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P-1 3 7 Z > 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 Final Report Analysis of PFO A and PFO S in Aqueous Sam ples from 3M Cordova W ells 1 , 2 , 3 , 4 , 5, and Drinking W ater Distribution Laboratory Request Number E06-0302 Method Requirement: 3M Method ETS-8-154.1 (modified) R e p o rt D ate - 0 8/16/06 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 P h o n e :(6 5 1 )7 7 8 -5 1 5 0 Fax: (651) 778-7203 The testing reported herein meet the requirements of ISO/1EC17025-1999 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2062-01. Testing that complies with this International Standard also operate in accordance with ISO 9001/ISO 9002 (1994). Certificate #2052-01 PAGE 1 OF 14 P-2 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 3M E nvironm ental Lab oratory 3M Environmental Laboratory Technical Manager. W illiam K. Reagen, Ph.D. 3M Principal Analytical Investigator Susan W olf Report A uthor Susan W olf AnalyticalReport EQ6-0302 Report Date: August 16,2006 ;23W fr'|&,r The 3M Environmental Laboratory prepared arid analysed w ater samples collected by Weston Solutions personnel on August 2,2006, from Cordova w ells 1 ,2 ,3 ,4 , 5, and Drinking W ater Distribution. Samples were returned to the 3M Environmental Laboratory for analysis o f perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFCS) under laboratory project num ber E06-0302. Analysis was completed following 3M Environmental Laboratory method ETS-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 Spectrometry". The 3M Environmental Laboratory prepared sets o f sample containers for six sampling locations. Each sample set consisted o f a field sample, field sample duplicate, low field spike, mid field spike, and high field spike. W ell 3 had an additional mid-high field m atrix spike prepared. Each empty container was marked with a "fill to here" line that corresponded to a final volume o f 450 mL. Containers reserved for field m atrix spikes were fortified with an appropriate m atrix spike so*ution containing all analytes prior to being sent to the field for sample collection. Samples were prepared on August 3,2006 and analyzed on August 3 and 4,2006. Table 1 lists the sampling locations and corresponding '/.ell ID # that w ill referenced throughout the report Table 2 summ arizes the sample results using the analytical method identified above. A ll results for quality control samples prepared and analyzed with the samples w ill be reported and discussed elsewhere in this report Table 1. Sampling Locations SamplingLocation Building 11; W e ill Building 12; W ell 2 Building 13; W ell 3 Building 24; W d l 4 Building 37; W ell 5 Bldg 1; DW Distribution See field sampling raw data file. Feld SamplingCodem CILGW PW 11 CILG W PW 12 CILG W PW 13 CILG W PW 24 CILG W PW 37 CILPW PW L1 Ia c c h e d it b p ! Certificate #2052-01 The testing reported herein meet the requirements of ISO/IEC 17025-1999 "General Requirements for 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 with ISO 9001/ISO 9002 (1994). PAGE 2 OF 14 P-3 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 Table 2. Sample Results Sum m ary(1> 3MUMSID SampleDescription : PFOS PFOA *>; Concentration (ng/mL). Concentration JngfinL) E06-0302-068 W ei 1; Sample 060802 0.386 0.181 ` I E06-0302-069 W ei 1; Sample Duplicate 060802 Avratf.We'1 r'--! %RPDSampWSample Dup Well t 0.462 3 !4 2 4 ^' 'f 18" 0.250 . - Jo .2 16 32 E06-0302-073 E06-0302-074 W ei 2; Sample 060802 ' * Well 2; Sample Duplicate 060802 Average Well 2 %RPD Sampie/Sample DupWell i .7 2 ' ' 3.10 2.91 ' ! 0.692 -0.777 *8 . 0.735 ___ 11 .____, E06-0302-078 W el3; Sample 060802 - 7 T .