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3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 Amended Final Report Analysis of PFBS, PFHS, PFOS and PFOA in W ater Samples Collected at 3M Guin Laboratory Request Number: E05-0662 Method Requirement: 3M Method ETS-8-154.1 (modified) 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 3M CONFIDENTIAL Page 1 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 3WI E nvironm ental Laboratory 3M Environmental Laboratory Manager: William K. Reagen, Ph. D. 3M Technical Lead and Report Author: Michelle Malinsky, Ph.D. 3M Environmental Laboratory Professional Service Personnel Cindy Carlson, Pace Analytical, Lab Ops Kevin Eich, Qualify Associates Marlene Having, Pace Analytical, Lab Ops ValtabhaTantry, Pace Analytical, Lap Ops Amended Analytical Report E05-0662 Water Samples from 3M Guin November 23,2005 9M p3 HU The 3M Environmental Latxjratory extracted and analyzed water samples from two locations within the 3M Guin facility. Samples were collected by Weston Solutions personnel on September 15,2005. The first sampling location was a surface water sample designated as SW in the sample description. The second location was a municipal water line located in the 3M Guin plant designated as PW. Samples were returned to the 3M Environmental Laboratory for analysis of perfluorobutane sulfonate (PFBS), perOuorohexane sulfonate (PFHS). perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA) and analyzed under laboratory project number EO5-0662 using 3M Environmental Laboratory Method ETS 8-154,1 "Determination o f Perfluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extractions arid High Performance Liquid Chromatography/Mass Spectrometry". The 3M Environmental Laboratory prepared sets of sample containers for the two sampling locations. Each sample set consisted of a field sample, field sample duplicate, low field spike (0.10 ng/mL) mid fiefd field spike (1.0 ng/mL) and high field spike (10 ng/mL). Each empty container was marked with a "fill to here" line and was fortified with a surrogate spike or an appropriate matrix spike solution containing the surrogate and the target analytes prior to being sent to the field for sample collection, Additionally, a set of trip blanks was also prepared and sent to the field with the other sample collection containers. Samples were extracted on September 22,2005 and analyzed on September 23,2005. Table 1 below summarizes the sample results. All resuits for quality control samples prepared and analyzed with the samples will be reported and discussed elsewhere in this report. 3M CONFIDENTIAL Page 2 of 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 T able 1. ,1,5am ple R esults Sum m ary 3M U M S ID S am p le D escriptio n E05-0622-88564 GAL SW PC01 0 050915 (Sample) E05-0622-88565 GAL SW PC01 DB 050915 (Sample Duplicate) Average Concentration (ng/mL) %RSD E05-0622-88569 GAL PW FWQ1 0 050915 (Sample) E05-0622-88570 GAL PW FWC1 DB 050915 (Sample Duplicate) Average Concentration (ng/m L) %RSD p)P FB S <0.0249 <0.0249 <0.0249 NA <0,0249 <0.0249 <0.0249 NA C o n cen tratio n (n g/m L ) PIpFH S (4Ip f o s (SJPFO A 0.0395 0.0351 0.0373 12% 0.029 0,0266 0.0278 8.60% 0.121 0.0908 0.106 23% 0.0575 0.145 0.101 87% <0.0246 <0.0245 <0.0246 NA <0.0240 <0.0246 <0.0246 NA (1) Results, averages, and %RPD values rounded to three significant-figures according to EPA rounding rules. Values may vaiy slightly from those listed in the raw data. (2) The analytical uncertainty for PFBS is 1D05.4% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFBS LOG was 0.0249 ng/mL. (3) The analytical uncertainty for PFHS is 10B7.5% based on method accuracy and precision. See Section 3.7 lor additional