Document NGKeGxR0OVR4nYZyYbNDbEm4w

P. Final Report 3M ENVIRONMENTAL LABORATOR Y REPORT NO. E07-0584 Z2(a - 3 Analysis of PFBA and PFOA in Aqueous Samples collected from Cottage Grove Private Residences Laboratory Request Number: E07-0584 Report Date : 1013/2007 Method Requirement: 3M Method ETS-8-44 .0 Method of Analysis for the Determination of Perfluorinated Compounds in Water by 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-2 7 PO Box 333 1 Saint Paul, MN 55133-3331 Phone: (651) 778-5150 Fax: (651) 778-7203 This laborato ry maintains A2LA accreditation to fSOlIEC 17025 :2005 for the specific testslcalfbrations listed In A2LA Certificate R 2052-01 and meets the relevant quality systems requirements of ISO 9001 :2000 . The tests results included in this report, however, are not covered by this accreditation 3M CONFIDENTIAL PAGE 1 OF 1 1 2 p. 2 3M ENVIRONMENTAL LABORATOR Y REPORT NO, E07-0584 3M Envi ronmental Laborato ry 3M Environmental Laboratory Manager : William 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 Gro ve Private Residences Report Date: October 3, 2007 ail . .. . . .. . . ILI . . .. . .. .. The 3M Environmental Laboratory analyzed water samples collected from nine private residences in Cottage Grove, MN . Water samples were collected by Pace Analytical Field Services personnel on September 12, 2007 . Samples were retumed to the 3M Environmental Laboratory for analysis of perftuorobutanoic acid (PFBA) and perfluorooctanoate (PFOA) under laboratory project number E07- 0584 . 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 matrix spikes were fortified with an appropriate matrix 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 of PerFluorinated Compounds in Water by LCIMSIMS ; Direct tinjection Analysis" on September 13-14,2007 , Table 1 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. The 3M Environmental 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 9001 :2000 . However, ETS 8-044 .0 does not fall under the lab's current scope of accreditation . This laborato ry maintains A2LA accreditation to ISOIIEC 17028:2005 for the specifi c tests/cal ib rations listed in A2LA Certificate # 2052-01 and meets the relevant quality systems requirements of ISO 9001 :2000. The tests results included in this re port , however, a re not covered by this accreditatio n 3R, . .., ., .~ ., , ... PAGE 2 OF 11 ~ p. 3 3M ENVIRONMENTAL LABORATOR Y REPORTNO. E07-0 584 Table 1 . (')Results Summary . 31N 1.hNS ID pesc~ ' PFBA rFoA Concen6ailon conoentraton E07-0584001 9675 Miller Road, sample E07 -0 584-002 9675 Miller Road, sample dup 2,23 1 .09 2.23 1 .09 Aver-age %RPD e E07-0584-005 9735 Miller Road, sample E07-0 584-006 9735 Miller Road, sample dup 2.23 1.09 0.00 0.00 1 .88 0 .747 1 181 0.720 Awrage 1.85 0.734 %RPD 3.8 3.7 E07-0584-009 9747 Miller Road, sample 2 .50 1 .12 E07-0584-0 10 9747 Miller Road, sample dup 2,45 1 1 3 %RPD S E07-0584-013 9501 Islay Road, sample E07-0584014 9501 Islay Road, sample dup 9bRPD ane~ Average 248 1 .13 2.0 0.89 Average 1 .82 1 .76 1.79 0.254 0.254 0.254 e 3: t 0.00 E07-0584-017 9564 Islay Road, sample 1 .39 0 .980 E07-0584-018 9564 Islay Road, sample dup 1 .42 0 .97 3 35RPP E07-0584-021 9567 Islay Road, sample E07-0584-022 9567 Islay Road, sample dup Average 1.41 e 2! 