Document 6wDEQr91D60LE9DYz7dMQd2E3

Katherine E. Reed, Ph.D. Staff Vice President 3M Environmental, Health and Safety Operations RECEIVED 900 Bush Avenue, Building 42-2E-26 PO Box 33331 St. Paul, MN 55133-3331 651 778 43B1 V. ; n t V /A f -ftBjfifo) im p * SO- 3 5c 3 Certified Mail " _ M H Q - 0 k 0 6 , OO3 V/- CD O' * April 14, 2006 3* -X} yo Document Processing Center M EPA East - Room 6428 Attn: Section 8(e) Office o f Pollution Prevention and Toxics US EPA 9.9.6 _ 5 6 3 / fsi T J O --- t f T' S3* O ; SE c o r n Q m CD GO 1200 Pennsylvania Avenue N W Washington DC 20460-0001 89060000298 6 9 0 6 0 0 0 0298 no css ' 0"*1 Re: TSCA 8(e) Substantial Risk Notice: Sulfonate-based and Carboxylic-based Fluorochemicals, Docket Nos. 8EHQ-1180-374; 8EIIQ-0381-0394; -3 " P r:: 8EHQ-0598-373 - Results from Analysis o f Groundwater in the vicinity o f : Oakdale Disposal Site To whom it may concern: tv crt .C D 3M is submitting this notice to supplement its previous submissions on sulfonyl and carboxylic- based fluorochemicals. 3M has recently received the enclosed analytical report (3M Environmental Laboratory Report No. 06-0151) for groundwater samples collected in the vicinity o f the former Oakdale Disposal Site (Site) in Oakdale, MN. From the late 1940's until 1960, a variety o f industrial and municipal wastes were disposed o f at a property know as the Abresch site in Oakdale, MN. This location is also known as the Oakdale Disposal Site and underwent an extensive site remediation/cleanup in 1983-84. In 1985, a pump out system was installed to remove and contain solvent-impacted shallow groundwater at the Site. This system has been in continuous operation since installation. 3M has been leading a study, with involvement from the Minnesota Pollution Control Agency (MPCA) and Minnesota Department o f Health (MDH), to characterize the presence o f fluorochemicals at the Site. In an early phase o f this assessment, existing on-site and near site monitoring and pump-out wells were monitored for fluorochemicals. Results from this work are provided in Exygen Study No. P0001400, Interim Report #1, enclosed. A map depicting the locations o f these wells is also enclosed as Figure 1. The results from this early work were used as a basis for locating nine additional monitoring wells. Four o f these monitoring points are on site and five are in close proximity to the Site. The location o f these wells is provided on Figure 2, enclosed. Results from the first round o f sampling for these wells are contained in the aforementioned 3M Environmental Laboratory Report (No. 06-0151). The new wells were constructed to sample from four different geological strata: alluvium, Platteville limestone, St. Peter sandstone and the Prairie du Chien group. These are depicted on Figure 3 for the Site. Results for four o f the five offsite wells are below the limit o f quantitation 000001 <7 ^ 7 0 7 (0.025 ng/mL) for all analytes. Levels in the fifth offsite welfare significantly less than 1 ng/mL (ppb) for each analyte. While 3M does not believe that any o f these data taken alone or cumulatively meet the "substantial risk" reporting threshold, we nevertheless recognize die ongoing work by U.S. EPA to assess fluorochemical exposure pathways. Therefore, we are placing these results in the 8(e) docket as a supplement to previous submissions. If you have any questions, please do not hesitate to contact Gaiy Hohenstein at (651)778-5150. Sincerelv. Katherine E. Reed Staff Vice President Environmental, Health and Safety Operations Enclosures 000003 LEGEND A Piattevaie Weil St. Peter Well Plume of Isopropyl Ether in Plattevilla - 2003 StK3aESSOS Plume of Isopropyl Ether in Platteville - 1984 Source: Digital Aerial Photos, Metropolitan Council, 2 0 0 0 & Barr Engineering Co. 0SP-O98-1O A Figure 1 FC MONITORING PROGRAM WELLS G akdaie D isposa i S ite O akdale, M innnesota LEGEND | ] Basal Alluvium W ell | | Pump-out Well Water Table W ell Surface W ater Sampling Location ; Inferred Limits ot Abresch Disposal Site Area ' Form er Pum p-Out W ell, Converted to a Monitoring W ell tNORTH . . H * -. ? v , ` * v e ' I fi ;r #"*** AR226-3633 v. % , V l. * f f l f c . t -' ` '* 0 P V e S P y * .'* <f V 1- 4? M ,, . , >. $ & : % ; ** ^ Washmsiun Cu / i'ropci l\ ?* _ ... .W V rtf& L i i r u l -jaut * r ** ,: j ' r 5 r'v^ * .* * " ' i S k l f t f c * a L E G E N D [ `W ^ .,. * . - J t l i . ' S i ^ Res.duum Water Tabic Well pi - 1 Residuum Base Well q " Platteville Limestone Well J Si. i'eter S.mJsioiK Well a Prairie du Chien Well Aerial View o f the former 3M Oakdale disposal area showing the locations of the newly constructed wells. Figure 2 B 1100 1000 900 AR226-3634 B1 800 700 05P-0185-2 1 Sand to Silty Sand (Alluvium) 2 Silty Sand (Alluvium) 3 Sandy Silt (Till) 4 Silty Sand (Till) 5 Gravelly Sand (Alluvium) 6 Silty Sand (Alluvium) 7 Gravelly Sand (Alluvium) 8 Silty Sand (Alluvium) 9 Peat Grain size distribution and permeability data available W ell screen 0 250 500 750 1000 Horizontal Scale (Feet) Source: Barr Engineering Co. ,, GEOLOGIC CROSS SECTION B-B' Figure 3 OAKDALE DISPOSAL SITE, MN ooooos AR226-3635 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-Q151 Final Report Analysis of PFOA, PFOS, PFHS, and PFBS From Newly Constructed Wells at the Oakdale, Minnesota Disposal Site Laboratory Request Number: E06-Q151 Method Requirement: 3M Method ETS-8-154.1 (modified) Testing Laboratory 3M EHS Operations 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Requester Gary Hohenstein 3M Building 42-02-E-27 PO Box 3331 Saint Paul, MN 55133-3331 Phone: (651) 778-5150 Fax: (651) 778-7203 n ^ jp iT g p i Certificate #2052-01 The testing reported herein meet the requirements of ISO/iED 17025-1999 "General Requirements for the Competence of Testing and Calibration Laboratories" in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate in accordance with ISO 9001/ISO 9002 (1994). 3M CONFIDENTIAL PAGE 1 OF 18 ` .'I 0 0 0 0 .0 6 3M ENVIRONMENTAL LABORATORY REPORT NO. E0&0151 3NI Environmental Laboratory 3M Environmental Laboratory Manager William K. Reagen, Ph.D. 3M Technical Lead: Michelle Malinsky, Ph.D. Report Author: Michelle Malinsky/Susan W olf 3M Environmental Laboratory Professional Service Personnel Gabriel McMurtry, Pace Analytical, Lab Ops Cindy Carlson, Pace Analytical, Lab Ops Analytical Report E06-0151 Ground Water Samples from Newly Constructed Wells near the Oakdale, Minnesota Disposal Site ' . ; 1 March 13,2006 The 3M Environmental Laboratory extracted and analyzed ground water samples collected by Weston Solutions, Inc. personnel on March 2-3,2006 from newly constructed wells on and/or near the Oakdale, Minnesota 3M disposal site. Samples were returned to the. 3M Environmental Laboratory for analysis of perfluorooctanoate (PFOA), perfluorooctane sulfonate (PFOS), perfiuorohexane sulfonate (PFHS), and perfluorobutane sulfonate (PFBS) under laboratory project number E06-0161 using 3M . Environmental laboratory Method ETS 8-154.1 "Determination of Perfluorinated Adds, Alcohols, . , Amides, and Sulfonates in Water by Solid Phase Extractions and High Performance Liquid Chromatography/Mass Spectrometry1. The 3M Environmental Laboratory prepared sets of sample containers for nine sampling locations. Each sample set consisted of a field sample, field sample duplicate, low field spike (1.0 ng/mL) and . high field spike (.10 ng/mL). Each empty container was marked with a "fill to here" line which ; t . corresponded to a final volume of 450 mL. Containers reserved for field matrix spikes were fortified with an appropriate matrix spike solution containing the four target analytes prior to being sent to the field for sample collection. ; :' ( All samples were extracted on March 3,2006 and analyzed on March 3,2006 and on March 6,2006. 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. I\ fACCREOiTEPj Certificate #2052-01 The testing reported herein meet the requirements of ISO/1ED17025-1999 "General Requirements for the Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052-01. Testing that complies with this International Standard also operate ip accoidance with ISO 9001/ISQ 9002 (1994). 3M CONFIDENTIAL PAGE 2 OF 18 o o o e i 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 1. Sample Results Summary. 3MLIMSID SampleDescription WPFOA 0PFOS 0PFHS '" PPFBS Concentration Concentration Concentration .Concentration (ng/mL) v (ng/mL) . (ng/mL) x (ng/mL) E06-0151-Q82 E06-0151-083 OKMN GWS RW40 0 060302 OKMN GWS RW40 DB 060302 Average <0.0250 <0.0250 <0.0250 <0.0249 <0.0249 <0.0249 <0.0252 <0.0252 <0.0252 <0.0397 <0.0397 <0.0397 E06-0151-086 E06-0151-087 E06-0151-090 E06-0151-091 E06-0151-094 E06-0151-095 %RPD Sample/Sample Dup NA NA OKMN GWS1SP42 0 060302 <0,0250 <0.0249 OKMN GWS SP42 DB 060302 <0.0250 <0.0249 Average %RPD Sample/Sample Dup <0.0250 NA <0.0249 NA OKMN GWS PL43 0 060302 ,, s/! , .<p.025p , f0.0249.. . OKMN GWS PL43 DB 060302 .. '<0.0250 : , ; y;< 0.0 249 ' -v Average1: : I <0.0260 ; ' <0.0249 %RPD Sample/Sample Dup ' ' NA - ' na ' 1OKMN GWS RW39 0 060302 : <0.0250 ` ' y < 0.0 249 '; ' OKMN GWS RW39 DB 060302 ' <0.0250 ' - <0.0249 Average <0.0250 ' <0.0249 %RPD Sample/Sample Dup NA NA NA <0.0252 <0.0252 <0.0252 NA i <0.0252 <0.0252 <0.0252 NA <0.025,2 <0.0252 <0.0252 NA NA <0.0397 <0.0397 <0.0397 NA i . <0.0397 <0.0397 <0.0397 NA <0.0397 <0.0397 , <0.0397 NA E06-0151r098 * - OKMN G W S .P0450.060303 ' . -0.592. .y... . . 0.390 >.V ' 0.0649 E06-0151-098 v ' OKMN GWS PC45 0060303 i. E 06-0151-099 OKM N GWS 1*045 DB 060303 ^ .rr-i ' ' '' ^ AvdreWe:: %Rs6sam ple/Sampie DUb/Lab b ij|S ' ooi:. 3^ . 0.522 ' 0.464 - ' ' \ 0.449 'ir ' ' 0.543 ' ! ; ' k'b .b 4 ;'r v ,r ^ 7.9 ' r " . . 0.0635 0.0547 0.0610 J 9.1' E06-0151-102 E06-0151-103 OKMN GWS SP44 0 060303 OKMN GWS-SP4j4 D B 060303 <0.0250 .<0.0250. <0.0249 <0.0249 <0.0252 <0.0252 " ,'.;r , i '-.",0.1 v l Aysras-; <0.0250 <0.0249 . i <0;0252 % R PD Sam ple/Sam pleD up; ;-.NA ' ' 'N A ' \ NA E06-0151-106 E06-0151-107 OKMN GWS RW38 0 060303 OKMN GWS RW38 DB 060303 0.0525 0.0556 0.187 0,195 <0.0252 <0.0252 Average 0.0540 0.191 <0.0252 %RPD Sample/Sample Dup 5.7 4.2 NA E06-0151-110 OKMN GWS RW37 0 060303 0.312 2.47 <0.0252 E06-0151-110(5i E06-0151-111 OKMN GWS RW37 0 060303 OKMN GWS RW37 DB 060303 Average %RSD Sample/Sample Dup/Lab.Dup .. 0.282 0.298 0.297 5.0 ' ; 2.51 2.56 2-51 ,4 -` ,1.8 .= . <0.0252 <0.0252 <0.0252 NA E06-0151-114 v OKMN GWS PL41 0 060303 0.0766' * 0.0268 <0.0252 E06-0151-115 OKMN GWS PL41 DB 060303 Average 0.0796 0.0781 <0.0249 (6>0.0268 <0.0252 <0.0252 %RPD Sample/Sample Dup 3.8 NA NA <0.0397 <0.0397 <0.0397 NA <0.0397 <0.0397 <0.0397 NA <0.0397 <0.0397 <0.0397 NA <0.0397 <0.0397 <0.0397 <0.0397 NA : <0.0397 <0.0397 <0.0397 NA (1) The analytical uncertainty fo r PFOA was 1005.8% based on method accuracy and precision. See Section 3.7 for additional explanation. The lim it o f quantitation (LOQ) was 0.0250 ng/mL. Results and average values are rounded to three significant figures according to ERA rounding rules. %RPD values are rounded to tw o significant figures. 3M CONFIDENTIAL PAGE 3 OF 18 000008 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Because o f rounding, values may vary slightly from those listed in the raw data. Samples with reported results less than the LOQ o f 0.0250 ng/mL may or may not have PFOA present. Results less than the LOQ are not quantified. (2) The analytical uncertainty for PFOS was 1003.7 % based on method accuracy and.precision. See Section 3.7 for additional explanation. The lim it o f quantitation (LOQ) was 0.0249 ng/mL. Results and average values are rounded to three significant figures according to EPA rounding rules. %RPD values are rounded to tw o significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Samples With reported results less than the LOQ o f 0.0249 ng/mL may or may not have PFOS present. Results less than the LOQ are not quantified. (3) The analytical uncertainty for PFHS was 1008.6% based on method accuracy and precision. See Section 3.7 for additional explanation. The lim it o f quantitation (LOQ) was 0.0252 ng/mL. Results and average values are rounded to three significant figures according to EPA rounding mies. %RPD values are rounded to tw o significant figures. Because o f rounding, values may vary slightly from those listed in the raw data. Samples with reported results less than the LOQ o f 0.0252 ng/mL may or may not have PFHS present. Results less than the LOQ are not quantified. (4) The analytical uncertainty for PFBS was 1006.6 % based on method accuracy and precision. See Section 3,7 for additional explanation. The lim it o f quantitation (LOQ) was 0.0397 ng/mL. Results and average values are rounded to three significant figures according to EPA rounding rules. %RPD values are rounded to two significant figures. Because of rounding, values may vary slightly from those listed in the raw data. Samples w ith reported results less . than the LOQ o f 0.0397 ng/mL may or may not have PFBS present. t Results less than the LOQ are not quantified. (5) Sample results are for a laboratory extraction duplicate. The relative standard deviation (%RSD) is reported using ail three results (sample, laboratory duplicate, and sampierduplicate). (6) The average value listed is the concentration for the sample or sample duplicate that produced a vale above th e ' LOQ. A true average and %RPD between the sample and sample duplicate was not determined. M 2.1 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 of an appropriate matrix spiking solution containing the i analytes o f interest (PFOA, PFOS, PFHS, and PFBS). Collected sample bottles were returned to the laboratory at ambient conditions on March 3,2006. Table 2 below details the bottles prepared and the corresponding spike levels for each sampling location. Samples were collected from nine individual sites. Table 3 provides the key code for the sample descriptions. Table 2. Sample Collection and Spike Information. Final Concentration(ng/mL) Description Nominal. Final Volume (mL) PF0* PFOS PFHS S am ple : 450 Sample Duplicate " 450 ' Low Field Matrix Spike : 450 High Field M atrix Spike' 450 Trip Blank . 450 Trip Blank Low,Matrix Spike 450 Trip Blank High M atrix Spike 450 : V NA ' NA. : 0.999 ? 9.99 NA 0.999 : 9.99 NA : : NA 0.997 9.97 NA 0.997 9.97 NA . NA 1-01 , 10.1 . NA 1.01 10.1 PFBS . NA NA 0.992 9,92 NA 0.992 9.92 : 3M CONFIDENTIAL PAGE 4 OF 18 3MENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 3. Sample Description Key Code; SampleID Code Definition . RW- " : ' Residuum w ell ' PL Platteville Limestone w ell SP :: V >S t Peter Sandstone w ell P C .., OKMN , : Prairie du Chein well r Oakdale Minnesota s ite , \ . i ; . - GW ' Groundwater-Sample ' ' " 0. Sample . . DB Duplicate LS Low Spike HS High Spike The ground water samples, sample duplicates, and field matrix spikes returned for analysis all had visible sediment present which "colored" the water sample when Shakento disperse the solids. .-All collected samples were centrifuged to remove particulate before extraction. See Section 2.2 for more information. Additionally, the samples associated with RW37 generated a fairly strong petroleum odor. Thp table below describes additional observations noted for each of the sample locations. Table 4. Sample Observations. Observations WellIdentification SedimentColor SedimentAmount Other RW 37 G rey-brow n (1)M oderate Strong petroleum odor present RW 38 RW 39 ''. > R ust-brow n : : Rust-brown f Light ' NA > : V - - 'n p ly g n t , :'' NA ' RW 40 ;n ! RuS-brown ' * '' ' '^M d'rate' ' ' ' " NA PL41 SP42 `. : '' ' ! 'Vi ' Rubt-broW n:i ! ,?;' ' RuStrbrowri ' ! \\ V (,)M oderat .^ o d o ra te ' .. ' ' 't NA NA PL43 ' *" !" ' V ''U ' , Rust-brown . . . .... `.''Moderate ' ' NA . , SP44 " ' G re y-brow n / .....`''Moderate , , ; ' NA . PC45 R ust-brow n lijh t NA supernatant M V t ' (2) Light: after centrifugation o f a 40 mL aliquot solids present, but minimal. 