explanation, th e PFHS LOG was 0.0247 ng/mL. (4) The analytical uncertainty for PFOS is 10012% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFOS LOG was 0.04S5 ng/mL. (5} The analytical uncertainty for PFQA is 10010% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFOA LOG was 0,0246 ng/mL. is 0 .jaasa . it; 2.1 S am ple C ollection Samples were collected in pre-rinsed NatgeneTM (low-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, all bottles were spiked in the laboratory with a known volume o f either a surrogate solution or an appropriate matrix spiking solution containing the analytes o f interest (PFBS, PFHS, PFOS, and PFOA) and the surrogate. The "fill to here" line was marked at 450 mL. Table 2 below details the samples collected and spikes added to each bottle. 3M CONFIDENTIAL Page 3 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 Table 2. Sam ple Collection and Spike Information. Final Spike Concentration fnonL) 3MUMS io 88564 88565 88566 88587 88568 88568 88570 88571 88572 86573 88574 88575 88576 88577 Location GALSWPC01 GALSWPC01 GALSWPCCI1 G ALSW PCO f GALSWPC01 GALFWFW01 GALPWFW01 GALFWFWOT G ALFW FW 01 GALFWFW01 Trip Blank Trip Blank Trip Blank Trip Blank DoacrioSon Sample Sample DupScate Lew Field Matrix Spfta Md FieW MafrocSpfe High Field Matrix Spike Sample Sample Duplicate Lew Field Matrix Spfte MW Field Matrix Spike High FieW Matrix Spike Sample Low Field Matrix Spike Md Field Matrix Spike Hteh Field Matrix Strike PFOAf1.2aa 5.00 5.00 0.0398 0.998 9.88 5.00 5.00 0.0988 0.998 9.98 5.00 0.0088 0.998 9.98 PFBS NA NA 0.0998 0.998 8.88 NA NA 0.0988 0.898 9.98 NA 0.0988 0.998 9.9 PFHS NA NA 0.0987 0.887 9.87 NA NA 0.0987 0.987 9.87 NA 0.0987 0.967 9.87 PFOS NA NA 0.0992 0.992 9.92 NA NA 0.0992 0.992 9.92 NA 0.0992 0.992 9.92 PFOA NA NA 0.0984 0.984 9.84 NA NA 0.0984 0.984 9.84 NA 0.0984 0.984 9.84 2.2 Extraction All samples, calibration standards, and associated quality control samples were extracted using a modified procedure o f ETS-8-154.1 "Determination o f Perfluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extractions and High Performance Liquid Chromatography/Mass Spectrometry". 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 o f methanol. This extraction procedure concentrates the samples by a factor o f eight (Initial volume = 40 mL, final volume = 5 mL). Samples were extracted on September 22,2005 and analyzed on September 23,2005. 2.3 Analysis All sample and quality control extracts were analyzed for PFBS, FFHS, PFOS, PFOA.and PFOA (1,2 13C) using high performance liquid chromatography/ landem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in toe tables below. 3M CONFIDENTIAL Page 4 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. 05-0662 Table 3. Instrument Parameters Instrum ent Name Liquid Chromatograph Guard column Analytical column Injection Volum e Mass Spectrom eter Electrode Ion Source Polarity S o ftw a re ETSOIfe Agilent 1100 Botasi C ta 2 X 100,5 um BetasflC18(2.1 mm X 100 mm), Sum 5 hL Applied Biosvstems API 4000 O trap Z-sprav TurtKi Spray Negative Analyst 1.4.1 Table 4. 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 (iiJmin) 300 300 300 300 300 300 PercentA (2 mMammonium acetate) 80.0 80.0 10.0 10.0 80.0 80.0 P e rce n ts (Methanol) 20.0 20.0 S0.Q 90.0 20,0 20.0 Tables. Mass Transitions A n a lyte *PFB5 W HS *PFOS *PFOA PFO AI1.2,1C! Mass Transition Q1433 29099 29980 3G9/13G mm 399/80 499/130 499/99 499/80 413/369 413/219 413/169 415/370 OvreflTme /msec) 100 100 100 100 100 100 100 100 100 100 100 100 *AII transitions were summed to produce a "total Ion chromatogram" (TIC). The TICs were used for quantitatioa 3M CONFIDENTIAL Page 5 o f 13 3MENVIRONMENTAL LABORATORY REPORT NO. E05-Q662 3.1 C alib ratio n Calibration standards were prepared by spiking known amounts of stock solutions containing the target analytes plus the surrogate into 40 mL o fASTM type I water. Each spiked water standard was then extracted in the same manner as the collected samples. A total often spiked standards ranging from 0.025 ng/m Lto 25 ng/mL (nominal) were prepared. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data was 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 extracted calibration standard used to generate the final calibration curve met the method calibration accuracy requirement of 25%. Coefficients of determination (r2) were greater than 0.993 for all analytes. 3.2 L im it o f Q uantitation (LO Q ) The LOQ for this analysis, as defined in E-TS-8-154.1, is the lowest non-zero calibration standard in the curve in which the area counts are twice `hose of the method b!ank(s). The LOQs for PFBS, PFHS, PFOS, PFOA, and PFOA [1 ,2 13C] were 0.0249ng/mL, 0.0247 ng/mL, 0.0495, 0.0246, and 0.0249 ng/mL, respectively. Area count comparison for the method blanks and the lowest calibration standard will be provided in Section 3.5.1. 3.3 S ystem S u ita b ility The 10 ng/mL extracted-calibration standard was analyzed in triplicate at the beginning and end of the analytical sequence to demonstrate overall system suitability. All analytes met method acceptance criteria of less than 5% relative standard deviation (RSD) for peak area and less than 2% RSD for retention time except for PFOA[1,2 WC], The initial percent RSD for PFOA[1,2 13C] area counts was 6.7%. As PFOA[1,2 13C] is a surrogate and not a target analyte, the data was accepted. Closing percent RSD for area counts for this analyte m et method criteria (4.8%). 3.4 C ontinu ing C alib ration 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 was still in control. The final CCV standard analyzed produced recoveries exceeding 125% for all analytes. This standard was disabled during initial calibration as it did not meet accuracy requirements. System suitability standards analyzed immediately after this non-compliant CCV produced recoveries within 100*25% demonstrating that the instrument was stil! in control. Samples were not reanalyzed. 3.5 Blanks Three types of blanks were prepared and analyzed with the samples: method blanks, solvent blanks, and field/trip blanks. Each blank type is described below. 3.5,1 Method Blanks Several method blanks were prepared by loading 40 mL of ASTM Type I water onto a C18 SPE cartridge and eluting with 5 mL of methanol using the same extraction procedure as the samples. Method blanks were prepared to evaluate the levels of background contamination in the overall extraction process (reagent water, glassware, SPE cartridges, etc.) T ables lists the area counts for the method blanks and the LOQ standard associated with the given data se t For this data set, four of the eight method blanks were spiked PFOA [1 ,2 13C] surrogate solution to achieve a final concentration of approximately 5 ng/mL. Surrogate recoveries ranged from 106-152%. 3M CONFIDENTIAL Page 6 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-Q6$2 Table 6. Method Blank Area Counts Area Counts Sample ID PFBS PFHS PFOS PFQA PFOAf1,2 ,}CJ MB-050922-1 TOM 39372 3757Q 6949 836 MB-050922-2 5390 6721 26516 3460 521 MEJ-050922-3 7697 9579 48281 13361 761 MB-050022-4 4950 4434 26430 5015 372 MB-050922-5 7968 6355 24397 4875 `"1635963 MB-050822-6 47106 5153 26032 6388 (1,1962006 MB-050922-7 7670 6434 23076 3782 `"2241749 MB-050922-8 10151 6872 30147 2221 `"1606083 2* area counts of highest Method Mark 20302 19158 93562 12776 1672 LOQ Standaid Area Counts B9239 74737 214922 21924 18683 LOQ Standard Cone. iraftnU 