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3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0381 Final Report Analysis of PFBA, PFOA, PFBS, PFOS, FBSA, and FOSA in Aqueous Samples from 3M Decatur, Alabama 3M Decatur NPDES Permit Number AL0000205: Quarterly FC Monitoring of Outfall DSN001; June 2007Sampling Laboratory Request Number: E07-0381 Method Requirement: 3M Method ETS-8-044.1 & ETS-8-154.1 Report Date -September 12,2007 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 E30 (CCREDITED The testing reported herein meet the requirements o f ISO/IEC 17025-1999 ' `General Requirements fo r the Competence o f Testing and Calibration Laboratories" , in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance w ith ISO 9001/ISO 9002 (1994). Certificate #2052-01 PAGE 1 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0381 3M Environmental Laboratory 3M Environmental Laboratory Technical Manager: William K. Reagen, Ph.D. 3M Principal Analytical Investigator: Susan Wolf Report Author: Susan W olf Analytical Report E07-0381 3M Decatur NPDES Permit Number AL0000205: Quarterly FC Monitoring of Outfall DSN001; June 2007 Sampling Report Date: September 12, 2007 1 Introduction/Summary The 3M Environmental Laboratory prepared and analyzed outfall samples collected by Enersolv Corporation personnel on June 19, 2007, from 3M Decatur location DSN001. Samples were returned to the 3M Environmental Laboratory for analysis of perfluorobutanoic acid (PFBA), periluorooctanoic acid (PFOA), perfluorobutane sulfonate (PFBS), perfluorooctane sulfonate (PFOS), perfluorobutanesulfonylamide (FBSA) and perfluorooctanesulfonylamide (FOSA) under laboratory project number E07-0381. The 3M Environmental Laboratory prepared sample containers for one sampling location. Each 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 450 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-8-044.0 "Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis" on July 20, 2007. Due to QC not meeting method acceptance criteria for PFOS, FBSA and FOSA, samples were extracted and analyzed on August 2, 2007 using ETS-8-154.1 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in Water by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". ETS-8-154.1 is specifically listed under the laboratory's A2LA scope of accreditation; however, ETS-8-044.0 currently is not. 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 Ia c c r e d it e p I The testing reported herein meet the requirements of ISO/IEC 17025-1999 "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 (1994). Certificate #2052-01 PAGE 2 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 1. Sample Results Summary (1) 3M LIM S ID S am ple D escriptio n P F B A (1) C oncentration (ng/m L) P F O A (1) P F B S (1) p f o s (2) F B S A *2' Concentration Concentration Concentration Concentration (ng/m L) (ng/m L) (ng/m L) (ng/m L) f o s a (2) C oncentration (ng/m L) E07-0399-001 DSN001, Sample E07-0399-002 DSN001 Sample Duplicate 3.80 3.59 2.67 25.3 7.64 7.30 Not Reported 2.45 24.3 7.37 6.89 Not Reported Average 3.70 2.56 24.8 7 .5 1 <3) 7 .1 0 N o t R e p o rte d *4' % R PD Sam ple/Sam ple Dup 5.7 8.6 4.0 3.6 5.8 NA NA = Not Applicable (1) Sample results for PFBA, PFOA, and PFBS were analyzed by direct Injection using method ETS-8-044.0 on June 20,2007. ETS-8-044 .0 is not included on the 3M Environmental Laboratory's ISO 17025 scope of accreditation. The analytical method uncertainties associated with the reported results are as follows: PFBA 29%, PFOA 23%, and PFBS 21%. Refer to Sections 3 and 4 for data acceptance criteria and discussion. (2) Sample results for PFOS, FBSA, and FOSAwere analyzed by solid phase extraction using methodETS-8-154.1 on August 2, 2007. ETS-8-154.1 is included on the 3M Environmental Laboratory's ISO 17025 scope of accreditation. The analytical method uncertainties associated with the reported results are as follows: PFOS 22% and FBSA 30%. (3) The analytical uncertainty for PFBS is 52%. See section 4 of the report for additional information. (4) Sample results not reported. Field matrix spike recoveries were <50%. PAGE 3 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 2 Methods - Analytical and Preparatory 2.1 Methods Analysis for PFBA, PFOA, and PFBS was completed following 3M Environmental Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis". Analysis for PFOS, FBSA and FOSA was completed following 3M Environmental Laboratory method ETS-8-154.1 "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 (low-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 July 6, 2007. 