Document om29JDyk7MKrEONg7E5aRjYR8

3M ENVIRONMENTAL LABORATORY REPORT NO. 05-0662 Amended Final Report Analysis of P FB S, PFH S, P FO S and P FO A in Water Samples Collected at 3M Guin Laboratory Request Number: E05-0662 Method Requirement: 3M Method ETS-8-154.1 (modified) Testing Laboratory 3M E H S Operations 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue S t Paul, MN 55106 Requester Gary Hohenstern 3M Building 42-02-E-27 P O 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 3M Environm 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 Etch, Quality Associates Marlene Heying, Pace Analytical, Lab Ops VallabhaTantry, Pace Analytical, Lap Ops Amended Analytical Report 05*0662 Water Sam ples from 3M Guin November 23,2005 :jcS&7 !* & The 3M Environmental Laboratory extracted and analyzed water sam ples from two locations within the 3M Guin facility. Sam ples were collected by Weston Solutions personnel on September 15,2005. The first sampling location was a surface water sample designated as S W in the sam ple description. The second location was a municipal water line located in the 3M Guin plant designated as PW . Sam ples were returned to the 3M Environmental Laboratory for analysis of perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHS), perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFO A) and analyzed under laboratory project number E05-0662 using 3M Environmental Laboratory Method ETS 8-154.1 `'Determination of Perfluorirtated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extractions arid High Performance Liquid Chrornatography/Mass Spectrometry'1. The 3M Environmental Laboratory prepared sets of sample containers for the two sampling locations. Each sam ple 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 w as 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 w as also prepared and sent to the field with the other sample collection containers. Sam ples 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 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-0662 T a b le ! <1,Sample Results Summary 3 M LfM S ID S am ple Description E05-0622-885S4 GAL SW PC01 0 050S15 (Sample) EO5-0622-88565 G AL SW PC01 DB 050915 (Sample Duplicate) Average Concentration (ng/mL) %RSD E05-0522-88569 G AL PW FW01 0 050915 (Sample) E05-0622-88570 G AL PW FW01 DB 050915 (Sample Duplicate! Average Concentration (ng/mL) % RSD PFBS <0.0249 <0.0249 <0.024 NA <0.0249 <0.0249 <0.0249 MA Concentration (n g /m L ) &PFHS W PFO S &PFOA 0.0395 0.0351 O.0373 12% 0.029 0.0266 0.0278 8.60% 0.121 0.0908 0.106 28% 0.0575 0.145 0.101 87% <0.0246 <0.0246 <0.0246 NA <0.0246 <0.0246 <0.0246 NA (1) Results, averages, and %RPD values rounded to three significant figures according to E PA rounding rules. Values may vary slightly from those listed in the raw data. (2) The analytical uncertainty for P F 8 S is 100*5.4% based on method accuracy and precision. Sea Section 3.7 tor additional explanation. The PFB S LCQ was 0.0249 ng/mL. (3) The analytical uncertainty tor PFH S is 100*7.5% based on method accuracy and precision. See Section 3.7 (or additional explanation. The PFH S LOQ was 0,0247 ngAnl. (4) The analytical uncertainty for PFO S is 10012% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFO S LOQ was 0.0495 ng/mL. (5) The analytical uncertainty for PFO A is 10010% based on method accuracy and precision. See Section 3.7 for additional explanation. The PFO A LOQ was 00248 ng/mL. ' " "3 ?Cw. l ta ..Site.:: -.i# 2.1 S am p le C ollection Sam ples were collected in pre-rinsed NaigeneTM (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 of either a surrogate solution or an appropriate matrix spiking solution containing the analytes of interest (PFBS, PFH S, PFO S, and PFOA) and the surrogate. The ' fill to here" line w as marked at 450 mL. Table 2 below details the samples collected and spikes added to each bottle. 