0.0249 0.0247 00495 0.0246 0.0249 (1) Method blank spiked with 5.0 ngAnL{nacTuna!) PFOA[12 IJC] surrogate. Area counts not used for LOQ cwnparision. (2) Determined to be a statistical outlier using Dbcors Q-test. Data [xw it excluded for LOQ comparison. Table 7. '''Surrogate Recoveries o f Spiked Method Blanks. Samte ID JTworatfcaf Surrogete Concentration (ngimlJ Calculated Concentration (rtgfoil) MB-050922-5 MB-050922-6 MB-O50922-7 MB-050922-6 5.06 5.06 5.06 5.06 5.47 6.68 7.70 5.36 Average %RSO Pm oftt R&cov&y 108 132 152 106 124 17.5 (1) Table displays rounded values for all concentration and percent recovery values (3 significant figures). Values may vary slightly from the values in the raw data. (2) The same solution used to prepare the spiked method blanks was used to spike the sarople/sample duplicate flection bottles. 3 & 2 Solvent Blanks Several methanol solvent blanks were analyzed to assess system contamination and/or instrument carryover. Analyte peak area counts in all blank samples were less than half the area counts o fthe calibration standard used to establish the LOQ. 3.5.3 Fietd/Trfp Blanks Prior to sample collection, one sample container was filled with 450 m l of ASTM Type I water, sealed, and shipped to the sample collection te along with the empty containers. This sample was analyzed as field/trip blank. The trip blank serves as an additional method blank that accounts for any storage conditions and/or holding time issues that the samples may experience. The target analytes were not detected above the stated LOQ in the trip blank. 3M CONFIDENTIAL Page 7 o f 13 3M ENVIRONMENTAL LABORA TORY REPORT NO. E05-0662 3.6 Lab C ontrol Spikes (LC Ss) Low (0.25 rtg/mL nominal concentration) and high (7.5 ng/mL nominal concentration) lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spiking known amounts o f 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 same manner as the samples. Table 8 summarizes the LCS recovery results. All LCSs met method acceptance criteria o f 10025% for accuracy and <15% relative standard deviation (RSD) for precision. The accuracy and precision o f LCS data will be used to determine overall method uncertainty In Section 3.7. Tables. I1,Lab Control Spike Results. Sample ID LCS-050922-1 LCS-05Q922-2 LCS-050922-3 LCS-050922-4 LCS-0S0922-5 LCS-05092Z-6 Average %RSD Spike Amount fngAMJ 0.249 0.246 0.249 7/48 7.48 7.48 PFBS Cone. fn g rtn y 0242 0.233 0.241 7.30 728 7.70 97.6 3.10 Percent Recovery 972 93.8 96.8 07.S 97.3 103 Spike Amount (n&mL) 0.247 0247 0.247 7,40 7,40 7.40 PFHS Cone. (ng/mL) 0.235 0.223 0.236 7.47 7.10 7.38 96.3 3.93 Percent R ecovery 95.1 903 95.5 101 95.9 90.7 Spike Amount (natoti) 0.248 0.248 024 744 7.44 7.44 PFOS Cone. (natoti) 0.224 0207 0232 7.56 7.54 7.76 96.8 S.43 Percent R e co ve ry 90.3 83.5 93.5 102 101 104 Santola ID LCS-050922-1 LCS-050922-2 LCS-050922-3 LCS-050922-4 LCS-050922-5 LCS-050922-3 Average %RSD PFOA ________ P F O A lV 1tC]________ SpJke Amount (natoti) 0246 0246 0.246 7.36 7.38 7.38 Com. (ngtoiL) 0266 0252 0243 7.76 7.47 829 105 4.73 Spike Percent Amount Recovery (ngtotL) 108 0249 102 0246 96.8 0249 105 7.48 101 748 112 743 Cono. (ngtoil) 0294 0265 0297 8.84 7.47 8.93 113 7,19 Percent Recovery 118 108 119 116 99.9 119 (1) ADreeulls, averages, and %RSO values listed to three significantfigures according to EPA rounding rules. Values may vary slightly from those in the raw data. LCS Percent Recovery =Calculated Concentration 100% Spike Concentration LCS% RSD = standard deviation LCS replicates 100% average LCS recovery 3M CONFIDENTIAL Page 8 o f 13 3MENVIRONMENTAL LABORATORY REPORT NO. 05-0662 3.7 Analytical Uncertainty Both the accuracy {percent recovery) and precision (%RSD) o f the lab control spikes were used to estimate the overall method's analytical uncertainty for a given analyte. For example, the overall accuracy and precision for PFOA based on LCS results was 105% 4.73%, The measured precision (%RSD) is then used to determine the range o fthe accuracy. Example: 105^(0.0473) = 4.966 105 + 4.966 =109.966; 105-4.866 = 100.0335 Thus, LCS accuracy results range from 100% to 110%. The absolute difference of the low and high ends o f this range, when compared 100%, are then calculated. 