 .3 :9 9 .9 -5 .4 = 94.5
Thus, LCS accuracy results range from 94.5% to 105.3% . The absolute difference of the low and high ends of this range, when compared to 100% , are then calculated.
100% -105.3= 5.3% 100% -94.5 = 5.5% .
The most conservative (largest) absolute difference is then used as the analytical uncertainty for the given analyte.
Table 6. Analytical Method Uncertainty
A nalyte PFBA NFPA PFHA PFOA PFBS PFHS PFOS
M ethod U ncertainty 1 0 0 % + /-a 0 % 10 0% + /-8.4 % 100% +/- 20% 100% +/- 8.9% 10 0 % + /-4 .6 % 100% +/- 3.3% 100% +/- 5.5%
3.8 Field Matrix Spikes (FMS)
Low and high field matrix spikes w ere collected at each sampling point to verify that the analytical method is applicable to the collected matrix. Field matrix spikes are generated by adding a measured volume of field sample to a container spiked by the laboratory with the target anaiytes prior to shipping sample containers for sample collection. Field matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown' components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. Field matrix spikes are presented in section 4 of this report.
FMS Recovery = (Sam ple Concentration or FMS - Average Concentration: Field Sample & Field Sample Dup.) Spike Concentrator)
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3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
Table 7. Field Matrix Spike Concentrations
L o c a tio n W ells We 7 W eK8 W ell 9 Trip Blank W ell 1 W ell 2 we 3
D escription Low Field Matrix Spike High Field Matrix Spike Low Reid Matrix Spike High Field Matrix Spike Low Field Matrix Spike High Field Matrix Spike Low Field Matrix Spike High Field Matrix Spike Low Field Matrix Spike High Field Matrix Spike Low Field Matrix Spike . High Field Matrix Spike ' Low Field Matrix Spike High Field Matrix Spike (Low Fiefcl Matrix Spike High Field Matrix Spike
Final C oncentration (ng/m L)
PFBA NFPA PFHA PFOA PFBS PFHS PFOS
0.0987 0.0990 0.101 0.508 0.0999 0.101 0.503
0 .9 8 7
0.990
1.01
1.02
0 .9 9 9
'.0 1
1.01
0.0987 0.0990 0.101 0.102 0.0999 0.101 0.101
0 .9 8 7
0.990
1.01
1.02 0.999 1.01 1.01
0.0987 0.0990 0.101 0.305 0.0999 0101 0.302
0^987
0.990
1.01
1.02 0.999 1.01 1.01
0.0987 0.0990 0.101 0.305 0.0999 0.101 0.302
0.987
0.990
1.01
1.02
0.999
1.01
1.01
0.0967 0.0990 0.101 0.0508 0.0999 0.101 0.503
0 .9 8 7
0.990
1.01
1.02 0 9 9 9 1.01 1.01
0.0987 0.0990 0.101 0.102 0.0999 0.101 0.101
0.987 0.990
1.01
1.02
0.999
1.01
1.01
0.0987 0.0990 0.101 0 .` 02 0.0999 0.101 0.101
0.987 0.0987
0.990 0.0990
1.01 0.101
1.02 0 .1 0 2
0.999
1.01
0.0999 0.101
1,01 0.101
0.987 0.990
1.01
1.02 0.999 1.01 1.01
' '\`l " v
f'r'-
The tables below summarize the sample results and field matrix spike recoveries for the seven locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference (R PD) of the sample and sample duplicate.