-b ''A 11-'7 E06-0302-079 W ei 3; Sam ple Duplicate 060802,, , .p tr-.n ,,, - US' 1 :'' '.'X .O' ' '> ' ' MW AverageWet3 !' v x t1 .8 %Rf*DSampie/SampleDupWelli ' ' T ;-' 1.8 E06-0302-083 Vie14; Sample 060602 ` c f; s : :v 1.7 E06-0302-034 W ei 4; Sample Duplicate 06080 ' ' ' 1.73 .v O rif'S P lJlH * a a; 0 .r,.v :-vq ' ' 1 . ' i- v ' r ; - o.43' : n 0.3&8 ' r..? - ,.j. ,1 .7 2 d r " ' '? v, %RPDSampie/Sample Dup WeilA: ' . >1.0 E06-0302-088' W e i 5; Sample 060802 ; K. 0.152 r E06-0302-089 W e i 5; Sample Duplicate 00802 i 0.166 ' ' ` ' -I > 1' Average Well3 0.159 %RPD Sampie/Sample Dup Will i 8.8 .... ^0.,417;-,(-,h -- 9 .1 -* '"v. !0.601 ' : 0;S62 ;o 6 9 , 33 E06-0302-093 E06-0302-094 '' DW Distribution; Sample 0606Q2 , , DW Distribution; Sample Dupicate 060802 ' Average DWDistribution %RPDSample/SampleDup DWDistribution - 3.10 3.13 3.11 1.1 1.30. 1.29 1.30 1.1 N/A = Not AppScable (1) The analytical method uncertainties are as follows: PFOA is 100% 17%, PFOS is 100% 24% . Refer to Sections 3 and 4 fo r data acceptance criteria and discussion. (2) The Relative Percent Difference between the Sampie/Sample Duplicate exceeds 15%. !'` 2.1 Methods , Analysis was completed following 3M Environmental Laboratory method ETS-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 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 fo r field m atrix spikes were - spiked in the laboratory w ith a known volum e o f an appropriate m atrix spiking solution containing the analytes o f interest Collected sample bottles wre rtumd to the laboratory at am bient conditions on August 3,2006. ' PAGE 3 OF 14 P-4 3MENVIRONMENTAL LABORATORY REPORT NO. E06-0302 2.3 Sample Preparation All samples, calibration standards, and associated quality control samples were extracted using a m odified procedure o f ETS-8-154.1. Briefly, 40 mL o f 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 o f methanol. This extraction procedure concentrates the samples by a factor o f e ig h t (Initial volum e = 40 mL, .final volum e = 5 mL). Lab control spikes extracted in the same manner crogs-vaiidate all the method modifications/deviations from ETS-8-154.1. See Section , 3.6 fo r additiona` l inform ation. 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 colum ns were not rinsed with 40% methanol after sample loading. A fter 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. 2.4 Analysis A ll samples and quality control sam ples were analyzed for PFOA and PFOS using high performance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Pertinent instrum ent parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below. Table 3. Instrument Parameters. Instrum ent Name A n a lytica l M ethod follow ed L iq u id C hrom atograph G uard colum n A n a lytica l colum n Injection Volum e M ass Spectrom eter Ion Source E le c tro d e P olarity Softw are E T S G inger ETS-8-154.1 Agilent 1100 Prism RP (2 mm X 50 mm), 5 um Betasil C18 (2.1 mm X 100 mm), 5 um 5uL Applied Biosystems API 5000 Turbo Spray Z-spray Negative Analyst 1.4.1 PAGE 4 OF 14 P -5 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 Table 4. Uquid Chromatography Gradient Program. ,, r '' ' ,W 'i E T 8 G in g e r________________________________ i . ________ .n-, . : " . ao .,>( S to p Number 0 1 2 3 ... 4 S' . . . Total time i (min) : Flow Rat4 > (tiYmtn) r*3 ' . Q too Percent'A ;!- i* : PercentB mMAmmoniumacetate)' ' - (Median61) ' "> o .b : 1.0 300 ' ' 30.0 ` ' 4 0 0 ' 11.0 300 i ..... . . 10-0 , , ; \ 90.0-, T-y ,. 13.5 14.0 , 300 , 300 - .... 10.0 ,. 60.0 yj ' 900, -,v . .,4 0 0 ,,. . 