2.70 2.86 0.977 0.72 0.278 0.282 3GRPD E07-0584-025 9655 Islay Road, E07-0584-028 9655 Isla Road, sample dup %RPD E07-0584-033 8724 95th St. South, sample E07 -0 58"34 8724 95th St. South, sample dup Average 278 e DUP 5.8 sample 3.03 2.89 Average 298 4.7 1 .81 1 .69 0.280 1.4 0.912 0 .89 8 Q803 1.5 0 .332 0 .333 Arrerage %RPD e E07-0584.037 8811 West Point Douglas Road, sample E07-0584 .038 8811 West Point Douglas Road, sample Dup 1 .75 6.9 2.92 2.99 0 .333 0.30 0 .433 0.425 Average 298 0.429 %RPO e LXE 2 .4 1.9 (1) Samples were analyzed by direct Injection using method ET5-8-044 .0. ETS-$-044 .0 is not included on the 3M Environmental taboratory's ISO 17025 scope of accredRation . The analytical method uncertainties associated with the reported results are as follows: PFBA t 30r6, PFOA t 25%. Refer to Sections 3 and 4 for data acceptance orReria and discussion . 3M CONFIDENTIAL PAGE 3 OF 1 1 ~ p. 4 3M ENVIRONMENTAL LABORATOR Y REPORT NO. E07-0584 . ! .. 2.1 Methods Analysis for PFBA and PFOA was completed following 3M Environmental Laboratory method ETS-8044.0 "Determination of Pesfluosinated Compounds in Water by LClMS1MS; Direct Injection Analysis" . 2 .2 Sample Collection Samples were collected in NalgeneT''" (!ow-density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, bottles designated fnr field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing the analytes of interest. Collected sample bottles were retumed to the laboratory at ambient conditions on September 12, 2007 . 2.3 Sample Preparatio n An aliquot of a well mixed sample was removed for analysis and placed in an autovial . 2.4 Analysi s All samples and quality control samples were analyzed for the target analytes using high performance liquid chromatography/ tandem mass spectrometry (MPLCIMSIMS) . Pertinent instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below . Table 2 . Instrument Parameters . Instrument Name ETSOIIie Analytical Method followed ETS-8-044.0 Li id Chromatograph A iient 1100 Guard column Betasil C8 4 .6 mm .X 150 mm), 5 prn Analytical column Betasil C18 4 .6 mm X 150 mm , 5 Iniecdon Volume 100 PL Mass 3 meter Applied Bi tems API 4000 Ion Source Turbo Spray Electrode Z-s ra Polarity Negative Software Ana 1 .4 .2 3M CONFIDEN'riAL PAGE 4 OF 11 p. 5 3M ENVIRONMENTAL LABORATORY REPORTNO . E07-0584 Table 3 . Liquid Chromatography Gradient Program . stop row riffle Row Rate Number (min) &LmuR) Percent A Pmterrt 8 mM amnronlum 0 0 1000 97 3 1 0-5 1000 97 3 2 11 .0 1000 5 95 3 13.5 4 13.6 1000 1000 5 95 97 3 5 17.0 1000 97 3 Table 4 . Mass Transition s Analyte Mass Transition Dwell Time (msec) Qi/Q? ET301Ke PFBA 213/1 69 200 S')PFOA 4131369 200 413/219 200 413/169 200 (1) The ind'n+idual transitions were summed to produce a"total Ion chromatogram" (rIC). The TICs were used for quantita6on. .. T . . 1 . . . . . .. .. . ::14 . .. - . . .. . . . 3.1 Calibratio n Calibration standards were prepared by spiking known amounts of stock solutions containing the target analytes into reverse-osmosis purified water. A total of thirteen calibration standards ranging from 0 .025 nglmL 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 of each curve point . Each calibration standard included in the final calibration curve met the method calibration accuracy requirement of t25% . Correlation coefficients (r) were greater than 0 .99 for both analytes . 3 .2 Limit of Quantitation (LOQ) The LOQ for 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 at 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 LOO for PFBA and PFOA was 0 .0491 ng1mL and 0.0727 ng/mL, respectively . 