Document x5wzvEmbM4jMVNbg27eeraXQ1

Katherine E. Reed, Ph.!>. Stuff Vice President II 3M Environmental, Health and Safety Operations M - is 'C 7 `)00 Bash Avenue, Buiklinu 42-2B-26 PO Box 33331 St. Paul, MN 53133-3331 651 778 433i : n 2HQ - HOST- 0 O 5 7 U Via Hand Delivery November 25,2005 Document Processing Center (Mail Code 7407M ) Room 6428 Attention: TSCA 8(e) Coordinator Office o f Pollution Prevention and Toxics U.S. Environmental Protection Agency 1201 Constitution Avenue, N.W, Washington, D.C. 20460 No CB1 CD cn O 'VT 733 r\j c.rt O . -.1 CO Re: TSCA 8(e) Supplemental Submission: Docket No. 8EHO-Q598-373: 8EHO-Q381-0394: 8EHO-1180-374 Dear Sir/Madam: feOer>ar o rn C~> X C* *23 "O pA -3 (7 --im 3M has previously submitted data showing very low or non-detect levels o f vMt Gperfluorooctanesuifonate (PFOS) or other perfluorinated compounds in variousmunicipal w atie o samples. As a supplement to those submissions, 3M provides additional results as described -Jr below. UO PFOS has been detected at approxirnately 0.1 parts per billion (ppb) in a sample of surface Water and a sample o f municipal water used as intake water at a 3M production facility in Guin, Alabama. The plant previously used a PFOS-related surfactant material in product manufacture. The laboratory report showing the results of this sampling is enclosed, and also includes analyses of PFI-IS (detected at 0.03 ppb), PFOA (non-detect), and PFBS (non-detect). If you have any questions, please do not hesitate to. contact Deanna Luebker at (6 5 1 ) 737-1374. Sincerely, Katherine E. Reed, PhD Staff Vice President Environmental Technology and Safety Services Enclosure 89060000093 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-Q662 Method Requirement; 3M Method E TS -8-154.1 (modified) Testing Laboratory 3M EHS Operations 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue S t Paul, MN 55106 Requester Gary Hohenstein 3M Building 42-02-E-27 PO Box 3331 Saint Paul, MN 55133-3331 Phone: (651) 778-5150 F a x :(6 5 1 )7 7 8 -7 2 0 3 3M CONFIDENTIAL Page 1 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 3!U1 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, Quality Associates Marlene Heying, Pace Analytical, Lab Ops Vallabha Tantry, Pace Analytical, Lap Ops Amended Analytical Report E05-0662 Water Samples from 3M Ouin November 23, 2005 Iff--1 r* m Srnrnv:,: . The 3M Environmental Laboratory 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 perfluonobutane sulfonate (PFBS), perfiuorohexane sulfonate (PFHS), perfluorooctane sulfonate (PFOS) and perfluoraoctanoate (PFOA) and analyzed under laboratory project number E05-0662 using 3M Environmental Laboratory Method ETS 8-154.1 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extractions and High Perfonnance 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 field 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 results 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 a b le ! <1)Sam ple R esults Sum m ary 3 M L !M S ID S a m p le D e s c rip tio n E05-0622-88564 GAL SW PC01 0 050915 (Sample) E05-0622-88565 GALSW PCQ1 DB 050915 (Sample Duplicate) Average Concentration (ng/mL) %RSD E05-0622-88569 GAL PW FWD1 0 050915 (Sample) E05-0622-S8570 GAL. PW FW01 DB 050915 (Sample Duplicate) Average Concentration (ngAnL) %RSD vpFB S <0.0249 <0.0249 <0.0249 NA <0.0249 <0.0249 <9.0249 NA C o n c e n tra tio n (n cf/riiL ) &PFHS <4iP F O S p)P F O A 0.0395 0.0351 O.0373 12% 0,029 0.0265 0.0278 8.60% 0.121 0.0908 