17.0, , : - , 300 . v y , : ' 60.0 - ; v .: 40.0-, : i r. :.!i ,r ~* ?P, Table 5. Mass Transitions .. ,, ,, ^ ^ . .. , \ 1 *,/ - " Analyte M M Transition Q1/Q3 413/369 PFOA 413/219 413/169 499/99 PFOS 499/80 499/130 in -- , : > .n - Dwelt Time (msec) " Et^Ginger 150 150 150 150 150 150 '.i'1. t vrViV'M': 3.1 Calibration ' Calibration standards were prepared by spiking known amounts o f stock solutions containing th e ' analytes o f interest into 40 mL o f ASTM type I water. Each spiked w ater standard was then extracted in the same m anner as the collected samples. A total of twelve spiked standards ranging from 0.025 ng/m L 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 o f each curve point Each curve point was quantitated using the overall calibration curve and reviewed fo r accuracy. Method calibration accuracy requirements o f 10025% (10030% for the lowest curve point) were m e t The correlation coefficients (r) w ere greater than 0.998 for each analyte. 3.2 Limit of Quantitation (LOQ) The LOQ for this analysis, as defined in method ETS-8-154.1, is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirem ents and which the area counts are at least tw ice those o f the appropriate blanks. The nominal LOQ for PFOA, and PFOS was 0.025ng/mL. 3.3 System Suitability The 1.0 ng/mL extracted-calibration standard was analyzed five tim es a t the beginning and end o f the analytical sequence to dem onstrate overall system suitability. All compounds m et the acceptance PAGE 5 OF 14 P -6 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 criteria o f less than 5% relative standard deviation (RSD) for peak area and less than 2% RSD for retention tim e fo r the opening and closing system suitability injections. 3.4 Continuing Calibration During the course o f the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrum ent response and the initial calibration curve were still in control. All CCVs m et method criteria. 3.5 Blanks Three types o f 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 determ ine the LOQ ter each analyte. The trip blank (E06-0302-098) contained trace amounts o f both PFOA and PFOS. However, the amounts detected were at least a factor o f 3x less than the sample with the lowest reportable value for either PFOA or PFOS. Samples have not been corrected for the trip blank concentration. 3.6 Lab Control Spikes (LCSs) Low and high lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spiking known amounts o f the analytes into 40 mL o f ASTM Type I water to produce the desired concentration. The spiked w ater samples were then extracted and analyzed in the same manner as the samples. Analysis o f triplicate LCSs at the two specified levels cross-validates the analytical method as used here fo r any m odifications/deviations from ETS 8-154.1. Additionally, LCS results are used to determ ine overall method uncertainty (see Section 3.7). Eight LCS at three different levels were prepared with the samples. LCS-060803-1 prepared at a concentration o f 0.203 ng/mL, had a recovery o f 173% for PFOA. This sample results was determ ined to be a statistical outlier. The other two LCS prepared at the same level m et method criteria and dem onstrate the analysis w as in control. The following calculations were used to generate data in Table 6. Calculated Concentration LCS Percent Recovery = 100% Spike Concentration standard deviation LCS replicates . ^ average LCS recovery PAGE 6 OF 14 3M ENVIRONMENTAL LABORATORY REPORT NO. 0 6-0302 Table 6. (1)Lab Control Spike Results. LabID LCS-060803-1 LCS-060803-2 LCS-060803-3 LCS-060803-4 LCS-060303-5 LCS-060803-6 LCS-060803-7 LCS-060803-8 LCS-060803-8 Average+ %RSD PFOS - PFOA Spiked Calculated Spiked j UpCURR--W Concentration Concentration Concentration Concentration (ngtoiL) (ngfaiL) %Recovery (ng/mL) (ng/mL) %Recoverv 0.2 ppb Lab Control Spice 