Document ZBK5qOKNX5QVZNR61m3aoLGr0
3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Final Report
Analysis of PFBAS, aPmFOplAes, PfrFoBmS3,MPFDOeSc,atFuBr,SAAla, baanmd aFOSA in Aqueous
3M Decatur NPDES Permit Number AL0000205: Quarterly FC Monitoring of Outfall DSN001; 1st Quarter 2008 Sampling
Laboratory Request Number: E08-0010
Method Requirement: 3M Method ETS-8-154.3
Report Date - February 18,2008
Testing Laboratory
3M EHS Operations 3M Environmental Laboratory
Building 260-5N-17 Maplewood, MN 55144-1000
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
1IF
& CCREDITEDI C ertificate #2052-01
The testing reported herein meet the requirements of ISO/IEC17025-2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001/ISO 9002 (2000).
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
3IV1 E nvironm ental Laboratory
3M Environmental Laboratory Technical Manager: William K. Reagen, Ph.D. 3M Principal Analytical Investigator and Report Author: Susan Wolf
Analytical Report E08-0010
3M Decatur NPDES Permit Number AL0000205: Quarterly FC Monitoring of Outfall DSN001; 1st Quarter 2008 Sampling
Report Date: February 18,2008
1 Introduction/Summary
The 3M Environmental Laboratory prepared and analyzed outfall samples collected by Enersolv Corporation personnel on January 16, 2008, from 3M Decatur location DSN001. Samples were returned to the 3M Environmental Laboratory for analysis of Perfluorobutanoic acid (PFBA), Perfluorooctanoic acid (PFOA), Perfluorobutane sulfonate (PFBS), Perfluorooctane sulfonate (PFOS), Perfluorobutanesulfonylamide (FBSA) and Perfluorooctanesulfonylamide (FOSA) under laboratory project number E08-0010.
The 3M Environmental Laboratory prepared sample containers for one sampling location. The sample set consisted of a field sample, field sample duplicate, low field spike, mid field spike, and high field spike. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 200 mL. Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution containing all analytes prior to being sent to the field for sample collection.
Samples were prepared and analyzed using ETS-8-154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". Samples were extracted on January 23, 2008. Due to field matrix spikes not meeting method acceptance criteria for PFBA on sampling location DSN001, this sample set was re-extracted on February 4, 2008 analyzed for PFBA only on February 5, 2008.
Table 1 summarizes the sample results using the analytical method identified above. All results for quality control samples prepared and analyzed with the samples will be reported and discussed elsewhere in this report.
I 1L ACCREDITED!
The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001/ISO 9002 (2000).
C ertificate #2052-01
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 1. Sample Results Summary*1'
3M LIMS ID
E08-0010-001 E08-0010-002
Sample Description
p f b a (2) Concentration
(n g /m L )
DSN001, Sample DSN001 Sample Duplicate
8.20 8.97
Average %RPD Sample/Sample Dup
8.59 9.0
PFOA Concentration
(n g /m L )
2.77 3.01
2.89 8.3
PFBS C o n c e n tra tio n
(n g /m L )
30.5 33.0
31.8 7.9
3M LIMS ID
E08-0010-001 E08-0010-002
Sample Description
PFOS Concentration
(n g /m L )
FBSA Concentration
(n g /m L )
FOSA C o n c e n tra tio n
(n g /m L )
DSN001, Sample DSN001 Sample Duplicate
9.65 9.68
35.7 0.947 38.5 0.955
Average %RPD Sample/Sample Dup
9.67 0.31
37.1 7.5
0.951 0.84
{1) Samples were extracted by solid phase extraction using method ETS-8-154.3 and analyzed on January 23,2008. The analytical method uncertainties associated with the reported results are as follows: PFBA 100% 19%, PFOA100% 17%, PFBS 100% 21%, PFOS 100% 9.8%, FBSA 100% 14%, and FOSA 100% 17%.