PAGE 12 OF 21
3M ENVIRONMENTAL LABORATORY REPO RT NO. E06-0294
Table 8. Well 5 Results
3M UM SID
Description
E06-0294-001 E 0 6 -0 2 9 4 -0 0 2 E 0 6 -0 2 9 4 -0 0 3
Rottte 1, W ell 5, Sample Bottle 2. W ell 5. Sam ple Duplicate Bottle 3, W ell 5, Field Matrix Spike Low
E06-0294-004 Bottle 4 , W e i 5, Field Matrix Spike High A verage Concentration (ng/mL) %RPD
PFBAm
NFPA
PFHA*
PFOA*
Concentration
(ng/mL)
%Recoverv
1.74 NA
1.75
NA
1.92
NR
2 .8 2
109
1.74 ng/mL 1.0%
Concentration
(n&mL)
^Recovery
0 .0 7 6 5
NA
0.0781
NA
0.181
10b
1.03 96.2
0.0773 nstfnL2.1%
Concentration
Concentration
(ng/mL)
%Recovery
(ng/mL)
'/Recovery
0203
NA
0 .7 3 2
NA
0.198
NA
0.722
NA
0294
NR
1.23
99.0
1.29
108
1.36
'''62.1
0.203 ng/ml 4.9%
0.727 ng/mL 1.4%
3MUMS ID
Description
E06-Q294-001 E 0 6 -0 2 9 4 -0 0 2 E 0 6 -0 2 9 4 -0 0 3 E 0 6 -0 2 9 4 -0 0 4
Bottle 1,W ell 5. Sample Bottle 2, W ell 5, Sample Duplicate Bottle 3, W ell 5, Fieki Matrix Spike Low Bottle 4, W ell 5, Field Matrix Spike Hii
Average Concentration (ng/mL) tiRPD
PRBS
PFHS1*
PFOS
Concentration
(ng/mL)
`Recovery
0 .0 4 2 6
NA
0 .0 3 8 5
NA
0.151
111
1.00
96.0
0.0406ng/mL 10%
Concentration
(ng/mL)
%Recovery
0.0858
NA
0.0817
NA
0 .2 3 8
153
1.13
104
0.0838 ngfinLA9%
Concentra Son
(ng/mL)
%Recovery
1.02
NA
0 .9 0 5
NA
1.55
117
1 93
95.8
0.962ng/mL 12%
N/A = Not Appicabl NR = N rf Reported = Endogenous concentration d analyte exceeded 2x the spiked level and therefore an accurate recovery cannot be calculated. (1) Sample results for PFBA were determined foflcwing method ETS-8-11.0. This method is currently not covered on the laboratories A2LA scope o f accreditation. (2) Sample results for NFPA, PFHA, PFOA, PFBS, PFH S, and PFOS were determined fodowirig method ETS-8-154.1 <3) One o f two field matrix spikes prepared and analyzed did not m eet method criteria of 100% 30% . As one of the two matrix spikes did m eet melhod criteria, the data quality is not
affected.
p. 13
PAGE 13 OF 21
p. 14
1
f
> Q
3M ENVIRONMENTAL LABORATORY REPO RT NO. E0&-0294
Table 9. Well 7 Results
3MUMS ID
E06-0294-005 Bottle 5, W ell 7, Sample E06-0294-006 Bottle 6, Well 7. Sample Duplicate E06-0294-007 Bottle 7, W ell 7, eld Matrix Spike Low 0^ 0294-008 RntHe B W ell 7, Field Matrix Spike High I Average Concentration (ngfmL) %RPD
PFBAm
NFPA1*
PFHA1*
PFOj1 *
Concentration
(ng/mU
%Recovery
0.824
NA
0.828
NA
0.910
NR
1.81 99.8
0.826 ngfmL 0.56%
Concentration
(ng/m l)
%Recovery
0 .0 3 0 6
NA
0 .0 2 6 9
NA
0132
104
0 .9 9 8
97.9
0.0288 ngfmL 13%
Concentration
Concentration
(ngfmL)
%Recovery
(ngfmL)
^R ecovery
0.0793
NA
0 .2 5 6
NA
0.0727
NA
0.236
NA
0.192
115
0 .3 2 4
NR
1,18
. 109
0.996
73.8
0.0760ngfmL 8.7%
0.246 ngfmL 7.7%
3M UM SID
Description
E0&D294-005 Bottle 5, W elt 7, Sample E06-0294-006 Bottle G, Well 7. Sam ple Duplicate E06-0294-007 Bottle 7, W ell 7, Field Matrix Spike Low E06-0294-008 Bottle 6, W ell 7. Field Matrix Spike High
Average Concentration (ngfmL) %RPD
PFBS1*
PFHS
PFOS
Concentration
Concentration
(ngfmL)
%Recovery
(ngfmL)
%Recovery
0 .0 2 5 0
NA 0.0343
NA
0 .0 2 5 0 0 .1 1 4
NA 0.0315 NA 114 0.121 87.2
1.05
105 1.09 105
<0.0250 ngfmL
0 .0 329ngfmL 8.5%
Concentration
(ngfmL)
%Recovery
0.204
NA
0.198 0.282 1.11
NA 802 90.0
0.201 ngfmL 3.0%
N/A = Not Applicable NR = Not Reported = Endogenous concentration of analyte exceeded 2x the spiked level and therefore an accurate recovery cannot be calculated. (1) Sam ple results for PFBA were determined following method ETS-8-11.0. This method is currently not covered on the laboratories A2LA scope of accreditation.
