Document daKM9z9ERDkwZy1aBJDdywzg9

3M ENVIRONMENTAL LABORATORY REPORT NO. E07-05S4 Final Report 2 2 ^ -3 7 ^ Analysis of PFBA and PFO A in Aqueous Sam ples collected from Cottage Grove Private Residences Laboratory Request Number: E07-0584 Report Date: 10/3/2007 Method Requirement: 3M Method ETS-8-44.0 "Method of Analysis for the Determination of Perfluorinated Compounds in W ater by 7 1 LC/MS/MS; Direct Injection Analysis" : Testing Laboratory 3M EHS Operations 3M Environmental Laboratory Building 260-5N-17 Maplewood, 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 This laboratory maintains A2LA accreditation to 1SQ/1EC 17025.2005 for the specific tests/calfbrationa listed In A2LA Certificate 2052-01 and meets the relevant quality systems requirements o f ISO 9001:2000. The testa results included In this report, however, are not covered by this accreditation 3M CONFIDENTIAL PAGE 1 OF 11 P -2 3M ENVIRONMENTAL LABORATORY REPORT NO. 607-0584 3M E n viro nm e nta l L a b oratory 3M Environmental Laboratory Manager: W illiam K. Reagen, Ph D 3M Technical Lead and Report Author: Michelle D. Malinsky, Ph.D. Analytical Report E07-0584 Analysis of PFBA and PFOA in Aqueous Samples Collected from Cottage Grove Private Residences Report Date: October 3,2007 The 3M Environmental Laboratory analyzed water samples collected from nine private residences in Cottage Grove, MN, W ater samples were collected by Pace Analytical Field Services personnel on September 12,2007. Samples were returned to the 3M Environmental Laboratory for analysis of perfluorobutanoic acid (PFBA) and perfluorooctanoate (PFOA) under laboratory project number E070584. The 3M Environmental Laboratory prepared sets of sample containers for eleven sampling locations, Each sample set consisted of a field sample, field sample duplicate, low field spike, and high field spike. Each empty container was marked with a "fill to here" line that corresponded to a final volume of 450 mL. Containers reserved for field m atrix spikes were fortified with an appropriate m atrix spike solution containing both analytes prior to being sent to the field for sample collection. Samples were prepared and analyzed using ETS-8-044.0 "Determination o f Perfluorinated Compounds in W ater by LC/MS/MS; Direct Injection Analysis" on September 13-14,2007. Table 1 summarizes the sam ple results. All results for quality control samples prepared and analyzed with the samples w ill be reported and discussed elsewhere in this report. The 3M Environmental Laboratory maintains A2LA accreditation to ISO/IEC 17025:2006 for the specific tests/calibrations tisted in A2LA Certificate #2052-01 and meets the relevant quality systems requirements of ISO 9001:2000. However, ETS 8-044.0 does not fell under the lab's current scope of accreditation. This laboratory maintains A2LA accreditation to ISO/IEC 17025:2005 for the specific tests/calibrations listed in A2LA Certificate # 2052-01 and meets the relevant quality systems requirements of ISO 001:2000. The tests results Included In this report, however, are not covered by this accreditation PAGE 2 OF 11 3 p .3 3M ENVIRONMENTAL LABORATORY REPORTNO. E07-0584 Table 1. <1)Results Summary. 3M UM SID Samte Description PFBA PFOA Concentration Concentration fno/lnU (ng/m E07-0584-001 E07-0584-002 9675 Miller Road, sample 9675 Miller Road, samle duo 223 2.23 1.09 1.09 Average %RPD Samole/Sample Duo Z23 0.00 109 0.00 E07-0584-005 E07-0584-006 9735 Miller Road, sample 9735 Miller Road, sample dup 1.88 0.747 1.81 0.720 Average 185 0.734 %RPD Sample/Sample Dud 3.8 3.7 E07-0584-009 EO7-O504-O1O 9747 Miller Road, sample 9747 Miller Road, sample dup 2.50 2.45 1.12 1 13 Average XRPD Sample/Sample Dup Z 48 2.0 1.13 0.89 07-0584-013 E07-C584-014 9501 Islay Road, sample 9501 Islay Road, smola duo 1.82 0.254 1.76 0.254 Average 1.79 0.254 E07-0584-017 EQ7-0584-018 %RPD Sample/Sample Duo 9564 Islay Road, sample 9564 Islay Road, sample dup 3A 1.39 1.42 0.00 0.980 0.973 E07-0584-021 E07-0584-022 Average %RPD Sample/Sample Duo 9567 Islay Road, sample 9567 Islay Road, sample dup 1.41 Z1 2.70 2.86 0.977 0,72 0.278 0.282 Average XRPD Sample/Sample Duo Z78 5.8 0.280 14 E07-0584-025 E07-0584-026 9655 Islay Road, sample 9655 Islay Road, sample duo 3.03 2.89 0.912 0.898 Average %RPD Sample/Sample Dup Z96 4.7 0.905 1.5 E07-0584-033 E07-0584-034 8724 95th St. South, sample 8724 95th St. South, sample dup 1.81 0.332 1.69 0.333 E07-0584-037 E07-0584-038 Average %RPD Sample/Sample Duo 8811 West Point Douglas Road, sample 8811 West Point Douglas Road, sample Dup 1.75 8.9 2.92 2.99 0.333 0.30 0.433 0.425 Average Z96 0429 %RPD SamoferSarnDfe Dup 2.4 1.9 (1) Samples were analyzed by direct injection using method ET5-B-O44.0. ETS-8-044.0 is not included on the 3M Environmental Laboratory's ISO 17025 scope of accreditation. The analytical method uncertainties associated with the reported results are as follows: PFBA 30%, PFOA 25%. Refer to Sections 3 and Afor data acceptance criteria and discussion. 3M CONFIDENTIAL 4 P A G E 3 0 F 11 3M ENVIRONMENTAL LABORATORY REPORTNO. 07-0584 2.1 Methods Analysis for PFBA and PFOA was completed following 3M Environmental Laboratory method ETS-8044.0 "Determination o f Perfluorinated Compounds in W ater by LC/MS/MS; Direct Injection Analysis". 2.2 Sample Collection Samples were collected in NalgeneTM (low-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume o f an appropriate m atrix spiking solution containing the analytes of interest. Collected sample bottles were returned to the laboratory at ambient conditions on September 12,2007. 2.3 Sample Preparation An aliquot o f a well mixed sample was removed for analysis and placed in an autovial. 2.4 Analysis All samples and quality control samples were analyzed for the target analytes using high performance liquid chrom atography/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 2. Instrument Parameters. Instrument Name Analytical Method followed Liquid Chromatograph Guard column Analytical column Injection Volume Mass Spectrometer Ion Source Electrode Polarity Software ETSOllie ETS-8-044.0 Agilent 1100 Betasil CS (4.6 mm.X 150 mm), 5 wn Betasil C18 (4.6 mm X 150 mm), 5 um 100 uL Applied Biosystems API 4000 Turbo Spray Z-spray Negative Analyst 1.4.2 3M CONFIDENT!AL PAGE 4 OF 11 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-0584 Table 3. Liquid Chromatography Gradient Program. Step Number Total Tima (min) 00 1 0.5 2 11.0 3 13.5 4 13.6 5 17.0 Table 4. Mass Transitions Row Rata (pUmin) 1000 1000 1000 1000 1000 1000 Percent A (2 mM ammonium acetate) 97 97 5 5 97 97 Percent B (Methanol) 3 3 95 95 3 3 !----------------- -- ------------Analyte Mass Transition Q1/Q3 Dwell Time (msec) ETSOWe PFBA ''PFOA 213/169 413/369 200 200 413/219 200 413/169 200 (1) The individual transitions ware summed to produce a "total ion chromatogram" (TIC). The TICs were used for quantitation. 3.1 Calibration Calibration standards were prepared by spiking known amounts o f stock solutions containing the target analytes into reverse-osm osis purified water. A total o f thirteen calibration standards ranging from 0.025 ng/m L to 50 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 calibration standard included in the final calibration curve met the method calibration accuracy requirem ent of 25%. Correlation coefficients (r) were greater than 0.90 for both analytes. 3.2 Limit of Quantitation (LOQ) The LOQ fo r this analysis, as defined in ETS-8-44.0 is the lowest non-zero calibration standard in the curve in which the area counts are a t least twice those of the method blanks. Table 5 lists the LOQ for each analyte for each analysis day from which sample results were reported. The LOQ for PFBA and PFOA was 0.0491 ng/m L and 0.0727 ng/mL, respectively. 3M CONFIDENTIAL PAGE 5 OF 11 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-Q584 3.3 Continuing Calibration During the course of the analytical sequence, continuing calibration verification samples (CCVs) were analyzed to confirm friat the instrument response and the initial calibration curve were still in control. All samples were bracketed by method compliant CCVs with recoveries o f 10025%. 