(2) Samples were re-extraction for PFBA only on February 4,2008 and analyzed on February 5,2008. Samples were diluted 1:10 prior to extraction.
2 Methods - Analytical and Preparatory
2.1 Methods
Analysis was completed following 3M Environmental Laboratory method ETS-8-154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry".
2.2 Sample Collection
Samples were collected in NalgeneTM (high-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample 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 were returned to the laboratory at ambient conditions on January 17, 2008.
2.3 Sample Preparation
All samples, calibration standards, and associated quality control samples were extracted using ETS-8154.3. Briefly, 40 mL of sample were loaded onto a pre-conditioned Waters 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).
2.4 Analysis
All samples and quality control samples were analyzed for six target analytes using high performance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters,
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below.
Table 2. Instrument Parameters.
Instrument Name Analytical Method followed Liquid Chromatograph Guard column Analytical column Injection Volume Mass Spectrometer Ion Source Electrode Polarity Software
ETS Stan ETS-8-154.3 Agilent 1100 Betasil C18 (2.1 mm X 50 mm), 5p Betasil C18 (2.1 mm X 100 mm), 5g
5 pL Applied Biosystems API 4000
Turbo Spray Turbo ion electrode
Negative Analyst 1.4.2
Table 3. Liquid Chromatography Gradient Program.
Step Number
0 1 2 3 4 5
Total Time (min)
0 1.0 14.5 15.5 16.5 20.0
Flow Rate (pL/min)
300 300 300 300 300 300
Percent A (2 mM ammonium acetate)
90.0 90.0 10.0 10.0 90.0 90.0
Percent B (Methanol)
10.0 10.0 90.0 90.0 10.0 10.0
Table 4. Mass Transitions
Analyte
Mass Transition Q1/Q3
PFBA
213/169
413/369
PFOA
413/219
413/169
PFBS
299/80 299/99
499/99
PFOS
499/80
499/130
FBSA
298/78
FOSA
498/78
The individual transitions were summed to produce a "total ion chromatogram" (TIC),
which was used for quantitation.
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
3 Data Analysis
3.1 Calibration
Calibration standards were prepared by spiking known amounts of stock solutions containing the analytes of interest into 40 ml. of laboratory reagent water. Each spiked water standard was then extracted in the same manner as the collected samples. A total of twelve spiked standards ranging from 0.025 ng/mL to 25 ng/mL (nominal) were prepared. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data were 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 coefficient (r) was greater than 0.995 for all analytes.
The stock standard used to prepare the calibration standards contained neat materials that have expired. The expired neat materials were not the analytes of interest in this report. The expired neat materials have been sent out for recertification and are not expected to have any impact on the results contained in this report.
3.2 Limit of Quantitation (LOQ)
The LOQ as defined in method ETS-8-154.3 is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate blanks. The nominal LOQ for PFOA, PFBS, PFOS, FBSA and FOSA was 0.025 ng/mL, and 0.050 ng/mL and 1.00 ng/mL for PFBA.
Table 5. Limit of Quantitation (LOQ).
Analysis Date
Analysis Date
1/23/08
2/5/08
Analyte
LOQ, ng/mL
LOQ, ng/mL
PFBA
0.0502
1.00(1)
PFOA
0.0249
NA
PFBS
0.0249
NA
PFOS
0.0250
NA
FBSA
0.0252
NA
FOSA
0.0250
NA
(1) Samples were diluted 1:10 prior to extraction. Analytical LOQ was 0.100 ng/mL
3.3 Continuing Calibration
During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. Method acceptance criteria is 100% 25%. All CCVs met method criteria.
3.4 Blanks
Four types of blanks were prepared and analyzed with the samples: method blanks, solvent blanks, field/trip blanks, and equipment blanks. Each blank result is reviewed and used to evaluate method performance to determine the LOQ for each analyte.