0.10S 23% 0.0575 0.145 0.101 87% <0.0246 <0.0246 <0.0248 NA <0.0245 <0.0245 <0-0248 NA (1) Results, averages, and %RPD values rounded to three significant figures according to EPA rounding rules. Values may vary slightlyfrom those listed in the taw data. (2) The analytical uncertainty for PFBSis 1Q05.4% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFBS LOQ was 0.0249 ng/mL (3) The analytical uncertainty for PFHS is 1G07.5% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFHS LOQ was 0.0247 ng/mL. (4) The analytical uncertainty for PFOSfe 10012% based on method accuracyand precision. See Section 3.7 for additional explanation. The PFOS LOQ was 0.0495 ng/rnL (5) The analytical uncertainty for PFCAis 1C010% based on method accuracy and precision See Section 3.7 for additional explanation. The PFOA LOQ was 0.024$ ngAnL. vi*5"'. ,. i.f u0 2.1 Sample Collection Samples were collected in pre-rinsed NafgeneTM (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. EOS-0662 Table 2. Sample Collection and Spike Information. Final Spike CcncenFstlonfnst/mU 3M U M S 10 Location DoscrtoOon 88564 88565 88566 38567 88568 88569 88570 88571 88572 88573 88574 88575 88576 88577 GALSWPC01 GAL SW PCM GALSWPC01 GAL SW PCM GALSWPC01 GALPW FVfol GALPW FW 1 GALFWFWOt GALFWFWOt GALFWFWOt Trip Blank Trip Blank Trip Blank Trip Blank Sample Sample Dupfcate Low Field Matrix Sp&a kfid Field MakerSpike High Field Matrix Spike Sample Sample Duplicate Lew Field Matrix Spite MW Field Matrix Spike High Field Matrix Spike Sample Low Field Matrix Spike Mki Field MatrixSpike Htoh Field Matrix Seiko PFOAf1.2a a 5.00 5.00 0.0698 0,998 9.68 5.00 5.00 0.0998 0.998 9.98 5.00 0.0998 0.998 9.98 PFBS NA NA 0.0998 0.898 9.98 NA NA 0.0998 0.998 9.98 NA 0.0998 0.998 9.98 PFHS NA NA 0.0987 0,887 9.87 NA NA 0.0987 0.987 9.87 NA 0.0987 0.987 9.S7 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 0.0384 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 Perfiuorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extractions and High Performance Liquid Chromatography/Mass Spectrometry". Briefly, 40 m l 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 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 arid quality control extracts were analyzed for PFBS, PFHS, PFOS, PFOA,and PFOA [1,2 13C] 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. 3M CONFIDENTIAL Page 4 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. EQ5-0662 Table 3. Instrument Parameters Instrument Name Ltauld Chromatograph Guard column Analytical column Injection Volume Mass Spectrometer Electrode Ion Source Polarity Software ETSOIfe Aa#ent 1100 Betas! CIS 2X100,5 tun Belasti C16 (2.1 mm X 100 mm). 5 urn 5 uL Applied Biosystems API 4000 Q trap Z-sprav Tubo Spray Negative Analyst 1.4.1 Table 4. Liquid Chromatography Gradient Program Step Humber 0 1 2 3 4 5 Total Tima (mini 0 1.0 14.5 15.5 16.5 20.0 Flaw Rata O lfatto ) 300 300 300 300 300 300 PercentA (2 mM ammonium acetate) 80.0 80.0 10.0 10.0 80.0 80.0 PercentB M entanoli 20.0 20.0 00.0 90.0 20.0 20.0 T ab le s . Mass Transitions Analyte *PFBS W HS *PFOS *PFOA p F O A ri,2 "a Mass Transition Q1/Q3 299199 29980 399^30 39999 39980 490/130 499/99 490/80 413/369 413/219 413/169 415/370 Dwell Time (msec) 100 100 100 100 100 100 100 100 100 100 100 100 'All transitions were summed toproduce a total Ion chromatogram"(TIC). The TICswere used forquantitation. 