3.4 Blanks Several blanks o f reverse osmosis purified water were analyzed throughout the analytical sequence and were used to evaluate method performance and to determ ine the LOQ for each analyte 3.5 Lab Control Spikes (LCSs) Low and high lab oontrol spikes were prepared and analyzed in triplicate. The LCS samples were prepared by spiking known amounts of the analytes into 40 mL of reverse osmosis treated deionized w ater to produce the desired concentration. The spiked water samples were then analyzed in the same manner as the samples. The method acceptance criteria states that the average recovery of LCS be 100% 20% with a RSD 520%, when evaluated independently at each concentration level. All LCS recoveries were used in the determination of the analytical uncertainty. The following calculations were used to generate data in Table 5. Calculated Concentration 1 LCS Percent Recovery Spike Concentration standard deviation LCS replicates. 100% LCS%RSD = average LCS recovery Table S. Lab Control Spike Recoveries. (1) Average PFOA reoovery for the low level LCSs exceeds method acceptance criteria of 10020%. A method deviation has been issued. 3M CONFIDENTIAL 7 PAGE 6 OF 11 p .7 3MENVIRONMENTAL LABORATORY REPORT NO. 07-0554 LCS Percent Recovery = P ^ l a* d Concentration 100% Spike Concentration LCS% RSD = standard deviation LCS replicates , , 0Q% average LCS recovery 3.6 Analytical 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 fo r the set o f accuracy results (In %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by factor of 2, which correspond with a confidence level o f 95%. Table 6. Analytical Method Uncertainty. Analyte PFBA PFOA Number of data points used for determining uncertainty 50 50 Standard Deviation 14.8 12.6 Method Uncertainty 30% 25% 3.7 Field Matrix Spikes (FMS) Low and high field m atrix spikes were collected at each sampling point to verify that the analytical method is applicable to the collected matrix. Field m atrix spikes are generated by adding a measured volume o f field sample to a container spiked by the laboratory with the target analytes prior to shipping. Field m atrix spike recoveries w ithin method acceptance criteria o f 10030% confirm that "unknown" components in the sample m atrix do not significantly interfere w ith the extraction and analysis of the analytes o f interest. Field m atrix spikes are presented in the section 4 o f this report Generally two spike levels are prepared as ETS 8-44.0 states that FMS levels should be between 0.5 to 10 tim es the endogenous sample concentration. If a given FMS level does not m eet this criteria, the recovery is labeled as NR, not reportable, and the other FMS level is used to evaluate the sample. The spike levels for each analyte are provided below FMS Recovery = (Sample Concentration of F M S - Average Concentration :Field Sample & Field Sample Pup.) Spike Concentrator 00 Table 7. Field Matrix Spike Concentrations Description Low Field Matrix Spike High Field Matrix Spike PFBA Spike Cone. rtgtoiL 0.504 4.58 PFOA Spike Cone. ng*nl_ 0.256 2.33 3M CONFIDENTIAL 6 PAGE 7 OF 11 p .8 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-QS84 The table below summarizes the sample results and field matrix spike (FMS) recoveries for the nine locations as well as the Trip Blank. The table provides the average concentration and the relative percent difference (RPD) of the sample and sample duplicate. Results and average values are rounded to three significant figures. 