2.2 Extraction All samples, calibration standards, and associated quality control samples'were extracted using the procedure outlined in ETS-8454.1 "Determination of PeHiubrinated Aci% , AJdohols, Amides, and Sulfonates in Water by Solid Phase Extractions and High Performance Liquid Chromatography/Mass Spectrometry". Briefly, 40 mL of sample were loaded onto a pre-conditioned Waters C18 solid phase extraction (SPE) cartridge (Sep-Pak, 1.0 g ,6 c c ) using a vacuum manifold. The loaded SPE cartridges were then eluted with 5 mL of methanol. This extraction procedure concentrates the samples by a factor of eight. (Initial volume = 40 mL, final volume = 5 mL). The calibration standards, lab control spikes, method blanks, and trip blank sample and spikes were extracted as described above, Because the collected ground water samples contained visibly significant amounts of sediment/particulate, the 40 mL aliquot was centrifuged at 3500 rpm for ten minutes for all samples, sample duplicates, low field , matrix spikes and high field matrix spikes prior to extraction. After centrifugation, the supernatant was ' loaded onto the SPE cartridge for extraction similar to the calibration standards and laboratory quality control samples. The remaining solids were retained if further extraction was deemed necessary. ETS-8-154.1 does not describe sample centrifugation prior to extraction. This method modification was 3M CONFIDENTIAL PAGE 5 OF 18 O O O O lO 3MENVIRONMENTAL LABORATORY REPORT NO. E06-0151 necessary as the sediment completely clogged the SPE cartridges almost immediately preventing complete loading of the water sample. The final methanol sample extracts had a slight yellowish color. Recoveries of laboratory matrix spikes and field sample matrix spikes demonstrated that the centrifugation step did not significantly impact the method performance. Samples were extracted and initially analyzed on March 3, 2006. The trip blank spikes for all four analytes produced recoveries of approximately 60%. Additionally, most field sample matrix spike recoveries were between 60-80%. Upon further review of the data, it was determined that an older standard was used to prepare the upper range of the calibration curve on March 3,2006 and that this standard was not the same one used to prepare the collection bottle spikes. On March 6,2006, anew extracted calibration curve was prepared using the same (newer) standard used to prepare the collection bottle spikes. Method blanks and lab control spikes at 1 ng/mL and 10 ng/mL were also prepared with the new curve. Additionally, the trip blank and trip blank field matrix spikes along with two samples (E06-0151-098 and E06-0151-0110) were also re-extracted. Furthermore, low and high lab matrix spikes at 1 and 10 ng/mL were prepared for the two samples selected for re-extraction. For the lab matrix spiked samples, an appropriate amount of spiking standard was added to the 40 mL sample aliquot before it was centrifuged to remove the solids. Analysis o f selected calibration points from the first curve (March 3,2006) against the the new curve (March 6,2006) demonstrated that a systematic bias of 20-30% Was present in the first analysis. All sample extracts from March 3,2006 were then reanalyzed against the new curve. All results presented here are from foe March 6,2006 analysis against foe new calibration curve. -, 2.3 Analysis All sample and quality control extracts were analyzed for the target analytes using high performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters, foe liquid chromatography gradient program, and foe specific mass transitions analyzed are described in the tables below. - Tables, instrument Parameters ' ' 7V ; . V ' ' 7 Instrum e nt Name L iq u id C hrom atograph G uard colum n A n a lytica l colum n In je ctio n V olum e M ass S pectrom eter Ion S ource E lectrode P o la rity S oftw are , ETSStan Agilent 1100 Betasil C18 {2.1 mm.XlOO mm), 5 urn Betasil C18 (2.1 mm X 100 mm), 5 urn 5 uL 1 Applied Biosystems A P I4000 Turbo Spray ' .....2-spray Negative Analyst 1.4.1 Table 6. Liquid Chromatography Gradient Program Step Number 0 1 2 3 4 5 Tom Time (min) 0 1.0 14.5 15.5 16.5 20.0 FlowRate (juUmin) 300 300 300 ;; 300 300 300 PercentA (2 mMammonium acetate) 80.0 80.0 10.0 io.o : 80.0 80.0 PercentB (Methanol) 20.0 20.0 90.0 ; 90.0 20.0 20.0 3M CONFIDENTIAL PAGE 6 OF 18 O O O O ll `M tr' 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 7. Mass Transitions Analyte (1)PFBS V . ' . !1)p f h s (1>PFOS (1>PFOA Mass Transition Q1/Q3 Dwell Time(msec) 299/80 299/99 . 125 . 125 '! 399/80 - 125 399/99 125 : 499/130 499/99 499/80 413/369 413/219 413/169 .. 125 , 125 ; 125 ' 125 ? T ' ' 125 " 125 ` Individual transitions wane summed to produce a "total ion chromatogram" (TIC). The TICs were used for quantitation. 3.1 Calibration Calibration standards were prepared byspiking known amounts o f methanolic, stock solutions containing PFQA, PFOS, PFHS, and PFBS into 40 mL of ASTM type I water. Each spiked water ; standard was then extracted in the same manner as the collected samples. A total of twelve spiked standards ranging from 0.025 ng/mL to 25 ng/mL (nominal) were prepared. A quadratic, 1/x weighted, calibration curve was used to fit the data for each analyte. The data was not forced through zero during the fitting process. Calculating the standard concentration using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point. Each extracted calibration standard used to generate the final calibration curve met the method calibration accuracy requirement of 25%. Th correlation coefficients (r) were greater than 0.999 for all analytes. 3.2 Limit of Quantitation (LOQ) The LOQ 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 limit of quantitation for PFOA, PFOS, PFHS, and PFBS is 0.0250 ng^mL, p,Q249 ng/mL, 0.0252 ng/mL, and 0.0397 ng/mL respectively Area count comparision for the rhethod .blanks and the lowest calibration standard will be provided in Section 3.5.1. , . 3.3 System Suitability Fiver replicate injections of the 5 ng/mL extracted-calibration standard was analyzed at the beginning of the analytical sequence to demonstrate overair system suitability, th e same standard was analyzed in triplicate at the end of the analytical sequence. All analytes met method acceptance criteria of less than 5% relative standard deviation (RSD) for peak area and less than 2% RSD for retention time for both opening and closing system suitability injections. ` 3.4 Continuing Calibration During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve was still in control. All CCVs produced recoveries within 1Q0%25%, which met method criteria. 3M CONFIDENTIAL I S -'5 ,; V PAGE 7 OF 18 000012 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 3.5 Blanks Three types of blanks were prepared and analyzed with the samples: method blanks, solvent blanks, and field/trip blanks. Each blank type is described below. 3.5.1 Method Blanks Several method blanks were prepared by loading 40 mL of ASTM Type I water onto a C18 SPE cartridge and eluting with 5 mL of methanol using the same extraction procedure as the samples. Method blanks were prepared to evaluate the levels of background contamination in the overall extraction process (reagent water, glassware, SPE cartridges, etc.) Table 8 lists the area counts for the method blanks and the LOQ standard associated with the given data set. Table 8. Method Blank Area Counts for Extractions performed on 3/6/2006. Sample Name Sample Comment SampleID s060306a025 Method Blank-1 M B -060306- s060306a026 Method Blank-2 MB-060306-2 s060306a027 Method Blank-3 M B -060306-3 s060306a028 Method Blank-4 M B -060306-4 s060306a029 Method Blank-5 MB-0S0306-5 s060306a030 Method Blank-6 M B -060306-6 s060306a031 Method Blank-7 M B -060306-7 sQ60306a032 Method Blank-8 MB-060306-6 Area Countsofhighestmethodblankmultipliedbytwo Area CountsLOQstandard LOQconcentration, ng/mL , : PFOA 11741 11689 11131 6189 8872 5558 20205 15076 40410 50284 0.0250 Area Counts PFOS PFHS (,)2880 1412 1814 993 1510 655 1982 5939 2265 ' 5101 1824 1613 1218 5292 1802 3964 . 5254 0.0249 4387 11878 21147 0.0252 PFBS 13417 4009 18787 4178 4717 1874 11821 14398 37574 54306 0.0397 (1) Determined to be a statistical outlier at the 80% confidence level using Dixon's Q -test Area value not used td establish the LOQ for PFOS. . ' ` 3.5.2 Solvent Blanks Several methanol solvent blanks were analyzed to assess system contamination and/or instrument carryover. Analyte peak area counts in all blank samples were less than half the area counts of the calibration standard used to establish the LOQ. 3.5.3 Field/Trip Blanks v Prior to sample collection, one sample container was filled with 450 mL of ASTM Type I water, sealed, and shipped to the sample collection1site along with the empty containers. This sample was analyzed as field/trip blank. The trip blank serves as an additional method blank that accounts for any storage conditions and/or holding time issues that the samples may experience. The target analytes were not detected above the stated LOQ in the trip blank. . 3.6 Lab Control Spikes (LCS6) For the extractions performed on March 3, 2006, low (0.25 ng/mL. nominal concentration) and high (7.5, ng/mL nominal concentration) lab control spikes were prepared and analyzed in triplicate. LCSs were prepared by spiking known amounts of the analytes into 40 mL of ASTM Type I water to produce the desired concentration. The spiked water samples were then extracted and analyzed in the same manner as the sample's. Analysis of triplicate LCSs at the two specified levels cross-validates the 3M CONFIDENTIAL PAGE 8 OF 18 000013 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 analytical method as used here for any modifications/deviations from ETS 8-154,1. Additionally, LCS result^ w ill be used to determine overall method uncertainty in Section 3.7. Table 9 summarizes the LCS recovery results from the March 6,2006 extraction set.. LCS recoveries from the March 3,2006 extraction are not given here as no sample results were reported from this run.1 Table 9. <1>Lab Control Spike Results. PFOA SampleDescription LabID 1 ppb Lab Control Spike LCS-060306-1 1 ppb Lab Control Spike LCS-060306-2 1 ppb Lab Control Spike LCS-0603Q6-3 10 ppb Lab Control Spike LCS-060306-4 10 ppb Lab Control Spike LCS-060306-5 10 ppb Lab Control Spike LCS060306-6 Average %Recovery %RSD Spiked Cone. (ng/mL) 0.999 0.999 0.999 9.99 9.99 9.99 Calculated ConC. % (ng/mL) Recovery \ 1.00. 1 101 0.961 ' 9.19 o o.5, , 9.85..... 97.4%U% 100 . 101 96.2 92.1 96.6 98.6 . Spiked Cone. (ng/mL) 0.997 0.997 0.997 9.97 , 9.97 9.97 PFOS Calculated Cone. % (ng/mL) Recovery ; 1.04' 1.03 1.00 9.91 10.2 10.1 102%1.8% 104 103 100 99.4 102 101 Sample Description LabID ' Spiked Cone. (ng/mL) 1 ppb Lab Control Spike 1 ppb Lab Controi Spike LCS-060306-1 ' 1.01 LCS-060306-2. 1.01 1 ppb Lab Control Spike LC S080306-3 : ! 1.01 10 ppb Lab Control,Spike LCS-060308-4 10.1 10 ppb Lab Control Spike LCS-060306-5 10.1 10 ppb Lab Control Spike LCS-060306-6 10.1 Average %Recovery%RSD PFHS . * ''\ k Calculated ' Cone. .WnQ 1.08 % Recovery '\07 1.11 110 1.08 107 9.85 97.7 9.93 98.5 9.84 103%i5.5% 97.6 i Spiked Cone. (ng/mL) ! 0.992 0.992 0.992 992 9.92 9.92 PFBS Calculated Cone. ....(ng/mL) 1.04 1.05 1.03 9.17 9,32 9.49 99.4%dS.1% % Recovery 105 106 104 92.4 94.0 95.7 (1) A ll results and average values listed tp three significantjfiguresaccording to E P ^ rounding rules. %RSP.values given to two significant figures, D u e to r6 u n d in g /va lu e sm a yva iy'ilig h tly% )m th o se 'in frie ra w a a ta . C alculated C oncentration LCS P ercent R ecovery = 100% S pike C oncentration . LCS% RSD _ ------- --------", ; '---- - r ------ 100% ' ' a v e ra g e tC S recovery ... 3.7 Analytical Uncertainty Both the accuracy (percent recovery) and precision (%RSD) of the lab controfspikes were used to estimate the overall method's analytical uncertainty for a given analyte. For example, the overall accuracy and precision for PFOA based on LCS results was 97.4% 3.3%. The measured precision (%RSD) is then used to determine the range of the accuracy. , ' Example: '' 97.4*(0.033) * 3.25 97.4 + 3.25 = 100.7; 97.4-3.25 = 94.20 . . 3M CONFIDENTIAL PAGE 9 OF 18 000014 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Thus, LCS accuracy results range from 94.2% to 100.7%. The absolute difference of the low and high ends of this range when compared 100%, are then calculated. . .. 100.7%-100% = 0.70% 100%-94.2% = 5:8%. . The most conservative (largest) absolute difference is then used as the analytical uncertainty for the given analyte. Therefore, the analytical uncertainty for PFOA is given as 100 5.8% for these results. For PFOS, PFHS, and PFBS, the analytical uncertainty, as defined here, is 100 3.7%, 100 8.6%, and 100 6.6% , respectively. , i; 3.8 Field Matrix Spikes (FMS) Low (nominal concentration of 1.0 ng/mL) and high (nominal concentration 10 ng/mL) field matrix spikes were collected at each sampling point to verify that the analytical method is applicable to the collected matrix. Field matrix spike recoveries within method acceptance criteria of 10030% confirm that "unknown" components in the sample matrix do not interfere with th extraction and analysis of the analytes of interest. Field matrix spike results w ill be presented in the next section with'the sample data. , ` ..: FMS Recovery - (Calculated Sample Concentration - Average Concentration : Field Sample & Field Sample Pup.) 1QQ% Spike Concentratori ' ; The tables (Tables 10-19) below summarize the sample results, field matrix spike recoveries, and lab matrix spike reovoeries (if applicable) for the nine locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference (RPD) or relative percent standard deviation (RSD) of the sample and sample duplicate (and laboratory duplicate - if applicable). All field matrix spike recoveries were within 100+30% for all analytes except for the high level PFOS field matrix spike associated with PC45 (LIMS ID# E06-0151-101) which produced a recovery of 148%. The analytical accuracy for the PFOS results associated with this well have not been adjusted as the low field matrix spike, as well as the low and high level lab matrix spikes, produced recoveries within 100+30%.- .. : 3M CONFIDENTIAL PAGE 10 OF 18 000015 is . 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 10. (1)Sample Results for OKMN GWS RW40. 3MIMIS ID Description PiFOA Cone. (ng/mL) %Recovery PFOS Cone. (ngAnQ %f?ecomy P iCHS Cone. (ng/mL) %Recovery PFBS Cone. (ngfinL) s' %Recevery E06-0151-82 OKMN GWS RW40 0 060302 <0.0250 . NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-G83 OKMN GWS RW40 DB 060302 <0.0250 .. NA <00249 NA <0.0252 NA <0.0397 NA E06A151-084 OKMN GWS RW40 LS 060302 1.15 115 . 1.22 122 1.15 , 114 0.976 98.4 E06-0151-085 OKMN GWS RW40 HS 060302 726 72.7 9.93 99.6 9.05 90.0 8.4 84.6 Average Concentration(ng/mL)%RPD <0.0250 <0.0249 <0.0252 <0.0397 NA= Not Applicable. / (1) Table displays rounded values fo r all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in the raw data. %RPD values not given with both foe samfrfe and sample duplicate concentrations are less than foe reported LOQ. Table 11. (1)Sample Results for OKMN GWS SP42. PFOA PFOS PFHS P F BS 3MUMSID Description Cone. (ngAnL) %Recovery Cone. (ng/mL) %Recovery Cone. (ng/mL) Cone. %Recovefy (ng/mL) %Recovery E06-0151-086 OKMN GWS SP42 0 060302 <0.0250 NA . <0.0249 NA <0.0252 * . " NA <0.0397 NA E06-0151-087 OKMN GWS SP42 DB 060302 <0.0250 . NA <0.0249 NA <0.0252 - * NA . <0.0397 NA E06-0151-088 OKMN GWS SP42 LS 060302 0.93 93:1 .. 1.18 118 1.03 102 ' 0.963 97.0 E06-0151-089 OKMN GWS SP42 HS 060302 725 72.6 10.1 101 8.54 84.9 821 82.7 Average Concentration(ng/mL)%RPD <0.0250 ' <0.0249 <0.0252 <6.0397 NA= Not Applicable. -. (1) Table displays rounded values for all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in foe raw data. %RPD values not given with both foe sample and sample duplicate concentrations are less than the reported LOQ. 000016 3MCONFIDENT1AL PAGE11 OF 18 3MENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 12. mSample Results for OKMN GWS PL43. PFOA PFOS P F HS PFBS MUMS ID Description Cone. (ng/mL) %Reco ve iy Cone. (ng/mL) %Recovety Cone. (ng/mL) %Recovetv Cone. (ng/mL) %Recoverv E06-0151-090 OKMN GWS PL43 0 060302 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-091 OKMN GWS PL43 DB 060302 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-092 OKMN GWS PL43 LS 060302 1.02 102 1.2 120 1.09 108 0.982 99.0 E06-0151-Q93 OKMN GWS PL43 HS 060302 8.29 83.0 11.7 117 10.1 100 9.31 93.8 Average Concentration (ng/mL) %RPD <0.0250 <0.0249 <0.0252 <0X1397 NA= Not Applicable. (1) Table displays rounded values fo r all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in the raw data. %RPD values not given w ith both the sample and sample duplicate concentrations are less than the reported LOQ. f Table 13. '''Sample Results for OKMN GWS RW39. PFOA PFOS PFHS PFBS 3MUMSID Description Cone. (ng/mL) %Recovery Cone. (ng/mL) %Recovery Cone. (ng/mL) %Recovmy Cone. (ng/mL) E06-0151-094 OKMN GWS RW39 0 060302 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-095 OKMN GWS RW39 DB 060302 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-096 OKMN GWS RW39 LS 060302 0.954 95.5 1.07 107 0.968 96.2 0.951 95.8 E06-0151-097 OKMN GWS RW39 HS 060302 7.43 74.4 10.5 105 9.52 94.6 9.25 93.2 Average Concentration (ng/mL) %RPD NA= Not Applicable. <0.0250 ' <0.0249 - <0.0252 <0.0397 . (1) Table displays rounded values fo r all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in the raw data. %RPD values not given with both tee sample and sample duplicate concentrations are less than the reported LOQ............................ 3M CONFIDENTIAL PAGE 12 OF 18 O O O 0 1 *? 