(2) Sam ple results for NFPA, PFHA. PFOA, PFBS, PFHS, and PFOS were determined following method ETS-8-154.1
PAGE 14 OF 21
3MENVIRONMENTAL LABORATORY REPORT NO. 06-0294
Table 10. Well 8 Results
I---------------------------------------------...
-- --<
3UUM SID
Description
E06-0294-009 Bottle 9, W ell 8, Sam ple E06-0294-010 Bottle 10. W ei 8. Sample Duplicate E06-0294-011 Bottle 11, W ell 8, Field Matrix Spike Low E06-0294-012 Botde 12, Wed 8, Reid Matrix Spike High
Average Concentration (ng/mL) %RPD
PFBATM
NFPATM
PFHATM
PFOATM
C o n c e n tra tio n
Concentration
(ng/mL)
%Recovety
(ng/mL)
.R ecovery
1.28
NA 0.0468
NA
128
NA 0.0491
NA
1.36
NR
0.162
1152
2.46
120
1 2 8 ng/mL 0.078%
0.961
922
0.0480 n gM iL i 4.8%
Concentration
Concentration
(ng/mL)
%Recovery
(ng/mL) %Recovery
0 .1 1 2
NA
0.431
NA
0.131
NA
0 .4 3 7
NA
0263
,3i140
0 .6 8 9
63.6
1.21 108 1 2 3 78.0
0.122 ngrinL 16% *
0.434 ng/mL 1.4%
3U U U SID
Description
E06-0294-009 Battle 9, W e i 8, Sample E06-0294-010 Bottle 10. W e i 8 Sample Duplicate E06-0294-011 Bottle 11, W ell 8, Field Matrix Spke Low E06-0294-012 Bottle 12. W ell 8, Field Matrix Spike High ______ Average Concentration (ng/mL) %RPD
PFBSP
PFHS's
PROS
Concentration
(ng/mL)
^R ecovery
0.0251
NA
< 0 .0 2 5 0 0 .1 3 7 1.05
NA 114 103
0.0257
Concentration
(ng/mL)
^R ecovery
0.0518
NA
0 .0 5 0 8
NA
0 ,1 7 6
123
1.09 103
0.0513 ng/mL 1.9%
C oncentration (ng/mL)
%Recavery
0.596
NA
0.647
NA
0.981
- NR
T .5 9 '
95.9
0.622 ng/mL 8.2%
NfA = NotApplicable
NR = Not Reported = Endogenous concentration ct analyte exceeded 2x the spiked level and therefore an accurate recovery cannot be calculated
(1) Sample results for PFBA were determined following method E TS -8-11.0. This method ts currently net covered on tie laboratory's scope of accreditation to ISO/1EC 17025:1999. (2) Sample results for NFPA, PFHA, PFOA, PFBS, PFHS, and PFOS vwre determined foHowing method ETS-8-154.1
(3) One of two field matrix spikes prepared and analyzed did not m eet method criteria of 100% 3 0 % . As one of the two matrix spikes did meet method criteria, the data quality is not affected.
(4) RPD exceeded 15% acceptance criteria.
p. 15
PAGE 15 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
Table 11. Well 9 Results
-------- -- ------------------------------ ---- ..............