3M CONFIDENTIAL PAGE 5 OF 11 p. 6 3M ENVIRONMENTAL LASORA TOR Y REPORT NO. E07-0584 3.3 Continuing Calibratio n During the course of the analytical sequence, continuing calibra ti on verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control . All samples were bracketed by method compliant CCVs with recoveries of 100125% . 3.4 Blanks Several bianks of reverse osmosis purified water were analyzed th ro ughout the analytical sequence and were used to evaluate method performance and to determine the L OQ for each analyte 3.5 Lab Control Spikes (LCSs ) Low and high lab control spikes were prepared and analyzed in triplicate. The LCS samples were prepa red by spiking known amounts of the analytes into 40 mL of reverse osmosis treated deionized water to produce the desire d 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 independentl y at each concentration level . All LCS recoveries were used in the determina ti on of the analytical uncertainty . The following calculati ons were used to generate data in Table 5 . LCS Percent Recovery = Calcul` ate1 d Co0 ncen0 tratio% n Spike Con centration LCS% RSD = standard deviation LCS replicates .100% average LCS recovery Table 5 . Lab Control Spike Recoveries . PFea PicoA Spiked Sample conc. Comment Sample 1D n CaIC. Spiked Conc. Conc. n /rRec. n Cak. Conc. n i6Rea LOS-1 LCS070913-1 0.198 0.183 92.5 0.195 0.261 134 LCS-2 LCS0709132 0.198 0 .195 90 .4 0 .195 0.248 127 LCS-3 LCS070913-3 0.198 0 .235 119 0 .195 0.245 125 LCS-4 LCS070913-4 3.96 4 .14 105 3 .91 3 .97 101 LCS-5 LCS070913 -5 3.96 4.34 110 3 .91 4 .26 109 LCS-6 LCS070913-6 3.96 4 .04 102 3 .91 3.9 99 .8 Average LCS-1 through-3 103 () 1 29 %RSD LCS-f triro h-3 13 3.7 Average LCS-4 through-6 108 103 9GRSDLCS-tlhro h-8 3.8 4.8 OveraN A ye/age 40 4 116 Overall %RSD 89 13 (1) Average PFOA recovery 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 3M ENVIRONMENTAL LABORA TOR Y REPORT N0. E07-0584 LCS Perce nt Recovery = Calculated Concentration ,100k Spike Concentration LCS1o RSD = standard deviation LCS replicates .100% average LCS recovery 3.6 Analytical Uncertaint y Analytical uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision . The method unce rtain ty is calculated following ETS-1 2-012 .2 . The standard deviation is calculated for the set of accuracy results ( in %) obtained for the QC samples . The expanded uncertainty is calculated by multiplying the standard deviation by factor of 2, which co rrespond with a confidence level of 95% . Table 6 . Analytical Method Uncertainty . Number of data points used for Standard Analyte determining uncertainty Deviati on Method UrK:ertat PFBA 50 14.8 130% PFOA 50 12.6 t 25P/6 3.7 Field Matrix Spikes (FMS ) Low and high field matrix spikes were collected at each sampling point to verify that the analytical method is applicable to the collected matrix. Field matrix spikes are generated by adding a measured volume of field sample to a container spiked by the laborato ry with the target analytes p rior to shipping. Field matrix spike recoveries within method acceptance c rite ri a of 100 30rb confirm that'unknown' components in the sample mat rix do not significantly interfere with the extraction and analysis of the analytes of interest . Field matri x spikes are presented in the section 4 of this report Generally two spike levels are pre pared as ETS 8-44 .0 states th at FMS levels should be between 0 .5 to 10 times the andogenous sample con ce ntration . If a given FMS level does not meet this cri te ria, the rec overy 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 FMS- Average Concentration : Field Sample & Field Sample Dup .) * ~ Spike Con centraton 1 DOn Table 7. Field Matrix Spike Concentration s PFBA Spike PFOA Spike Description Conc. Conc. n L ngkn L Low Field Matrix Spike 0 504 0.256 High Field Matrix Spike 4 5 8 2 .33 3M CONFIDENTIAL PAGE 7 OF 11 ~ p. 8 ..,,. 