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 14. (1)Sample Results for OKMN GWS PC45. PFOA PFOS P F iH S PF BS 3MUMSID Description Cone. (ng/mL) Cone. ' - Cone. %Recovery _ (ng/mL) %Recovery (ngAnL) %Recovery Cone. (ngfinQ %Recovery EQ6-0151-098 OKMN GWS PC45 0^060303 0.522 NA - - . 0.464 NA 0.0649 NA <0.0397 NA E06-0151-099 OKMN GWS PC4S DB 060303 0.514 N 0.449 NA 0.0547 NA <0.0397 NA EO6D15-O980 OKMN GWS PC45 0 06033 . 0.592 NA 0.390 NA 0.0635 NA <0.0397 NA E06-0151-100 OKMN GWS PC45 LS 060303 ~1A5 90,6 1.64 121 1-11 105 1.05 106 EQ6-0151-101 OKMN GWS PC45 HS 060303 .' 993 - . .94.0 ....... A . 152 . . ^148 10.3 102 9 .7 4 . 982 (4!E064)151098-LMS Low Laboratory M atrix Spike at 1 ng/mL 1.59 105 141 97.5 1.07 100 0.944 95.1 H!E06-0151098-LMS High Laboratory M atrix Spike a t 10 ng/mL ~ 11.3 ' ' 108 - 11.0 106 10.5 104 9.05 912 Average Concentration (ng/mL) % R S P v - <2 2 0,5437.9 0.4349.0 0.06109.1 <0.0397 NA= NotApplicable. '" * '' (1) Table displays rounded values for all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in the raw data. (2) Sample results are from a duplicate laboratory exfraction o f the sample. A ll three replicate values used to determine average and %RSD. (3) FMS recovery exceeded method acceptance criteria o f 10Q30%. (4) Laboratory matrix spikes were prepared by spiking the40 mL sample aliquot prior to centrifugation. ... 3M CONFIDENTIAL PAGE 13 OF 18 000018 3M ENVIRONMENTAL LABORATORY , REPORT y o . E06-0151 Table 15. (1)Sample Results for OKMN GWS SP44. PFOA PFOS PFHS PFBS 3MLMISID Description Cone. (ngAnL) %Recovery Cone. (ngAnL) Cone. (ngAnL) %Recovety Cone. (ngAnL) %Recoverv l cc 5? E06-0151-102 OKMN GWS SP44 0 060303 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-103 OKMN GWS SP44 DB 060303 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-104 OKMN GWS SP44 LS 060303 0.943 94.4 1.08 108 0.991 98.5 0.942 94.9 E06-0151-105 OKMN GWS SP44 HS 060303 Average Concentration(ng/mL)%RPD NA= NotApplicable. 8.82 88.3 <0.0250 11.9 119 <0.0249 9.60 95.4 <0.0252 9.16 92.3 <0.0397 (1) Table displays rounded values for all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in the raw data. %RPD values not given w ith both foe sample and sample duplicate concentrations are less than foe reported LOQ. Table 16. (1)SampIe Results for OKMN GWS RW38. PFOA PFOS PFHS PFBS 3MUMSID Description Cone. (ngAnL) %Recovery Cone. (ngAnL) %Recoverv Cone. (ngAnL) %Recoveiy Cone. (ngAnL) %Recovery E06-0151-106 OKMN GWS RW38 0 060303 0.0525 NA 0.187 NA <0.0252 NA <0.0397 NA E06-0151-107 OKMN GWS RW38 DB 060303 0.0556 NA 0.195 NA <0.0252 NA <0.0397 NA E06-0151-1Q8 OKMN GWS RW38 LS 060303 1.02 96.7 1.42 123 1.06 105 0.969 97.6 E06-0151-109 OKMN GWS RW38 HS 060303 7.94 78.9 10.2 100 9.27 92.1 8.86 89.3 Average Concentration(ngAnL)%RPD NA= Not Applicable. ................ 0.0540 5 .7 0.1914.2 <0.0252 .* * <0.0397 (1) Table displays rounded values for all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary, slightly from foe values in foe raw data. %RPD values not given with both foe sample and sample duplicate concentrations are less than the reported LOQ. .v~ . 3M CONFIDENTIAL PAGE 14 OF 18 000019 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 Table 17. (1)Sample Results for OKMN GWS RW37. PFOA PFOS P F HS P F BS MUMS ID Description Cone. (ng/mL) , %Recovery Cone (ng/mL) %Recovery Cone. (ng/mL) %Recovery Cone. (ng/mL) %Recovery E06-0151-110 E06-0151-111 E06-0151-110 E06-0151-112 E06-0151-113 OKMN GWS RW37 0 060303 OKMN GWS RW37 DB 060303 OKMN GWS RW37 0 060303 OKMN GWS RW37 LS 060303 OKMN GWS RW37 HS 060303 0.282 0.298 0.312 1.22 ' 7.73 NA - 2.51 .........N A <0.0252 NA <0.0397 NA NA . 2.56 NA . <0.0252 NA <0.0397 NA NA 2.47 NA <0.0252 NA <0.0397 NA 92.3 3.43 '92.2 1.19 118 1.16 117 74.4 11.7 92.1 10.2 101 9.83 99.1 plE 06-015t110-LM SLow Laboratory M atrix Spike a t 1 ng/mL 1.47 ...... ... _ . - 117 3.71 120 0.983 97.7 0.941 94.8 PIE06-0151110-LMS Hiah Laboratory Matrix Spike at10nq/m L Average Concentration (ng/mL) %RSD 9.62 * 93.3 0.297 5 .0 12.3 98.2 2.51 1^8 8.91 88.6 <0.0252 8.82 88.9 <0.03S7 NA= NotApplicable. . ... ., (1) Table displays rounded values for aB coricentratfons arid percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values to the raw data. (2) Sample resutts ate from a duplicate laboratory extraction o f the sample. A ll three replicate values used to determ ine average and %RSD. (3) Laboratory matrix spikes were prepared by spiking a 40 mL sample aliquot prior to centrifugation............... 3M CONFIDENTIAL PAGE 15 OF 18 000020 3M ENVIRONMENTAL LABORATORY . RERORmgE06-0151 Table 18. (1,Sample Results for OKMN GWS RW39. PFOA PFOS PFHS PFBS 3MUMSID Description Cone. (ng/mL) %Recovery Cone. (ngfatL) %Recovery Cone. (ng/mL) Cone. YoReeovery (ng/mL) %Recoverv E06-0151-114 OKMN GWS PL41 0 060303 0.0766 NA 0.0268 NA <1.0252 NA <0.0397 NA E06-0151-115 OKMN GWS PL41 DB 060303 0.0796 NA <0.0249 NA <0.0252 NA ' <0.0397 NA E06-151-116 OKMN GWS PL41 LS 060303 1.11 103 1.13 111 1.10 109 0.995 100 E06-0151-117 OKMN GWS PL41 HS 060303 9.93 98.6 12.1 121 11.7 116 10.3 104 Average C oncentration (ng/mL)%RPD 0.0781 3.8 ^0 .0 2 6 8 <0.0252 <0.0397 NA= Not Applicable. (1) Table displays rounded values for all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from tie values In the raw data. %RPD values not given with both the sample and sample duplicate concentrations are less than the reported LOQ. (2) The average value reported reflects the single result that was above the LOQ. A true sample average and %RSD were not determined. Table 19. (1,Sample Results for the Trip Blank. ' PFOA PFOS PFHS PFBS 3MUMSID Description Cone. (ng/mL) YoReeovery Cone. (ng/mL) YoReeovery Cone. (ng/mL) Cone. YoReeovery (ng/mL) %Recovery mExtracted3-3-06 E06-0151-079 OKMN PW TRIP2 0 060302 <0.0250 NA <0.0249 NA <0.0252 NA <0.0397 NA E06-0151-08Q E06-0151-081 Extracted3-6-06 OKMN PW TRIP2 LS 060302 OKMN PWTR1P2 HS 060302 0.808 7.47 80.9 74.8 0.788 79.0 0.808 825 82.7 8.04 80.3 79.9 0.783 7.67 78.9 77.3 E06-0151-079 OKMN PW TRIP2 0 060302 <0.0250 NA <0.0249 NA <0.0252 NA _ <0.0397 NA E06-0151-080 OKMN PW TRIP2 LS 060302 1.04 104 0.928 93.0 1.04 103 0.982 99.0 E06-0151-081 OKMN PW TRIP2 HS 060302 9.04 90.5 10.2 102 10.0 99.4 9.58 96.5 NA= Not Applicable. . (1) Table displays rounded values for all concentrations and percent recovery values (3 significant figures), %RPD values (2 significant figures). Recovery and RPD values may vary slightly from the values in the raw data. %RPD values not given w ith both the sample and sample duplicate concentrations are less than the reported LOQ. .. ' (2) Samples extracted on 3-3-06 but analyzed against the calibration curve prepared on 3-6-06. 3M CONFIDENTIAL PAGE 16 OF 18 000021 3M ENVIRONMENTAL LABORATORY REPORT NO. E06-0151 PFOA, PFOS, PFHS, and PFBS results for the collected samples were presented in Table 1. *** Laboratory control spikes were used to determine the method accuracy and precision for all analytes. The accuracy and precision were then used to estimate the analytical uncertainty for the results (100 5.8% for PFOA; i 00 3.7% for PFOS, 10 8.6% for PFHS, and 100 6.6% for PFBS). Field matrix spike recoveries within 100 30% demonstrated that the analytical method was appropriate for the given sample matrix. ,1 All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures. J ? 3M CONFIDENTIAL PAGE 17 OF 18 000022 7 Signatures 3M ENVIRONMENTAL LABORATORY r e p o r t n q eotrofs: :m ' * -?M 'i f . : ;lr Mi The 3M Environmental Laboratory's Quality Assurance Unit has audited the data and report for this p ro te c t Quality Assurance Representative a/ / i..y 0 {'; Date i i 3M CO^O&NTJAl 000023 AR226-3636 INTERIM REPORT #1 Analysis of Oakdale Water Samples STUDY TITLE Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 Phone: 610-701-3761 INTERIM REPORT COMPLETION DATE May 19, 2005 PERFORMING LABORATORY Exygen Research 3058 Research Drive State College, PA 16801 . Phone:814-272-1039 STUDY SPONSOR 3M Company 3M Building .0236-0 l-B-10' St. Paul, M N 55144 Phone:651-733-6374 PROJECT Protocol Number: P0001400 Exygen Study Number: P0001400 Total Pages: 110 000024 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0001400, entitled "Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesul fonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research. . John Flaherty f Principal Investigator Exygen Research Jaisimha Kesari P.E., DEE Study Director Weston Solutions, Inc. Robert A Paschke Sponsor Representative 3M Company Exygen Research Date Date Page 2 of 110 4*00025 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0001400, entitled, "Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulforiate (FFHS), and Perfluorooctanesulfomte (PFOS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program." A ll reviewed phases1 were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director. Phase 1. Protocol Review Date Inspected 03/24/05 Date Reported to Date Reported to Principal Exygen Date Reported to Investigator Management Studv Director 03/25/05 03/29/05 05/19/05 2. Extraction Review 03/24/05 03/25/05 03/29/05 05/19/05 3. Raw Data Review and Interim Analytical Report Review 05/16-17/05 05/18/05 05/19/05 05/19/05 ^ o t e : A ll inspections w ill be documented in the QA statement for the final analytical report at the conclusion o f the study. , Exygen Research X V '.v o Page 3 o f 110 000026 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No; : P0001400 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number POO014OQ, is a true and complete representation o f the raw data, Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814)272-1039 Principal Investigator, Exygen; Exygen Research Exygen Research Facility Management Richard A. President Exygen Research Study Director, Weston Solutions, Inc J--aisim1ha KTesan* PT' .ET -i ., DEETp**TTT~3 Weston Solutions, Inc, Sponsor Representative, 3M Company; ~ ~ ^ D $ c u . r S L J lS L Robert A: Paschke Manager, 3M Corporate Environmental Programs Exygen Research Date c,I o rlo s - Page 4 of 110 000027 */<- Interim Report #1-Analysis o f Oakdale Water Samples ; . Exygen Study No,: P0001400 STUDY IDENTIFICATION Analysis o f Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perihiorooctanesulfonate (PFS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program PROTOCOL NUMBER: P0001400 EXYGEN STUDY NUMBER: P0001400 TYPE OF STUDY: Residue SAMPLE MATRIX: Water TEST SUBSTANCE: Perfluorooctanoic acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) SPONSOR: 3M Company 3M Building 0236-01-B-10 S i Paul, M N 55144 , . STUDY DIRECTOR: Jaisimlia Kesari P.E,, DEE Weston Solutions, Inc, 1400 Weston Way West Chester, PA 19380 SPONSOR REPRESENTATIVE: Robert A. Paschke 3M Company 3M Building 42-02-E-27 S i Paul, M N 5.5144 ' PERFORMING LABORATORY: Exygen Research 3058 Research Drive State College, PA 16801 . ANALYTICAL PHASE : TIMETABLE: Study Initiation Date: 03/03/05 Interim Analytical Start D ate:" 03/21/05 Interim Analytical Termination Date: 04/21/05 Interim Report Completion Date: 05/19/05 Exygen Research . Page 5 o f 110 000028 Interim Report #1-Analysis o f Oakdale Water Samples : Exygen Study No, ; P0001400 PROJECT PERSONNEL The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc, The following personnel from Exygen Research were associated with various phases o f this interim portion o f the study; ........................ Name Title ................ John Flaherty Vice President Karen Risha Scientist Paul Connolly Technical Lead-LC/MS Chrissy Edwards Technician Mark A m m erm an ................... Sample Custodian Amy Sheehan .......... Associate Scientist Eric Edwards Sample Custodian James Miller Scientist Edward Kaiser .............................. Scientist - Exygen Research Page 6 of 110 000021 interim Report #1 -Analysis o f Oakdale Water Samples Exygcn Study No.: P0001400 TABLE OF CONTENTS Page TITLE PA G E ..................................................... ,....................... ...... ...... ...........................................1 GOOD LABORATORY PRACTICE COMPLIANCE STATEM ENT.............................. 2 QUALITY ASSURANCE STATEMENT .................... I............................ 3 CERTIFICATION OF AUTHENTICITY................................. ..................... ...... ...................... A STUDY IDENTIFICATION................................ ......... ,................................................................5 PROJECT PERSONNEL............ ................. ....................................................................................6 TABLE OF CO NTENTS......................................... ............................ ...... ......................................7 LIST OF TA B LE S...... ..................................... .................... ................ .................. ............. ..........8 LIST OF FIGURES..... ....................................................... ................................................................9 O S T OF APPENDICES........................ .......................... .............................................................. 11 1.0 SUM M ARY.............................................................. 12 2.0 OBJECTIVE........ ...................................... ..................... ...... i.................................................12 3.0 INTRODUCTION................................................................ 12 4.0 ANALYTICAL TEST SAMPLES.......................................................................................13 5.0 REFERENCE M ATERIAL................................... ............................................................... 13 6.0 DESCRIPTION OF ANALYTICAL M ETHOD.. ........ ..............................................15 6.1. Extraction Procedure..................................... 15 6.2. Preparation o f Standards and Fortification Solutions...... ...............................16 6.3. Chromatography ..................................... ...................... ...... ................................................ 17 6.4. Instrument Sensitivity............................ 17 6.5. Description o f LC/MS/MS Instrument and Operating Conditions........... .................17 6.6. Quantitation and Example Calculation................................ ............................................18 7.0 EXPERIMENTAL D E SIG N ............................................ 19 8.0 R E SU L T S................................................... .............................................................................20 9.0 CONCLUSIONS................................................ 20 10.0 RETENTION OF DATA AND SAMPLES ............. .........................................................20 Exygen Research y&u Page 7 o f 110 ooooao Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: POQQ1400 Table I. LIST OF TABLES .. Page Summary o f PFBS, PFHS, PFOS and PFOA in Water Sam ples..... ...................................................................... ........... ,..... v......................22 Table 33. Matrix Spike Recovery o f PFBS and PFHS in Water Samples........................24 Table IH. Matrix Spike Recovery o f PFOS and PFOA in Water Samples....,.................30 Table IV. Surrogate Spike Recovery o f 13C PFOA in Water Sam ples............................. 36 Exygen Research Page 8 of 110 000031 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P000I40 Figure 1. LIST OF FIGURES Page Typical Calibration Curve for PFOA in Reagent Water.................................... 