-----
PFBAm
NFPATM
3M UM SID
EOS-0294-013 E 0 6 -0 2 9 4 -0 1 4 E 0 6 -0 2 9 4 -0 1 5
Description Bottle 13, W ell 9, Sample Bottle 14, W ell 9, Sample Duplicate Bottle 15, Well 9, Reid Matrix Spike Low
Concentration (ng/mL) t %RPD
Concentration
(ng/mL)
^R ecovery
2.04
NA
202
NA
2.21 NR
I 3.15
114
2.03 ng/mL 0.79%
Concentration
(no/mL)
^R ecovery
0.0895
NA
0.0914
NA
0.169
79.3
1.1 102.0
0.0904 ng/mL 11%
PFHATM
PFO*
Concentration
(ng/mL)
^R ecovery
0.225
NA
0.235
NA
0.384
NR
1.27
103
0.230 no/mL 4.3%
Concentration
(ng/mL)
^R ecovery
0.726
NA
0 652
NA
0.949
85.2
1.51 80.5
0.689 no/mL 11%
3M LIMS ID
Description
E06-0294-013 Bottle 13, Well 9, Sample E06-Q29+-014 Bottle 14, W ell 9, Sample Duplicate E06-0294-015 Bottle 15, W ell 9, Field Matrix Spike Low F n 6-0 ? M -n i6 Bottle 16. W ell 9. Retd Matrix Soike High
Averagt Concentration (ng/mL) %RPD
PFBSn
PFHSi*
PFO,S "
Concertfratfon
Concentration
(ng/mL)
^R ecovery
(no/mL)
^R ecovery
0.0521 NA 0.106 NA
0.0492
NA
0.166
115
1.08 103
0.0506 ng/mL 5.7%
0.103
NA
0.211
105
1.14 103
0.10* no/mL 19%
Concentration
(ng/mL)
^R ecovery
0.567
NA
0.544 0.633
NA 91.9
1.51 94.5 0.556 ng/mL 41%
NfA = Not Applicable NR = Not Reported = Endogenous concentration of analyte exceeded 2x ttie spiked level and therefore an accurate recovery cannot be calculated. (1) Sample results for PFBAwere determined following method ETS-6-11.0. This method is currently not covered on the laboratory's scope of accreditation to ISO/1EC 17025:1999.
(2) Sample results for NFPA, PFHA, PFOA, PFBS, PFH S, and PFOS were determined following method ETS-8-154.1
p. 16
PAGE 16 OF 21
p. 17
r I
3MENVIRONMENTAL LABORATORY REPORT NO. E06-0294
Table 12. Well 1 Results
3M UM SID
Description
E06-0294-020 Bottle 20, W ell 1, Sample E06-0294-021 Bottle 21, W ell 1, Sam ple Duplicate E06-0294-022 Bottle 22. W ell 1. Field Matrix Spike Low E06-0294-023 Bottle 23, W ell 1, Field Matrix Spike Hioh
Avenge Concentration (ng/mL) %RPD
PFBA1"
Concentration (ng/mL)
0 .2 9 5
NA
0.287
NA
0.416
126
1.35
107
0.291 ng/mL 3.0%
NFPA1*
PFHATM
PFOA
Concentration
(ng/mL)
%Recoverv
<0.0248
NA
<0.0248
NA
0.100
101
1.01 102
0.0249 ng/mL
Concentration
Concentration
(ngAnL)
%Recoverv
(ng/mL)
`/Recovery
<0.0252
NA
0.0781
NA
<0.0252
NA
0.0801
NA
0 .1 4 2
*141
0.172
91.1
1.18
117
0.924
8 2 .8
<0.0252 ng/mL
0.0791 ng/tnL 2.5%
3M UMS ID
DescripBon
E06-0294-020 Botile 20, W ell 1, Sample E06-0294-021 Botile 21, W ell 1, Sample Duplicate E06-0294-022 Botile 22, W ett 1, Field Matrix Spike Low E0&O294O23 Botte 23. W ell 1, Fiald Matrix Spire High
Average Concentration (ng/mLi V.RPD
PFBSTM
PFHS?*
PFOS
Concentration
Concentration
(ng/mL)
%Recovery
(ng/mL)
%Recovery
<0.0250
NA <0.0252 NA
<0.0250
NA
0 .0 9 7 8
9 7 .9
1.12
112
<0.0250ng/mL
<0.0252
NA
0.117
116
1.19
109
<0.0252 ng/mL
Concentration
(ng/mL)
% fleco verv
0 .0 4 1 5
NA
0.0381 0-128 1.06
NA 87.3 101
- 0.0398 ng/mL 8.5%
W A = Nol Applicable
(1) Sample results for PFBA were determined following method E TS -8-11.0. This method is currently nol covered on (he laboratory's scope o f accreditation lo S O IE C 17025:1999.' (2) Sample results for NFPA, PFHA, PFOA, PFBS, PFH S, and PFOS were determined following method ETS-8-154.1 (3) One of two field matrix spikes prepared and analyzed did not m e t method criteria of 100% 30% . As one of the two matrix spikes did m eet method criteria, the data quality is not
affected.