2.3 Sample Preparation 2.3.1 ETS-8-044.0 An aliquot of a well mixed sample was removed for analysis and placed in an autovial. 2.3.2 ETS-8-154.1 All samples, calibration standards, and associated quality control samples were extracted on June 27, 2007 using a modified procedure of ETS-8-154.1. 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). Lab control spikes extracted in the same manner cross-valldate all the method modifications/deviations from ETS-8-154.1. See Section 3.5 for additional information. Modifications from ETS-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 sample as possible. 2.4 Analysis All samples and quality control samples were analyzed for seven target analytes using high performance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. PAGE 4 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 2. Instrument Parameters. Instrum ent Nam e A nalytical M ethod follow ed Liquid C hrom atograph G uard colum n A nalytical colum n Injection V o lu m e M ass Spectrom eter Ion Source E le c tro d e P o la rity Softw are ETS Stan ETS-8-044.0 Agilent 1100 Betasil C18 (4.6 mm X 150 mm), 5 u Betasil C18 (4.6 mm X 100 mm), 5u 100 uL Applied Biosystems API 4000 Turbo Spray Turbo ion electrode Negative Analyst 1.4.2 ETS Stan ETS-8-154.1 Agilent 1100 Prism RP (2.1 mm X 50 mm), 5 u Betasil C18 (2.1 mm X 100 mm), 5p 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 Step Number 0 1 2 3 4 5 Total Time (min) 0 0.5 11.0 13.5 13.6 17.0 Total Time (min) 0 2.0 14.5 15.5 16.5 20.0 ETS-8-044.0 Flow Rate (p L /m in ) Percent A (2 m M am m onium acetate) 1000 97.0 1000 1000 97.0 5.0 1000 5.0 1000 97.0 1000 97.0 ETS-8-154.1 Flow Rate (pL /m in ) Percent A (2 m M am m onium acetate) 300 90.0 300 90.0 300 10.0 300 10.0 300 90.0 300 90.0 Percent B (M e th a n o l) 3.0 3.0 95.0 95.0 3.0 3.0 Percent B (M e th a n o l) 10.0 10.0 90.0 90.0 10.0 10.0 PAGE 5 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 4. Mass Transitions Analyte M ass Transition Q 1 /Q 3 PFBA 213/169 413/369 PFOA 413/219 413/169 PFBS 299/80 299/99 499/99 PFOS 499/80 499/130 FBSA 298U8 FOSA 498/78 Note: D w ell tim es vary with m ethod and instrum ent a n d are recorded with the raw data for each run 3 Data Analysis 3.1 Calibration 3.1.1 ETS-8-044.0 Calibration standards were prepared by spiking known amounts of the stock solution containing the target analytes into 50 mL of carbon-filtered matrix matched water. An aliquot of the spiked water standard was removed for analysis. A total of eleven spiked standards ranging from 0.025 ng/mL to 10 ng/mL (nominal) were analyzed. 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. Method calibration accuracy requirements o f 10025% (10030% for the lowest curve point) were met with the exception of the 0.05 ng/mL curve point for PFHA. This point was disabled as the backcalculated concentrations did not meet method acceptance criteria. The correlation coefficients (r) were greater than 0.990 for all analytes. The FOSA reference material used for preparing the matrix spikes and analytical standards expired on 3/14/2005. The reference standard has been sent out for recertification. The purity o f this reference material is not expected to change, based on the known stability of this compound and results of previously re-certified compounds. 3.1.2 ETS-8-154.1 Calibration standards were prepared by spiking known amounts of stock solutions containing the analytes of interest into 40 mL of carbon-filtered matrix matched water. Each spiked water standard was then extracted in the same 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 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. PAGE 6 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 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 0.999 for PFOS. 3.2 Limit of Quantitation (LOQ) The LOQ as defined in method ETS-8-44.0 and ETS-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, PFOA, PFBS, PFOS, and FOSA was 0.025 ng/mL, and 0.030 ng/mL for FBSA. 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 Three types of blanks were prepared and analyzed with the samples: method blanks, solvent blanks, and field/trip blanks. Each blank result is reviewed and used to evaluate method performance to determine the LOQ for each analyte. 