43 Figure 2. . Extracted Standards o f PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively.............. ......................................... ........................................................44 Figure 3. PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively............................................. 45 Figure 4. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR).......................... ............................. ........................... ............. 46 Figure 5. Typical Calibration Curve for t3C PFOA in Reagent W ater........ ....................47 Figure 6. Extracted Standards o f 13C PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively.... .............................. ............ .........................................48 Figure 7. 13C PFO A in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively....... ................... .............. 49 Figure 8. Chromatogram Representing an Oakdale Water Sample Analyzed for 13C PFOA (Exygen ID: C0064522, Data Set: 032405C ).......... 50 Figure 9. Typical Calibration Curve for PFBS in Reagent Water...................................... 51 Figure 10. Extracted Standards o f PFBS in Reagent Water, 25 ng/L and 50 ng/L, Respectively.......................................................... ............. .........................................52 Figure 11. PFBS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively................................................ .53 Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, D F -100 (Exygen ID: C0064522, Data Set: 0 3 2 4 0 5 C R )............................................ 54 Figure 13. Typical Calibration Curve for PFHS in Reagent W ater.................................... 55 Figure 14. Extracted Standards o f PFHS in Reagent Water, 25 ng/L and 50 ng/L, Respectively........ ........ .......................... 56 Figure 15. PFHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively......................... ........................ 57 Fi gure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=100 (ExygenID: C0064522, Data Set: 032405C R )................................... 58 Figure 17. Typical Calibration Curve for PFOS in Reagent W ater..................................... 59 Exygen Research Page 9 o f 110 00003? Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 LIST OF FIGURES Continued Figure 18. Extracted Standards o f PFOS in Reagent Water, 25 ng/L and 50 ng/L, R e sp e c tiv e ly ................................... 60 Figure 19- PFOS in Reagent Water, 50 ng/L Fortified Reagent Water, and : 500 ng/L Fortified Reagent Water, Respectively..................................................61 Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, D F -100 (Exygen ID: C0064522, Data Set: 0 3 2 4 0 5 C R )................................ 62 Exygen Research Page 10 of i 10 #00033 Interim Report #1-Analysis o f Oakdale Water Samples Exygen. Study No.: P0001400 LIST OF APPENDICES A ppendix A Study Protocol P0001400 (Exygen Study No. P0001400) with Analytical Method: V0001780:"Method o f Analysis for the .......................Determination o f Perfluorooctanoic Acid (PFOA) in Water by . LC/MS/MS" .................. .............................................. ...................... Page ,63 Exygen Research Page 11 of 110 000034 Intrim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 10 SUMMARY Exygen Research extracted and analyzed water samples for the determination o f perfluorooctanoic acid (PFOA), perfiuorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) according to .Exygen Method V01780 (Appendix A). . The limit o f quantitation for PFOA, PFBS, PFHS and PFOS in water was 50 ng/L and the limit o f detection for PFOA, PFBS, PFHS and PFOS in water was 25 ng/L. Analytical results for the analysis o f PFOA, PFBS, PFHS and PFOS in water samples are summarized in T able 1. The overall average percent recoveries standard deviations for all fortifications o f PFOA, PFBS, PFHS and PFOS in water samples were 93% 19, 141% 21,96% 1 5 and 109% 32, respectively. The overall average percent recovery standard deviation for all fortifications o f the surrogate field spike compound, 1 3 CPFOA, in water samples was 83% 2 1 . 2.0 OBJECTIVE The objective o f the analytical part o f this study was to determine levels o f perfluorooctanoic acid (PFOA), perfluorobutanesuliFonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) in water according to Protocol P0001400 (Appendix A), 3.0 INTRODUCTION This report details the results o f the analysis for the determination o f PFOA, PFBS, PFHS and PFOS in water using the analytical method entitled, "V 0001780 Method o f Analysis for the Determination o f Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS." The study was initiated on March 03, 2005, when the study director signed protocol number P0001400, The analytical start date for this interim report was March 21, 2005, and the analytical termination date for this interim report was April 21,2005. Exygen Research Page 12 of 110 oQ oons Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 4*0 ANALYTICAL TEST SAMPLES One hundred and twenty-one water samples, which correspond to twenty-nine sample sites, (Exygen ID 00064404-00064438/ C0064442-C0064461, C0064467-C0064532) were received at ambient temperature on March 15, 2005 from Tim Frinak at Weston Solutions, Jnc. The samples were logged in by Exygen 'personnel and placed in refrigerated storage. Sample log-in and chain o f custody information is located in the raw data package associated with this interim report. Storage records will be kept at Exygen Research. 5.0 REFERENCE MATERIAL The analytical standard, PFO A /w as purchased from Sigma Aldrich and was received at Exygen on December 08, 2003. The surrogate spiking standard, 13C labeled perfluorooctanoic acid (13C PFOA), was received at Exygen on April 15, 2004 from the 3M Company. The analytical standards, PFBS and PFHS, were supplied by 3M. PFBS was received from 3M at Exygen on July, 06, 2000. PFHS was received from 3M at Exygen on January 20, 2003. PFOS was purchased from Fluka Corporation and was received at Exygen on April 23 2003. The available information for the reference materials is listed below. PFOA was stored ambient PFBS, PFHS and !3C PFOA were stored frozen and PFOS was stored refrigerated. Compound PFO A 1JC PFOA PFBS PFHS PFOS Exveen Inventory.No.. / L ot# SP0003800 23116HB SP0004184 :v 3507-195 SP0000252 - 101 SP0002401 . : : . SE036 SP0002694 430180-1 Puritv (%1 97.64 . 97 , 96.7 98.6 1 0 1 .2 Expiration E 12/08/05 03/29/09 12/04/06 10/18/06 04/23/06 The molecular structures o f PFOA, 13C PFOA, PFBS, PFHS and PFOS are given on the following pages:' " .* . Exygen Research Page 13 o f 110 000036 Interim Report #1-Analysis o f Oakdale Water Samples . Exygen Study No.: F0001400 PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 ~> 369 (for quantification) and 413 -> 219 (for confirmation) Structure: 13C PFOA Chemical Name: 1,2-13C perfluorooctanoic acid Molecular Weight: 416 Transition Monitored: 4 1 5 -> 370 Structure: PFBS Chemical Name; Perfuorobutanesufonate Molecular Weight: 338 supplied as the potassium salt (C4 F9 SO3 TC*) Transitions Monitored: 299 -> 99 ' Structure: : v' ' '; Exygen Research Page 14 of 110 000037 Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No.: P0001400 PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (CeFiaSOjTC4) Transitions Monitored: 399 80 Structure: PFOS Chemical Name: Perfluorooptanesulfonate . Molecular Weight: 538 supplied as the potassium salt CCsFiySOaTC4) Transitions Monitored: 4 9 9 -> 80 Structure: 6*0 DESCRIPTION OF ANALYTICAL METHOD The analytical method "V0001780: Method o f Analysis for the Determination o f Perfluorooctanoic A cid (PFOA) in Water by LC/MS/MS'' was used for this study. 6.1, Extraction Procedure A 40 mL aliquot o f the water sample was used for the extraction procedure. After fortification o f appropriate samples the samples were loaded onto a Cis SPE cartridge conditioned with 10 mL o f methanol and 5 mL o f water. The eluate was discarded. Approximately five milliliters o f methanol was added to the cartridge. Five milliliters o f eluate was collected into a graduated 15 mL polypropylene centrifuge tube. Each sample was analyzed by LC/MS/MS electrospray. Exygen Research 'jCH'j Page 15 of 1 10 000038 Interini Report #1-Analysis o f Oakdale Water Samples Exygen Study No.': PGG1400 62 Preparation of Standards and Fortification Solutions , Individual stock standard solutions o f PFOA, 13 PFOA, PFBS, PFHS and PFOS were prepared as specified in Exygen method V0001780. The stock standard solutions were prepared at a concentration o f 100 pg/mL by dissolving 10 m g o f each o f the standard (corrected for purity and salt content, i f necessary) in methanol. From these solutions, .0 pg/mL fortification standard solutions were prepared by taking 1 mL o f the appropriate stock and bringing the volume up to 100 mL with methanol. By taking 10 mL o f the appropriate 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, 0,1 pg/mL fortification standards were prepared. B y taking 10 mL o f the appropriate 0.1 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, 0.01 pg/mL fortification standards were prepared, Several sets o f standards containing PFOA, 13C PFOA, PFBS, PFHS and PFOS were prepared in water and processed through the extraction procedure, identical to samples. The following concentrations were prepared: Cone, o f Fort Fort Volume o f Solution Volume Fortified Sample (ng/m L)' 0 10 ..m o . 0 \ ;1 0 0 "(mL) 40 40 10 2 0 0 40 10 400 ' 40 100 100 . 40 100 2 0 0 . 40 1 0 0 400 , 40 1o f PFOA, l3C PFOA, PFBS, PFHS and PFOS Final Cone. Calibration! (ng/L) 0 25 50 100 250 . 500 1000 An additional m ixed stock solution o f PFOA, n C PFOA, PFBS, PFHS, and PFOS was prepared at 1000 pg/mL and diluted to 100 and 10 pg/mL for bottle spiking purposes. Complete details can be found in the raw data package associated with this study. The stock standard solution and all fortification and calibration standard solutions were stored in a refrigrator (4 : 2C) when not in use. Documentation o f standard preparation is located in the raw data package associated with this interim report, Exygen Research Page 16 of 110 0000Q 9 Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No. : POOO1400 6.3 Chromatography Quantification of-PFO A , PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray. The retention time o f PFOA, PFBS, PFHS and PFOS was ~12 min, ~5 mins, -1 1 mins, and ~13 mins, respectively. Peaks above the LOD were not detected in any o f the reagent blank samples corresponding to the analyte retention time. 6.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentration o f 25 ng/L o f PFOA, PFBS, PFHS and PFOS. 6.5 Description of LC/MS/MS Instrument and Operating Conditions . Instrument: . API 4000 Biomolecular Mass Analyzer Interface: Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 ' ' Software: WindowsNT,Analyst 1.4.1 ......... HPLC: ............................ Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Thermo Fluophase RP, 50 mm x 2.1 mm Column Temp. : 30 C Injection Voi.: 15 pL M obile Phase (A): 2m M Ammonium Acetate in water M obile Phase (B): Methanol Time Omni . 0.0 1 ,0 ^8 . 0 .1 0 0 . 1 1 .0 . 18.0 Total run time: ~ 18 min Flow Rate: 0.3 tnL/min : ; % 65 : 65 25 25 65-:. : 65 ; ;%B 35 35 75 ; ,75 ' 35 35 Exygen Research Page 17 o f 110 000040 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.; P0001400 Ions monitored: Analvte PFOA PFOA Confirm Ion 13CPFOA PFBS PFHS PFOS Mode negative negative negative negative negative negative Transition Monitored 413 - 369 413 -> 219 4 1 5 -> 3 7 0 299 -> 99 399 80 499 80 Approximate Retention Time (min) - 1 2 min. - 1 2 min. - 1 2 min. - 5 min. - 1 1 min. ~13 min. 6.6 Quantitation and Example Calculation Fifteen microliters o f sample dr calibration standard were injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by .Analyst software using six concentrations o f standards. The concentration was determined from the equations below. Equation 1 calculated the amount o f analyte found (in ng/L based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program. Equation 1: - . . . . . . ,. , .. .. Analyte found (ng/L) = iPeak area - intercept) x DF ' . . . slope . . , ....... .. Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary. For samples fortified with known amounts o f PFOA,, PFBS, PFHS, PFOS and 13C PFOA prior to extraction, Equation 2 was used to calculate the percent recovery. Equation 2: , . .'. . . . . . > Recovery (% )= .s . (analvte found (W L ) - analyte in control (ng/L)) xlQ0% amount added (ng/L) . An example o f a calculation using an actual sample and results from the PFOA analysis follows; Water sample Exygen ID CG064432 Spk. F (Set; 032105BR), fortified at 50000 ng/L with PFOA where; peak area : intercept ' 'slope :. . ^ . = 1170161 26200 --. 1330 dilution factor = ng/L PFOA added (fort level) = amt in corresponding sample (ng/L)* ~ 100 50000 37600 (The primary sample result was used for all calculations) Exygen Research Page 18 of 110 ;Interim Report #1-Analysis o f Oakdale Water Samples , . Exygen Study No.r P0001400 From equation 1: Analyte found (ng/L) = fl 170161 - 262001 x 100 1330 From equation 2: % Recovery = 86012 ng/L* = (86012 ng/L 37600 ne/Li x 100% 50000 ng/L ,, = 97% (values are slightly different from raw data due to rounding) 7.0 EXPERIMENTAL DESIGN 13C PFOA was used as a surrogate for all the samples, 13C PFOA was added to the sample collection bottles in the laboratory before being shipped to the field for sampling. For samples designated as field matrix spikes, PFBS, PFHS, PFOS and PFOA were also added at a known concentration to the bottles in the laboratory before being shipped to the field. The samples were filled to a 200 mL volumetric fill line in the field. The samples were extracted in five sets. Each set consisted o f one reagent blank and two reagent blanks fortified at known concentrations. The first set contained six sample sites, the second set contained six samples sites, along with a trip blank and two trip blank spikes. The next two sets contained seven sample sites each. The fifth set contained three sample sites, along with a second trip blank and two trip blank spikes. For each site, a sample, a field duplicate arid two-matrix field spikes were collected. For each site, a laboratory duplicate o f the primary sample was extracted and two laboratory matrix spikes were also extracted. For the two laboratory matrix spikes, two 40 mL portions o f the primary sample collected for the site was poured from the bottle and fortified. Not only were PFBS, PFHS, PFOS and PFOA added in the laboratory prior to extraction, but also l3C PFOA was added. The .additional l3C PFOA was added because the levels o f PFBS, PFHS, PFOS and PFOA spiked, into the samples were known to exceed the calibration ranges and were not analyzed without dilution; therefore, l3C PFOA levels were adjusted to require the same dilution as the other analytes. For each primary sample collected, between the, field and lab, seven individual QC results were reported for 13C PFOA. Some samples gave recoveries for ,3C PFOA outside o f the normal acceptance range o f 70-130%. Because laboratory control spikes for 13C PFOA were acceptable in every set, instrument washes were free o f 13C PFOA, at least one ,3C PFOA recovery per the seven done for the sample was acceptable and no evident errors in spiking or extracting could be found, no re-extractions were performed. 13C PFOA recoveries outside o f 70-130% are deemed indicative o f matrix effects. Exygen Research Page 19 of 110 000042 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 8.0 RESULTS Analytical results for the analysis o f PFOA, PFBS, PFHS, and PFOS in water samples are summarized in Table I. Fortification recoveries for PFOA, PFBS, PFHS and PFOS in the water samples are detailed in Tables II and III. The overall average percent recoveries standard deviations for all fortifications o f PFOA, PFBS, PFHS and PFOS in water samples were 93% 19, 141% 21, 96% 15 and 109% 32, respectively. Fortification recoveries for 13C PFOA in the water samples are detailed in Table IV. The overall average percent recovery standard deviation for all fortifications o f 1 3 C-PFOA in water samples was 83%2L 9.0 CONCLUSIONS The water samples were successfully extracted and analyzed for PFBS, PFHS, PFOS and PFOA according to analytical method V0001780. There were no circumstances that may have affected the data quality or integrity. 