3M CONFIDENTIAL Page 3 o f 13 3MENVIRONMENTAL LABORATORY REPORT NO. E05-0662 T a b le 2. S am ple C o lle ctio n and S p ike Inform ation. PlnM Spike C cncrntm tion fno/m O 3M U M S ID 88564 88565 88566 $8587 88568 88569 88S70 88571 88572 86573 88574 88575 88576 88577 Location GALSW PC01 GALSW PC01 GALSW PC01 GALSW PCOI GALSW PCOI g alpw fvkh GALFW FW W GALFW FW OI GALPW FW OI GALFW FW OI Trip Blank Trip Blank Trip Blank Trio Blank D e sc iM b fl Sample Sample Eupfcate Low Field Matrix Spite M d Field MatrocSpike High Field Matrix Spike Sam ple Sample Duplicate Low Field Matrix Spike MW Field Matrix Spike High Retd Matrix Spike Sam ple Low Field Malrix Spike bid Field Matrix Spike Htoh Field Matrix Spike P F O A f1.2a a 5.00 5.00 0.0998 o.m 9.98 5.00 5.00 0.0998 0.998 9.96 5.00 0.0998 0.998 9.98 PFBS NA NA 0.0998 DM98 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 9.37 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 Alt samples, calibration standards, and associated quality control sam ples were extracted using a modified procedure of ETS-8-154.1 "Determination of Perfluorinated Acids, Alcohols, Amides, and Sulfonates in W ater by Solid Phase Extractions and High Performance Liquid Chromatography/Mass Spectrom etry. Briefly, 40 m l 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 S P E cartridges were then eluted with 5 m L of methanol. This extraction procedure concentrates the sam ples by a factor of eight (Initial volume =40 mL, final volume = 5 mL). Sam ples were extracted on September 22,2005 and analyzed on September 23,2005. 2.3 A n a lysis A ll sample and quality control extracts were analyzed for PFB S, PFH S, PFO S, PFOA,and P FO A [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 m ass transitions analyzed are described in the tables below. 3M CONFIDENTIAL r Page 4 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. EQ5-0662 Tabi 3. Instrument Parameters Inetrum ent N am e U au ld C firom atoflraD h G uard colum n A nalytical colu m n Injection V olum e M ass S p ectrom eter E lectrod e Ion Sou rce P o la rity Softw are ETSO lie Aailent 1100 B etas! C182X100,5urn Betasil C18(2.1mm X 100mm l, 5urn 5hL Applied B iosystem s API 4000Q trap Z -sp rav Turbo Spray N egative Anatrai 1.4.1 Table 4. Liquid Chromatography Gradient Program S te p N u rrib s r 0 1 2 3 4 5 T o ta l T im (m in ) 0 1.0 14.5 15.6 16.5 20.0 F lo w R e t* (tiJm srt) 300 300 300 300 300 300 P ercen tA a n M am m onium a ceta te) 80.0 80.0 10.0 10.0 80.0 80.0 Percent 8 (M e th a n o l) 2 0.0 20.0 90.0 90.0 20.0 20.0 Tables. Mass Transitions A n a ly te V FB3 *PFHS *PFOS PFO A PFO A1.2,5C] M a s s T rm tslto /} 01/03 299/99 299/80 39/130 399/99 399/80 499/130 499/99 49960 413/369 413/219 413/169 415/370 D w e lt T im e (m sec} 100 100 100 100 100 1C0 100 100 100 100 100 100 All transitions were summed to produce a Total Ion chromatogram" (TIC). The TICswere used for quantitation. 3M CONFIDENTIAL Page 5 o f 13 G 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-Q662 is 3.1 Calibration Calibration standards were prepared by spiking known amounts of stock solutions containing the target analytes plus the surrogate into 40 mL ofASTM type I water. Each Spiked water standard w as then extracted in the same manner as the collected samples. A total often spiked standards ranging tram 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 of 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 0.999 for all analytes. 3.2 Lim it of Quantitation (LOQ) The LO Q for this analysis, as defined In ETS-8-154.1, is the lowest non-zero calibration standard In the curve in which the area counts are twice those of the method blank(s}. The LO Q s for PFB S, PFH S, PFO S, PFO A, and PFO A [1,213C] were 0.0249ng/mL, 0.0247 ng/mL, 0.0495,0.0245, 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 Suitability 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% R SD for retention time except for PFO A[1,2 1SC], The initial percent RSD for PFO A[1,2 1iC] area counts was 6.7%. A s PFO A[12 13C] Is a surrogate and not a target analyte, the data w as accepted. Closing percent RSD for area counts for this analyte met method criteria (4.8%). 