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. Field matrix spikes meeting the method acceptance criteria of 10030% dem onstrate that the method is appropriate for the given matrix. Table 8. Data Summary with QC. S575 Miller Road PFBA 3M UM SID E07-0584-001 E07-0584-002 E07-0584-003 E07-0584-004 Sample Description 9675 Miller Road, sample 9675 Miter Road, sample dup 9675 Miller Road, low spike 9675 Miller Road, high Spike Average %RPD Cone. (nglmL) 2.23 2.23 2.32 7.10 223 0.0 FMS ^ R e c o v e ry NA NA NR 106 9735 Miller Road PFBA 3M UM SID Sample Description Cone. (nytnL) ^Recovery E07-0584-005 E07-0584-Q06 E07-0584-007 E07-0584-008 9735 Miller Road, sample 9735 Miller Road, sample dup 9735 Miller Road, low spike 9735 Mlter Road, high spike Average %RPD 1.88 1.81 2.29 6.59 1.85 3.8 NA NA NR 104 9747 Miner Road PFBA 3M UM SID Sampie Description Cone. (ngftnL) FMS `Recovery E07-0584-009 E07-0584-010 E07-0584-011 E07-0584-012 9747 Miller Road, sample 9747 Mller Road, sample dup 9747 Miller Road, low spike 9747 Miller Road, high spike Average %RPD 2.50 2.45 2.98 7.30 2.48 20 NA NA NR 105 PFOA Cone. (ngfmU FMS %Recoverv 1.09 1.09 1,40 3.34 1.09 0.0 NA NA NR 96.6 PFOA Cone, (ng/n fltfS %Recovery 0.747 0.720 0.994 3.00 0.734 3.7 PFOA NA NA NR 97.3 Cone. (ng/mL) 1.12 1.13 1.38 3.39 1.13 0.89 FMS ^ R e c o v e ry NA NA NR 97.2 3M CONFIDENTIAL 7 PAGE 8 OF 11 3M ENVIRONMENTAL LABORATORY REPORT NO. E07-C584 Table 8 Continued. 9501 Islay Road PFBA m u m ip Sarwfcytesgtotion FMS _Coflcj>ig4Tjy_ ^Recovery E07-0564-013 E07-0584-014 EO7-0584-015 E07-0584-016 9501 Islay Road, sample 9501 Islay Road, sample dup 9501 Islay Road, low spike 9501 Islay Road, high spike Avenge %RPD 1.82 1.76 2.40 7.03 1.79 5.4 NA NA NR 114 9564 Islay Road PFBA 3M UMS ID Sample Description E07-0584-017 E07-0584-018 ED7-0584-019 E07-0584-02Q 9564 Islay Road, sample 9564 Islay Road, sample dup 9564 Islay Road, low spke 9564 Islay Road, high spike Average %RPD 9567 Islay Road FMS '/Recovery 1.39 1.42 2.01 6.65 1.41 2.1 NA NA NR 115 PFBA 3M UM SID E07-0584-021 9567 Islay Road, sample E07-0584-022 E07-0584-023 E07-0584-024 9567 Islay Road, sample dup 9567 Islay Road, low spike 9567 Islay Road, high spike Average %RPD 9655Islay Road <Ccwc. 2.70 2.86 3.15 7.47 2.78 5.8 FMS ^Recovery NA NA NR 102 PFBA E07-O584-O25 E07-0584-026 E07-05B4-027 E07-Q584-028 JCon&Jngmi^_ 9655 Islay Road, sample 9655 Islay Road, sample dup 9655 Islay Road, low spike 9655 Islay Road, high spike Average %RPD 3.03 2.89 3.53 8.03 96 4.7 FMS '/Recovery NA NA NR 111 PFOA Cone. (nglmL) FMS %Recovery 0.254 0,254 0512 2.74 0.254 0.0 NA NA 101 107 PFOA Cone. {n&mLl FMS %Recovery 0.960 0.973 1.23 3.54 0.977 0.72 NA NA NR 110 PFOA 0.278 0.282 0.565 2.74 0.280 1.4 PFOA NA NA 111 106 j0ono_)g4nU 0.912 0.898 1.19 3.76 0.905 1.5 FMS %Recevery NA NA NR 123 3M CONFIDENTIAL PAGE 9 OF 11 3M ENVIRONMENTAL LABORATORY REPORT NO E07-0584 Table 8 Continued. 8734 95ttSl$O trfh 3M UMS ID E07-0584-033 E07-0584-034 E07-0584-035 E07-0584-035 Sample Description 8724 95th St. South, sample 8724 95th St. South, sample dup 8724 95th St. South, low spike 8724 95th St. South, high spike Average %RPD PFBA cogjfrg*gy_ 1.81 1.69 2.18 6,83 1.75 FMS `Recovery NA NA NR 111 PFOA FMS onc^JngSm_ `Recovery 0332 0.333 0600 2.73 0.333 0.30 NA NA 104 103 8811 west Point Douglas Road PFBA PFOA 3M LfflfS ID Sample Description FMS C onJjg]i_ ^Recovery FMS E07'0584-037 E07-0584-038 E07-0584-39 E07-0584-040 Trip Blank 8811 West Point Douglas Road, sample 6811 West Point Douglas Road, sample Dup 8611 West Point Douglas Road, Low spike 8811 West Point Douglas Road, High spike___________________ Average %RPD 2.92 NA 2.99 NA 3.51 NR 8.73 2.98 2.4 PFBA 126 0.433 NA 0,425 NA 0.745 123 2.94 0.429 1.9 PFOA 108 3M IM S 10 Sample Description FMS /.Recovery Cone. (nc/mL) E07-0584-045 Trip Blank <0.0491 NA E07-0584-046 Trip Blank Low Spike 0.629 125 E07-Q584-047 Trip Blank High Spike 5.35 117 NR= Not Reportable. FMS concentration was <0.5 times the endogenous sample concentration. <0.0727 0.328 2.77 FMS Recovery NA 128 119 3M CONFIDENTIAL // PAGE 10 OF 11 3M ENVIRONMENTAL LABORATORY REPORT NO. EQ7-0584 .......... I. i **% ' a f s*'i S" %' .? s?: Sample results for PFBA and PFOA were presented in Table 1. Field m atrix spike recoveries for all locations m et m ethod acceptance criteria of 10030% for both