10.0 RETENTION OF DATA AND SAMPLES All original paper data generated by Exygen Research that pertains to this interim report will he shipped to the sponsor. This does not include facility-specific raw data such as instrument or temperature logs. Exact copies o f ail raw data, as well as a signed copy o f the interim analytical report and all original facility-specific raw data, w ill be retained in the Exygen Research archives for the period o f time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792. Exygen Research Page 20 o f 110 00004a Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No,; POOO1400 Exygen Research Page 21 of 110 000044 Interim Report #1 -Analysis o f Oakdale W at Samples Exygen Study No.: POOO1400 Table !. Summary of PFBS, PFHS, PFOS and PFO in Water Exygotl ID 00064404 C0064404-Rep C0064405 Client Cample ID OKLMN-GW-W3-O-O50310 OKLMN-GW-W3-O-O50310' CKLMN-GW-W3-0-050310 Dup Samples Analyte Found {ppf, ngfL) C4 Sulfonate PFBS COSulfonatB PFHS C6Sulfonate PFOS C# AcWPFOA 312 162 4750 6330 296 160 3350: 6220 303 : 159 . 3190 v . 5990 C0064408 0LMN-GW-W84M>50310 57.0 ND 59.0 ' 290 C00644408 Rep 0KLMN-GW-W&OOS0310* 63.8 ND 55.7 275 C0064409 OKLMN-GW-Wfi-G-050310 Dup 60.1 ND 56.3 284 C0054412 C0064412 Rep C00S4413 OKLMN-GW-W264W50310 OKLMN-GVV-W26-0-050310* OKLMN-GW-W2&-CMD50310 Dup . 73400 75700 . 71400 222000 244000 214000 . 13500000 14400000 12200000 79300000 70200000 71800000 G00M418 C0064416 Rep C0064417 OKLMN-GW-W33-0-05Q310 OKLA1N-GW-W33-O-O50310* . OKLMN-GW-W33-0-050310 Dup 26800 28800 28500 92300 , 84600 81600 4810000 4870000 4540000 1750000 2020000 2790000 00064420 C0064420 Rep C0064421 OKLMN-GW-W205-0-060310 OKLMN-GW-W205-04)50310* OKLMN-GW-W2Q5-Q-050310 Dup 8260 8800 7850 6740 6610 7070. 146000 119000 116000 147000 150000 158000 CX1084424 C0064424 Rep C0064425 OKLMN-GW-W215-04)50310 OKLMN-GW-W215-0-050310* OKLMN-GW-W215-0-05031 Dup 801 81.2 75.8 769 37100 256 . 27000 . 270 36900 , 4400 3510 4070 C0064428 C0064426 Rep 00064429 OKLMN-GW-W2010-0-05031D OKLMN-GW-W2010-0-050310* OKIMN-GW-W2D1WWE0310 Dup ND ND ND ND , , ND ' ND: ND ND ND . NQ ND ND CO064432 00064432 Rep C0064433 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310* OKLMN-GW-PW7-0-050310 Dup 4460 4340 4630 4800 5080 ; 5080 ' 71600 37600 67600 . ' 38400 72400 . 38200 C0064436 C0064442 C0064442 Rep C0064443 C0064446 03064446 Rep C0064447 C006445O 00064450 Rep C0064451 C0064454 CQ064434 Rep C0O6445S OKLMN-GW-TRIP1 -0-050310 OKLMN-GW-PW8-C-05Q310 OKLMN-GW-PW8-0-050310* . OKLMN-GW-PW8-0-050310 Dup OKLMN-GW-PW9-O-OS0310 OKLMN-GW-PW0-0-050310` OKLMN-GW-PW9-0-050310 Dup OKLMN-GW-W61G2-0050310 0 KIM N-GW-W8102-0-050310* OKLMN-GW -W6102-0-050310 Dup OKLMN-GW-W8104-0-050310 OKLMN-GW-W8104-0-05031Q* OKLMN-GW-W6104-0-050310 Dup ND 13300 14100 14100 - 2110 2140 1930 NQ 53.5 ' ' NO NQ NQ 51.2 ND 23800 23900 23000 5160 5000 5140 ND ND : ND ND ND ND . ' ND 34300 35600 33400 64400 84900 ; 88800 , NQ NQ ND 109 1 125 118 ND 81400 80600 56500 49000 46700 49900 214 228 227 207 189 184 C0064458 C0064458Rep C0O64459 C0O64467 CO064487 Rep C064468 , C0064471 C0064471 Rep C0064472 OKLMN-GW-W6201-0-050310 OKLMN-GW-W6201 -0-050310* OKLMN-GW-W8201-O-O5O31Q Dup OKLMN-GW-W2O-O-O503O9 OKLMN-GW-W20-0-05C309* OKLMN-GW-W20-04)50309 Dup OKLMN-GW-W22-0-0503D9 OKLMN-GW-W22-0-050309* OKLMN-GW-W22-0-050309 Dup 74.0 74.f 7B.0 13900 10700 10000 36600. 32200 37500 ND ND ND 12900 9040 7660 31400 29500 25700 . . N : NO NQ 46600 : 3B300 30100 45800 34000 28100 . 95.5 66.3 132 . 285000 243000 190000 317000 301000 244000 Laboratory Duplicale ND Natoet&ctedai or above 25 ng/L. NO s Not quantifiable = Weasuradconcentration between 25 noH.andft Limitof Quantitation (LOQ) wtiich is SOnj/L. Exygen Research Page 22 o f l l O Interim Report # 1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table I. Icxynen ID Summary ofPFBS, PFHS,PFOS and PFOA in Water Client Samte 10 Samples Continued Anatyfo Found (ppt, ng/L] C4Sulfonate PFBS Ct Sulfonate PFHS C8 Sutfonat* PFOS C* Acid PFOA C0D64475 CO064475 Rep 0084476 OKLMNGW-W31-0-050309 OKLMN-GW-W31-0-050309* OKLMN-QW-W31-0-050309 Dup 1300 1380 1360 5130 4780 5190 132000 : 132000 156000 23100 22300 24900 C0084478 C0064478 Rep 0064479 OKLMN-GW-W32-OC6O3O0 I DKLMN-GW-W32-0-050309* OKLMN-GW-W32-0-050309 Dup 2180 " 2290 2960 3000 3120 2940 47100 44400 83000 v 117000 93300 125000 0064482 0064482 Rep C0064483 OKLMN-GW-W217-0050309 OKLMN-GW-W217-0-050309* 0KLMN-GW-W217-0-050309 Dup ND ND- -. ND -N D ; ' ND .... ND NQ NQ 128 . NQ NQ NQ C0064466 C0O64486 Rp CO064487 CO064490 C0064490 Rep 0064491 OKLMN-GW-W2OO8-O-O5O309 OKLMN-GW-W2OQ8-0-O5Q3O9* . CKLMN-GW-W20Q8-0-050309 Dup OKLMN-GW-W2Q12-0-050309 OKLMN-GW-W2O12-0-O5O3O9* ! OKLMN-GW-W2012-O-060309 Dup 6780 7170 -v - 6930 2210 1960 1920 10100 10800110300 4700 4470 ' 4420 15500 17800 18800 . 117000 118000 , 139000 59300 58700 60300 48900 46400 51400 00084494 C0064494 Rep 00084495 OKLMN-GW-W8Q-CK>50309 ' OKLMN-GW-W80-0-050309* OKLMN-GW-W80-0-050309 Dup ND ND ND ND ' ND ND .ND N D .-: ND 302 280 328 00064498 C0064493 Rep C00644B9 0KLMN-GW-PW143-050310 OKLMN-GW-PW1-0-050310' OKLMN-GW-PW1-0-050310 Oup 5620 5650 5580 - 4180 . 4150 : 4170 66900 71600 70S00 . 37300 39300 39100 00064502 C0064502 Rep C0064503 OKLMN-6W-PW2-0-O5O31O OKLMN-GW-PW2-0-050310*' . OKLMN-GW-PW2-0-O5O310 Dup $41 - 624 894 -so r . 491700 351 , 383 303 3630 3890 5160 C0064508 COO64508 Rep' C0064507 OKLMN-GW-PW3-D-050310 OKLMN-GW-PW3-0-050310* / ' OKLMN-GW-PW3-0-050310 Dup - , 8970 8740 - 6570 ' / 10000 - . 9740 . ; 9990 . 32700 25500 32300 177000 160000 176000 00064510 C0064510Rep 00064511 DKLMN-GW-PW4-0-Q50310 OKLMN-GW-PW4-0-050310* " ' . OKLMN-GW-PW4-0-050310 Dup : 8130 7700 7810 ';. .. 7890 7480 i 7550 33800 30300 27800 . 72100 67800 65900 00064514 C0064514 Rep 0064515 00064518 C006451B Rep C0064519 OKLMN-GW-PW6-0-050310 OKLMN-GW-PW8-D-050S10* ... OKLMN-GW-PW6-0-050310 Dup.!,: OKLMN-GW-PW10-0-050310 OKLMN-GW-PW10-0*050310* v 0KLMN-GW-PW10-0-050310 Dup 7930 8000 8130\ 13100 12700 . 11900: . 14500 . . 14600 14600- 29200 27400 : 26800 90000 86000 85400 1400000 1780000 1740000 78400 78700 78600 719000 781000 614000 C0064522 0064522 Rep C0064523 0KLMN-GW-PW11-0-050310 OKLMN-GW-PW11-0-060310* i . 0KLMN-GW-RW11-0-050310 Dup- 6520 ' 8490. . 7150- ' 8820 10000 ; 9050 40800 50800 43400 . 60300 71600 60600 C0064526 C0064526 Rep CO064527 OKLMN-SW-Q-050310 . OKLMN-SW-0-060310* V-X; OKLMN-SW-0-050310 Dup 0 , NQ NQ y. , NQ . NQ NQ NQ 1190 1200 1270 491 . 529 537 CO064530 OKLMN-GW-TRIP2-0-050310 ND ND ND ND LaboratoryDupilcete . ,\ NO = Mot c>et6<!tocla(oi above 25 ng/L. -NQ * Notquantifiable =Measured concentrationbetween 25 ngIL anattt Limit ot Quantitation (LQQ) which is $0 ng/L. Exygen Research Page 23 of 110 000046 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples ' S am p l . O ee c rttrtle n . C4 SuliaMla PF88 A m ount A nrt Found A m ount S p iked In Sant pi R co vrd R *c o v ry .... m A m ourd S p lke d {n o .) C t SuHonat* PPHS A m i Found Am ount k i C a m p i* R ecovered RSCOvwry {n o /t) {n g A 4 (* ] Q K U U N ^ 3 W -W 3 n M W 1 0 <CdOSU04S(ikCt 2600neA .U b^plks) O K LM N C W -W O -0 -0 6 01 10 ICCOdUM S et 0,50000 i * * . U b sp ila) O K LM N -S W -V Y 3-0 -0 50 3 10 L o ie S p lk a 5 ppb [COO*MO1*WH>ftflil. Fiele 3 p lte ) O K LM N -G W -W 3-0 -56 0 31 0 H ig h S p tt 5 0 ppb (060*44*7.50000 m /L Fiele S plte ) 6000 50000 6000 50000 312 6980 133 312 ' ' 67400 ' 134 312 7450 , 143 312 74700 : 148 5000 50000 5000 50000 162 5130 162 . . 47500 162 5140 182 54400 B8 E5 100 100 O K L M N -C W -W I-O -0 *0 3 1 0 (cooeaeoe s t* e . 5oc njA . L*b api*) O K LM N -G W -W 5-0-0 3 03 10 (C00M4M 3 jtfF , r o note La* Splhel O K L M N -G W -W -C -0 4 03 10 LOW S p lk PpO (COOSMIO, MOO n *L FtWU S p ila > O X L M fW W -V V 6 -0 -0 5 0 3 ia H ig h S p lk e S p p b {co cA tm , sixxion. Fiele E ptte) 5000 50000" 5000 50000 5 T .0 5 7 .0 5 7.0 6 7.0 7020 138 70000 140 7410 147 70600 . 141 5000 50000 5000 50000 ND ND ND ND 5120 51400 6610 53300 102 103 110 107 O K LM N J3W -W 2S-0-0 5 03 10 (CMKU12 Beh G, SC<H n h .U b Spila) O K U IN -G W -W 3 # -0 -0 W 1 fl (CW>W 412Sphe3W 00rii^)_bSpJk| 0K L M N -O W -W 26-0-0B 0310 to w S p lk ppb (0061414. SIOO ng/L Fiale S p iti} O K U M M -Q W W 2 -0 - 1 *W H ig h S p lk * ppb (CM M 413, et nh. Fleld 5(>k* ) 6000 50000 5000 60000 73100 - 73100 73400 125000 73400 78200 78400 147000 "e" 5000 222000 103 soooo 222000 * SODO 222000 147 SOCQO : 2 2 2 00 0 207000 52000 210000 266000 - 0K LM M -G W -W S 3-0 -0 *0 1 1 0 . (C00441* 8p * 1, v m n (A .U b S fila ) Q K LM N G W -W J3-0-0503 10 (0006441* S # J .iO t *n g (L U b Spili*) O K LM N -C W -V tfU -O -O S dllO Lt>w S p lk * S ppb 3M 9 * . Mete S p ila ) O K LM M -G W -W 3S -0-080110 H igh S p lk * SO ppb (C006441*. 50000 no*. Fiele SpUoi ) OKLMN-QlV~W20S-0-0$a310 (COOM-ttO Bpn K, 500C no*. U b Splk* ) O K LM N-QW -W 205-O-O 8 03 10 lCSOM420Spk usoeoo n e l. U b S p lk i) O K U U IN -G W -W 20B -W 60910 U m Splk fi ppi> (Coagula. &66t 9IL fUA Spile > O K L M N -Q W ^ Q O S 44 6 01 1D H ig h S p ie * 50 ppb (COflMeaa, scotio n **. Fiele Spili j 6000 soooo 5000 50000 5000 50000 Sotto 50000 20000 26600 26800 26800 6200 8280 0200 0260 33600. 133000 38700 106000 15400 .72 5 00 1S200 82800 *` 600 212 sooq 5000 102 50000 82300 78000 92300 122000 82300 85200 82300 . 150000 143 5000 126 soooo 130 SOQC 140 soooo- 740 6740 740 6740- 12500 53100 11 BOO 60600 * 59 115 115 83 101 100 0 K D J N ~ Q W < m i5 -a -0 5 6 3 1 0 ' (C O C *4W 5i*M ,O O n ^L Ut> Spi* ) O K L H N -B W -W 2 15-0*060310 jC O O I44W liitft, *0000 n p *.U b Sptke) O K L M H -Q W -W 216-0-0 5 03 10 U h v 5 p lt * ppb (c o *e 2, seco "a *-n W S e tte ) . O K L M M -d W -W 2 1 M -C iC 3 1 0 H tijh S p lk 60 ppb (COOMW , SOCCOn *. Fiele Spille ) 5000 soooo 5 0 0 0 .' SOOOO 0 0 1 .0 7200 128 8 0 1 .0 , 67200 133' 801.0 . 0 72 0 ' 118 it.o 66900 132 .5 0 0 0 60000 5000 SOOOO 789 ?; 769 76 5260 50300 ; 5240 " 48S 80 99 aa &$ Swmple ra k lu e exceeds the spSdng level HQrUheanHy; therefoie, an accort** recovery value cannot be tabulated ND - NDtdett'CtSd 31 o r above 25 rlQfl. (ppt). N Q b Mol quarX)table s Measured concentraBOfi between 25 r * / t (ppt) and the Limit of Quantitation (LOQ) which IS SO n&fl- {ppt). Note: Since th t* untimely table how rounded r w u ltt, recovery vatuee may vary itfttty troni the v a t u in the raw data. Exygen Research Page 24 o f 110 Q Q O fh r Interim Report #1-Analysis o f Oakdale Water Samples . Exygen, Study No,: P0001400 Table IL Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued C4 SuMtMiaUPF8S C* Sultonat* PFHS Amount Am t Found Amount Amount Am t Found A m ount Satnpl :; , Spiked In S am pl* R a cu w e d Racovaty SpHnd In S am pl* Recovered Recovery D **crH )tlort ,W {StfLJ fn-} - .< * ... b ig .} fri .) (%> CW LM N-G W W ttia-O -O 50310 (CbM442SpfcC.4M pft. Lab Spike) OKLMN-G W -W 2C1O -0-Q 50310 (C0M442I $pk D, *eew natu Lab Spike) O K U IN -O W -W H <W )-a10 U ow S pIk* 5 ppb (00044436,M l rwt. Hak) pik* | QK1MN-GW-W2Q10-0-050310 High S p in SO ppb 1004*4431.OWOQiwAFMdSivIk*) . 5000 SOOOO . X 50000 ND ND: NO NO 6590 68600 6700 83B00 132 5000 ' ND 4800 139 50000 ND 48700 134 .5000 , ND ` ' ' 700 128 50000 ND '. _ 43700 % 97 94 87 O K U 4 N ^W W T -W ftS 10 (COMa29p]te.BOOOn9n.UibapHui O K LM N -G W -l>W 7-fl-05iai (CM04U2SpkF,l0004 n g lta li Iptka) OKLMN-GW -f*W 7--05M10 Low p ik 6 ppb (CMM4M.SM nA. FWd pik* ) 0K LM M -0W -W 7-0O W J10 High S p ft* SO ppb |COO441,MPO m /L nld Split* ) 5000 4400 50000 - 4450 SODO 4480 80000 446 12200 72800 13200 eoooo 155 SOOO 4000 . 137 50000 4800 175 5000 : 4800 151 50000 4800 9310 50900 0370 99000 90 G2 91 108 O K LU N -G W -TR IP lO O M 31tt Low S plit > ppb (C00U4I7, EQ04upA. FM* 3pllu ) OKLAIN-GW -TRIP10 0 8 0 3 1 0 High S pika W ppb ICOOSM3,WM Bflrt. Ftald Splk* > 5000 50000 NO NO 5 *0 44400 131 5000 88 50000 ND ND 4600 46100 92 92 OXLM N-O W -fW M M W M I0 {C60t4442iBkG,IMMOnL U b3plkl OKLMN-OVW W aOOSOSIO (CP0M4U pvH.KICOOnah.Ljib SpHw) OKLMN-GW -PW 4-0-C50310 Low Splk S ppb (COOe+aM. sioorprt FWdSpIta } OKLMN-QW-PWSOOSOJ10 High plka SO ppb (COO04443.9CO40aplt Fl* Splk ) ` 5000 50000 5000 50000 13300 13300 13300 13300 21400 78700 21000 80700 162 5000 2 3 0 0 0 ', ' 28700 133 50000 23800 70300 154 ' 5000- 23600 : : 30000 135 50000 23800 76100 110 90 124 10S O K LW N -O W -W S-0 >060310 {C O M M aU *1 id t\Q fLLab Splk) OKUMN-GW 'PW S-O-OnSICI (C W *W * SpKJ, COtKWnpIL lab -SpH*) OKLMM-GW-PWS-O-CKMIO Low S p ik e s ppb (Coe*4+M, tw u p iL fin o S p t ) 0 KLM N-QW -PW -0-060310 High Splko 50 ppb tCO04444S,3 m * N id Spike) O raM N -O W -W *1M >-060310 ICOOOUM Spk K,lOOOrwl Labs*) O KLMN-W -W 6102-fl-050316 (C0M44S0 Spk L, SOOflOnpL la * 9pH) OKLMM-GW^rti102-O4k5O*1O Low Spika $ ppb <co m au , eooo gii. f i*m B p i ) QKLM N-GW*W0 1D2-<M)30310 High S p lk* 30 ppb 1006*4493,MOO npL Fleld Botk* 1 5000 50000 sooo ' 50CO0 5000 50000 5000 50000' 2110 2110 2110 2110 NQ NQ NQ ' NQ : 8280 8800 ' 8290 ' 74800 7360 ! .67500 712Q 70700 ! 144 ' 5000 134 60000 144 6000 148 50000 147 6000 135 50000 142 3000 141 60000 5160 5160 5160 5160 9310 64400 9350 54600 ND ND " ' 4890 47400 ND 5040 ND 50600 83 98 04 90 08 95 101 101 Sample idu* weeds the spik|r>8 level Igntflcantiy. tlwster, m accurate rscovaiy value cannot be calculated NO Not detected at or above 25 ngMppl>. NQ NotQantltlabte=MeMuie<lc<XK!6nVB(i<Hibetyiteeh2SnBrt. (ppt)*ntiaK !U m *of , C3niUllon(LCX)}vtitehl*5Prig/L [ppt). . Motet Sine* thla auiwnary table ihowa roonaod raiutt, reeevwy vaiudi may vary lightly fmmiM value* Inthe raw data. Exygen Research Page 25 of 110 000048 Interim Report#!-Analysis o f Oakdale Water Samples Exygen Study N.: PQ001400 Table II. Matrix Spike Recovery of FFBS and PFHS in Water Samples Continued Swnphi , D e ac rip tlo n ' Am ount Spiked C4 Sulfonate PFBS Am t Found Am ount In S em p i* Recovered Recovery (flJ- ...... < * ) .... Am ount S p ire d m C8 Sulfonate PFKS Am t Found A m ount Sem ple Recovered in o /U <ng/U Recovery m OKLM M -OW JilV1W >-OSQ31b {CMtM54SteiM,9W Oak.Ub9aUl 500C NQ 6680 . Q KLMN-GW -W B1044M I9I310 ICm u te * Bahm, som re. u Spia) SOCCO NQ 73000 OKLMN-GW -W 6104-0-060110 Low S p ll Sppb (COMM,eoa dqIL FWd SiUlv } 5000 NQ , 6730 OKLMhMSW *Weit>aJ>-06M1ll HtflhSplW efcOppb tcoctektrr, soooon ai. ri*w pik. | 50000 NQ 60700 154 5000 : NO 146 50000 ND 135 5000 N 139 50000 ND ' 5050 48000 4720 51200 101 96 94 102 OKLMN-OVW 201-C-0>S40 (COMteie Se* C.W nflL U h io ite | QKLMN-GW -W 2O1-0-OSO10 (C0M44SI 9pk 0,50000 n/L U bS pIte) O KLM N-G W -W 1-0>S0310 Low B plk* 0 3 ppb (COOM4*d,SQOfi4|LfM dSplk>) OKLMN4W -W N2P1HMM031P Hip b 8pBce ppb tceO M 4M .*IM i#ILF1aliS|9k*) 5000 50000 6 5000 74.0 74.0 74.0 74.0 5580 65500 877 7560 130 6000 131 50000 121 500 ISO 5000 ND NO ND ND 4810 44400 543 5360 92 68 109 108 O K M U M ^ w a a -iw is a jt . (Coo*47 8jA i . scoo nao.u* spi** ! QKLMN-GW-W 20-O-O603M ICOOMW7BpKF, MMOitgA. UH SpWt ) OKLMN-GW-WJXl-O-OSOW Low S pili 5 ppb fC N M e*;sootiiLndii Spilo) O KLM N^W -W 20>O-Q IM Hlflh S p i) SO ppb . <ooo4ro>soooa o t FUte Spik. ) 5000 500C 5000 60000 13000 19400 13800 7T100 13800 20500 13S00 83000 110 6000 12900 126 50000 12900 140 5000 142 . SOOOO 12900 12900 16200 55200 10200 48400 66 85 66 71 OKLMN .W U ^P S O S O B (CM444714(*G,BOOOn *fl U b Bpfl) OKLMN-GW-WBMJ-OSOSdB (C0CM47I spk K. tOQOD ngO. Ufo S p i) OKLM N-eW -W Z24H)B030 LOW S p H te lp p b (Cocan, sodo oiu fw w S p i ) O K LM N -6W 4V2244SO M High Splfcs SO ppb (CW5M474. SOOOOn4- Fiate Spi 1 O KLMN-GW -W 31-a-050108 (C0004479$ f* 1,SOM nplU-lfc 3plk> 0KUMN-<SW -W 31-<MaM e ICOOS447S3pk J, wooa TL U b S fU k . ) OKLM M -OW -W 31-0-050M High S p lk* SO ppb (C0054477.50000 IL H.W S p i } 5000 50000 5000 50000 5000 60000 50000 36300 36600 36600 38800 1300 1300 1300 44100 109000 44000 111000 . . . " 5000 145 50000 5000 149 50000 .31400 31400 31400 31400 450 70500 00900 143 138 .. 179 5000 5130 SOOOO . 5130 SOOOO 5130 37000 73000 35000 62200 9090 51200 63200 . 