3.4 C ontinuin g Calibration During the course of the analytical sequence, several continuing calibration verification sam ples (CCVs) were analyzed to confirm that the Instrument response and the initial calibration curve w as still In control. The final C C V 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 C C V produced recoveries within 10025% demonstrating that the instrument was still in control. Sam ples 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 M ethod B lanks Several method blanks were prepared by loading 40 mL of ASTM Type Iwater onto a C18 S P E 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, S P E cartridges, etc.) Table 6 lists the area counts for the method blanks and the LOQ standard associated with the given data set. For this data set, four of the eight method blanks were spiked PFO A [1,213C] 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 1 3M ENVIRONMENTAL LABORATORY REPORT NO. EOS-0662 Table 6. Method Blank Area Counts A/ Counts Sam ple ID PFBS PFHS PFOS PFOA PFOJV1.2 " CJ MB-O50922-1 7005 <*39372 37570 5949 836 MB-050922-2 5390 5721 23516 3460 521 MB-OM922-3 7687 9579 48281 *13361 761 MB-050922-4 4950 4434 26430 5015 372 MB-050922*5 7968 6355 24397 4875 <" 1635963 MB-050922-8 47106 5153 26032 6386 <" 1962006 MB-050922-7 7670 6434 23076 3782 (112241749 MEWK0922-8 10151 6872 30147 2221 >1606083 2* area count* of highest Method Mark 20302 19156 98502 12776 1672 LOQ Standard Area Counts 89239 74737 214922 21924 18663 LOQ Standard Cone. (ngfthU 0.0249 0.0247 03495 0.0246 0.0249 | l) Method blank spiked with 6,0 ngAnL^nomin^) PFO A [12 ,JC} surrogate. Area courts not used for LOQ oomparteicm. (2) Detetmlned to be a statistical outlier using Dixon's Cutest. Date peart w riudsd for L O Q comparison. Table 7. `"Surrogate Recoveries o f Spiked Method Blanks. Sam ple ID MB-050922-5 MB-050922-6 MB-050922-7 MB-050922-8 Theoretical Surrogate Concentration (ngfm L) ... 5.06 5.06 5.06 5.06 Calculated Concentration fn fl* ! 5.47 6.68 7.70 5.36 Average %RSO Percent Recovery 108 132 152 106 124 17.5 (1) Table displays rounded values for all concentration and percent racovBiy values (3 ajgniScanl figures). Values rray vary sligfttyyfrom the values in ttw raw data. (2) T lie sam e ablution used to prepane the spiked method blanks was used to spite the sampla/sampte duplicate coBect'an bottles. 3J&2 Solvent Blanks Several methanol solvent blanks were analyzed to assess system contamination and/or instrument carryover. Analyte peek area counts in all blank samples were less than half the area counts ofthe calibration standard used to establish the LOQ. 3.5.3 Field/Trip Blanks Prior to sample collection, one sample container was tilled with 450 m l of ASTM Type Iwater, sealed, and shipped to the sample collection ate along with tie empty containers. This sam ple was analyzed as field/trip blank. "The trip blank serves as an addilfonal 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 LO Q in the trip blank. 3M CONFIDENTIAL Page 7 o f 13 % 3M ENVIRONMENTAL LABORA TORY REPORT NO. E05-0662 3.6 Lab Control S p ik e s (LC S s) Low (0.25 ng/mL nominal concentration) and high (7.5 ng/mL nominal concentration) lab control spikes were prepared and analyzed in triplicate. LC S s were prepared by spiking known amounts of the analytes into 40 mL of ASTM Type Iwater to produce the desired concentration. The spiked water sam ples were then extracted and analyzed in the same manner as the samples. Table 8 summarizes t ie LC S recovery results. All LC Ss met method acceptance criteria of 10025% for accuracy and <15% relative standard deviation (RSD) for precision. The accuracy and precision of LC S data will be used to determine overall method uncertainty in Section 3.7. Table 8. t1,Lab Control Spike Results. Sam ple ID LCS-050922-1 LCS-050922-2 LCS-050922-3 LCS-050922-4 LCS-050322-5 LCS-05O922-6 Average % RSD S p ik e Am ount (n g fa tlj 0.249 0.249 0.249 7/48 7.48 7.48 ARBS Cone. (ng/m L) 0242 0.233 0.241 7.30 728 7.70 97,6 3.10 Percent R e co v e ry 972 93.0 93.8 67.S 97.3 103 Spate Am ount 0.247 0247 0.247 7,40 7,40 7.40 PFHS Cone. (ng/m L) 0,235 0.223 0236 7.47 7.10 7.38 96.3 3.93 Percent R e co v e ry 95.1 902 95.5 101 95.9 99.7 Spare Am ount p tfirirtU 0.248 0.248 0248 7/44 7.44 7.44 PFOS Cone. (n g M .) 