analytes. A ll remaining sam ple and data (hardcopy and electronic) associated with this project w ill be retained and archived according to 3M Environmental Laboratory standard operating procedures. W illiam K. Reagen, Ph.D., Environmental Laboratory Management Date The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report fo r this project. Quality A s^irp n ce Representative Date 3MCONRDEIVT1AL /Z PAGE 11 OF 11 Material Description: Light aromatic solvent naphtha (petroleum) is a complex mixture of 70-80% C9 aromatic hydrocarbons (primarily ethyltoluene and trimethylbenzene isomers), with the remainder primarily C8 and CIO aromatic molecules. It has a boiling point range of 135-210 deg C (275-410 deg F). Note: Due to analytical limitations and known variability in refinery process stream composition, identification of every specific individual molecular compound in every refinery process stream under all processing conditions was impossible. Recognizing these problems, the American Petroleum Institute (API) recommended to the EPA a list of generic names for refinery streams consistent with industry operations and covering all known processes used by refiners. Properties of representative samples of distillates are then used to demonstrate the toxicity for substances within the category. This HHP is based on specific information for light aromatic solvent naphtha (petroleum). Whenever possible, this information is supplemented by general information for comparable aromatic naphthas, as appropriate. Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB rogram Name: Superfund-PFC Samples: 200729212 - 200729212 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729212 j Receiving Comments: Coll Date Coll Time 12 -SEP-2007 1420 Fields No - 1 Sampling Point Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Orqanic Results are indicated by BOLD. Result Codes Result Rept Level 55 PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 2.6 J 0.2 J 0.07 0.3 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dati 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1This report was modified by 3M prior to TSCA 8(e) submission to remove the property owners' names from the "sampling point" field of the report form Group 312473 p. 14 Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB Program Name: Superfund-PFC Samples: 200729213 - 200729213 j Date Received: 12 -SEP-2 007 Date Generated: 20 -SEP-2 007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729213 Receiving Comments: Coll Date Coll Time 12-SEP-2007 1105 Field No - Sampling Point1 Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Organic Results are indicated by BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 2.2 0.3 J 0.1 1.0 < 0.3 < 0.3 J 0.06 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dat 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18 -SEP-07 18 -SEP-07 18 -SEP-07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1This report was modified by 3M prior to TSCA 8(e) submission to remove the property ow ners' names from the "sampling point" field of the report form Group 312474 /6 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program: TB Program Name: Superfund-PFC Samples: 200729214 - 200729214 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page : 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729214 ; Receiving Comments: - Coll Date Coll Time 12-SEP-2007 1050 Field No - Samp 1inq Poi n t1 Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Organic Results are indicated bv BOLD. Result Codes Result Rept Level 555 PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 2.4 J 0.2 J 0.1 1.0 < 0.3 < 0.3 J 0.1 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dati 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1 This report was modified by 3M prior to TSCA 8(e) submission to remove the property owners' names from the "sampling point" field of the report form. Group 312475 p. 16 Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB c.