63 * 62 79 92 110 O K LM N 'G W -W M -O -O SO M S <ax44?4 Spk K, sooa non. l* u 3p<h| OKLMN 43W -W 32-0 <050108 (C4064471 SpK L.50000 nIL l*b 8pik* } O K lM N ^W -W U -0-000309 U)W Splk Sppb (C0064450.5009 ngfl. Fitte S pi ) O K U *N -0W -W 32<<W O l0H H |hS plkaippb <00004451, SOOOOIL Fitte 3 p | 5000 50000 5000 50000 2160 2180 2180 2180 0910 130 67300 130 1.0800 172 65500 127 5000 50000 5000 60000 3000 -3000 3000 3000 T400 SOOOO 7010 52800 66 94 96 100 Somple (estere mcaecii the p ik in g level therefore, an accurate recovery value cannot be calculated NO * Net detected et OCSbov SnQ/U(ppt), NQ * hkriquantffiitoe * Measured concentration tetween 2$ n g ll iPPQ and the U n it 1 Q jam )teifon(LO Q ) which fe 50 ns/t-fepi). - - -........... < Note; 6ln e * th i* aum m ary ta b ). how ro u n d id (ulte, rtc o w r y v a lu ta m ay vary Rghtly fromth. value* Inthe rawdata. . Exygen Research ,k\; Page 26 of 110 000049 :Interim Report #1 -Analysis o f Oakdale Water Samples Exygen. Study N o.: P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued . S am ple. . D e sc rip tio n 04 Sulfonate HFB3 Am cunt Am tFound Am ount S p ked in Sam ple Rn o v I f m .(BflL) .... ia tfU - R pcovtry { * > .. Am ount S piked ( II -} Cl SulfonatePFHS Am t Found Am ount In Sam ple Recovered Recovery tn a /U in tfl) ... JS ). O K U *N -aw -vrair-c-4>503M (0M44K $pkM. M neA.Lab 8plte ) 0KLM IW 3W .W J1 7 -0 4 8 0 3 0 * |Cso*44*s spk n, w o t n*iL Lab Spite > O KLMN-OW .W 217-0.6503D Low Spike l ppb (pOMUM,SSnaA-HtkiSpite ) 0 4O M N ^ W -W a iT 4 H M M | H igh Spike SO ppb (CD**4m MOWr>*rt_Fi.li Spite 1 5000 .60000 . 0 0 50000 ND NP NO ND 6680 86800 7570 71200 134 5000 ' ND ' 1S4 60000 ND 151 5000 ND 142 50000 ;. ND 48 BO 46500 4580 51300 86 93 92 103 OKLN N43W -W 20084I4W 03W (CMS44IS Spie0 , K M n*A . Lab Spite 1 O K L M h M W ^ 200^M I60M > ICDOeUUSpkP. SMOCnglLLab Spite) OKLMN4JW-W200B-0-W OMM Low Spike S ppb fCOOSMSS,MQt n p l Flaw Spite ) O K U IN W 4W U K M 4m M M H igh Spike SOppb (0*0*4411, MOM ng/L Field Spite ) 000 50000 5000 50000 0780 6780 6780 6780 14300 73800 16600 87000 150 6000' 10100 134 50000 10100 194 6000 10100 162 50000 10100 16000 56500 18300 84800 118 93 184 109 OKLMN-QW -W MIi-O-OBOaO* (GMS44W Spk C, 5009n*A. Lab Spite 1 0K LM N W -W 2tH 2449 30 . (CKOteO* Spkp, BOOMnalL Lab Spite | O KLM N 4IW -W 2012-0480309 Low S p in ppb tcooeaB ,o*naiLn.i4S a) OKLMN4JW -W 20I3.O4IW SO# H igh S p k * SOppb ICDW44W, 50000 ngL field Splk) ,60p0 50C00 5000 50000 2210 8800 2210, ' 06400 ' 2210 8210 2210 71500. 132 .. 5000 4700 128 50000 :470o 120 : 8000 .. 4 70 0' . 138 ' ' 50000 4700 8140 46900 8950 53800 SB 84 85 96 OKLMN-OW-WBO-0-OE0309 (cm aaw sp e, twoa p ita b spun r O K U i*N -Q W 4yiB 4l4>M l3( (0*064494 SpkF 00 npL Lab Spite j OlUJHN'4!MNB04Mt5030S Lew Spike S ppb (CM644BA.SOMned. Field Spite ) OKLM NW -W B04M IS030B H igh S p lk* GOppb (Cootuer, sooponan. n s p i*. ) OKLMN^iW4F>WHM>50310 . (0*0*44*1 Spk B, *0*0 npiLLab Spite ) OKLMN43W4=W 1-0.0TO10 jC0M44*a Spk H, OOOOOnpA Lab Spite) OKUAN-GW -fW I-O-tMM Low Spike 6 ppb (000*4300,MOOnprt. Reid Spite) OKLMN45W-PW1 -0-05030* High S p ik e ppb (CDO04MH, 50000 ngA-FUdSpO) OKLMN^W-PW2-1>-050310 <CM45C2 5pk L CMr&L U) SpUc*1 0KLM N4>W -f>W 24)484310 (000*4002Spk4,SOMr>#ILLabSpite ) OKLMN-OVK-FWJ-045M310 Low S p k * $ ppb ' (CMMSM.BBOB eg/l. Field Spite) ' OKLMN43W 4W 2-<MiH810 High S pike SO ppb (C04S4MS.50*00npA Raid Spite ) 5000 ND 8850 137 m o aooo 's o c o 50000 ND NO ND " 64700, 7390 69700 12B 60000 14B " 5000 139 30000 8000 5620 13600 160 5000 50000 5000 5820 r 25620 72000 13100 ,135( 60000 ISO 5000 50000 6620 60700| 128 50000 5000 641 7720 142 5000 soooo 641 65900' 131 ' 50000 600CT' - 641 - 7030 ....128 5000 SOOOO 641 6300 , 127 50000 ND 4860 ND 46200 NQV " S2D0 NO 4S200 4160 ease 4160 . 52000 41 BO 7680 4180 , . 47700 501 5280 501 47700 501 5160 501 ' 44300 100 92 104 96 94 86 71 87 95 84 94 88 ,m'Samplo residue eKceeds the spiking level signmcaolV, therefore, aocuralc rocovary value, caorerf be calculated ND = Not detected acor above 25 n^L <ppt). ' '' NQ a Not quantitable " M ew ured concentroUan between 25 n0 l_ (ppt) and ttiB Limit of Quantfallen (lO Q } which It 50 nftA. (ppi). Not*: nc* this suitm ary table sltowe rounded suits, recovery values may vary sightly from the value* b>th* aw data. Exygen Research Page 27 of 110 000050 interim Report #1-Analysis o f Oakdale Water Samples Exygen Study N a : P0001400 Table II. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued Sam ple D e ec rip tto n O K U *N -O W -P w a-o-oso3io (COCMSO* SoleK, SOWmart. Lab Sptka) O Ki.M h-G VV-PW 3-0*05310 <COOt* SpbU 40*00 no. Lab Spike) OKLMN-QW-PW34-OS031O Low Spike S ppb (CoosesM, 5000 npL FM0 Splice) OKUtfM-GW -PWS-o-oSOHO Hlgh Splke SO ppb (OOOWSW, SWOOn#*. Field Spike) C4 Sulfonate PFBS Amount Am t Found Am ount Spiked h Sample Recovered R e c o v e ry (nglL) (n s /L ) tnoOJ (%> A m ount Spiked .. ("3A -> C6 Sulfonate PFHS Am t Found In Sam ple Am ount Recovered (n o n .) Race vary |W> 5000 SOOOO 5000 50000 5970 . 13800 8970 98900 6970 1,5200 B970 92300 137 5000 10000 13600 180 50000 10000 . 54400 185 ,, 5000 ' 10000 _ 16300 ' 171 60000 10000 54900 72 as 126 ec QKUUN-GW-F'W t-tW M J IO : (CireeiSII Spit M.SOM ng/L Lab Spike ) OKLMN-GW -PW M-MSOStO (COtreUtt SakN, OOtOOnvLLab Spike) OKLMN-<3W-PW4-0-C5<IJ10 Low SpBw 3 ppb (COOMSU,00 np/L Field Spike) OKUUN-GVW-PVM-0-0S0M1) M ghS pareS a ppb (COMMIT 5W BgiLftol|l spike) 6000 50000 5000 50000 8130 8130 8130 8130 17400 95000 16300 88800 185 6000 78 9 174 50000 . 7890 163 5000 7890 162 50000 7880 13900 53600 13500 58200 120 91 112 101 O KLM N -(5W -fW 9-<M )M 310 <C0<M4 $pk 0,9000 ngJl- Lab Apikm } Q KUW N-O W -fW S-045031 0 <CMM3U Spk P,90000nL Lafa Spike) O K LM lW iW -P W S dW im i 9 LOW S p fl S ppb (C00445H. 90M eWL Rad Spike) OKUMN'GW -PVM-O.OSMtO H igh S plit SC ppb (COOUI7,50000 ngO. Field Spike) 5000 79aO . . 17200 50000 7930 90600 6000 7930 17100 50000 7930 04800 186. 166 183 173 5000 " 14500 SOOOO 14500 5000 14500 50000 14500 20600 58800 20800 69400 122 89 128 90 OKLM N-GW -PW 10 4 -0 6 0 H C (C w 1* Spk C,4ooq n * t Lab Spike 1 O KUdN-G W -PW 10-05031C |COOMM*SpK P, 50MO npL U b Spike) OKLMM43W-PW O-M5B0310 Low S pIkftSppb (COOMAi^ 6<NWna*. PM4 SfUl ) OKLMN-OW-RW1 D-0-OS0310 High S pike SO ppb (CDOUast. SHOO npft. Field Spfce) 5000 50000 5000 50000 13100 13100 13100 13100 19300 70700 19000 74000 124 6000 29200 133 50000 29200 118 5000 29200 122 50000 29200 34300 71000 33500 71300 102 84 88 84 OKLMN43W -PW 114-060310 (CWMSZZ SpkE. 9000 nglL Lab Spike 1 O KLM N-G W -PW 114-0O aiO (C00*UQ1 SpkF,SOtt n/LLeb Spike | OKLM N-GW JPW 114-050310 Low Spike 5 ppb ICOOMf&L 500 "Oh. Field *dk ) O K LM N -tiW -P W It-0-050310H igh 8pkB#0ppb (06044S2, S000nglL Field Spike) 5000 60000 5000 50000 6520 6620 6320 8520 IZ700 68300 13200 63800 124 5000 8820 124 SOOOO 8820 134 6000 8 320 114 50000 8820 14200 55100 13300 54800 100 93 90 92 'Senwle reek** exceeds Vw aplklna levd isnificaiWy; tflefetare, an sccuraMrecoveryvalue cannol be calcutoterJ NO Not detected ator above 25 ngM pcflNQ = NotqvinS0lWo~ Wcajured concenIraSon between25 ng/L (ppl) and the Limit ol Quantitation (LQQ)wtilch fct 50 ngA. (ppl), Note: Sine* th is eumenary table h o w * ro u n ie issues, recovery values m ay vary s lig h tly b n the values In ifre raw d*tp. Exygen Research Page 23 o f 110 000091 Interim Report #1 -Analysis o f Oakdale Water Samples' Exygen Study No.: P0001400 Table II. Matrix Spike Recovery of PFRS and PFHS in Water Samples Continued ` .' . . . > Sam ple D escrip tio n ! .y 0 4 S ulfonate PFBS Amount Amt Found Amount Spiked In Sam ple Recovered Reoovey .....--fo tfw < * *) ft Am ount S p ited w C* Sulfonate PFH3 Am t Found Am ount In Sam ple Recovered Recovery in o ....... ( * > OKLMN-SW -O-OMJIO (Conee#*a* 0 , SWOsrt.Lab 9p* } OICU4N.8W 4J-CIM81 (COOMsatBhH, 5W m >rLUb8)>lf*) . O K LM N -8W -0-W aaiO Low S pike E ppb (cee*M3,i>on.nidSi>MM) OKLMN-8W 4W J5W 10 H h Spc sd pp ij [Coomsw, aoaoo non. Fuin spin. ) 5000 50000 ' 5000 50000 NQ UQ NQ NQ 5690 63800 7280 65000 120 6000 128 50000 145 5000 NQ NQ NQ 4780 45100 5250 130 50000 NQ ' : 48400 06 80 105 88 0KLM hW 3W -TW P3-C-0M 310 l o w Spike S ppb (coorueti, sodo non. Seika DKLMN-QW -TRIP2-04)60310 HH)h Spike SO ppb rCOMU%O40 nelL Spnu | 5000 50000 NO NO 4480 28100 BO : 5000 58 soooo NO : NQ 4370 48000 88 9B A verag e: Standard Deviation! 141 ' 21 `Sample lealdue exceed f t * tp W n g level IflnMqwiBy, therefore, an accurals recovery value cernol be calculated WO * detected lo ra b o v e 25 n g /l (pplj. NQ Not quanM Ubte Measured cdnoebtralfori between 28 nolL(ppt) and the lim it o t Quanfitaaurt (LOQ) which >s$0 og/L (ppi>. N o tti Since tbla eunm iytabla show* raundad rMuHe.racovefy vefue* may vary alightty from the values In the raw data. A v a r* ; Standard Deviation: Exygen Research Page 29 o f 110 000052 interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No. : POO014OO in.Table Matrix Spike Recovery of PFOS and PFOA in Water Samples Simple ' - D escription {CHOM4UOKLMN-GW -W 3"0-O50310 8p* C. 0 bIL U b ecu* ) tcnoefttfO KLM N 43W -W 3O -<lSO ai0 ape d , woo n*iL te e spike ) ppb0KLMN-GW -W 3--QS310 L o w Spike 5 OdIW 44W , Field S ote > ICMM487,MMO FWdOKLMN-GW<W 3-tWfSW 10 H iflli S pike 50 ppb *. pite CSSuM anateFFO S Amount FoundAmt Am ount Am ount Spiked SpikedIn Sem ple Recovered Recovery AlamStaFmoupnled C S AtW PPOA RAecmoovuenretd Recovery w (rtflfl.) - B t i ______f f ) . ____ (nflft.) in o lL ) ... m 5000 50000 5000 50000 4750 4750 4750 4750 12400 73500 10900 84500 153 6000 138 50000 123 6000 160 50000 6330 8330 6330 6330 . 11900 59200 9470 40100 111 106 83 80 O K U ! H -G W -W -0-050310 (C M eedt 3k e, MOO n tfl. Lall Spite} 3000 59.0 . 4940 OKLM N-GW -W B-C-050310 (C0M44M Spk F, HMOdnpIL Lab Spite ) OKLMM-IGCOWW-W44109-O,-CW5e0e3e1RO-LFMowdSSpplkfk.las ppb HighOKLMN-GW -W -O-O503f0 S pike 50 ppb (C00411. W O cpILPWU Spite t 50000 5000 ,5 0 0 0 0 69.0 6 9 .0 59.0 55000 5380 50500 96 5000 110 50000 10 5000 101 50000 290 . 5350 250 51900 290 6050 290 30900 101 103 115 77 MOOngfLLabopte)OKLMN-CW -W2S-0-0SO310 {Ccoeuuapk G. (OaOM441 LabOKLWN-SW-W28m^WSOJ SpkH, toco nIL Spite) -0-0 Spike5ppbOKLMN-GW -W 24 50310 Low WM )|CW4414. n jfl. Field Spite Spike ppb0KLMN-GW -W 2&-0-C5031C High 50 (CotHH4li, SdbW ngll Fted Spite ) 5000 50000 5000 50000 13500000 9450000 13500000 7390000 13600000 9050000 13500000 7210000 5000 79300000 86300000 50000, 70300000 68300000 5000 79300000 73100000 50000 79300000 57WOOO UrtaOKLMN-GW -W 33.<f-050310 IOWM41 Spk 1, 00 BBS. Spite) 5000 4610000 4720000 5000 1750000 Spkj.saooa )DKLMN-OW -W 33*0"O8O31O (C008U1* cqit-U b Spite 50000 4010000 4730000 * 50000 1750000 {CODM411, &fk*>O K W H -G W *m M 4 $ Q m U w S p i**5 p p t> K K n^Ln*ki 3000 4610000 4920000 5000 1750000 OKLMN-G<WCM-VMV+MU-,0M-CM5OOn31p0f.HFieigldhSSppiteik)e50ppb 50000 10000 4520000 * 50000. 1750000 1520000 1650000 2350000 1630000 * (C0OMK4LCMHNSp-GkKW.-SWM2S0p5p-0IL-0L3tb0S31p0ite) OKLM N-G W JW 05-00 50 3 10 tC m o Spk L, s e w nplL lab Spite i ppb0K LM N O W -W 2050-050310 Low S pike 5 (COOmu,kW noH FieldSpite ! oxLm-G(wC9-MmMo33s,-SibHOaMQam*.FhkMmUSpsitpe}soppb 5000 50000 5000 50000 14800 140000 146000 146000 , 136000 166000 129000 221000 . ' ... 500C 20 50000 v 5003150 50000 147000 160000 147000 190000 147000 143000 147000 184000 .* 86 * 74 O ia M N ^ W -W 2 1 5 0 0 5 0 3 1 0 . {CoaeHMSpkM. MOfl ittfL Lab Spite) (caOeeKML2M4SNp-6kWN.O90V0(21n5p0lt0-,3U0.b3S1p0ite) QKLMN-O(CWP0*W*42iM15,-O-0n5#Ov3n1O*>LdowSpSitep1lk S ppb HighO K LM M -G W -V1 15O O 5031O S p ik e ppb (C90*U2A Spite)npiL FMd 5000 50000 5000 50000, 37100 52400 >. 5000 317100 96900 '3 7 1 0 0 ' 5800 120 .. 5000 5000 37100. 101000 , , '2 8 50000 4400 4400 4400 4400 8650 56700 8600 39200 89 105 85 TO "Sample residua exceed! the splWno level g iito n tly; therefore, an accurate recovery value cannot be calculated ND Not detected at or above 25 ngfLCppt). NQ * Not quantifiable * Measured concentration between 25 na/L (ppl) and the lim it oi Quanttetlon (LOQ) which SO npA. (ppt). N o d : Since this *unvnry u tile sh o w * founded rw ralt*, recovery value* may very llphpy from Uw v a in ** In th raw data. Exygen Research Page 30 of 110 QOOQ53 .Interim Report #1-Analysis o f Oakdale Water Samples ; Exygen Study No.: PGOO1400 Table HI* Matrix Spike Recovery of PFOS and PFQA in Water Samples Continued S em ple C8 Sulfonat PFOS C* Add PFOA Amount Amt Found Amount Amount Amt Found Amount Spiked In Semple Recovered Recovery Spiked In SampI* Recovered Recovery O KLM N -G W -W 201CHHIS0310 {Coteens pa c, a m n.Lt>spn* ) OKLWN-GW-W2010-0-050310 tCOMMatgpkO.SMMtnsA.UlOSfU) OKLWN-OW-W2010-C<50310Low Spike 5ppb <C00fU0, MODnon FhHd3fJk ) OXLMN-GW-W201IH K tM 310H igh S p i 50ppb {cneceui, win ngn.FMdSplk| 500C . 50000 : 5000 50000 . ND nd NO ' NO 5170 103 54600 109 5270 105 54800 " 110 O K L M N - W ^W r- S m itl (COM4aape,M M n0l(.Lai>ptet) O K LM H -SW .PW 7-CM)50310 (CeotMai 8p* F.**e *gA U b Sete ) OKLMN-G(CWeo4ewWM7.-900<00Mxe31rc0nLtwowpSikp*iki e 5ppb O KU tN -G(CW004-f4W40-5h, -SOOOSMWnfIfDlL H igh Spike FI*W Uptk ) SOppto 5000 71600 7BSQ0 . 50000 71600 i 119000 95 5000 71600 72800 ' ' . .'. 60000 71600 118000 88 OKLMN-G(WCM-TMR4J1PT1,S-0M-005iiB63n1.F0lLkorSwi>Sllnp)ike 5ppb 5000 OKLM M-GW-TWP1-0-050310H igh Spike 50ppb (C00C44M. MODO(ltd. FMd Spill > ' 50000 ND ND 5780 1.16 53500 107 OKLMN-OW-PW8-W W 0310 tcoaei4iasp fcG ,ia H ii9iLijibSpik ) C>KLMN-QW-PWB^M>90310 ICWM44I spa H,MM npL lab Bp* | - OKLMN-G(CWO-WPW+*4M,M50W0enOBS>IOLFiLWowpSlWpri)ke S ppb OKUHN-G(CW00-0PWW4S9.-dSO-0M3O03up1*0. FHteigWhSSpiap*)* SOppb 5000 34300 50000 34300 5000 34300 50000 34300 3B500 80800 38400 63100 - 111 - 166 OKLMN-GW-PW#-P-C0J10 tC*M4444Spk 19M non.U b W Hi I OKLMN-GW-PWS-O-O50S10 (c *44e i sp* j, ooo on. u n spite) OKJJ4N-GVV-PW9-0-060110Low Spike 5ppb (0604444$,MOOnglLFtek) 8pU>*) G KU W N^W 4*VTO*0-OW3tO $09* rtfr*. PH%igMht$0Jph**&) SOppfe (CQS0KML4MNS4p5KWK-,W9060100n2fl-d0-L3a5b0S3p1ia0* ) OKLM N-Q W-W B1CZ'-O-050310 (coaeuw Spau, boom nod. Lb apea i OKt.MN-G|CWBO-w-ei5OJ,25W 5W Fl0MLdo9w(JSklp)ike $ ppb OKUM K^W(C*ftW**4f4t1S0t,2S4H-O5tn0&3iLaPHlaildfijZb&Skmp|H\ 850ppb 5000 84400 soooo 84400 5000 B4400 $oqoq 64400 5000 NQ 50000 NQ 5000 ' NQ 50000 NQ ; 83200 138000 88400 778000 '. 107 v 183 5300 ; . 106 , 55800 112 5480 110 53200 106 5000 ' NO 50000 V NQ 5000 m 50000 NQ $000 37800 60000 37600 5000 37600 SOOOO 37600 5000 - ND soooo- ND 5000 61400 50000 61400 5000 81400 50000 61400 5000 48000 50000 48000 5000 49000 50000 49000 5000 214 50000 214 5000 '214 SOOOO J 214 ' 5290 54300 4710 ' 32300 41800 86100 42800 87100 5360 50500 61000 113000 58300 82200 50400 87900 55200 83200 5880 52700 6610 35300 ' Sample m*Woe exceeds the spkino level spnlficarMly, thamfoce, an accurate r e c t w y value eawiM be calculated NO Not delected at or above 26 ngA. (ppQ, ' NQ = Not qusndftaWe * Measured concentration between 25 n j/L (pp<) and the lim it of Quai>tiltian(Loa)ymi<iliIs50io'U(ppi). . .. ......... ............. Note: Since th l* eummary U b l* hows rounded reauita. recovery vala* may vary liahfly from the v *lu *s In th raw oat*. '' ; 106 108 84 55 ,, 87 . 59 107 101 . 103 . 42 .' 98 - 80 113 105 108 70 Exygen Research Page 3 l o f i 10 000054 Interim Report #1-Analysis o f Oakdale Water Samples Exygeti Study No.: P0001400 Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued S im p l . . D escription C8Sulfonate PFOS Am ount Am t Found Am ount Am ount Spiked In S im p le R e to w e d Recovery Spiked fPD>U in u /U - W W _____ l fc L C8Add PFOA Am t Found A m ount In Sam ple Recovered in jtf.) W4 R eco very W O KLM M -G W -W 6104-0-050310 (O M M 4M Sph hl, W K ) al|, Lao plk* ) - O KLM N -G W -W 5104-0-05C310 (CooeeeM Spk N. SOM n o t Lab Spike > O KLM N <CW -W 104-0-090310 Low S pike 5 ppb (CeOOUM, SOM npIL FlfW Spike | O KLM N -G W -W 6104-0-030310 H igh S pike 50 ppb I C M t u n , COM no- rie Id Spike ] 6000 50000 5000 60000 100 109 109 109 5540 58100 5700 58700 108 5000 116 50000 112 5000 113 50000 207 207 207 207 5290 57300 5470 3SS00 102 114 105 71 O KLM N -G W -W S201-0-050310 (COO** Spk C, 50POOh. L0 SpOtf) O KLHN-G W -W S2 1-0-050310 (CW44S*pkD, 90040 IL Lab Spike) O KLM N -G W -W 8201-0-050310 Low S p ila 0 .5 ppb (000(44*4, SMngiL Field Splka) OKLMN-GVy-W 82014J4150310 H igh S p ilt* 5 ppb (C4044441, X ItfFL Field Spile* | 6000 50000 500 5000 NQ NQ NQ NQ : 4S80 50000 670 6600 too 5000 ' 95.5 4W0 100 50000 9 5 .5 50800 134 500 9 5 .5 006 132 5000 ' 95.5 ' ! ' 8130 97 101 102 121 O KLM N-CW -W 2 -0-O 5M 09 ICOOM447 Spk E, 50M dpIL Lab 8p*l# > OKLW N-GW -W aa-O-OSHO IC0004407 Spk F. MOW nglL U b Spike ) , O KLM MOWtVSO-O-OSOSO Low S pike S p p b (COOM 4*e.PM nBlLFhM Selkl O K LM N -G W -W 2O -O -O 50JO 8 H i t) S pike 5 0 ppb (00*4470, SOCCO nod. FW d Spike ) 6000 50000 5000 50000 46600 46800 46600 46800 49900 92800 41900 59500 5000 92 WOOD * 5000 26' , 50000 285000 Z850PD 285000 285000 289000 295000 278000 264000 * * 0K LM K -G W -W 2S -0-050309 (CUUM47 SpkG , SAM n e l Leh Spike) OKLMN4SW -W 2S-O-OS030 (C0404471 Spk H. SOM ng/L Lab S p k* I O K L M M -G W -W 2 2 -0 -0 5 0 3 0 9 L aw S pike S p p b (C0044473,9400HfiA.Field Spike) O KLM H -G W -W 4W I50JO 9 H I0 h S pike 50 ppb (090*4474,90000 ntt/L Field Spike ) O K LM N -C W -W 31-0-05030 (CP04447SSpk 1,9000 npiL Lab Spice ) O KLM N -O W -W 31-0-050309 |COOV<79S p k 3,9000 it)pL lafaSpIke) O K U * tN -t;W -W 3 1 -0-050SOS H lp tt s p ik e 5 0 p p b (CAM44TI, MOM A p t Field Spike ) 5000 45800 6 0 0 0 0 . .45800 5000 . 