PAGE 17 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. E06-Q294
Table 13. Well 2 Results
3M UM SID
Descriptor}
E 06-0294-024 Bottle 24, Well 2, Sample E06-0294-025 Bottle 25, W ell 2, Sam ple Duplicate E06-0294-026 Bottle 26. Well 2, Reid Matrix Spike Low EO&0294-Q27 Bottle 27. W ell 2. Field Matrix Spike H gh
Averagt Concentrator} (ng/mL) t %RPD
PFBAn
NFPAm
pfha!v
pfop!*
Concentration
(ng/mL)
%Recovery
0.381
IMA
0.373
NA
0 .4 8 9
NR
1.47 111
0.377 ngfmL 2.0%
Concentrator}
(ng/mL)
Recovery
<0.0248
NA
< 0 .0 2 4 8
NA
0 .1 1 7
118
. .1 .0 5 .
106
<0.0248ng/mL
Concentrator}
Concentration
(nofmL)
'Recovery
(ng/mL) %Recovery
0 .0 3 7 6
NA 0.0931 NA
0 .0 3 6 4
NA
0.0915
NA
0 .1 5 7
119
0.222
127
1.19
114
0.838
73.1
0.0370ng/mL 3.2%
0.0923 ng/m Lt 1.7%
3MUMS ID
Description
E0O-0294-024 Bottle 24. W ell 2. Sample E 06-0294-025 Bottle 25, W ell 2, Sam ple Duplicate E06-0294-026 Bottle 26, W ell 2, Field Matrix Spike Low E06-0294-027 Bottle 27. Well 2. Field Matrix Spike High
Average Concentration (ng/mL) %RPD
PFBSf*
PFHS
PROS
Concentration
(ng/mL)
'Recovery
<0.0250
NA
<0.0250
NA
0.107
107
1.11 111
<0.0250 ng/mL
Concentra (fon
(ng/mL)
%Recovery
<0.0252
NA
< 0 .0 2 5 2
NA
0 .1 1 8
117
1.02
101
<0.0252ng/mL
C oncentration
(ng/mL)
'/Recovery
0.0387
NA
0 .0 3 2 4
NA
0 .1 3 5
9 8 .5
0.961
91.6
0.0356ng/mL i 18%
M/A = Not Applicable NR = Not Reported = Endogenous concentration of analyte exceeded 2x ihe spiked level and therefore an accurate leixjvesy cannot be calculated. (1) Sam ple results for PFBA were determined following method ETS-S-11.0. This method is currently not covered on the laboratories laboratory's soope of accreditation to ISO/IEC
17025:1999. (2) Sample results for NFPA, PFHA, PFOA, PFBS, PFHS, and PFOS were determined following method ETS-8-154.1. (3) RPD exceeded 15% acceptance criteria.
p. 18
PAGE 18 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
Table 14. Well 3 Results
PFBA1
3M UM SID
Description
06-0294-028 Bottle 28, W e 3, Sam ple
iE 0 6 -0 2 9 4 -0 2 9 E 0 6 -0 2 9 4 -0 3 0
Bottle 29, W ell 3, Sam ple Duplicate Bottle 30, W e i 3, Field Matrix Spike Low
E06-Q294-031 Bottle 31, W efl 3, Field Matrix Spike High
Average Concentration (ng/mL) t %RPo
Concentration
= = 222 y= 0.0949
NA
0.0855
NA
0.213
124
1.19 111
0.0902 ng/mL 10%
NFPA
PFHA
PFOA
Concentration
(ng/mLj
`Recovery
< 0 .0 2 4 8
NA
<0.0248
0.101
NA
102
0.967
98
<0.0248 ng/mL
Concentration
Concentration
(ng/mL)
'Recovery
(ng/mL)
`/Recovery
< 0 .0 2 5 2
NA 1 <0.0254
NA
< 0 .0 2 5 2
NA
<0.0254
NA
0 .1 0 6 108
105 0.0745 73.0 107 0.671
<0.0252 ng/mL
<0.0254 ng/mL
PFBS
PFWS
PROS
3M LUIS ID
Description
E06-0294-028 Bottle 28. W ell 3, Sample E06-0294-029 Bottle 29, W ell 3, Sam ple Duplicate E06G 294-030 Bottle 30. W ell 3, R eid Matrix Spike Low E06-0294-031 Botte 31, W ell 3, Field Matrix Spike High _ Average Concentration (ng/mL) %RPD
C o n c e n tra tio n
Concentration
(ng/mL)
%Recovery
(ng/mL)
'Recovery
<0.0250
NA <0.0252 NA
<0.0250
NA <0.0252 NA
0 .1 1 5
115
1.05 105
<0.0250 ng/mL
o .io i
100
1.04
103
<0.0252 ng/mL
Concentration
(ng/mL)
`/Recovery
<0.0252
NA
<0.0252
NA
0 0 7 3 4
72.7
0.881
87.2
< a 0 2 5 2 ing/mL
N/A = Not Applicable