0.224 0207 0232 7.56 7,54 7.76 9S.8 8.43 Percent R e co v e ry 90.3 83.5 93.5 102 101 104 Sample ID LCS-050922-1 LCS-050822-2 LCS-050922-3 LCS-050922-4 LCS-050922-5 LCS-050922-S Average %RSD PFOA P F O A I1 2 1JC l S p ik e Am ount (ng/m L) 0246 0246 0.248 7.38 7.38 7.38 CMC. (n g M .J 0266 0252 0243 7.76 7.47 6.29 105 4.73 Percent Recovery 108 102 98.8 105 101 112 Spike Am ount (n g fa L ) 0249 0249 0.249 7.48 7.48 7/48 Cone. (ng/m L) 0294 0265 0297 8.64 7.47 8.93 113 7.16 Percent R eco very 118 106 119 116 99.9 119 (1) All results, averages, and %RSD values listed to three significant Agues according to EPA rounding rules. Valuesm ayvaty slightly from those Inthe raw data. Calculated Concentration L C S Percent Recovery = Spike Concentration 100% LCS% RSD standard deviation L C S replicates , 10)% average LC S recovery 3M CONFIDENTIAL Page 8 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. 05-0662 3.7 A nalytical Uncertainty Both the accuracy (percent recovery) and precision (%RSD) of 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 PFO A based on LC S results was 105% 4.73%. The measured precision (%RSD) is then used to determine the range ofthe accuracy. Example: 105^(0.0473) = 4.966 105 + 4.966 =109.966; 105-4.966 = 100.0335 Thus, L C S accuracy results range from 100% to 110%. The absolute difference of the low and high ends of this range, when compared 100%, are then calculated. 110%-100%= 10% 100%-100%=0%. The most conservative (largest) absolute difference Is then used as the analytical uncertainty for the given analyte. Therefore, the analytical uncertainty for PFO A Is given a s 10Q10% for these results. The analytical uncertainty, as defined here, for PFB S, PFH S, and PFO S is 1005.4%, 1007.5%. and 10012%, respectively. 3.8 Surrogates Although not specified in the ETS 8-154.1, PFO A [1,213C] was added to all sam ples and sam ple spikes as a surrogate to evaluate overall method performance. The final PFO A (1,213C] concentration was 5.00 ng/mL Surrogate recoveries are reported in the next section with sam ple data. Surrogate Recovery = C a ta 'a t^ S^mpje gonoemratloj i Spike Concentration 3.9 Field Matrix S p ik e s (FMS) Low (nominal concentration of 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 verity that the analytical method is applicable to the collected matrix. Reid matrix spike recoveries within method acceptance criteria of 1003D% confirm that "unknown" components in the sample matrix do not interfere with the extraction and analysis ofthe analytes of interest R eid matrix spikes will be presented in the next section with the sample data. f m s Recovery tCalculat6d Sample Concentration - Average Concentration: Field Sample & Field Sample Pup.). 1M ., Spike Concentrator 3M CONFIDENTIAL Page 9 o f 13 ID 3M ENVIRONMENTAL LABORATORY REPORT NO. E05-OS62 i f m- '.mi. ms.:- e r. 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 for the low level P F O S spikes (recoveries <70%). Poor reproducibility between the sample and the sam ple duplicate (RPD>15%) may have contributed to the low recovery. The mid and high level matrix spikes for PFO S exhibited good recovery (>86%). Therefore, the sample results for alt analytes, including PFO S, are reported and considered to be accurate within 100+30%. A ll samples, sample duplicates, low, mid, and high spikes exhibited sporadic P FO A [1,213C] surrogate recoveries ranging from 3.83% to 93.6%. A l 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. 