45800 50000 45800 44600 S850 41200 .65800 5000 13200p , . 116000 50000 132000 50000 132000 169000 216000 - .5000 105 50000 * ' 5000 40 50000 317000 317000 317000 317000 * 5000 72 50000 168 50000 23100 23100 23100 330000 412000 324000 288000 26400 71300 65700 * * * S fi 85 OKLM N-GW -W 32-0-OS0304 (C000447I S pk K. *900 (Ip*. Lab Spike) DKLM N-<5W -W 52-0-030309 (CM*447*9p<tL 90000 nglL Lab Spike) OKLMN-GW -W 324)-050309 Low Spfce 5 ppb (000*44*0, MOO npn. Field tp ik * ) KLM N-G W -W 32- -050309 H igh S pate SO ppb (CM W-U 1, BOOOOnp*. Field Spike ) 5000 50000 6000 50000 47100 4T100 47100 47100 62200 5000 115000 138 500 0 0 74000 ` 5000 120000 14. 50000 117000 117000 117000 117000 10S000 151000 131000 1S700 - - * "Sarr.pte residua exceed* the sp*kirg level slgnWcanay; tterefors, an a c e ta te recovery value cannot t calculated MD Not detected al or above 25 r>aVL(ppii. : . , NQ Not quatiSfiable = Mea6ured concentration between 25 n jA (ppt) and the Umlt of ' . QuanBlaBon (LOQJ vdilch Is SO n plL(ppt).' . , ' . ' V ., , Not: Since this ium m erytaW e * h a w * rounded reeull*, recovery value* may vary iiantiy '. from the v ilu e f in the raw data. .. Exygen Research Page 32 o f l l O 000055 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 f Table III* Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued V. ' - v : Sam ple . . s c rip tion OKLM N-GW -W 217-0<05e30S (CMSMU 3pfcM.00C4 n g l Lab Spilo 1 Q KLM N-G W -W 717-0-O 50309 (080*4+12 Sek N. SMM no. Lab Splka ) O KLM N -G W -W 217-0-050309 Low S pike S ppb . <C*0444.4**IL FliM Sp*o } O K LM N -Q W -W 217-0-<0 H lflli Spike 50 ppb {C W H 4tS,ti0M nalU fM dint) Cl SulfonatePFOS Am ount Am t Found Am ount Am ount S piked in Sam ple Recovered Recovery S piked fro m <08^4 .. W ____. B L . ...fo a M . CSAeld PFOA Amt Found hn Sam pi# Am ount R e co ve red < nen-) ...... (nart->..... 5000 NQ 4790 96 5000 NO 4860 .50 0 00 5000 NO . , NQ 60000 NQ . 49700 5800 65300 99 50000 ' NQ - 52200 '116 5000 NQ 4880 131 50000 NQ . 42600 OKLM N-G W -W 200B-C-0SOSOS ICMM 4M SkO. 6900 a g l Lab Splka ) Q KLM N -G W -W 2006-0'Q 50399 (Ce*+4*e*pfc, MOOn*n.Labelka | O KLMN-GW -W 2008-0-050309 Low S p ike 5 ppt) , <C0044M. MOOnolFlaKI # 0 **) OKLMN-GW-W2OOB-O-O503O9 W ehS ptko 50 ppb ... (COMMM, neoo'ngl Wald ip * ) 5000 50000 . 5000 50000 15500 15500 15500 15500 20800 09300 Z70D0 71300 106 5000 106 50000 230 5000 112 ; 60000 59300 . 04800 59300 114000 59300 59300 73600 94600 OKLM N-Q W -W 2012-C-O 503W <C09M4*Sab C, OS ngti. Lab SplM } 5000 .117000 O KLM tW 5W -W 201W )-O 50a0 <coM 44*esbD .M eeengn.ubS aii*) SDOOO 117000 O K L M I^ W -W 1 2 -0 -0 5 M M Low S pike 5 ppb (c m m m * . soce p i pi -, .5000 ; 1,117000 OKLMN-GW -W 2012-9-0SO3D9 H igh S pike 0 ppb (000044*2.96090!nglL Flak) Sgrfloi ) 60000 " 117000 143000 .186000 115000 203000 6000 46900 138 ! 60000 46900 5000 . 46900 172 - 50000 46900 57700 64700 48500 89500 QKLMN-GVV-WBO-O-OSOM (C0eM4S4 Spk * , SS09 a g l Lab Spike ) 5000 : . -ND * 5280 J06 5000 OKLM N -G W -W i0-0-050300 (C00M4M Spk r , SOOCtitip i Lab Sp* ) 50000 - ' N D . OKLM f+43W -W 80-04 5 0 3 0 9 Low Bpfcb 5 DPfc (CMNM4*. 8*00 n g l n *m Spbua) ' " 5000 ' ' ' ' ; ND j OKLMN-GW-W SO-0-050109 H ig h S pike 50 ppb <CM*u7, (ftooe n i FiaM Op*> ' ' '50000 N D .' '52900 1 5720 1 57600 106: > 50000 114' '6000 115 50000 . O KLM N ^SW -PW I-0-050310 (00*444*1 Spk G,(409 n g l Lab Spilo} 6000 . O K tM N ^ W -W 1 -O H M a iC {COM44M Sc* H.POCOngILtMb 90U* ) 500C' OKLMN-GW -PW I-O-OSOJtO Low S p lk * 5 ppb ' . 1. , (Cdo*+ o, teas ngn. naie Spie* i 5000 O K L M N -6W -P W 1-O 45 3TO H l0tlS plk*S 0ppb (Ceos, MOODn g l Flak tf+ka ) SOOO 66900 *66800 60900 6690 ' 72000 116000 36900 '' 95200 5000 102' 50000 5000 5 7 ' SOOO O KLM H-Q W -jPW 2<M a031O ' |C*9*4S*i6pk 1, ai)M n g l Lab Sail i 5000 ' OKLM N-G W -PW 2-0-050310 (COtxasa Spk *, SMee ngJLLab Splka I ' . ( 50000 OKLMN-GW -PW 2-<M)50310 to w S p lk * 5 ppb (CBObiitx, Jeeoign.F)*apai . 6000 , 0K LM N -G W -P W 2-0450310 H igh 3 p lk * 50 ppb (C0644HS, 04*0 n e lFM 4 Splk*) ;v 50000 351 5480 351 59800 . 351; ..... ..4 2 6 0 . 351 40500 ,. . 103. , a . 119. .6000 50000 . 79 5000 8 0- 60000 302 1 302 302 3CQ 37300 37300 37300 37300 3630 3630 3630 3630 5810 53100 5860 42200 47700 90200 40400 80500 8720 58800 7860 39500 R ecovery m 97 104 98 86 . 109 . 71 . 96 . 85 110 106 111 &4 . 106 ' 86 102 110 65 72 Sample residue eaceeda the apiklnglevd signtfcanay; therefore, an accurate recovery vJu* cannot&e eeleutoted NO * Ngtde8CttdJitoraDove2SnQ/t jppti . .. NQ a NW qwnWtabte Uaajred MWcamreBoti between 25 no. IppQ and the U nit o l Quantitation (IO Q ) which i 50 not. (ppt). Wo**Since W u*m tary table how rouided result*, reccwary values mayvary nightly from the vxlu*s In the raw data. Exygen Research Page 33 of 110 000056 interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: PD001400 Table HI. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sample Dewipoon Ct Sulfonate PFOS CSAcid PfCA Amount Amt Found Amount Amount Amt Found Amount Spiked In Sample Recovered Recovery Spiked in Sample Recovered (nan.) (nnflj (nq>U (%) (tftlL) tn q /U In o /U Recovery (%) O KLM ht-G W -PW S-0-050310 <C0W4#M Sph K, SOMpplLlari)Spilo* ) O K LM N -G W -P W 3-W 0J10 {ceeMooespkt, secoogn.ub apu> OKLUN-GW-RW3.4MH0310 Low Splka Sppb CCSe*4.8Mn8/LFItWr<k> aK LM N 43W -P W 34J-05i10 High Splk 50 ppb (h o m m , im m irari, violeselle ) OKLM M 5W -PW 4-0-0S C 310 1C0M4319SpAN, SOM nfl/L lab Uplke) QKLMN-GVV-PW 4-e-950310 (co*s4ftespi ^ swoonei. u apo*) OKLMN-GW-PW4-0-05Q3V) LOW Splk5 ppb tC0M4412.5000nolLFIeMSplk 1 O KLM N-0W HPW 4-0-O5M10 HlQhSpiKe 50 ppb team. joomn nidsptiu) 6000 50000 5000 50000 5000 50000 5000 50000 32700 32700 32700 32700 33800 33800 33800 33600 43300 .6 6 1 0 0 33800 60000 42500 75700 42200 81200 SODO 177000 67 60000 ' 177000 . .. r, 5000 177000 55 50000 177000 * 5000 72100 8 4 V . 50000 . 72100 5000 72100 85 50000 72100 138OQ0 190000 196000 204000 77500 121000 80700 118000 m 26 * 54 . 98 68 OKLM N -G W -P W i-C -080310 (C0W5U spk0 . r n t no*. LekSpili ) K LM N -G W -f'W C -fl-050310 (paOMSt* ftpk P. MOM nplL Labtytt* I 0K L M N -G W -W 6-0-C 50310 Low Sp8(* 5 ppb <C00Wf1.RM ftgfLFMdSplk*) O KLM N -G W -PW fi-0-050310 High Splka 50 ppb (CM*45ir,SOOOCngfl. FMd Sfrik ) 5000 50000 5000 50000 90000 . 97600 . * ; ' 5000 90000 139000 ' 98 50000 90000 94100 5000 90000 124000 68 50000 78400 78400 78400 78400 82900 133000 87000 116000 - 109 * 75 O KLMN-GW -PW 1(W M5d310 (CSMW1spk C. setBfl.L*b SplM | O K LM N -G W -FV H 0-fl-050310 |CW*431*Bpk 0, 500C0nt- Lk Spll } O K U M N 4W 4W 1O 4W O 3*0 Li>wSpikt Sppb pfiOMSM,5000n&L FIWSpA*) OKLM N-GW -PW 1D-0-050310 High Spk* 80 ppb fCMUKI,SOnpA. FMd Spile | 5000 50000 5000 50000 WOOOOO 1400000 1400000 1400000 1410000 1390000 955000 1210000 5000 50000 6000 * 50000 719000 719000 719000 719000 868000 840000 92000 747000 * * * O K LM H -C W -FW 11-0-050310 (caetMSBl Spke, som noe.Laespiin) OKLM N -tfW -FW 11-M 5 0 3 1 0 (C0M4S22Spk F,SMKXH9>LLUkSpfW > O K LM N -C W -fW 11-0-050310 Low S plka 5 ppb tCMMSK.SOMnqlLW*ldSplk*) OKLMN43W-FW11-0-050310 High Splka SOppb (COJItKK. SMMng/L Ft*U Spile> 5000 50000 5000 5DOOO 40800 40800 40800 40800 48900 83100 45400 88500 5000 60300 85 50000 80300 * 5000 60300 95 50000 60300 84700 105000 63300 96100 * 89 76 Sample residue exceeds the spiking level significantly; therefore, an accurate ntcovnry value cannot be calculated NO - Not detected at or above 25 nQ/t<ppl). HQ - Hot quanSteblB * Measured concentration between 25 r>g/L {ppt| and tha Limit of Quantitation (U X I) which Is 50 ngiL (ppt>. NdUt; Sine* th l* summary table snows rounded suit, recovery values may vary slightly from the value* In the rent data. Exygen Research Page 34 of 110 OOO0S7 ' Interim Report -A nalysis o f Oakdale Water Samples ' .Exygen Study No,: P0001400 Table III* Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued Sample CSulftW>aPPaS C l Acid PFOA Amount ArmFound Amount Amount Amt Found Amount Splkod In Sample Recovered Rocoveiy Spited InSampt* Recovered Recovery (naffj | M U ' W ) : : .W U (ngd-) (*) OK1MNJ-SW-0-CS0310 (CM i2 Bp* O.WMnert.Lab Spite | DKJLMN5W-0*050310 {Com#* ip * M.WOODn*fl. L ib Spite I OKLMM-SW-0-0563H> Low SpHc S ppb (C0094S2I, SOMn#L FMO Spite ) OKLMM-5W-0-050510 H kflh S p lk* SOppb <C00W, MOWHA- Flew Spite I OKLMN-GW-TRJP2-M)50310 Low 9 p k * I ppb (CMMUt, MO npii. Spite) OKLMN-0W-TTOPi-0-050310 High SpIkeSO ppb (COOewn.SMOJrtiA Spite) 5000 soooo 5000 50000 5000 50000 1190 1190 1180 1190 6270 51600 7220 58000 ND ' 61TO ND 57-400 102 5000 101 50000 121 5000 114 50000 123 5000 115 50000 491 401 491 481 ND NO 5520 $3200 6020 44200 5040 57300 101 105 111 B7 121 115 Average: 110 Stand! Deviation: 32 - - ``Sample residue exceed] the spfcing level sIjniScsntly, therefore, an accurate recovery value cannot be calculated NO * Not detected el or above 23 ngfl- (ppt). NO a No! quartifeM " Measured concentration between 2 fin o /l (ppt) and Uie Uitill of Q uareudon(LO Q )-w hlc>ilt50ngA .(ppt). . N o ti:8<r>celhiiuinrrairvtatilt*lciw rourvkdr*i)i.rcoveryvli>t*m eyvaryillB W 1y from the values in the rew date. '' Average: Standard Deviation: *S 1* Exygen Research Page 35 o f 110 000058 Interim Report #1-Analysis o f Oakdale Water Samples ; Exygen Study No.: P0001400 Table IV, Surrogate Spike Recovery of l3C PFOA in Water Samples Exygen ID S am ple D e s c rip tio n 13c -p p o a Am ount Am ount S piked R ecovered {n g /L l -.....("o n -l R ecovery {*0 C0064404 Spk C C0064404 Spk D C0064404 C0064404 Rep C0064405 CO064406 C0064407 KLMN-GW -W 3-0-D5310 ....... DKLMN-GW -W 3-0-D50310 OKLM N-GW -W 3-0-050310 OKLMN-G W -W 3--050310 O KLM N-G W -W 3-0-050310 Dup OKLM N-GW -W 3-0-050310 LowSpike 5 ppb OKLM N-GW -W 3 -050310 High Spike .50 ppb . 5500 50500 500 500 500 5000 50000 5580 53900 431 . 422 416 4730 . 34500 101 107 86 B4 83 95 69 C0064408 Spk E C0064408 Spk F C0064408 C0064408 Rep CQ064409 C0064410 C0064411 O KLM N-G W -W 8-0-050310 OKLW N-GW -VV 8 -0 -0 5 0 3 1 0 OKLMN-GW -W 8-0-50310 OKLM N-GW -W 8-0-050310 OKLM N-GW -W 8-0-050310 Dup OKLM N-GW -W 8-0-C50310 Low S pike 5 ppb O KLM N-G W -W 8-0-050310 KiQh Spike 50 ppb C0064412 Spk G. C0064412 Spk H COO64412 , C0064412 Rep C0064413 CO064414 C0D64415 QKLM N-GW -W 26-0-050310 OKLMN-GW -W 26-CH)50310 O KLM N -G W -W 28-Q - 5031 O KLM N -G W -W 26-0-050310 O KLM N-G W -W 26-0-050310 Dup 0 KLMN-GW -W 26-0-05Q310 lo w S pike 5 ppb OKLMN-W -W 26-0-50310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5500 50500 500 500 500 5000 50000 5840 55900 466 452 . 483 . 5550 39400 5430 32900 7720 7660 7540 5210 28000 106 111 93 90 97 111 79 99 65 A * 104 56 C0064416 Spk 1 COO64410 S pk J C0064416 C0064416 Rep C0064417 C0064418 C0064419 OKLM N-GW -W 33-0-050310 . 0 KLM N-GW-W 33-Q-05Q310 OKLM N-GW -W 33-0-050310 OKLMN-G W -W 33-0-050310 OKLMN-GW-W33-Q-05Q31Q Dup OKLMN-G W -W 33-0-050310 Low S pike 5 ppb OKLM N-GW -W 33-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 3160 48000 262 256 ' 261 2750 42500 . 57 95 52 51 52 55 85 C064420 Spk K C0064420 Spk L 00064420 : CQQ64420 Rep C0064421 ; C0064422 C00S4423 O KLM N-GW -W 206-0-050310 OKLM N-G W -W 205-0-50310 OKLMN-GW -W 20S-0-06031Q O K LM N -G W -W 205- -0503.10 OKLMN-GW -W 205-C-050310 Dup OKLM N-GW -W 205-0-050310 lo w S pike 5 ppb OKLMN-GW-W205-CW3S0310 High S pike 50 ppb 5500 50500 500 500 500 5000 50000 4940 53000 279 280 .. 307 4240 38000 90 105 56 56 , 61 85 76 C0064424 Spk M C084424Spk N C0064424 C0064424 Rep C0064425 C0064426 C0064427 OKLM N-GW -W 215KJ-050310 OKLM N-GW -W 215-0-050310 OKLMN-G W -W 215-0-050310' OKLMN-G W -W 215-0-050310 OKLMN-GW -W 215K>-050310 Dup OKLM N-GW -W 215-0-0503tO Low Spike 5 ppb OKLMN-GW -yV215-<M)503l0 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5850 106 56700 1010 434 ... 112 20 2 87 464 93 4960 , 99 35600 71 T h e very high PFOA level In the undiluted sample Interfered with UG PFOA recovery. Note: Since thl* summary table show* rounded results* recovery values may vary slightly from the value* In the raw darta. Exygen Research . .Page 36 of 110 000059 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P000I400 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID Sample Description Amount Spiked ing/L) 1sC-PFO A Amount Recovered (ng/L) Recovery .. C0064428 Spk C CO064428 Spk D C0084428 CQ064428 Rep 00054429 C0084430 C0064431 OKLMN-GW-W2010-0-050310 OKLMN-QW-W2010-0-050310 OKLMN-GW-W2010-0-050310 OKLMN-GW-W2010-0-050310 OKLMN-GW-W2010-0-050310 Dup OKLMN-GW-W2010-0-050310 Low Spike 5 ppb OKLMN-GW-W2010-0-050310 High Spike 50 ppb 5500 50500 500 500 ' 500 5000 50000 . 5390 53000 432 417 510 4500 30200 98 105 86 83 102 90 60 C0084432 Spk E C0064432 Spk F C0054432 C0064432 Rep C0064433 C0064434 C0064436 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7,0-050310 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310 OKLMN-GW-PW7-0-050310 Dup OKLMN-GW-PW7--O50310 LpwSpike 5 ppb PKLMN-GW-PW7-0-050310 High SpikeSO ppb 5500 50500 500 500 500 5000 50000 5260 51000 341 335 325 4820 33200 96 101 68 67 65 96 66 00054436 C0064437 00084438 OKLMN-GW-TRIP1--050310 OKLMN-GW-TRIP1-O-050310 Low Spike 5 ppb OKLMN-GW-TR1P1 -0-050310 High Spike 50 ppb 500 5000 50000 510 5100 51300 102 102 103 C0064442 Spk G C0064442 Spk H C0064442 C0064442 Rep C0064443 COO64444 C0064445 OKLMN-GW-PW8-0-050310 OKLMN-GW-PW8-Q-05310 OKLMN-GW-PW8-0-050310 OKLMN-G1V-PW8H}H)50310 , ' OKlMNrGW-PW8-0-0503l0 Dup OKLMN-GW-PW8-0-050310 Low Spike 5 ppb OKLMN-GW-PW8-0-050310 High Spike 50 ppb 5500 50500 500 500 500' 5000. 50000 5270 52900 321 322 300 3910 25800 96 105 64 64 60 78 52 00064446 Spk I C0064446 Spk J r OKLMN.GW-PWS-0-050310 OKLMN-GW-PWB-0-050310 C064446 OKLMN'-QW-RW-O-OOSIO C0064446 Rep . OKLMN-GW-PW9-0-05310 ` COOS4447 . . OKLMN-GW-PW9--050310 Dp C0064448 OKLMN-GW-PW9-0-050310 Low Spik 5 ppb C0064449 OKLMN-GW-PW9-0-G50310 High Spike 50 ppb 6500 50500 500 500 500 5000 50000 5250 53000 315 317 338 4230 24800 95 10? 63 63 68 85 50 C006445Q Spk K 00064450 Spk L C0064450 C0064450 Rep G0064451 C0064452 C0064453 OKLMN-GW-W6102-0-05D31 OKLMN-GW-W61G2-0-050310 OKLMN-GW-W6102-0-650310 OKLMN-GW-W61G2--050310 OKLMN-GW-W6102-0-050310 Dup OKLMN-GW-W6102-0-050310 Low.Spike 5 ppb OKLMN-GW-W6102-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5640 53200 424 439 480 5050 32500 103 105 85 B8 96 101 65 Not: SFnce this summary tabt shows rounded results, recovery values may vary slightly from the values In the raw data. Exygen Research Page 37 of 110 000060 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No,: P0001400 Table IV* Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID Sample Description 13c -pfo a Amount Amount Spiked Recovered (ng/L) .. ( " 8 /L ) Recovery (%> CQ064454 Spk M C064454 Spk N C0064454 C0064454 Rep C064455 C0064466 CO0 6 4 4 5 7 0K LM N -G W -W 6104-0-050310 5500 O K LM N 'G W -W 6104-0-050310 50500 OKLM N-GW -W 6104--50310 500 OKLM N-GW -W 6104--050310 500 OKLMN-G W -W 6104-0-Q50310 Oup 500 OKLAIM-G W -W 6104-0-050310 Low S pike 5 ppb < 5000 O K LM N -G W -W 6104-0-050310 High S pike 50 ppb .50000 , 5510 54500 398 4 1 7 '. 487 4920 33800 100 108 80 83 97 98 68 C0064458 Spk C C0064458 Spk D C0064458 CQ64458 Rep CQ054459 C0084460 C0064461 OKLMN-GW -W 62C1-0-50310 O KLM N-GW -W 6201-0-Q 50310 OKLM N-GW -W 6201-0-05031Q O KLM N -G W -W 6201-0-050310 OKLM N-G W -W 8201-0-050310 Dup OKLMN-GW -W 621-0-5310 Low S pike 0.5 ppb O KLM N-GW -W 6201 ^-0 5 0 3 1 0 High S pike 5 ppb 5500 50600 500 500 500 500 . 