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
3.5 Lab Control Spikes (LCSs)
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 carbon-filtered matrix matched blank water to produce the desired concentration. The spiked water samples were then extracted and analyzed in the same manner 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 8-154.3. The method acceptance criteria states that the average recovery of all LCS be between 80%-120% with a RSD <20%. All LCS samples met method acceptance criteria and were used in the determination of analytical uncertainty where applicable. The following calculations were used to generate data in Table 6.
Calculated Concentration
100LCS Percent Recovery =
%
Spike Concentration
LCS% RSD = standard deviation LCS replicates 100% average LCS recovery
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 6. Lab Control Spike Results.
Extracted 1/23/08
Lab ID LCS-080123-1 LCS-080123-2 LCS-080123-3 LCS-080123-4 LCS-080123-5 LCS-080123-6 Average %RSD
PFBA
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
0.201
0.191
0.201 0.201 5.02 5.02 5.02
0.192 0.197 4.94 4.86 4.83
96.8% 1.6%
%Recovery
95.2 95.3 98.1 98.4 96.8 96.3
PFOA
PFBS
Spiked
Calculated
Spiked
Calculated
Concentration Concentration
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
(ng/mL)
(ng/mL)
0.199
0.213
107
0.199
0.217
0.199
0.225
113
0.199
0.219
0.199
0.23
116
0.199
0.215
4.98 5.14 103 4.99 5.01
4.98 5.35 107 4.99 4.88
4.98
5.10
102
4.99
A ll
109% 4.8%
105% 5.4%
%Recovery
109 110 108 100 97.8 95.6
Extracted 1/23/08 Lab ID
PFOS
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
LCS-080123-1 LCS-080123-2 LCS-080123-3 LCS-080123-4 LCS-080123-5 LCS-080123-6
0.200 0.200 0.200 5.00 5.00 5.00
0.203 0.212 0.205 5.00 4.94 4.95
101 106 103 99.8 98.8 99.0
Average %RSD
102% 2.8%
FOSA
FBSA
Spiked
Calculated
Spiked
Calculated
Concentration Concentration
Concentration Concentration
(ng/mL)
(ng/mL)
%Recovery
(ng/mL)
(ng/mL)
0.202
0.212
105
0.200
0.209
0.202 0.202 5.04 5.04 5.04
0.214 0.206 5.14 4.81 4.79
106 102 102 95.4 95.1
0.200 0.200 5.01 5.01 5.01
0.212 0.209 5.22 5.02 5.11
102% 4.1%
104% 2.1%
%Recovery
104 106 104 104 100 102
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 6 continued. Lab Control Spike Results.
Extracted 2/4/08
PFBA
Lab ID
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
LCS-080204-1 LCS-080204-2 LCS-080204-3 LCS-080204-4 LCS-080204-5 LCS-080204-6
0.201 0.201 0.201 5.02 5.02 5.02
0.212 0.204 0.209 5.19 4.98 5.13
Average %RSD
102% 2.3%
%Recovery
106 101 104 103 99.2 102
3.6 Analytical Method Uncertainty
Analytical uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS-12-012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by factor of 2, which correspond with a confidence level of 95%. A minimum of twenty data points is needed to determine method uncertainty by this method.
Table 7. Analytical Uncertainty.
Analyte PFBA PFOA PFBS PFOS FBSA FOSA
Number of data points used for determining uncertainty 50 50 50 50 29 48
Standard Deviation
9.37 8.41 10.7 4.92 7.20 8.71
Method Uncertainty 100%19% 100%17% 100%21% 100%9.8% 100%14% 100%17%
3.7 Field Matrix Spikes (FMS)
Low, mid, and high field matrix spikes were 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 analytes 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 the section 4 of this report.
FMS Recovery - (amPle Concentration of FMS - Average Concentration: Field Sample & Field Sample Dup.), 1 Spike Concentraton
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 6 continued. Lab Control Spike Results.