3M CONFIDENTIAL Page 5 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 % SS? S 3.1 C alib ration 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/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 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 o f determination (r2) were greater than 0.999 for all analytes. 3.2 L im it o f Q uantitation (LOQ) 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 those of the method blankfs). 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 System 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 o f less than 5% relative standard deviation (RSD) for peak area and less than 2% RSD for retention time except for PFOA[1,2 n C], 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 fo r this analyte m et method criteria (4.8%). 3.4 C ontinuing C alibration 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 w as disabled during initial calibration as it did not m eet accuracy requirem ents. System suitability standards anaiyzed im m ediately after this non-compliant C C V produced recoveries within 1 0 0*25% demonstrating that the instrument w as still in control. Sam ples w ere not reanalyzed. 3.5 B lanks 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 o f ASTWl Type I water onto a C18 SPE cartridge and eluting with 5 mL o f 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.) Table 6 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 (1,213CJ 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. E0S-06$2 Table 6. Method Blank Area Counts A n * Counts Sam nlelD PFBS PFHS PFOS PFOA fro m t" c i MB-050922-1 M0-O5O322-2 MB-Q50B22-3 MB-0508224 MB-050922-5 MB-050022-6 MB-050922-7 MB-050922-8 7005 6390 7687 4950 7968 47106 7670 10151 39372 5721 0579 4434 6355 5153 6434 6872 37570 26516 48281 26430 24397 26032 2307 30147 5949 3460 *13361 5015 4875 6386 3782 2221 836 521 761 372 *1635963 *1962006 *2241749 *1606083 2* area counts ofhighestMethod blank 20302 13158 96562 12776 1672 LOQ Standaid Area Counts 89239 74737 214922 21924 18683 LOQ Standard Cone. inoAnU 0.0249 0.0247 0.0495 0.0246 0.0249 ^i> Method blank spiked with 5.0 ngAnLfnoniinal) PFOA (1X "C] surrogate. Area counts not used ter LOQ coroparislon. (2) Determined to be a statistical outlier using Dtxon's Q-test. Data point excluded for LOQ comparison. Table 7. '"'S u rro ga te R ecoveries o f S piked M ethod B lanks. Sample ID MB050S22-5 MB-050S22-6 MB-050S22-7 MB-050922-8 Theoretical Surrogate Concentration '& * ) .... 5.06 5.06 5.06 5.06 Calculated Concenirsiron (no/mL) 5.47 6.68 7.70 5.36 Avenge %RSO Percent Recovery 108 132 152 106 124 17.6 {1} Table displays rounded values for all concentration and percent racowty values (3 significant figures). Values m ay vary slighltyfron the values inIhs rawdata. (2) The same solution used to prepare the spiked method blanks was used to spite the saroptateampte duplicate coBedion bottles. 3 & 2 Solvent Blanks Several methanol solvent blanks were analyzed to assess system contamination and/or instalment 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 Fletd/Trfp Blanks Prior to sample collection, one sample container was filled with 450 m l of ASTWI Type l water, sealed, and shipped to the sample collection a te along with the empty containers. This sample was analyzed as fiekl/Wp blank. The trip blank serves as an additional method blank that accounts tb r 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 3MENVIRONMENTAL LABORATORY REPORT NO. E05-0662 3.6 Lab Control Spikes (LCSs) Low (0.25 ngftriL nominal concentration) and high {7.5 ng/mL nominal