3M E1WfROMMENTAL LABORA TOR Y REPORT NO. E07-0684 The table below summarizes the sample results and field mat ri x spike ( FMS) recoveries for the nine locati ons as well as the T ri p Blank. The table p rovides the average concentration and the relative perce nt differenoe (RPD) of the sample and sample duplicate . Results and average values are ro unded to three significant figures . Percent relative difference (%RPD) values are rounded to two significant figures . Because of rounding, values may va ry slightly fro m those listed in the raw data . Field matrix spikes meeting the method acceptance c riteri a of 100 30% demonstrate that the method is app ro pri ate for the given matrix . Table 8 . Data Summary with Q C . 9673 Millet Road PFBA PFOA 3M UMS ID Sample Desni 'on Cona n FMS FMS %Recovery ConC. n %Reco E07-0584-001 9675 Milier Road, sample 2 .23 NA 1 .09 NA E07-0584-002 9675 Miller Road, sample dup 2 .23 NA 1 .09 NA E07-0 584-003 9675 Miller Road, low spike 2 .82 NR 1,40 NR E07-0584 -0 04 9675 Miller Road, high spike 7 .10 106 3 .34 96.6 Average 223 1.09 %RPD 0.0 0.0 9736 Milker Road PFBA PFOA 3M U M S I D FMS FMS Sa Descrl on Conc. (ngftL) ' eco Conc. n %fteco E07-0584-005 9735 Miller Road, sample 1 .88 NA 0 .747 E07-0584-006 9735 Miner Road, sample dup 1 .81 NA 0.720 E07-0584-007 9735 Miller Road, law spike 2.29 NR 0 .994 E07-0584-008 9735 Miler Road, high s Dike 6 .59 104 300 Average 1.85 0.734 %RPD 3.8 3.7 IVA NA NR 97 .3 974 7 Miller Road PFBA PFOA 3M L1MS ID e Desaf Conc. FMS FMS %Recovery Conc. n %Recovery E07-0584-009 9747 Miller Road, sample 2 .50 E07-0584-010 9747 Miller Road, sample dup 2 .45 E.07-0584-0 11 9747 Miller Road, low apike 2 .98 E07-0584-012 9747 Miner Road, h' h spike 7 .30 Average 2.48 g6itPD NA NA NR 105 P,0 1 .12 1 .13 1 .38 3.39 1.13 0.89 NIA NA NR 97 .2 3M CONFIDENTIA L ~ PAGE 8 OF 11 P-9 3M ENVIRONMENTAL lr46OR,4TOR Y REPORT NO. E07-9584 Table 8 Continued . 950i Is1a Road PFBA PFOA 3M LMS ID Sa le aescii yon Conc. n FMS FMS %Reco Conc n %Reco E07-0584-013 9501 Islay Road, sample 1 .82 NA 0 .254 NA E07-0584-014 9501 Islay Road, sample dup 1 .76 NA 0,254 NA E07-0584-015 9501 Islay Road, low spke 2.40 NR 0.512 101 E07 -0584-0 16 9501 Islay Road, high spike 7.03 114 2.74 107 Aveaye 1 .79 0t,254 %RPD 3.4 0.0 9564lsla Road PFBA PFOA 3M UMS ID Lamle Descrf Con Canc. n FMS FMS %Rooovwy Corrc. n %Rwoverv E07-0684-d17 9564 Islay Road, sample E07.0584-018 9564 Islay Road, sample dup E07-0584-019 9564 tslay Road, low spice E07-0584 -020 9564 Islay Road, high ike 1 .39 NA 1 .42 NA 2.01 NR 6.65 115 0.980 NA 0.973 NA 1 .23 NR 3.54 11 0 pve'age 1.4 1 0.977 S6RPD Y.? 0.72 95671s/a Road PFpA PFQA 3MLlMSlD Sa Descrr ffon Corrc. n FMS qUS %Recoverv Con c . n %Reco E07-0584-021 9567 Islay Road, sample 2.70 NA E07-0584-022 9567 Islay Road, sample dup 2 .86 NA E07-0584-023 9567 Islay Road, low spike 3 .15 NR E07-0584-0 24 9567 Islay Road, high spike 7 .47 102 Average 2.78 905 Isla Road %RPD -5.8 PFBA 0.278 NA 0.282 t,lq 0.565 111 2 14 106 01 Z80 y .4 PFOA 3M LIMS ID Sample Descrf Conc. 72tu FMS %Recovery E07-0584-025 9655 Islay Road, sample 3 .03 NA E07-0584-026 9655 tslay Road, sample dup 2 .89 NA E07-0584-027 9655 Islay Road, low spike 3 .53 NR E07-0584-028 96b5 Islay Road, high spike 8.03 111 A verage 296 %RPD 4.7 /'iNS Conc . Lnfi"g %Recovery 0.912 NA 0.898 NA 1 .19 NR 3 .76 123 0.905 1.3 3M CONFIDENTIAL PAGE 9 OF 11 16 P . 