-gram Name: Superfund-PFC Samples: 200729215 - 200729215 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729215 j Receiving Comments: Coll Date Coll Time 12 -SEP-2007 1205 Field No - Sampling PointJ Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Orqanic Results are indicated bv BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 1.5 J 0.1 < 0.3 J 0.26 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0 .3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Date 18-SEP-07 18 -SEP-07 18 -SEP-07 18 -SEP-07 18-SEP-07 18 -SEP -07 18 -SEP -07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1This report w as modified by 3M prior to TS C A 8(e) subm ission to rem ove the property ow ners' nam es from the "sam pling point" field o f the report form. Group 312476 17 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program: TB Program Name: Superfund-PFC Samples: 200729216 - 200J729216 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729216 Receiving Comments: - Coll Date 1 2 -SEP-2007 Coll Time 1240 Field No - Sampling Point1 Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Orqanic Results are indicated bv BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 1.7 J 0.2 J 0.06 J 0.2 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dat 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18 -SEP-07 18-SEP-07 18-SEP-07 Result Code Description J The analyte was positively identified. The result is below the report leve 1 and is estimated. 1 This report was modified by 3M prior to TSCA 8(e) submission to remove the property owners' names from the "sampling point" field of the report form Group 312480 Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB P U gram Name: Superfund-PFC Samples: 200729217 - 200729217 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729217 Receiving Comments: - Coll Date Coll Time 12 -SEP-2007 1250 Field No - Sampling Point1 Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Orqanic Results are indicated by BOLD. Result Codes Result Rept Level Units PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 2.6 J 0.28 J 0.1 0.7 < 0.3 < 0.3 < 0.3 0.3 ug/L 0.3 ug/L 0.3 ug/L 0.3 ug/L 0 .3 ug/L 0 .3 ug/L 0.3 ug/L Analysis Date 18-SEP-07 18 -SEP-07 18 -SEP-07 18 -SEP-07 18 -SEP-07 18-SEP-07 18-SEP-07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1This report w as m odified by 3M prior to TS C A 8(e) subm ission to rem ove the property ow ners' nam es from the "sam pling point" field of the report form Group 312471 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program: TB rogram Name: Superfund-PFC Samples: 200729218 - 200729218 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID Project Name 3M WOODBURY/COTTAGE GROVE _ Sampled By JEFFREY ARNDT Sample No: 200729218 ; Receiving Comments: - Coll Date Coll Time 12 -SEP-2 007 1215 Field No - Sampling Point^ Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Orqanic Results are indicated by BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 1.3 J 0.2 J 0.1 0.9 < 0.3 < 0.3 J 0.07 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Date 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Description The analyte was positively identified. The result is below the report level and is estimated.1 1 This report was modified by 3M prior to TSCA 8(e) submission to remove the property owners' names from the "sampling point" field of the report form. Group 312472 p. 20 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program: TB Program Name: Superfund-PFC Samples: 200729219 - 200729219 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729219] Receiving Comments: - Coll Date Coll Time 12-SEP-2007 1225 Field No - _ _____ Sampling Point1 Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Orqanic Results are indicated by BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 2.5 J 0.2 J 0.06 J 0.2 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Date 18-SEP-07 18-SEP-07 18 -SEP-07 18-SEP-07 18-SEP -07 18-SEP -07 