3.5 Lab Control Spikes (LCSs) 3.5.1 ETS-8-044.0 Low and high lab control spikes were prepared and analyzed in triplicate. The LCS samples were prepared by spiking known amounts of the analyte into 50 mL of carbon-filtered matrix matched water to produce the desired concentration. The spiked water samples were then analyzed in the same manner as the samples. The LCS results were used to determine overall method uncertainty in Section 3.6. The method acceptance criteria states that the average recovery of LCS be 100% 20% with a RSD <20%, when evaluated independently at each concentration level. The method acceptance criteria was not met for the mid-level LCS set for PFBA, which had an average recovery of 121%. All LCS were used in the determination of method analytical uncertainty. 3.5.2 ETS-8-154.1 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 8-154.1. The method acceptance criteria states that the individual LCS recovery be between 100%25% with a RSD<15% when both concentration levels are evaluated collectively. 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 5. LCS Percent Recovery Calculated Concentration * 1 Spike Concentration standard deviation LCS replicates LCS% RSD = 100% average LCS recovery PAGE 7 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 5. Lab Control Spike Results11*. ETS-8-044 PFBA Lab ID Spiked C a lc u la te d Concentration Concentration (n g /m L ) (n g /m L ) LCS-070719-1 LCS-070719-2 LCS-070719-3 LCS-070719-4 LCS-070719-5 LCS-070719-6 0.199 0.199 0.199 3.98 3.98 3.98 0.234 0.234 0.228 4.84 4.79 4.76 Low -Level LCS Average % RSD M id-Level LCS Average % RSD 117% 1 .5 % 1 2 1 % 1 .0 % (2) VoRecovery 118 118 115 122 120 120 PFOA Spiked Calculated Concentration Concentration (n g /m L ) (ng /m L ) 0.200 0.200 0.200 4.00 4.00 4.00 0.221 0.222 0.22 4.57 4.47 4.49 110% + 0.52% 113% 1 .0 % PFBS VoRecovery Spiked C a lc u la te d Concentration Concentration (ng /m L ) (n g /m L ) 110 0.200 0.222 111 0.200 0.222 110 0.200 0.224 114 3.99 4.04 112 3.99 4.08 112 3.99 3.98 111% 0 .52% 101% 1 .1 % VoRecovery 111 111 112 101 102 99.7 ETS-8-154 Lab ID PFOS Spiked C a lc u la te d Concentration Concentration (ng /m L ) (n g /m L ) VoRecovery FBSA Spiked Calculated Concentration Concentration (n g /m L ) (n g /m L ) FOSA % R eco very Spiked Calculated Concentration Concentration (ng /m L ) (n g /m L ) VoRecovery LCS-070802-1 LCS-070802-2 LCS-070802-3 LCS-070802-4 LCS-070802-5 LCS-070802-6 0.201 0.201 0.201 5.04 5.04 5.04 0.212 0.216 0.204 5.240 5.110 5.460 106 0.201 0.203 101 0.199 0.208 104 107 0.201 0.223 111 0.199 0.202 102 102 0.201 0.192 95.4 0.199 0.201 101 104 5.02 5.39 107 4.97 4.94 99.3 101 5.02 5.22 104 4.97 4.90 98.5 108 5.02 5.41 108 4.97 4.97 100 Average % RSD 105% 2.7% 105% 5 .4% 101% 2 .0 (1) PFBA, PFOA and PFBS were prepared and analyzed by method ETS-8-044. PFOS, FBSA, and FOSA were prepared and analyzed by ETS-8-154. (2) Average LCS recovery was outside of method acceptance criteria of 100% 20% PAGE 8 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 3.6 Analytical Method Uncertainty 3.6.1 ETS-8-044.0 The analytical uncertainty was determined by using laboratory control sample recovery data. The standard deviation was calculated for the set of accuracy results (in %) obtained for the control and field matrix spike samples. The expanded uncertainty is calculated by multiplying the standard deviation by factor of 2, which correspond with a confidence level of 95%. Table 6. Analytical Method Uncertainty Analyte PFBA PFOA PFBS Number of data points used for determining uncertainty 50 50 50 Standard Deviation 14.5 11.5 10.7 Method Uncertainty 100% 29% 100% 23% 100% 21% 3.6.2 ETS-6-154.1 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. This method of determining method uncertainty was applied to the PFOS results. In those instances where there was an insufficient number of laboratory control samples where available (FBSA and FOSA), field matrix spike recoveries were used to determine analytical uncertainty. Sampling locations with field matrix spikes meeting the acceptance criteria of 100% 30% were assigned an analytical uncertainty of 30%. A n a ly te PFOS N um ber o f data points used for determ ining uncertainty 50 S ta n d a rd D eviation 11.0 M ethod U ncertainty 100% 22% 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 (Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample Pup.) t ^qqq, Spike Concentraton PAGE 9 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 7. Field Matrix Spike Concentrations L o c a tio n D escription Low Field Matrix Spike 1 Mid Field Matrix Spike High Field