10 3M ENVIRONMENTAL LABORATOR Y REPORT NO E07-0584 Table 8 Continued . 8724 95tb SL South PFBA PFOA 3ML11NSID FMS S a D e s c r f bn C o n c. ' /. R O C O Conc. n FMS 96R000 E07-0 584 -0 33 8724 95th St. South, sample 1 .81 NA 0 .332 INA E07-0584-034 8724 95th St . South, sample dup 1 .69 NA 0.333 NA E07 -0 584-035 8724 95th St . South, low spike 2 .18 NR 0 600 104 E07-0584-036 8724 95th St . South, high spike 6 .83 111 2 .73 103 Average 1 .75 0.333 %RPD 6.9 0.30 8811 West Point DO las Road PFBA PF;OA 3M Ll1NS ID Descr! aon FMS FMS Conc. n %Reoo Conc. 8811 West Point Douglas Road , E07-0584-037 sample 2.92 NA 0433 NA 8811 West Point Douglas Road , E070584-036 sample Dup 2.99 NA 0.425 NA 8811 West Point Douglas Road, E07-0584-439 Low spike 3.51 NR 0 .745 123 E07- 0584 -040 8811 West Point Douglas Road, High spike 8 .73 126 2.94 108 Average 2.96 0.429 SSRPD 2.4 l.9 Tir B1ank PFSA PFOA 3 M VMS ID Sample D o s c i r C o n Cnne. n FMS fwlS :GReco C o n c. n Y.R E07-0584-045 Trip Btank <0.0491 NA <0.0727 MA E07-0584-046 Tri p Blank !_ow Spike 0 .629 125 0 .328 128 E07-0584-047 Trip Blank 1" 5 ike 5.35 117 2 .77 119 NR= Not Reportable . FMS ooncentration was <0.5 tirnes the endogenous sample concentration . 3M CONFIDENTIAL // PAGE 10 OF 11 p .11 3M ENVIRONMENTAL LABORATOR Y REPORT NO . E07-0584 x 9 Sample results for PFBA and PFOA were presented in Table 1 . Field matrix spike recoveries for all locations met meth od acceptance criteri a of 10030% for both analytes . All remaining sample and data (hardcopy and electronic) associated wi th this project will be retained and archived according to 3M Environmental Laboratory standard operating p ro cedures, .. ~ Y 14~ ~ ' 1~~~~' . , ~ f', ~ ~-'~~~~~, . ~ ~T ~~3 aG6~ Mic Ile D . Malinsky, h . Proj echnical Lead Da Clifft n . Jacoby, Ph ., Technical Reviewer Date % - ~~~..~~~C~C ~ William K . Reagen, Ph .D., Environmental Laboratory Management Dat e The 3M Environmental Laborato ry's Quality Assurance Unit has audited th e data and report for th is p roject . /0 C.>-) Quality As nce Representative Dat e 3M CONFIDENTIAL PAGE 11 OF 1 1 1Z p . 12 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 C10 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 . 13 p .13 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB Program Name : Superfund-PFC Date Samples : 200729212 - 200729212 Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID Project Name Sampled B y 3M WOODBURY/COTTAGE GROVE JEFFREY ARNDT Sample No : 200729212 1 1 Receiving Comments : - Coll Date Coll Time Field-No Sampling Poin t - - ---- ------------ --- ----- - 12-SEP-2007 1420 - Trip Blank Field Blank 200729223 20072922 2 *~***+*r**********r*********rr SAMPLE RESULTS * r***r*r**r**rr***r**r**r*r**r Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 555 PFC Expanded Lis t PFBA PFPeA J PF HxA J PFOA PFBS < PFHxS < PFOS < 2 .6 0 .2 0 .07 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . This report was modifi ed by 3M prior to TSCA 8(e) submission to remove the prope rty owners' names from the "sampling point" field of the repo rt form . Group 312473 ~~ p . 