18-SEP-07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1This report w as m odified by 3M prior to TS C A 8(e) subm ission to rem ove the property ow ners' nam es from the "sam pling point" field of the report form. Group 312477 9< / Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB rogram Name: Superfund-PFC Samples: 200729220 - 200729220 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729220 Receiving Comments: - Coll Date Coll Time 12-SEP-2007 1055 Field No - Sampling Point1 Trip Blank 200729223 Field Blank 200729222 **************************** SAMPLE RESULTS -fr*'*'*************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Organic Results are indicated by BOLD. Result Codes Result Rept Level 555 PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 1.7 J 0.2 J 0.1 0.6 < 0.3 < 0.3 J 0.05 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dat 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Description J The analyte was positively identified, is estimated. result is below the report level and 1This report w as m odified by 3M prior to TS C A 8(e) subm ission to rem ove the property ow ners' nam es from the "sam pling point" field of the report form. Group 312478 52. p. 22 Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB Program Name: Superfund-PFC Samples: 200729221 - 200729221 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729221 j Receiving Comments: - Coll Date Coll Time 12 -SEP-2007 1225 Field No - Sampling Point1 Trip Blank 200729223 Field Blank 200729222 ** * ** * * * ** + ** ** SAMPLE RESULTS + ^|r*'***'*'*'*'****'l|^,* * * * * * ,*, * * * * * '* * * * Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Organic Results are indicated by BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS 2.5 J 0.2 J 0.07 J 0.2 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dat 18-SEP-07 18-SEP-07 18-SEP-07 18 -SEP-07 18 -SEP-07 18 -SEP-07 18 -SEP-07 Result Code Description J The analyte was positively identified. The result is below the report level and is estimated. 1This report was modified by 3M prior to TSCA 8(e) submission to remove the property owners' names from the "sampling point" field of the report form. Group 312479 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program: TB Program Name: Superfund-PFC Samples: 200729222 - 200729222 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID - Project Name 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729222 I Receiving Comments: - Coll Date Coll Time 12-SEP-2007 1230 Field No - Sampling Point FIELD BLANK Trip Blank 200729223 Field Blank 200729222 ****************************** s a m p l e RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Organic Results are indicated by BOLD. Result Codes Result Rept Level 555 PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS < 0.3 < 0.3 < 0.3 < 0.3 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Date 18 -SEP-07 18 -SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 2< / Group 312464 p. 24 Minnesota Department Of Health - Environmental Laboratory- Final Report - Client Copy - Report Of Analytical Results Program: TB P c.gram Name: Superfund-PFC Samples: 200729223 - 200729223 Date Received: 12-SEP-2007 Date Generated: 20-SEP-2007 Request Page: 1 of 1 Date Reported: 20-SEP-2007 Site ID Project Name _ 3M WOODBURY/COTTAGE GROVE Sampled By JEFFREY ARNDT Sample No: 200729223 j Receiving Comments: - Coll Date Coll Time 12-SEP-2 007 1230 Field No Sampling Point TRIP BLANK Trip Blank 200729223 Field Blank 200729222 ****************************** SAMPLE RESULTS ****************************** Unit: ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-07 Note: Positive Oraanic Results are indicated bv BOLD. Result Codes Result Rept Level PFC Expanded List PFBA PFPeA PFHxA PFOA PFBS PFHxS PFOS < 0.3 < 0.3 < 0.3 < 0.3 < 0.3 < 0.3 < 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L Analysis Dat 18 -SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18 -SEP-07 18 -SEP-07 Group 312463