Extracted 2/4/08 Lab ID
PFBA
Spiked
Calculated
Concentration Concentration
(ng/mL)
(ng/mL)
L C S -08 02 04-1 L C S -0 8 0 2 0 4 -2 L C S -08 02 04-3 LCS-0802Q4-4 L C S -08 02 04-5 LCS-0802Q4-6 Average %RSD
0.201 0.201 0.201 5.02 5.02 5 .0 2
0 .2 1 2 0 .2 0 4 0 .2 0 9 5 .1 9 4 .9 8 5 .1 3 102% 2.3%
%Recovery
106 101 104 103 9 9 .2 102
3.6 Analytical Method Uncertainty
Analytical uncertainty Is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS-12-012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by factor of 2, which correspond with a confidence level of 95%. A minimum of twenty data points is needed to determine method uncertainty by this method.
Table 7. Analytical Uncertainty.
Analyte PFBA PFOA PFBS PFOS FBSA FOSA
Number of data points used for determining uncertainty 50 50 50 50 29 48
Standard Deviation
9.37 8.41 10.7 4.92 7.20 8.71
Method Uncertainty 100%19% 100%17% 100%21% 100%9.8% 100%14% 100%17%
3.7 Field Matrix Spikes (FMS)
Low and high field matrix spikes were 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 analytes 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 the section 4 of this report.
FMS Recovery - ^ ample Concentration of FMS - Average Concentration: Field Sample & Field Sample Pup.), ^ Spike Concentrator!
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 8. Field Matrix Spike Concentrations
Location
Description
Low Field Matrix Spike
DSN001 Mid Field Matrix Spike
High Field Matrix Spike
Low Field Matrix Spike
Trip Blank Mid Field Matrix Spike
High Field Matrix Spike
Final Concentration (ng/mL) PFBA PFOA PFBS PFOS FBSA FOSA 0.251 0.249 0.249 0.250 0.252 0.250 5.02 4.98 4.99 5.00 5.04 5.01
100 99.5 99.7 100 101 100 0.251 0.249 0.249 0.250 0.252 0.250 5.02 4.98 4.99 5.00 5.04 5.01
100 99.5 99.7 100 101 100
4 Data Summary and Discussion
The tables below summarize the sample results and field matrix spike recoveries for sample location DSN001 as well as the Trip Blank. An equipment blank sample was also collected in the field. The table provides the average concentration and the relative percent difference (RPD) of the sample and sample duplicate. Results and average values are rounded to three significant figures according to EPA rounding rules. Percent relative difference (%RPD) values are rounded to two significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Field matrix spikes meeting the method acceptance criteria of 30%, demonstrate that the method is appropriate for the given matrix.
Trip Blank - The low, mid, and high FMS recoveries for FOSA were analyzed twice with recoveries that did not meet method acceptance criteria, with recoveries ranging from 53.8% to 72.3%. However, the sample FMS recoveries did meet method acceptance criteria for FOSA, therefore, no further action was taken.
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 9. DSN001 Results
3M L IM S ID
Description
E08-0010-001 DSN001, Sample E08-0010-002 DSN001, Sample Duplicate E08-0010-003 DSN001, Field Matrix Spike Low E08-0010-004 DSN001, Field Matrix Spike Mid E08-0010-005 DSN001, Field Matrix Spike High
Average Concentration (ng/mL) %RPD
PFBAm
PFOAm
PFBS121
Concentration
(ng/mL)
%Recovery
8.20 8.97
NA NA
(3) NC
12.6
79.9
105 95.9
8.59 ng/mL 9.0%
Concentration
(ng/mL)
%Recovery
2.77 NA
3.01 NA
3.03 NC
7.81 98.9
105 103
2.89 ng/mL 8.3%
Concentration
(ng/mL)
%cRecovery
30.5 NA
33.0 NA
(4) NC (4) NC 140 109
31.8 ng/mL 7.9%
3M U M S ID
Description
E08-0010-001 DSN001, Sample E08-0010-002 DSN001, Sample Duplicate E08-0010-003 DSN001, Field Matrix Spike Low E08-0010-004 DSN001, Field Matrix Spike Mid E08-0010-005 DSN001, Field Matrix Spike High
Average Concentration (ng/mL) %RPD
PFOSf21
f b s a ,2>
FOSA121
Concentration
(ng/mL)
%Recovery
9.65
NA
9.68 9.53
NA NC
13.8 82.6
104 94.2
9.67 ng/mL 0.31%
Concentration
(ng/mL)
%Recovery
35.7 NA
38.5 NA
(4) NC (4) NC 140 102
37.1 ng/mL 7.5%
Concentration
(ng/mL)
%Recovery
0.947
NA
0.955
NA
1.19 NC
5.65 93.8
99.8 98.7
0.951 ng/mL 0.84%
NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. (1) Samples for PFBA were diluted 1:10 and extracted on February 4,2008 and analyzed on February 5,2008. The LOQ for PFBA on this sample is 1.0 ng/mL. (2) Samples were extracted on January 23,2008 and analyzed on January 23,2008. (3) Sample not extracted since the FMS level was not appropriate as compared to the sample concentration. (4) Sample concentration exceeded calibration range. A dilution of the sample was not prepared since the FMS level was not appropriate as compared to the sample concentration.