14 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB Date Received : 12-SEP-2007 Pc,qram Name : Superfund-PFC Date Generated : 20-SEP-200 7 -- - Request Page : 1 of 1 Samples : 200729213 - 200729213 ] Date Reported : 20-SEP-2007 Site ID Project Name Sampled By 3M WOODBURY/COTTAGE GROVE JEFFREY ARND T Sample No : 200729213 Receiving Comments : - Coll Date Coll Time Field No Sampling Pointl - -- -- - 12-SEP-2007 1105 - Trip Blank Field Blank 200729223 20072922 2 ******~*r********************* SAMPLE RESULTS *******+**********+**r******** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date PFC Expanded Lis t PFBA PFPeA PFHxA PFOA PFBS < PFHxS < PFOS J 2 .2 0 .3 J 0 .1 1 .0 0 .3 0 .3 0 .06 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is est imated . iThis report was modified by 3M prior to TSCA 8(e) submission to remove the prope rty owners' names from the "sampling point" field of the repo rt form . Group 312474 ~~ p .15 Minnesota Department Of Health - Environmental Laborator y Final Report - Client Copy - Report Of Analytical Results Program : TB Date Program Name : Superfund-PFC Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Samples : 200729214 - 2007292141, Date Reported : 20-SEP-2007 Site ID -- Proj ect Name S ample d By -- -- -- -- - - --- - - --- --- - - - --- 3M WOODBURY/COTTAGE GROVE JEFFREY ARND T ---- Sample No : 200729214, Receiving Comments : - Coll Date Coll Time 12-SEP-2007 1050 - Field-No - Sampling_Point i - - - Trip Blank Field Blank 200729223 20072922 2 +*rr***rrr**r******r+*t*tt*+*r SAMPLE RESULTS *****t**t***r*****rt***r**r*** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 555 PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA PFBS < PFHxS < PFOS J 2 .4 0 .2 0 .1 1 .0 0 .3 0 .3 0 .1 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . 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 16 p . 16 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB Prc :qram Name : Superfund-PFC Date Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Samples : 200729215 - 200729215 ] Date Reported : 20-SEP-2007 Site - 3M ID Pro- jec- t-N- ame-Sa- mple - d B y WOODBURY/COTTAGE GROVE JEFFREY ARNDT Sample No : 200729215! Receiving Comments : - Coll Date Coll Time Field No Sampling Pointi - 12-SEP-2007 1205 - Trip Blank Field Blank 200729223 20072922 2 ************r****r************ SAMPLE RESULTS ** **r*************rr*****r**** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date S PFC Expanded Lis t PFBA PFPeA J PFHxA < PFOA J PFBS < PFHxS < PFOS < 1 .5 0 .1 0 .3 0 .26 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 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 . 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 repo rt form . Group 31247 6 ~~ p .17 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB Program Name : Superfund-PFC Date Samples : 200729216 - 200729216 Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID Project Name - 3M WOODBURY/COTTAGE GROVE S ample d B y JEFFREY ARNDT Sample No : 200729216 Receiving Comments : - Coll Date Coll Time Field No - --- -- --- Sampli nq Pointi 1240 - -12SEP07 Trip Blank Field Blank 200729223 20072922 2 ********r*r*****r********rr*** SAMPLE RESULTS *** ****tttr**ttt*r**t**r*r**** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 555 PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA J PFBS < PFHxS < PFOS < 1 .7 0 .2 0 .06 0 .2 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . This report was modified by 3M prior to TSCA 8(e) submission to remove the prope rty owners' names from the "sampling point" field of the report form Group 312480 p . 