110%-1OO% = 1O% 100%-100% = 0%. The most conservative (largest) absolute difference is then used as the analytical uncertainty for the given analyte. Therefore, the analytical uncertainty fo r PFOA is given as 10Q10% fo r these results. The analytical uncertainty, as defined here, for PFBS, PFHS, and PFOS is 1005.4%, 1007.5%, and 10012%, respectively. 3.8 Surrogates Although not specified in the ETS 8-154.1, PFOA [1 ,2 13C] was added to all samples and sample spikes as a surrogate to evaluate overall method performance. The final PFOA [1 ,2 13C] concentration was 5.00 ng/m L Surrogate recoveries are reported in the next section with sample data. Suirogate Recovery = Calculated SampleCon^rrtrarion >1QQ% 3.9 Field Matrix Spikes (FMS) Low (nominal concentration o f 0.1 ng/mL}, mid (nominal concentration o f 1 ng/mL), and high (nominal concentration 10 ng/mL) field matrix spikes were collected at each sampling point to verily that the analytical method is applicable to the collected matrix. Field matrix spike recoveries within method acceptance criteria of 1003Q% confirm that "unknown" components in the sample matrix do not interfere with the extraction and analysis of the analytes o f interest. Reid m atrix spikes w ill be presented in the next section with the sample data. FMS Racove - tCalculat8<l Sample Concentration - AvBrage Concentration: Field Sample & Field Sample P up.). 1 Spike Concentrator 3M CONFIDENTIAL Page 9 of 13 3M ENVIRONMENTAL LABORATORY REPORT NO. 05-0662 it e lP f ls Ill : fit: - I P " 'oSfK? isms-. ;f .mi. The table below summarize the sample results, field matrix spike (FMS) recoveries, and surrogate spike recoveries for the two locations as well as the Trip Blank. Table 9 provides the average concentration and the relative percent difference (RPD) of the sample and sample duplicate. All field matrix spike recoveries were within method acceptance criteria of 100+30% exceptforthe low level PFOS spikes (recoveries <70%). Poor reproducibility between the sample and the sample duplicate (RPD>15%) may have contributed to the low recovery. The mid and high level matrix spikes for PFOS exhibited good recovery (>86%). Therefore, the sample results for alt analytes, including PFOS, are reported and considered to be accurate within 100+30%. All samples, sample duplicates, low, mid, and high spikes exhibited sporadic PFOA [1 ,2 13C] surrogate recoveries ranging from 3.83% to 93.6%. At this time, no explanation can be given for this behavior. The 3M Environmental Laboratory will be investigating this issue in depth in a future study. Because matrix spikes of the target analytes produced excellent recoveries, sample concentrations have not been corrected for surrogate recovery. m m ` i: .. .m * m P :* i Results for the two sampling locations are presented in Table 1. Laboratory control spikes were used to determine the method accuracy and precision for the target analytes. The accuracy and precision were then used to estimate the analytical uncertainty for the results (1005.4% for PFBS; 1QQ7.5% for PFHS, 10012% for PFOS, and 10Q10% for PFOA). Field matrix spike recoveries o f the target analytes demonstrated that the results for the sample matrix are accurate within 1003G%, 5.V % m # . i ist K : *>`*1* * Si,.,:* * ** * # w ii * r m n .: w All hardcopy and electronic data will be archived according to 3M Environmental Laboratory standard operating procedures. Remaining sample will be retained at the 3M Environmental Laboratory in accordance with current sample retention policies. 