7 f$ Kk a) EK U ** iy-frnf. 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 (1005.4% for PFB 5; 1007.5% for PFH S, 10012% for PFO S, and 1Q010% for PFOA). Field matrix spike recoveries of the target anaiytes demonstrated that the results for the sample matrix are accurate within 10030%. I*'!m : ms, i in * ,i. "" 1 :t. S* 1 I` A ll 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 m ENVIRONMENTAL LABORA TORY REPORT NO. E05-0662 Table 9. t1)Detailed Sample Results. PFBS PFHS PFOS PFOA PFOA [1f2 13C] Surrogate 9 M IM S ID Sample D escription Cone. (ngfaiL) ms Recovery Cone (ngtoit) ms Recovery Cone. (nofrttU FMS R e co v e ry Cone. ru ffin g ms R e co v e ry Cone. fa o fa iU R e ra sn f Recovery E5-Q622-6S564 G A LS W PC O t 0050015 <0.0249 NA 0.0395 NA 0.121 NA <0.0246 NA 329 65.7 E05O622-8S565 G A LSW PC 01 DB050015 <0.0246 NA 0.0351 NA 0-0908 NA <0.0246 NA 3.38 67.8 05-0622-88558 Q ALSW PC01 IS 050915 0.0996 99.8 0.128 91.9 0.171 p,65.6 0.101 103 0.0119 11.9 E05-Q622-88587 G A LS W PC O t MS 050915 0.956 96.0 0819 892 0.963 86.4 0.683 89.7 0.156 15.8 05-0622-88588 G A LS W PC O t H S 050915 9.88 99.1 9.73 982 926 92.3 10.8 110 2.85 28.8 Average Concentration <0.0249 0.0373 0.106 <00248 NA %RPD NA 12 28 N A NA E05-0622-88569 G ALPW FW 01 0 050915 < 0.02 NA 0.029 NA 0.0575 NA <0.0246 NA 1.75 35.0 05-0622-88570 G ALPW FW 01 DB 050915 <0.0249 NA 0.0266 NA 0.145 NA <0.0246 NA 223 44.6 E0506Z2-88571 G AL PW FW01 LS 050915 0.101 101 0.118 914 0.159 w58.5 04)961 97.7 0.00608 6.09 E05-0622-88572 GALPW FW D1 MS 050915 0.875 87.7 0864 84.7 1.05 95.7 0933 94.8 0.138 13.8 E050622-88573 G ALPW FW 01 HS 050915 944 94.6 9.12 92.1 9.17 914 9.1 92.5 1,95 19.6 Avaraga Concentration %RPD <0.0249 NA 0.0Z78 8.6 0.101 87 <0.0246 NA NA NA E0M622-88574 G ALQ ATRIP01 0050916 <0 NA <0.0247 NA <0.0495 NA <0.0246 NA 4.68 93.6 E05-0622-88575 GAL QATRIP01 0050915 E05-0622-88576 G A LG A T R IP0 10050915 0.0933 0.845 93.6 94.7 0.0884 0.904 89.6 91.6 0.0753 0.934 76.0 942 0.109 1.01 111 0.00382 3.83 103 0.142 14.2 0)5-0622-88577 G AL Q ATR IP010 050915 9.81 99.3 959 94.1 9.48 95.6 9.61 966 6.61 (1) Tabte displays rounded values for an concentration and percent recovery vaiues (3 significant Sgurea). Values may vary sfighfly from the values in the raw data. 66.2 (2) Recevety of field matrix spike exceeded method criteria of 10030%. FM S recovery calculated using just the sample duplicate =80.8%, The large %RPD (>15%) may contribute to the low spire recovery. (3) Recovery o fthe field matrix spike exoeeded method criteria of 100+30%. FM S recovery calculated ushg just tha sample value = 103%. The large %RPD 15%) may contribute to the low spike recovery. 3M CONFIDENTIAL S U Page 11 o f 13 3M ENVIRONMENTAL LABORATORY REPORT NO. EOS-0662 J '-lanr M ichelle D, Malinsky, PhiDCToM QAU Representative ITJ-1 -JooT Date Dale L. Bacon, 3M Environmental Laboratory Technical Director Date 8.1 Report A m endm ent Declaration 3M CONFIDENTIAL Pago 12 o f 13 I3 wcaii/ronAraecanrAr REPORT NO. E05-0662 3M Environmental Laboratory Final Project Report Amendment Projectnumber E05-0662 Project tide: Water Samples from 3M Girin Laboratory Project Lead: Mifbelle Malinsky Amendment date: November 23,2005 Amendmentnumber. 1 TMa amendmentmodifies the following-portion of the final report Title on ire cover page and page 2. Section 1. fotrodiwifon/Surmnaiy changed to clarify Hut one sample was form a Municipal water Sue located in the 3M Guin Plant. Added this amendment as an attachment increasing the total pages to 13 Reason for foe amendment To clarify that one sample was form a Municipal water line located in re 3M Guin Plant, instead ofnormal surface water. Approvedby: 3M CONFIDENTIAL Page 1 o f 1 Page 13 o f 13 Aerial Photograph of the Guin, AL facility showing the location of the two samples collected on 15 Sep 05. /r