18 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB P ,tam Name : Superfund-PFC Date Samples : 200729217 - 200729217 Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID - 3M Proje c t Name WOODBURY/COTTAGE - -- - Sampled B y GROVE JEFFREY ARNDT Sample No : 200729217I Receiving Comments : - Coll Date Coll Time Field No Sampling Pointl 12-SEP-2007 1250 Trip Blank Field Blank 200729223 20072922 2 r*r*+************************* SAMPLE RESULTS **************r*****+********* Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 1 .1,PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA PFBS < PFHxS < PFOS < 2 .6 0 .28 0 .1 0 .7 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 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 . This report was modified by 3M prior to TSCA 8(e) submission to remove the prope rt y owners' names from the "sampling point" field of the repo rt form . Group 31247 1 Iq p .19 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB Program Name : Superfund-PFC Date Samples : 200729218- 200729 21 8 Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID Proje ct Name - 3M WOODBURY/COTTAGE GROVE Sampl ed B y JEFFREY ARNDT Sample No : 200729218' Receiving Comments : - Coll Date Coll-Time Fi e l d No --- -- -- 12-SEP-2007 1215 - - S -- amp- l ing P- oi nt l Trip Blank Field Blank 200729223 20072922 2 r****r**r*rr********tt***r***r SAMPLE RESULTS * r***ttr*r**t****t*****r****** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 555 PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA PFBS < PFHxS < PFOS J 1 .3 0 .2 0 .1 0 .9 0 .3 0 .3 0 .07 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . 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 repo rt form . Group 312472 ~,~ p . 20 Minnesota Department Of Health - Environmental Laborator y Final Report - Client Copy - Report Of Analytical Results Program : TB P :c,c]ram Name : Superfund-PFC Date Samples : 200729219 - 200729219 Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID 3M Project Name WOODBURY/COTTAGE GROVE Sampled B y JEFFREY ARNDT Sample No : 200729219~ Receiving Comments : - Coll Date Coll Time Field No Sampling Pointl -- --- - 12-SEP-2007 1225 - Trip Blank Field Blank 200729223 20072922 2 **************t*****r******r*r SAMPLE RESULTS ********r*****************+*** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA J PFBS < PFHxS < PFOS < 2 .5 0 .2 0 .06 0 .2 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . ~ This report was modified by 3M prior to TSCA 8(e) submission to remove the propert y owners' names from the "sampling point" field of the repo rt form . Group 312477 p . 21 Minnesota Department Of Health - Environmental Laborator y Final Report - Client Copy - Report Of Analytical Results Program : TB Program Name : Superfund-PFC Date Samples : 200729220 - 2007292201 Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID - 3M Project Name Sampled B y WOODBURY/COTTAGE GROVE JEFFREY ARNDT Sample No : 200729220 Receiving Comments : - Coll Date Coll Time Field No Sampling Poin t l - - - - - 12-SEP-2007 1055 - - Trip Blank Field Blank 200729223 20072922 2 ***r*******r**rr*rr*****r****r SAMPLE RESULTS * **********rrt*t****r****r*rr* Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 555 PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA PFBS < PFHxS < PFOS J 1 .7 0 .2 0 .1 0 .6 0 .3 0 .3 0 .05 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . -- - - - iThis report was modi fi ed by 3M prior to TSCA 8(e) submission to remove the prope rty owners' names from the "sampling point" field of the repo rt form . Group 312478 ~ ~~ p . 