concentration) lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spildng 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 100125% for accuracy and <15% relative standard deviation (RSD) for precision. The accuracy and precision o f LCS data w ill be used to determine overall method uncertainty in Section 3.7. Table 8. (i)Lab C on trol Spike R esults. Sample ID LCS-050922-1 LCS-050922-2 LCS-050922-3 LCS-05Q922-4 LCS-50922-5 LCS-050922-6 Average %RSD Spike Amount (ngtotL) 0.249 0.249 0.249 748 7.48 7.48 ARBS Cone. fhffh iU 0242 0.233 0.241 7.30 728 7.70 97.8 3.10 Spike A m en t Amount Recovery 972 0.247 93.8 0.247 96.8 0.247 67.6 7,40 97.3 7,40 103 7.40 ARMS Cone. O 0.235 0223 0236 7.47 7.10 7.38 96.3 3.93 Percent Recovery 95.1 90S 95.5 101 95.9 99.7 Spike Amount fnpAnV 0.248 0.248 0248 744 7.44 7.44 PFOS Cone. (nghvL) 0.224 0207 0232 7.56 7.54 7.76 96.8 8.43 Percent Recovery 90.3 83.5 93.5 102 101 104 Sample ID LCS-050922-1 LCS-050922-2 LCS-050922-3 LCS-050922-4 LCS-050922-5 LCS-050922-S Avenge %RSD PFOA PFO A I121,CJ Spike Amount (n a m . 0246 0246 0.246 7.36 7.38 7.36 Cone. (nghnL) 0268 0252 0243 7.76 7.47 8.29 105 4.73 Percent Recovery 108 102 98.3 105 101 112 Spike Amount (nofmL) 0249 0249 0249 7.48 7.48 748 Cone. (n a h m 0294 0266 0297 8.64 7.47 8.93 113 7.16 Percent Recovery 118 106 119 116 99.9 119 (1) AUresufts, averages, and %RSO values listed to three significantfigures accordingto EPA rounding rules. Values may vary slightlyfrom those In the raw data. LCS Percent Recovery = Calculated Concentration 100% Spike Concentration LCS%RSD standard deviation LCS replicates , average LCS recovery 3M CONFIDENTIAL Page 8 o f 13 3MENVIRONMENTAL LABORATORY REPORT NO. E05-0662 3.7 Analytical Uncertainty Both the accuracy {percent recovery) and precision (%RSD) o f the tab control spikes were used to estimate the overall method's analytical uncertainty fo r 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; 105-1.966 = 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% -100% =10% 100%-100%=0%. The most conservative (largest) absolute diffrence is then used as the analytical uncertainty for the given analyte. Therefore, the analytical uncertainty for PFOA is given as 10Q10% for these results. The analytical uncertainty, as defined here, for PFBS, PFHS, and PFOS is 10Q5.4%, 1007.5%. and 10012%, respectively. 3.8 Surrogates Although not specified in the ETS 6-154.1, 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 w ith sample data. Surrogate Recovery = >10Q% 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 verify that the analytical method is applicable to the collected matrix. Field matrix spike recoveries within method acceptance criteria o f 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 will be presented in the next section with the sample data. fm s Recovery - (Calculat8d Sample Concentration - Average Concentration: Field Sample & FieldSample Pup.) , 1M% 3M CONFIDENTIAL Page 9 of 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 m :- 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% except fo r the 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 (>8S%). Therefore, the sample results for all 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%. A t 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 i 9# fe m h .. m , 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 (1Q05.4% for PFBS; 10Q7.5% for PFHS, 10012% for PFOS, and 100*10% for PFOA). Field matrix spike recoveries o f the target analytes demonstrated that the results for the sample matrix are accurate within 1003Q%. m .