Matrix Spike Low Field Matrix Spike Trip Blank Mid Field Matrix Spike High Field Matrix Spike PFBA 0.248 4.97 99.4 0.248 4.97 99.4 Final C on centration (ng/m L) PFOA PFBS PFOS FBSA 0.250 0.249 0.252 0.251 5.00 4.99 5.04 5.02 100 99.8 101 100 0.250 0.249 0.252 0.251 5.00 4.99 5.04 5.02 100 99.8 101 100 FOSA 0.249 4.97 99.4 0.249 4.97 99.4 4 Data Summary and Discussion The tables below summarize the sample results and field matrix spike recoveries for the eight locations as well as the Trip Blank. Each 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. DSN001 - All analytes had recoveries for the high field matrix spike around 50%. For all analytes, with the exception of PFBS, the mid level field matrix spike was most appropriate as compared to the sample result, therefore, no adjustment was made to the analytical uncertainty. For PFBS, the analytical uncertainty has been expanded accordingly. FOSA -Both the sample and trip blank had field matrix spike recoveries <50%. Therefore, no sample results were reported for this compound. PAGE 10 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 8. DSN001 Results 3M LIM S ID D e s c rip tio n E07-0399-001 E07-0399-002 E07-0399-003 E07-0399-004 E07-0399-005 DSN001, Sample DSN001, Sample Duplicate DSN001, Field Matrix Spike Low DSN001, Field Matrix Spike Mid DSN001, Field Matrix Spike High Average Concentration (ng/mL) % RPD PFBAm P F O A 111 PFBS*" Concentration (n g /m L ) % R eco very 3.80 NA 3.59 NA 3.93 NC 9.13 109 60.2 56.6(2' 3.70 ng/mL 5.7% Concentration (ng /m L ) % R eco very 2.67 NA 2.45 NA 2.78 NR 8.04 110 51.8 49.2(2) 2.56 ng/m L 8.6% Concentration (n g /m L ) % R eco very 25.3 NA 24.3 NA --70.4 45.7(2) 24.8 ng/mL 4.0% PFOSm F B S A ,2> FOSAm 3M LIM S ID Description E07-0399-001 E07-0399-002 E07-0399-003 E07-0399-004 E07-0399-005 DSN001, Sample DSN001, Sample Duplicate DSN001, Field Matrix Spike Low DSN001, Field Matrix Spike Mid DSN001, Field Matrix Spike High Average Concentration (ng/mL) % RPD Concentration (n g /m L ) % R eco very 7.64 NA 7.37 8.21 12.4 54.3 NA NC 97.2 46.5<3) 5.25 ng/mL 4 .2 % C o n c e n tra tio n (ng /m L ) % R eco very 7.30 NA 6.89 7.62 11.7 54.8 NA NC 92.0 47.5(3) 7.16 n g/m L 6 .0 % <4> C o n c e n tra tio n (n g /m L ) % R ecovery Not reported N o t R e p o rte d (SI NA = Not Applicable NC = Not Calculated; Endogenous sample concentration greater than 2x spike level. (1) PFBA, PFOA and PFBS were prepared and analyzed by method ETS-8-044. (2) PFOS, FBSA, and FOSA were prepared and analyzed by ETS-8-154. (3) Field matrix spike did not meet method acceptance criteria of 100% 30%. (4) The analytical uncertainty for PFBS is 52%. (5) The sample result for FOSA could not be reported as the field matrix spike recoveries were <50%. PAGE 11 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 Table 9. (1>Trip Blank Results 3 M U M S ID E07-03 99-009 E07-0399-006 E07-0399-007 E07-0399-008 E07-0399-010 Description Trip Blank Sample Trip Blank FMS Low Trip Blank FMS Mid Trip Blank FMS High Equipment Blank p f b A ') PFOA"' PFBS1" C o n c e n tra tio n (n g /m L ) <0.0248 0.287 5.73 111 <0.0248 % R eco very NA 115 115 111 NA Concentration (n g /m L ) <0.0249 0.283 5.60 106 <0.0249 % R eco very NA 113 112 106 NA Concentration (n g /m L ) <0.0249 0.279 4.91 97.8 <0.0249 % R ecovery NA 112 98.4 98.0 NA 3M L IM S ID D e s c rip tio n E07-0399-009 Trip Blank Sample E07-0399-006 Trip Blank FMS Low E07-0399-007 E07-0399-008 E07-0399-010 Trip Blank FMS Mid Trip Blank FMS High Equipment Blank P F O S ,2> f b s a ,2> FOSA Concentration (n g /m L ) <0.0252 0.216 4.91 89.0 <0.0252 Concentration % R eco very (n g /m L ) NA <0.0301 85.8 0.227 97.5 88.4 NA 5.01 89.8 <0.0301 % R eco very NA 90.5 99.9 89.5 NA Concentration (n g /m L ) <0.0249 0.0769 2.11 29.3 <0.0249 % R ecovery NA 30.9(3) 42.4(3) 29.5,3) NA N/A = Not Applicable (1) (1) PFBA, PFOA and PFBS were prepared and analyzed by method ETS-8-044. (2) PFOS, FBSA, and FOSA were prepared and analyzed by ETS-8-154. (3) Field matrix spike did not meet method acceptance criteria of 100% 30%. PAGE 12 OF 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0399 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-8044.0 "Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis" for PFBA, PFOA, and PFBS. Analysis for PFOS, FBSA, and FOSA was completed following ETS-8154.1 "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 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. Quality Assurance Representative '07 Date PAGE 13 OF 13