0.201 0.212 105% 0.203 0.352 173%P 0.2 ppb Lab Control Spice 0.201 0.204 102% 0.203 0.212 104% 0.2 ppb Lab Control Spice 0.201 0.206 102% 0.203 0.213 105% Z 0 ppb Lab Control Spice 2.0 ppb Lab Control Spice 2.01 2.01 2.02 101% 2.03 1.96 97.5% 2.03 , 2.08 2.02 102% 100% 2.0 ppb Lab Control Spice 10 ppb Lab Control Spice 10 ppb Lab Control Spice 10 ppb Lab Control Spice 2.01 10.1 10.1 10.1 1.90 94.5% 9.47 93.8% 9.88 97.8% 9.80 97.0% 99.0% 3.9% 2.03 1.94 10.2 10.1 i 10.2 , 10.5 1 0 .2' 10,5- - 101% 3.1% 95.6% 99.0% 103% m% ,T, Cr NA = Not applicable (1) AH results and average values listed to three significant figures according to EPA rounding rules. %R3D values given to two significant figures. Due to rounding, values may vary slightly from those in the raw data. -> ^ i (2) LCS recovery did not meet method criteria of 100%25% and was determined to be a statistical outlier. ' .. 3 r. PAGE 7 OF 14 p.8 3M ENVIRONMENTAL LABORA TORY REPORT NO. E06-0302 3.7 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 o f accuracy results (in %) obtained fo r the Q C samples. The expanded uncertainty is calculated by m ultiplying the standard deviation by factor o f 2, v.tiich correspond with a confidence level o f 95%. Table 7. Analytical Method Uncertainty A nalyte PFOA PFOS N um ber o f data pointa used fo r determ ining uncertainty - 203 189 Standard D eviation 8.604 11.89 M ethod U ncertainty 100% +/-17% 100% +/- 24% 3.8 Field Matrix Spikes (FMS) Low, mid, and high field m atrix spikes were collected at each sampling pcirtt to verify that the analytical method is applicable to the collected matrix. Field m atrix spikes are generated by adding a measured volum e o f field sample to a container spiked by the laboratory with the target analytes prior to shipping sample containers for sample collection. Field m atrix spike recoveries within method acceptance criteria o f 10030% confirm that "unknown' components in the sample m atrix do not significantly interfere with the extraction and analysis o f the analytes o f interest. Field m atrix spikes are presented in the section 4 o f this report. (Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample P u p )* * ' OniLii P n n M n l r e l A n PAGE 8 OF 14 P -9 3M ENVIRONMENTAL LABORATORY REPORT NO. 0 6 -0 3 0 2 Table 8. Field Matrix Spike Concentrations L o c a tio n D escription W ei 1 Low Field M atrix Spike M kl Field M atrix Spike High Field M atrix Spike Low Field M atrix S p ite W ei 2 M kl Field M atrix S p ike, High Field M atrix S p ite ... Low Field Matrix Spike W ei 3 Mkt Field M atrix Spike M M -HIgh Field M atrix Spate H g h Field M atrix S p ite l r, to w Field M atrix Spike ` W e li 1' : , .... ,f s- i ' r i M ki Field M atrix Spike High Field M atrix Spike' Low R eid M atrix Spike W e is Mid Field M atrix Spike High Field M atrix Spike lo w Field M rilrix Spike D W Distribution Mkl Field M atrix Spike High Field M atrix Spike Trip Blank Low Field M atrix Spike M kl Field M atrix Spike High Field M atrix Spike H n a i S pike C oncentratiO n/ngrm L) 'P F O A .' 'V f PFOS 0 .2 0 3 0 .5 0 8 ' ' :- ` 0 .2 V ' 0 .5 0 3 1.02 i.o f ' : 0 .5 0 8 : ' 'J 1 .5 3 ' 0 .5 0 3 - .d '- , . " ^ ~ . V f. 5 08 ` ' 5.03 ' 2 .4 8 2 .4 8 . 5 .0 8 5 .0 3 1 0 .2 , 1 5.2 . - . , .