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
Table 10. Trip Blank Results
3M U M S ID E08-0010-009 E08-0010-006 E08-0010-007 E08-0010-008 E08-0010-010 E08-0010-007; rerun E08-0010-008; rerun E08-0010-009; rerun
Description Trip Blank Sample Trip Blank FMS Low Trip Blank FMS Mid Trip Blank FMS High Equipment Blank Trip Blank FMS Low Trip Blank FMS Mid Trip Blank FMS High
PFBA
PFOA
PFBS
Concentration (ng/mL)
<0.0502 0.223 4.70 106
<0.0502 0.252 4.98 109
Concentration
%Recovery
(ng/mL)
NA 88.8 93.5 105 NA 100 99.1 108
<0.0249 0.286 5.41 112
<0.0249 0.297 5.13 107
%Recovery NA 115 109 113 NA 119 103 108
Concentration (ng/mL)
<0.0249 0.266 4.88 94.8
<0.0249 0.288 5.32 109
%Recovery NA 107 97.9 95.1 NA 116 107 109
3 M U M S ID E08-0010-009 E08-0010-006 E08-0010-007 E08-0010-008 E08-0010-010 E08-0010-007; rerun E08-0010-008; rerun E08-0010-009; ream
Description Trip Blank Sample Trip Blank FMS Low Trip Blank FMS Mid Trip Blank FMS High Equipment Blank Trip Blank FMS Low Trip Blank FMS Mid Trip Blank FMS High
PFOS
FBSA
FOSA
Concentration (ng/mL)
<0.0250 0.248
4.70 95.0 <0.0250 0.241 4.78 95.9
Concentration
%Recovery
(ng/mL)
NA <0.0252
99.1 0.250
93.9 4.43 94.9 91.0 NA <0.0252 96.3 0.273 95.5 4.87 95.8 98.5
%Recovery NA 99.2 87.9 90.3 NA 108 96.6 97.7
Concentration (ng/mL)
<0.0250 0.175
3.43 53.9 <0.0250 0.181 3.62 56.9
%Recovery NA 69.9
68.5(1) 53.8(1)
NA 72.3 72.3 56.8(1)
N/A = Not Applicable (1) Field matrix spike did not meet method acceptance criteria of 100% 30%.
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3M ENVIRONMENTAL LABORATORY REPORT NO. E08-0010
5 Conclusion
Laboratory control spikes were 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 matrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix. Analysis was completed following 3M Environmental Laboratory method ETS-8154.3 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates In Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". Analytical results are reported in Table 1 of this report.
q Data / Sample Retention
All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures.
7 Signatures
ClifftoryBUacoby, P h.D /3M Technical Reviewer
/rFd. zmt Date
--------------------------------J& z
William K. Reagen, Ph.D., 3M Environmental Laboratory Technical Manager
Date
The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project.
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