3M CONFIDENTIAL Page 10 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. EQ5-0662 Table 9. |1|Detailed Sam ple Results. PFBS PFHS PFOS PFOA PFOA [1 ,2 i3C] Surrogate 3M L M S ID Sample Descrfetfoo Cone. FMS (ngfoti) Recovery Cone (ngML) ms R ecovery Cone. (mtfaiU FMS R ecovery Cane. (ng/mL) ms R e co ve ry Cane. fitoAtti} Percent Recovery 05-0622-88564 GAL SW PC010050915 <0.0249 NA 0.0395 NA 0.121 NA <0,0246 NA 3.29 65.7 E05-0622-88565 GAL SW PC01 D6 050915 <0.0249 NA 0.0351 NA 0.0908 NA <0.0246 NA 3.38 67.8 05-0622-88568 GALSW PC01LS 050915 0.0996 99.8 0.128 91.9 0.171 p,65.6 0.101 103 0.0119 11.9 E05-0622-88567 GAL SW PC01 MS 050915 0.956 96.0 0.918 892 0.963 86.4 0.683 89.7 0.156 15.6 050622-86568 GAL SW PC01 HS 050915 9.89 99.1 9.73 982 926 92.3 10.8 110 2.85 28.6 Average Concentration <Qj0249 0.0373 0.106 <0.0246 NA %RPD NA 12 28 NA NA E05-0622-88568 GAL FWFVUD1 0 050915 <0.0249 NA 0.029 NA 0.0575 NA <0.0246 NA 1.75 356 E05-0622-88570 GALFWFW01 DB 050915 <0.0249 NA 0.0266 NA 0.145 NA <0.0246 NA 223 44.6 EQ5-0622-88571 GALPWFVUJ1 LS 050915 0.101 101 0.118 914 0.159 <*58.5 0.0961 97.7 0.00606 6.09 E05O622-88572 GALPWFW01 MS 050915 0.675 87.7 0664 84.7 1.05 95.7 0.933 94.8 0.138 13.8 E05O622-88573 GALPWFW01 HS 050915 944 94.6 9.12 92.1 9.17 91.4 9.1 92.5 1.95 19.6 Average Concentration <0.0249 0.0278 0.101 <0.0246 NA %RPD NA 8.6 87 NA NA E05O622-88574 GALQATRIP01 0050915 <0 NA <0.0247 NA <0.04 NA <0.0Z46 NA 4.68 93.6 E05-0622-88575 GALGATRIP01 0 050915 0.0933 93.6 0.0884 89.6 0.0753 76.0 0.109 111 0.00382 3.83 EQ5-0622-88576 GAL QATRIP01 0 050915 0.945 94.7 0.904 91.6 0.934 942 1.01 103 0.142 142 E05O622-88577 GAL GA TRIP010 050915 9.91 99.3 9.29 94.1 9.48 95.6 9.61 96.6 6.61 (1) Table displays rounded values for ail concentration and percentrecovery values (3 significant figures). Values may vary sSghli/lrom the values in ite raw data. 662 (2) Recovery of fieW matrix spike exceeded method criteria of 100+30%. FMS recovery calcu'atei using fjs t the sample duplicate * 60.9%, The large %RPD (>15%) may contribute to the low spire recovery. (3) Recovery o fthe field matrix spike exceeded method criteria o f 100+30%. FMS recovery calculated usingjust the sample value = 103%. The large %RPD (>15%) may contribute to the low spike recovery. 3M CONFIDENTIAL Page 11 of 13 3M ENVIRONMENTAL. LABORATORY REPORT NO. E05-0662 QAU Representative / / ^ 3 -J 0 Q 1 " Date Dale L. Bacon, 3M Environmental Laboratory Technical Director Date 8.1 Report Amendment Declaration 3M CONFIDENTIAL Paga 12 of 13 jitcwmofliiiimiirm t REPORT NO. E05-0662 3M Environmental Laboratory Final Project Report Amendment Project number: EQ5-0662 Project title: Water Samples from3M Gota Laboratory ProjectLead: Michelle Malinsky Amendment date: November 23,2005 Amendment number: 1 This amendment modifies the following portion of the final report Title an die cover page and page 2. Section 1. introduction/Summary changed to clarify that one wmple was from a Municipal water line located in the 3M Guin Plant. Added fins amendment as an attachment, increasing the total pages to 13 Reason for flic amendment: To clarify that one sample was f i w i Municipal water line located in the 3M Guin Plant, instead ofnormal surface water. Approved by; 3M CONFIDENTIAL Page 1 o fl Page 13 o f 13 Aerial Photograph of the Guin, AL facility showing the location of the two samples collected on 15 Sep 05.