-1 5 .1 v a t.;' * / ' 0.203' - I ' : ' 6.201 1 0 .5 0 8 1 ' " 0.503 r - !: ' ` ' ' ' ' 2 .0 3 " . ' ' .. < 2.1 " 203 , ,0.201 . , 0 .5 0 8 0 .5 0 3 2 .0 3 2.01 1.02 ' 1.01 1 2 .0 3 2.01 5 .0 8 5.03 0 .2 0 3 2 .0 3 1 0 .2 0.201 2.01 10.1 This was the third sampling round fo r these locations. The first sampling set collected on 5/18/06 was not reported due to QC requirements. The second sampling set collected on 7/27/06 was not reported due to sampling errors. Additional information on these two sampling events can be found in the raw data file. Tables 9 - 1 5 summarize the sample results and field matrix spike recoveries fo r the seven locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference (RPD) o f 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 o f rounding, values may vary slightly from those listed in the raw data. Well 1 For W ell 1, the RPD for both PFOA and PFOS did not m eet method criteria o f <15%. Additional samples from this location would need to be collected to determ ine if the variability is statistically re le v a n t PAGE 9 OF 14 3M ENVIRONMENTAL LABORA TORY REPORT NO. 0 6-03 02 Table 9. Well 1 Results FFOA PFOS 3MUMSID Description E06-03C2-068 W e ll; Sample 060802 E36-0302-069 W ei 1; Sample Duplicate 060802 E06-0302-070 W e ll; Field M atrix Spike Low 060802 E06-03C2-071 W ei 1; Field M atrix Spike Mid 060602 E06-0302-072 W ei 1; Field Matrix Spike Nigh 060802 A verace Concentration (ng/mL) %RPD Cor.certyation Concentration (ng/m %Recovery (ng/mL) `/Recovery 0.181 NA 0.386 NA ' 0.250 NA 0.462 NA 0.475 128 0.656 NR - 0.705 95.3 0.847 84.1 1.22 98.5 0.216ngtoiL32%m 1.23 80.1 0.424 ng/mL18%m NA = Not Applicable NR = Not Reported - Endogenous concentration ofanalyte exceeded 2x the spiked level and therefore an accurate recovery cannot be calculated. - . (1) RPD exceeded method acceptance criteria of <15%. Additional samples from this location would need to be collacted to determine If the variability is statistically relevant Field matrix spire recoveries were determined using the average concentration detected In the sample and sample duplicato. Table 10. Well 2 Results 3MUMSID Description E06-0302-073 W ei 2; Sample 060802 E06-0302-074 W ei 2; Sample Duplicate 060802 E06-0302-075 W ei 2; Field M atrix Spike Low 060802 E06-0302-076 W ei 2; Field M atrix Spke Mid 060802 E06-0302-077 W ei 2; Field M atrix Spke High 060802 Average Concentration (ngAnL) %RPD PFOA PFOS Concentration Concentration (ng/mL) HRecovery (ng/mL) %Recovery 0.692 NA 0.777 . NA 1.17 86.3 2.05 85.9 5.06 85.2 0.735 ng/mL1 11% 2.72 NA 3.10 NA 3.26 NR 4.24 87.5 6.95 80.3 2.91 ng/mL i 13% N A * Not Applicable NR - Not Reported * Endogenous concentration of analyte exceeded 2x the spked level and therefore an accurate recovery cannot be calculated. PAGE10OF14 p . 11 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 Table 11. Well 3 Results . tc, PFOA PFOS 3MUMSID Description ... Concentration Concentration (ngftnl) ^R e co ve ry, (ngfmU %Recover/ E06-0302-678 We 3; Sample 060802 . ,, 4 .^9 ' NA ,f > 11.7 NA E 06-0302-079 E06-0302-080 E06-0302^081 W ei 3;,Sample Duplicate 060802 r,; . f. W ei 3, Field Matrix S p ite Low 060802 ; : W ei 3; Field Matrix Spike Mid 060802 -f ~ f 4.68 6.66 9.*i4 in *--?s Li! , m . jf ; -;f .. 96.6. : 11.9 V 13.5 `M 16-7 NA NR NR E06-0302-082 W ei 3; Field Matrix S piro Mid High 060802 r NC , , NA < .299 90.1 E06-0302-102 W ei 3; Reid M atrix S pire High 060802 Average Concentration (ng/mL) 1 %RPD ^ ____ N______ NA 4.64 ngAnLt 1.9% , 23.7. 78.5 11.8ng^mLi 1.8% NA - N otApplicable ,K r . - ; .> < * NR Not Reported = Endogenous concentration o f analyte exceeded 2x the spiked level and therefore an accurate recovery canhotbecalculated.'1 . m -! 