(1) Sample results for PFBA were determined following method ETS-8-11.0. This method is currently not covered on the laboratory's scope of accreditation to ISO /IEC 17025:1999. (2) Sample results for NFPA, PFHA. PFOA, PFBS, PFHS, and PFOS were determined following method ETS-8-154.1 (3) Since the low FMS spike recovery met acceptance criteria and the measured values were below LOQ the data is arvptnhip
p. 19
PAGE 19 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
Table 15. Trip Blank Results
PFBAm
NFPATM
PFHATM
PFOATM
3M LIM SID E06-0294-017 E 06-0294 -Q 1 8 E 0 6- 2 94-019
Description
Concentration (ng/mL)
Bottle 17, NA, Trip Blank Bottle 18. NA, Trip Blank Matrix Spike Low Bottle 19, NA, Trip Blank Matrix Spike High
<0.0494 0 .1 0 3 1.08
"Recovery
NA 105 109
Concentration (ng/mL)
0.0295**'
0.097 1.00
Recovery NA
P>68.2 98
Concentration (ng/mL)
<0.0252 0 .1 0 4 1.10
Concentration
ARecovery
(ng/mL)
^R ecovery
NA
<0.0254
NA
103
0.053
104
109
0 821
80.5
PFBSf*
PFHSt*
PFCSTM
3M UM SID
E 0 6 -0 2 S 4 -0 1 7 06-0294 -01 B E 0 6 -0 2 S 4 -0 1 9
O es crfp tfo n
Bottle 17. NA, Trip Blank Bottle 18. NA, Trip Blank Matrix Spike Low Bottle 19, NA, Trip Blank Matrix Spike High
Concentration (ng/mL)
< 0 .0 2 5 0 0 .1 1 4 1.02
Concentration
%R e c o v e ry
(ng/mL)
NA <0.0252
114 0.0987
102 1.08
; Concentration
^R ecovery
(ng/mL)
N 97.7
<0.0252 0.0364
107 1.05
Recovery NA 7 2 .4
.. 104
N/A = Not Applicable (1) Sample results for PFBA were determined following method ETS-8-11.0. This method is currently not covered on the laboratories laboratory's scope o f accreditation to ISO /IEC
17025:1999. (2) Sample results for NFPA, PFHA, PFOA, PFBS, PFHS, and PFOS were determined following method ETS-8-154.1
(3) FMS or trip blank spike recovery did not m eet method criteria at 100% 30% . (4) The trip blank contained a trace amount of NFPA above the LOQ (0.0248 ng/mL). Samples have not been corrected for the trip blank concentration.
.
p. 20
PAGE 20 OF 21
3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0294
jr-.T.s?q-T
Laboratory control spikes w ere used to determine the analytical method accuracy and precision for all
analytes. The accuracy and precision were then used to estimate the method uncertainty for the
results. Field m atrix spike recoveries demonstrated that the analytical method was appropriate for the
given sample m atrix. A nalysis was successfully completed following 3M Environmental Laboratory
m ethod ETS 8-11.0 "Determination of C4 - C8 Highly Fluorinated A dds, AJcohols. Amides, and
Sulfonates in W ater by High Performance Liquid Chromatography/Mass S pectrom etry^nd ETS-8-
154.1 'D eterm ination of Perfiuorinated A dds, Alcohols, Amides, and Sulfonates in W ater by Solid
Phase Extraction and High Performance Liquid Chnomatography/Mass Spectrometry". Analytical
results are reported in Table 1 o f this report
'
p pp i
All remaining sample and associated project data (hardcopy and electronic) w ill be archived according to 3M Environmental Laboratory standard operating procedures.
William K. Reagen, Ph D., Environmental Laboratory Technical Manager D a te The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project.
Date
PAGE 21 OF 21