5000 5460 50300 388 391 496 491 5440 99 100 78 78 99 96 109 C064467 Spk E C0064467 Spk F C0064487 C0064467 Rep C0064468 C064469 C006447 OKLMN-GW -W 20-0-05309 O KLM N-G W -W 20-0-050309 0 KLM N-G W -W 20-0-050309 ; Q KIM N -G W -W 20-0-050309 O KLM N-G W -W 20-0-050309 D up O KLM N-GW -W 20-0-05309 Low. S pike 5 ppb O KLM N-GW -W 20-0-05309 High S pike 50 ppb 5500 4090 50500 . 46500 500 272 500 270 500 270 5000 3790 50000 26600 74 92 54 54 54 76 53 C0064471 Spk G C0064471 Spk H C0064471 C064471 Rep C0064472 COO64473 C0064474- OKLMN-GW -W 22-0-60309 OKLMN-GW -W 22-0-Q503D9 O KLM N-G W -W 22-0-050309 O KLM N-G W -W 22-0-050309 . OKLM N-GW -W22--05Q3Q9 D up : OKLMN-GW-W22-0-5Q3D9 LOW S pike 5 ppb OKLMN-GW 'W 22-0-05Q3Q9 H l8 h S pike 50 ppb 5500 50500 500 500 500 5000 50000 4380 50700 . 267 280 .. 256 3830 28800 80 100 53 56 51 77 58 C0064475 Spk 1 C0064475 Spk J C 0064475 : C0064475 Rep CQ064476 C0064477 OKLM N-GW -W 3 i -0-050309 O KLM N -G W -W 31-0-05Q309 O KLM N -G W -W 31-0-050309 0 KLMN-GW -W 31 -0-050309 0 KLM N-G W -W 31-0*050309 Dup O KLM N -G W -W 31-0-050309 High S pike 50 ppb C0064478 Spk K C0064478 Spk L C0064478 C0064478 Rep CO06447 CQ6448 C0064481 . OKLM M -GW -W 32-0-050309 OKLMN-GW -W 32-G-050309 O KLM N-G W -W 32-0-050309 . OKLMN-GW -W 32-0-05D309 OKLMNrGW -W 32-0-Q5D309 Dup OKLMN-GW -W 32-O-O50309:Low S pike 5 ppb OKLM N-GW -W 32-0-050309 High Spike 50 ppb 5500 50500 500 5 0 0 .. 500 50000 5500 50500 500 500 500 5000 50000 541Q 54200 391 391 ,371 44100 4840 51000 287 .2 8 9 328 4750 49000 98 107 78 78 74 88 88 101 57 58 66 95 98 Not: Sine th is sum m ary table shows rounded results, recovery values may vary s lig h tly from the value in the. raw data. . Exygen Research Page 38 o f 110 000061 Interim Report #1-Analysis o f Oakdale Water Samples . Exygen Study No.: P0001400 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen ID S am ple D e s c rip tio n Am ount S piked (mm ,aC-PFOA Am ount R ecovered (n o /L ) R ecove ry ....... % )..... - C0064482 Spk M COO644-82 S pk N C0064482 CQ064482 R ep Q0064483 C0064484 C0064485 OKLMN-GW -W 217--0503Q9 OKLM N-GW -W 217-0-050309 O KLM N-G W -W 217-0-050309 O KLM N-G W -W 217-0-050309 OKLM N-GW -W 217-0-050309 D up O KLM N-G W -W 217-0-050309 Low S pike 5 ppb O KLM N-G W -W 217-0-050309 High S pike 50 ppb 5500 50500 500 500 500 5000 50000 5410 52500 428 453 468 4850 44700 98 104 86 91 94 97 89 C0064486Spk 0 OKLM N-GW -W 2008-0-050309. CDQ64486 S pk P OKLM N-GW -W 2Q08-0-050309 C0064486 O KLM N -G W -W 2008-0-050309 C004486 Rep QKLM N-GW -W 200B-0-050309 C0064487 O KLM N-G W -W 2008-0-050309 Dup 00064488 KLM N -G W -W 2008-0-050309 Low S pike 5 ppb C 0064489 ^ OKLMN-GW-W20Q8*Q*05Q309 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5140 52100 318 326 357 6040 37800 93 103 64 65 71 121 76 00084490 Spk C 00064490 Spk D C064490 C0064490 Rep C064491 CD064492 -C 0064493 O KLM N -G W -W 2012-0-050309 O KLM N-G W -W 2012-0-050309 OKLMN-GW -W 2012--05039 OKLM N-GW -W 2012-0-050309 OKLMN-GW -W 2012-0-050309 D upi; O KLM N-G W -W 2012-0-050309 Low S pike 5 ppb O K IM N -G W -W 2012*0*050309 High S pike 50 ppb 5500 50500 500 500 500 5000 50000 5050 50700 ' 344 342 351 5010 37900 92 100 69 68 70 100 76 C0064494 Spk : OKLMN-G W -W 8-0-050309 , C0064494 Spk F OKLM N -0 W -W 80-0-050309 C0064494 OKLM N-GW -W 80-0-050309 C0064494 Rep O KLM N-G W -W 80-0-050309 C00S4495 ` OKLM N-GW -W 80-0-050309 Dup C0064496 O K IM N -G W -W 80^0-050309 Low S pike 5 ppb C0064497 OKLM N-GW -W 80-0-0503Q9 High S pike 50 ppb 5500 50500 500 500 500 5000 50000 5650 . 52400 486 438 502 5410 41700 103 104 97 88 100 108 83 C064498 Spk G OKLMN-GW -PW 1-Q-050310 00064498 Spk H OKLMN-G W -PW 1-0-050310 C064498 OKLMN-GW -PW 1-0-05Q310 C0QS4498 Rep C0064499 OKLMN-G W -FW 1-0-050310 1 O KLM N -G W -W 1-43-050310 D u p : C0064500 ' O KLM N -G W -FW 1-&-50310 Low S pike 5 ppb C0064501 OKLM N-GW -PW 1-0-050310 High S pike 50 ppb 5500 50500 500 500 500 5000 50000 C0064502 Spk I CO064502 S pk'J C0064502 C064502 Rep C0064503 C0064504 . C0064505. : O KLM N -G W --PW 2-O D 5C 310 OKLM N-0W -PW 2-CH)50310 OKLMN-GW -PW 2-O-05C310 ; O KLM N-G W -PW 2-0-050310 . OKLM N-GW -PW 2-0-05031Q Dup KLMN-GW -PW 2-0-05031Q Low S pike 5 ppb O KLM N-G W -PW 2-0-050310 H igh S pike 50 ppb 5500 50500 500 500 500 5000 50000 5150 53000 -331 350 352 4420 41600 5420 52600 - 440 : 440 431 4680 34000 94 105 66 70 70 88 83 99 104 88 88 86 94 68 Note: Slnca ttila summarytable shows roundsd rasults, recovery value* may vary sltflhtly from the value* In the> raw data. Exygen Research Page 39 o f HO 000062 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study Np.: FOOD1400 Table IV. Surrogate Spike Recovery of 13C PFOA in Water Samples Continued Exygen . ID S am ple D e s c rip tio n Am ount S piked -- O 0 41 1>C *PFO A Am ount R ecovered R ecovery m 0008*506 Spk K C0064506 Spk L C0064508 C0064506 Rep C0064507 C0064508 C0064509 OKLMKM3W -PW 3-0-Q50310 OKLM N -6W -PW 3-0- 50310 OKLM N -G W -PW 3-0-050310 OKLM N-GW -PW 3-0-050310 OKLM N-GW -PW 3-0-05031 Dup O KLM N -G W -PW 3-0-050310 Low Spike 5 ppb O KLM N -G W -PW 3-0-050310 High S pike 50 ppb 5500 50500 500 500 500 5000 50000 4640 53100 284 275 294 4080 38300 84 105 57 . 55 59 82 77 00064510 Spk M C0064510 Spk N C0064510 C 00645010 Rep C0064511 C0064512 C0064513 OKLM N-GW -PW 4-0-050310 0 KLM N -G W -PW 4-0-050310 GKLMN-GW-PW 4-0-OSO310 O K lM N -G W -P W 4-0-050310 OKLMN-GW -PW 4-0-O50310 Dup O KLM N-G W -FW 4-0-05Q 310 Low Spike 5 ppb Q KLM N -G W -PW 4-0-050310 H igh S pike 50 ppb 5500 50500 500 500 500 5000 50000 5100 52400 320 324 313 4870 38000 94 104 64 65 63 97 76 C0064514 S pkO C0064514 Spk P C0064S14 C0064514 Rep C0064515 C0064516 C0064517 OKIMN-GW -PW 6--05Q310 O KLM N-G W -PW 6-0-050310 OKLM N-GW -PW 64J-050310 OKLM N-GW -PW 6-0-050310 O KLM N-G W -PW 6-0-050310 Dup O KLM N -G W -PW 6-0-050310 Low Spike 5 ppb O K LM N -6W -P W 6-0-050310 H igh Spike 50 ppb 5500 50500 500 500 500 5000 50000 5050 52300 304 311 313 4740 35100 92 104 61 62 63 95 70 C0064618 Spk C 00084516 Spk D C0064516 C0064518 Rep C0064519 C0064520 C004521 OKLM N-G W -PW 10-0-050310 OKLM N-GW -PW 10-0-050310 OKLMN-GW -PW 1-0-050310 OKLMN-GW -PW 10-0-05310 OKLM N-GW -PW 10-0-050310 Dup Q KLM N-G W -PW 10-0-050310 Low Spike 5 ppb OKLM N -G W -PW 10-0-050310 High Spike 50 ppb 5000 50500 500 500 500 5000 50000 3670 48500 255 249 258 2980 34100 67 96 51 50 52 60 68 C0064522 Spk E C0Q64522 Spk F C0064522 C0064522 Rep C0064523 C0064524 C0064525 O KLM N-GW -PW 11-0-050310 O KLM N-GW -PW 11-0-050310 O KLM N-GW -PW 11-0-050310 OKLM N-GW -PW 11-0-050310 OKLMN-GW -PW 11-0-050310 Dup O KLM N -G W -PW 11-0-050310 Low Spike 5 ppb O KLM N -G W -PW 11-0-050310 High Spike 50 ppb 5500 50500 500 500 500 5000 50000 5180 51600 319 347 312 4400 36000 94 102 64 69 62 88 72 C0064526 Spk G C064526 Spk H C064526 C0064526 Rep C0064527 C0064528 C0064529 OKLMN-S W -O-050310 OKLM N-SW -0-050310 OKLMN-SW -O-050310 OKLM N-SW -0-050310 O KLM N-SW -0-050310 Dup O KLM N-SW -0-050310 Low Spike 5 ppb OKLMN-SW -Q-050310 High Spike 50 ppb 5500 50500 500 500 500 50DD 50000 5270 52000 124 132 505 5320 41200 96 103 25 26 101 106 82 Mote: Since th is sum m ary table shows rounded results, recovery values may vary s lig h tly from the values In the raw data. Exygen Research "'e : ' Page 40 of 110 000063 '' Interim Report #!-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Table IV. .........Exygen ID Surrogate Spike Recovery of 13C PFOA in Water Samples Continued ^P FO A Sample Description Amount Amount mSpiked Recovered Recovery (ng/L) . .. ino/L) COO64530 C0064531 C0064532 OKLMN-GW-TRIP2-0-05310 500 OKLMN-GW-TR1P2-0-050310 Low Spike 5 ppb 5000 OKLMN-GW-TRIP2-0-050310 High Spike 50 ppb 50000 494 5520 52900 99 110 106 Average; 83 Standard Deviatimi: 21 Not: Since this summary table shows rounded results, recovery values may vary slightly from the values In the raw data. Exygen Research C tO t|i Page 41 of 110 000064 Interim Report # 1-Analysis o f Oakdale Water Samples . . Exygen Study N o.: P0001400 Exygen Research Page 42 of 110 000065 'Intenm'Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 1, Typical Calibration Curve for PFOA in Reagent Water CtfMiXC Gw k I (PFOflJ: U r m r R *jr**iionO l^5*0C3 * +J.5CC4 (f > fiJWiJ) Alea, counts Exygen Research pU Page 43 o f 110 000066 interim'Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: POOO1400 Figure 2. Extracted Standards of PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively XCS32103-1 PFOA * m u - tH n p tr 2 o f 41 from O3240SC,>*r A r9K44n7eott<m Hitght: 6039&36 cp* KT:11A4amin ' 11,64 XEB32J-2 rrOACStandirt) 413iWW .0 fiiu - t m f i* 3 4l om #3M05C.iff A w : 78# eeuit> HWit: 127BS.770 cp* RT: 11M 2 min Exygen Research Page 44 of 110 000067 Interim Report #1-Analysis of Oakdale Water Samples Exygeti Study No.: P0001400 Figured* PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively KwggnrlCimirot - PFOA (U n m o w t1 l+ i3 0 fX $ amv a tm plt-9 a t *1 tK>m032# X Z m M A nn ; 5766 covata HakfAl: 664.122 o p t K7: (1.816 mlrr Reagtf* Spie A - PFOA (OD}413J)OG9.9 U rti - 10of 41 tram OMIfliC.nHi A w ; 90130 {W W 19073.491 afa RT. 1141* irtn 1iX)4. I SDCOjOO ODD ..t ............. I " .''T*......................... I...... " ! ' ' * * ', ' r ' f -.T -J k ... 9 4 0 7 8 B 10 t1 12 13 14 15 16 17 Tim *, mill Hmqm* tp k S /V O A C D C )4 l$ M O iJ Wnu- J*nple 11 a i 4 1ran HXiW C.mH A l* 700803H its m8l*1 113023.no op* RT: 11.93* rMtt <* 1.00*5 45 0 7 S . 0 ; 1D . 11 . ' 12 13 14 18 17 T in t.m il> Note: A linear lot o f PFOA was used to calibrate the instrument, The two peaks shown in Figure 4 are due to different isomers present in environmental samples. The area counts for all isomers present are included to report one total PFOA value. Exygen Research Page 45 o f 110 000068 interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 4. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF-100 (Exygen ED: C0064522, Data Set: 032405CR) ................... C69&4B27 -f>FQ* flithaaw n} t ik . M fn p it 3 8 o f ST from 0 32 *}iC R w ilf A r* * : 878784 oai#rt> 7 \S 0 t6 4 9 c p * RT; 1130min 11.S2 Intensity, cps Exygen Research Page 46 of 110 000069 Interim Report #1-Analysis o f Oakdale Water Samples .Exygen Study No.: P000I4O0 Figure s. Typical Calibration Curve for 13C PFOA in Reagent Water B325C OWJMWIfcwRwit.rMJ C ia tP F O ^ c T J n iM rR ^ iik in C 1 - U l. t O I tt + OJM041 01-* Arsa, courts Exygen Research Page 47 of 110 0000*7 Interim Report #1 -Analysis of Oakdale Water Samples - Exygen Study No*: P0001400 Figure 6. Extracted Standards of 13C PFOA in Reagent Water, 25 ng/L and 50 ng/L, Respectively 1 X003)05-1 - 13CPFOA(S1*Kl*rd)415.0l310.0vw **mp)92e/*1 fmitt03346BC.WW At: 3311X1 i-tuilrft H tivh i 5399,1)3 npw RT: 11J366 mh . Exygen Research Page 48 of 110 000071 Interim Report .#!-Analysis o f Oakdale Water Samples Exygen Study Np.: P00G14O Figure 7, 13C PFO Ain Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively f t * # g e M C r ir a f <3C PFOA (Untvravml +ia.fliJ!'0 n i / - w rm p te 9 o f 4 f ftw r r OH-tOGCMnlr A /M : 3 /f otmntf */() 36,86400 fl7 : I f A 34/nli/ 0X I R * * } * S |* 6 - I3C FFQA(QC)41SAWI0nu- tam fk 1>oM 1 fiwn 0324 C juM1 A w 1M8BW o a m 2038*1,01 qw K T ;ll.M 3ih 2.0*5 - I f i*aS S b a io T im * . rie iam 11 Exygen Research Page 49 of 110 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No!: P0001400 Figure 8. Chromatogram Representing an Oakdale Water Sample Analyzed for l3C PFOA (Exygen ID: C0064522, Data Set: 032405C) intensity, cps Exygen Research Page 50 o f 110 000073 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 9, Typical Calibration Curve for PFBS in Reagent Water Area, counts Exygen Research Page 51 o f 110 000074 intensify, cps Interim Report #1-Analysis o f Oakdale Water Samples ' Exygen Study No;: POOO1400 Figure 10, Extracted Standards of PFBS in Reagent Water, 25 ng/L and 50 ng/L, Respectively XOM0400-1 PFaS(Sta*{fant)299JHi9.Q9rm-**tpl92t>fBT*ttrQ314KCitM#r ootifris Height t0634 opt BT: &SOT mht . ' xo H C W i-? r r a csmmsm) zbo-d ab.# k i m p h 3*< 07 n o n M M o s c ft.w A w ; 7727 ccunCr tW * * : H T i4 a j R T:3M 4lrtn 3&S Tlm t, min Intensity, cps ` Exygen Research Page 52 o f 110 Q0075 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: POOO1400 Figure 11. PFBS in Reagent Water, SO ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively fittg vn f Cxmfoirooml iP)PBS o.ao 199&8&-0 rmu tampb 9 o ft7 front OSHOSCR.m# 3.65 nwgtM tpt< 6 m s [OQiBiJMfrii StftJ- 11 t f 17 (nm C524C6CR.tf M i; 1*2 W l* 1WM: 12M.W apt RT:3JHTirvri Exygen Research Page 53 o f 110 000076 Interim Report #1-Analysis o f Oakdale Water Samples ' Exygeri Study -No.: P0001400 Figure 12, Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR) O X * -P F B S flJn km > M ii2$ 90 a 9.0 *im > S M iip )ta6 of6 itiM t0 3i40 aC R .m ir A /,.-*r78oow f Haight 15.404 tip J?T>-5,924 min 3 J2 intensity, cps Exygen Research Page 54 of 110 000077 : Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.; P0001400 Figure 13. Typical Calibration Curve for PFHS in Reagent Water 0334WC GiwxxfWpltr ( T f H4J l i t * * * fagnmwnC1 * <WJ x + SOll j GJWiS) AfB, counts Exygen Research Page 55 o f 110. 00007S Interim Report #1 -Analysis o f Oakdale Water Samples . Exygcn Study Np.: P0001400 Figure 14. Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/JL, Respectively XC03210S-1 PFHS (S tK U f*n t)S 9 9 .0 ia 0 .0 a m t aampta 1 o f # t 1mm 032-IOSC.mlf Ana: 1296t coasla Malaht m o ja f o p j ST: 10.626 mm 10.63 I XCCOJIBi-a - PFHS C S tm dart) 3W D .O fnu parmph 3 o# 41 ftw T M M M C M ltt A m ; 2S03 M M * H < I9 :3 3 1 4 D 8 2 0! RT; ID J8I7m in 10.62 Exygen Research Page 56 o f HO 000079- Interim Report #1 -Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Figure 15. PFHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively Coffimi 7*ms |>>*Wi not fanad} * m t m m p i* 9 of-ff from o s i-io s c .w fir * 4TM01 Q. 10.B4 1 1 .7 B 13-^0 It 20- C m ' 0- i / i f f II 1 4 12 . * l| 12.70 326 73e7jM,844,880 001 I .1420 #ll.M f... ...*-- lu,--- lli, titi 3 4 S 8 7 B 0 10 11 12 13 14 15 15 17 I Ruw* Spk A- l*fWt $0)394.0/69.8 mtu ampli 10*141 frem093109Cfrf 7 ru :7 it* a c o u n t! Hl9ht;W22.Ui of RT: IS.Sfrlrrin T im *, m i 1050 I RM0MW 3 fk 9 - P 7H 5 (QCJ MC.OOB mu - j p n p l t I I <4 4 | fro m W 2W C . * *.39W oounto Half*: 29774.188 of* R7:105Mmin Tim, min 13 14 . 15 15 17 Exygen Research Page 57 of 110 ooooso Interim Report #1-Analysis of Oakdale Water Samples Exygen Study No,: P0001400 Figure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=JOO (Exygen ED: C0064522, Data Set; 032405CR) CP064377 PFHS (Uakimm)3S9j0td$jD Mmt - *j,m*tt* 38 <*67 PmmOiUOSCR.wm Am a:S 7368eaunU Hvigkl: 2 9 3 3 c p s XT: i035<rtk> Exygen Research Page 58 of 110 Jaterim Report #1-Analysis o f Oakdale Water Samples Exygen. Study No.: P0001400 f i g u r e 17. Typical Calibration Curve for PFOS in Reagent Water /, ,* CttMOJC (^udV *M rF (lW ^(F F 03)T jw f'R nran ' M l `.71wC3 fr 0 * 9 ' Exygen Research * Page 59 o f 110 0O 0O 8Z Interim Report #!'Analysis o f Oakdale Water Samples Exygen Study No: P0001400 Figure 18. Extracted Standards o f PFOS in Reagent Water, 25 ng/L and 50 ng/L, Respectively XCS3210S-I -P FO S (S t* tn t rd }-m M b O J ) i m u u m p l t o T - i i I h m 032-KSC.wiiT H eight iG BO .ilO ape XT; 13S3Bmm ; 12J04 I XCC32106-2 FF01 (SUndinl) 9 .0 *4 JU m j- sam pttO if 4! Twn p t 4 C j fi F ru : m OMrtu H*sM : 2S20.7 cp RT' 12,939 rl# i 2500' 2000 05 aL# 1800 f CD 1000 g 600' 0 12.34 1 4 5 B 7 0 C 10 11 12 19 14 15 1B 17 Tim, r Exygen Research kn\ i \ mh Page 60 of 110 00QO83 Interim Report #1-Analysis o f Oakdale Water Samples . . Exygen Study No.: P0001400 Figure 19. PFOS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively tffstwjHNrf Ctofrlro} (iflML-fO#-owwrt 9 o f4 1 lfc s n Q$340$C 4ft Intensity, cps Intensity, cps mteiwlty, cps Exygen Research i Page 61 of i 10 000084 Interim Report #1-Analysis o f Oakdale Water Samples Exygen Study No;: P0001400 Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF-100 (Exygen ID: C0064522, Data Set: 032405CR) 0)064622 PFOS{Unkta*Hj -m m 0,9*mu-smpl* 3fl </7Pern 032KG#.ttr A n . tst)7& io w ifc Htratrt. 6 0 3 3 2 apt ST: 1 2 min KW0 0500 - 12.14 1W ww>4000' ea. a- Tim, fnln Exygen Research Page 62 o f 110 0Q08S intrim Report #1-Analysis o f Oakdale Water Samples Exygen Study No.: P0001400 Study Protocol P0001400 ..... (Exygen Study No. P000X400) with Analytical Method: V0001780:"Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS" Exygen Research Page 63 of 110 000086