5 ' ' 5 ' NC = Not Calculated * Sample concentration was outside of the range of calibration. ' . ' ' ' r t.! . ' ` '1`* r.j . Table 12. Well 4 Results 3MUMSID Description E06-0302-083 Well 4; Sample 060802 E 060302-084 W ei 4; Sample Duplicate 060802 E06-0302-085 W ei 4; Field Matrix Spike Low 060802 E06-0302-086 W ei 4; Field M atrix Spire Mid 060802 E06-0302-087 W ei 4; Field Matrix S pite High 060802 Average Concentration(n&mL) t %RPD PFOA > PFOS Concentration Concentration (ngtotU MRecovery {ngfinQ %Recovery 0.436 NA 1.71 NA 0.398 0.604 NA ' 1.73 NR 1.89 NA NR 0.887 92.5 2.18 86.8 0.417ng/rriL 9.1% 2.04 NR 3.35 80.8 ' 1.72ng/mL 1.0% ' N A = Not Applicable NR = Not Reported " Endogenous concentration of analyte exceeded 2x the spired level and therefore an accurate recovery cannot be calculated. PAGE 11 OF 14 p. 12 3M ENVIRONMENTAL LABORATORY REPORT NO. 0 6-03 02 Table 13. Well 5 Results PFOA PFOS 3MUMS ID Description E06-0302-G88 Well 5; Sample 060602 : E06-0302-089 W ell 5; Sample Duplcat 060802 E06-0302-090 W ell 5; Field Matrix S pire Low 060802 E06-0302-091 We 5; Field Matrix S pire Mid 060602 E06-0302-092 W ei 5; Field Matrix S pire High 060802 Average Concentration (ng/mL) t %RPD Concentration Concentration (ng/mL) Recovery (ngAnL) %Recoverv - 0.501 " NA ' 0.152 NA 0.582 NA u 0.166 NA " 0.797 NR 0.357 98^6 1.05 90.9 0.576 82.9 1 2.16 71.2 0.591 ng/mL 1 3.3% 1.94 38.3 0.159 ng/mL 8.8% . NA = Not Applicable - '.r.- ; l.v. . f t . i : , >- ; r ...- i';`j . ^ .j: v' .. ... NR Not Reported = Endogenous concentration o f analyte exceeded 2x the spired level and therefore an accurate recovery cannot be calculated. Table 14. Drinking Water (DW) Distribution Results PFOA PFOS 3MIM SID Description E6-0302-093 DW Distribution; Sample 060802 E06-0302-094 DW Distribution; Sample Suplicate 060802 E06-0302-095 DW Distribution; Field Matrix Spike Low 060802 E06-0302-096 DW Distribution; Field Matrix Spike Mid 060802 E06-0302-097 DW Distribution; Field Matrix Spike High 060802 Average Concentration (ng/mL) t %RPD Concentration (ng/mL) 1.30 1.29 Recovery NA NA 2.10 79.0 3.04 86.0 5.69 86.6 1.30ng/mLt 1.1% Concentration (ng/mU R ecovery 3.10 NA 3.13 NA 3.82 NR 4.83 85.4 7.44 86.0 3.11 ng/mL 1 1.1% N/A= Not Applicable NR = Not Reported = Endogenous concentration o f analyte exceeded 2x the spired level and therefore an accurate recovery cannot be calculated. PAGE 12 OF 14 p. 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 Table 15. Trip Blank Results<1> PFOA PFOS 3MUMSID Description E06-0302-098 Trip Blank 060802 E06-0302-099 Trip Blank Spike Low 06Q802 E06-0302: ip 0 Trip Blank Spike Mid 060802 E06-0302-101 Trip Blank Spike High 060802 c' Concentration Concentration (ng/'mL) %Rec6verv . (ng/iriL) %Recoverv , 0.0615 . NA ... t . 0 0498 . NA ,, 0.248 92.0 , 0.231 ,,9 0 .2 1.98 - 1C-2 94.3 99.0 >,.* 192 . . 9.85. 92.9 97.1 N/A = Not Applicable ' . (1) The trip blank amounts detected were at least a factor of 3x less than the sample with the lowest reportable value for either PFOA or PFOS. Trip blank spikes recoveries were corrected for trip blank concentration. ' PAGE 13 OF 14 p. 14 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0302 Laboratory control spikes are used to determ ine the analytical method accuracy and precision for both analytes and are used to determ ine the method uncertainty for each analyte. Field m atrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix. Analysis w as successfully completed following 3M Environmental Laboratory m ethod ETS-8-154.1 "Determination o f Perfluorinated Adds, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extraction and High Performance Liquid Chromatography/Mass Spectrometry". Analytical results are reported in Table 2 o f this report. All remaining sam ple and assodated project data (hardcopy and electronic) w ill be archived according to 3M Environmental Laboratory standard operating procedures. tr Susan T. W olf, 3M Senior C h Date W illiam K. Reagen, Ph.D., 3M Environmental Laboratory Technical M anager Date The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this project. Quality Assurance I te n ta tiv e PAGE 14 OF 14