-. W; me. 1 Sii. : *1! & 5* *** * i fit P .; is ,3. p, .,f 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. 05-0662 Table 9. [1|Detailed Sample Results. PFBS PFHS PFOS PFOA PFOA [1 ,2 13C] Surrogate M U M S ID Sample Description Cone. (ngfaiL) A irs Recovery Cone (ngfaL) FMS Recovery Cone. mmo FMS Recovery Cone. ffle tn U FMS Cotie. Recovery fnstoO Percent Recovery 054622-88554 GALSW PC01005091S <0.0249 NA 0.03% NA 0.121 NA <9.0246 NA 329 657 05-0622-86565 GAL SWPC01DB 050915 <0.0249 NA 04351 NA 0.0908 NA <0.0246 NA 3.39 67.8 05-0622-88566 GALSWPC01 LS 05091$ 04996 99.8 6.128 91.9 0.171 Pl65.6 0.101 103 0.0119 11.9 05-0622-68567 GALSW PC01 MS 050915 0.956 96.0 0918 892 0.963 86.4 0.883 89.7 0.156 15.6 05-0622-88568 GAL SW PC01 NS 050915 9.89 SS.1 9.73 982 9.26 S2.3 10.8 110 2.85 28.6 Average Concentration <0.0248 0.0373 0.106 <04246 NA %RPO NA 12 28 NA NA E054622-86569 GAL FWFWB1 0050915 <0.0249 NA 0.029 NA 04575 NA <0.0246 NA 1.75 35.0 E05-0622-88570 GALPWFW01 OB 050915 05-0622-88571 GALPWFW01 LS 050915 <0.0249 0.101 NA 101 0.0266 0.118 NA 914 0.145 0.159 NA p 58-5 <0.0246 0.0961 NA 97.7 223 0.00608 44.6 6.09 E05-0622-88572 GALPWFW01 MS 050915 0.875 67.7 0464 847 1.05 957 0.933 94,8 0.138 13.8 054622-88573 GALPWFWQ1 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 <04246 NA %RPD NA 8.6 87 NA NA E05-0622-88574 GALQATRIP01 D050915 <0 NA <04247 NA <0.0495 NA <0.0246 NA 4.68 93.6 E054622-88575 GALGATRIP01 0050915 0.0933 93.5 0.0684 89.6 0.0753 76.0 0.109 111 0.00382 3.83 05-0622-88576 GALQATRIP01 0 050915 0.945 94.7 0.904 91.8 0.934 942 1.01 103 0.142 14.2 E054622-88577 GAL GA TRIP010 050915 9.91 99.3 9.29 94.1 9.48 95.6 951 96.6 6.61 (1) Table displays roundedvalues lor ail concentration and percentrecovery values {3 significant figures). Values may vary sf/gftiiyfrom the values in the raw data. 66.2 (2) Recovery of field matrix spike exceeded method criteriaof 100*30%. FMS recovery calculated using just 8 sample duplicate * 60.9%. The large %RPD (>15%) may contributeto the lowspire recovery. (3) Recoveryofthe field matrixspike exoeeded method criteriaof 100+30%. FMS recovery calculated usngjust tha sample value = 103%. The large %RPD (>15%) maycontribute to the lowspike recovery. 3M CONFIDENTIAL Page 11 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E5-0662 P ia -- T _____-- js f- X f Michelle D. Malinsky, PhdBCTW ieshriical L e a d / date 1 QAU Representative //' -'J O T Date Dale L. Bacon, 3M Environments Laboratory Technical Director f / y / ' Date 8.1 Report Amendment Declaration 3M CONFIDENTIAL Paga 12 o f 13 o n c *n o TM ii n rrv u / REPORT NO. 054662 3M Environmental Laboratory Final Project Report Amendment Project number: E05-O662 Project title: Water Samples from 3M Guin Laboratory ProjectLead: Michelle Malinsky Amendment date: November 23,2003 This amendmentmodifies the following portion of the final report: Title on tbe cover page and page 2. Section 1. Jntroductipn/Sumiimry changed to clarify that one sample was from a Municipal w aterline located jo the 3M Guin Plant. Added this amendment as an attachment, increasing the total pages to 13 Reason far file amendment: To clarify Oat one sample waa from a Municipal water line located in the 3M Gain Plant; instead ofnormal surface water. Approved by: 3M CONFIDENTIAL Page 1 o f1 Page 13 o f 13 Aerial Photograph of the Guin, AL facility showing the location of the two samples collected on 15 Sep 05.