22 Minnesota Department Of Health - Environmental Laboratory Final Report - Client Copy - Report Of Analytical Results Program : TB F-(,qram Name : Superfund-PFC Date Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 - -_ _____ Request Page : 1 of 1 Samples : 200729221 - 200729221 Date Reported : 20-SEP-2007 Site - 3M ID Project Name Sampled B y WOODBURY/COTTAGE GROVE JEFFREY ARNDT Sample No : 200729221', Receiving Comments : - Coll Date Coil Time Field No Sampling Pointl 12-SEP-2007 1225 - Trip Blank Field Blank - -- -2-20793 0072922 2 *rr**********r*********r****** SAMPLE RESULTS ****************r**********+*r Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Orqanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date > ,t)PFC Expanded Lis t PFBA PFPeA J PFHxA J PFOA J PFBS < PFHxS < PFOS < 2 .5 0 .2 0 .07 0 .2 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 0 .3 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 Result Code Descriptio n J The analyte was positively identified . The result is below the report level and is estimated . ~ This report was modified by 3M prior to TSCA 8(e) submission to remove the prope rty owners' names from the "sampling point" field of the repo rt form . Group 312479 ~ p . 23 Minnesota Department Of Health - Environmental Laborator y Final Report - Client Copy - Report Of Analytical Results Program : TB Date Program Name : Superfund-PFC Samples : 200729222 2 007 29222j Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Date Reported : 20-SEP-2007 Site ID - - - Project Name Sam pl ed B y -- - - -- - - - - - -- - --- - 3M WOODBURY/COTTAGE GROVE JEFFREY ARND T Sample No : 200729222 1 Receiving Comments : - Coll Date Coll Time Field No - -- - Sa- mpli- ng-P - o- in- t - 12-SEP-2007 1230 - FIELD BLANK Trip Blank Field Blan k 200729223 20072922 2 r*r***r*******r**r*****tt***** SAMPLE RESULTS **** r****t**t*rtt****r*tr***tt Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive Organic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 555 PFC Expanded Lis t 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 ug/L ug/L ug/L ug/L ug/L ug/L ug/L 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-07 18-SEP-0 7 c~2V Group 312464 p . 24 Minnesota Department Of Health - Environmental Laborator y Final Report - Client Copy - Report Of Analytical Results Program : TB Pc,(3ram Name : Superfund-PFC Date Received : 12-SEP-2007 Date Generated : 20-SEP-200 7 Request Page : 1 of 1 Samples : 200729223 - 200729223, Date Reported : 20-SEP-2007 Site ID 3M Project Nam e Sampled By WOODBURY/COTTAGE GROVE JEFFREY ARNDT Sample No : 200729223 Receiving Comments : - Coll Date Coll Time Field N o Sampling Point 12-SEP-2007 1230 - TRIP BLANK Trip Blank Field Blank 200729223 20072922 2 **r*******rr*********r***r**** SAMPLE RESULTS ** ***r*****r**************r*** Unit : ORGANIC CHEMISTRY Reviewed By PDS on 20-SEP-0 7 Note : Positive OrcTanic Results are indicated by BOLD . Result Codes Result Rept Level Units Analysis Date 1 1)PFC Expanded Lis t 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 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-07 ug/L 18-SEP-0 7 ,,~~~~ Group 312463