Document zd9mrpMG43zyv8M4z9aGLnYaz

received OPPT HCIC ^ HAY200 i 2 4i1 9: j q ^ Study Title T e n n e s s e e R iv e r V a ll e y S a m p le s 26" 1733 Author Mark E. Ellefson Revised Report September 12, 2003 Performing Laboratory 3M Environmental Laboratory Building 2-3E-09 935 BushAvenue St. Paul, MN 55106 Project Identification 3M Environmental Laboratory Study # E02-0443 Total Number of Pages 276 tm Report E02-0443 Tenn. River Valley Samples Table of Contents List of Tables.............................................................................................................................................3 Study Information..................................................................................................................................... 4 Summary................................................................................................................................................... 5 Purpose..................................................................................................................................................... 6 Test and Analytical Reference Substances............................................................................................ 6 Test Systems.............................................................................................................................................7 Method Summaries.................................................................................................................................. 8 Preparatory Methods................................................................................................................................ 8 Sample Analysis....................................................................................................................................... 11 Analytical Method..................................................................................................................................... 12 Analytical Results..................................................................................................................................... 13 Data Summary..........................................................................................................................................20 Statistical Methods................................................................................................................................... 2 5 Statement of Conclusion..........................................................................................................................26 References................................................................................................................................................ 2 6 List of Attachments................................................................................................................................... 26 Signature Page..........................................................................................................................................2 7 Attachment A: Analytical Method and SOP Deviations......................................................................... 2 8 Attachment B: Data Summary Tables.....................................................................................................4 0 Attachment C: Sample Chromatograms................................................................................................ 6 7 Attachment D: Sample Prep Sheets, Test Substance, and Test System Information....................... 230 Attachment E: Notes to File..................................................................................................................... 270 3M Environmental Laboratory Page 2 of 276 Report E02-0443 Tenn. River Valley Samples List of Tables Table 1. Sample Location, Sample Type, and Analytical Data Summary.......................................... 5 Table 2: Characterization of the Test and Analytical Reference Substances.................................... 6 Table 3a. Description of Fish Tissue Analyzed in this Study...............................................................7 Table 3b. Description of River Water Analyzed in this Study.............................................................. 7 Table 3c. Description of River Sediments Analyzed in this Study...................................................... 7 Table 4a. Fish Tissue Sample Preparation Method.............................................................................8 Table 4b. Preparation of Extracted Calibration Curves for the Fish Tissue....................................... 9 Table 4c. Fish Tissue Analytical Data Quality Objectives................................................................... 9 Table 4d. River Water Sample Preparation Method........................................................................... 9 Table 4e. River Water Sample Data Quality Objectives..................................................................... 10 Table 4f. River Sediment Sample Preparation Method........................................................................ 1 0 Table 4g. River Sediment Sample Data Quality Objectives.................................................................11 Table 5. Sample Analysis Information....................................................................................................11 Table 6a. PFOS Calibration Standard Reprocessing Summary.........................................................14 Table 6b. FOSA Calibration Standard Reprocessing Summary.........................................................1 5 Table 6c. PFOA Calibration Standard Reprocessing Summary........................................................ 16 Table 6d. PFHS Calibration Standard Reprocessing Summary........................................................ 17 Table 6e. PFBS Calibration Standard Reprocessing Summary..........................................................18 Table 7a. Catfish Analytical Data.......................................................................................................... 21 Table 7b. Large mouth and Small mouth Bass Analytical Data..........................................................22 Table 7c. River Water Analytical Data.................................................................................................. 23 Table 7d. River Sediment Analytical Data.............................................................................................24 Table 8. Sample Location, Sample Type, and Analytical Data Summary........................................... 2 5 3M Environmental Laboratory Page 3 of 276 Report E02-0443 Tenn. River Valley Samples Study Information Requestor Dale L. Bacon 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-4736 Study Director Mark E. Ellefson 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-5405 Study Location Testing Facility 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 William K. Reagen, Laboratory Manager Mark L. Anderson, Analytical Chemist Cindy M. Carlson, Analylical Chemist Ognjenka Krupljanin, Analytical Chemist Experimental Dates Sample Analysis Initiation: 26 June 2002 Sample Analysis Completion: 12 November 2002 Location of Archives All original raw data and the report have been archived at the 3M Environmental Laboratory according to 3M Standard Operating Procedures. Remaining specimens pertaining to the analytical phase of this study will be archived at the 3M Environmental Laboratory for as long as the quality of the preparation affords evaluation. 3M Environmental Laboratory Page 4 of 276 Report E02-Q443 Tenn. River Valley Samples S ummary Fish, river water, and river sediment samples were collected from three locations in the Tennessee River near the 3M Decatur, Alabama facility. The samples were analyzed for perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHS), perfluorooctanoate (PFOA).perfluorooctane sulfonylamide (FOSA), and perfluorooctane sulfonate (PFOS). The analyses were accomplished by extracting the samples using Solid Phase Extraction (SPE) and then analyzing them using HPLC-Electrospray/Mass Spectrometry (HPLC/ES/MS). Sampling Location 1 (SL-1 ) was located downstream of the 3M facility near Fox Creek at river mile 296. Sampling Location 2 (SL-2) was across the river from the 3M facility at river mile 301. Sampling location 3 (SL-3) was upstream from the 3M facility at river mile 307,5. Analytical results are presented in Table 1: Table 1. Sample Location, Sample Type, and Analytical Data Summary. Fish Tissue Sampling Location & Species Sampled PFBS (ng/g) PFHS ig/g) PF (ng/g) FOSA (ng/g) PFOS (ng/g) SL-1, C (n=6) SL-2, C (n=7) SL-3. C (n=6) SL-1, LM (n=6) SL-2, LM (n=4) SL-3, LM (n=7) SL-3, SM (n=1) <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ River Water <LLOQ <LLOQ <LLOQ <LLOQ1 <LLOQ <LLOQ <LLOQ 60.9 (6/6)2 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 113 (6/6)2 <LLOQ 15.2 (4/6)2 553 (6/6)2 169 (2/4)2 <LLOQ <LLOQ SL-1, RW SL-2, RW SL-3, RW PFBS (py/m L) 84 <LLOQ <LLOQ PFHS (pg/m L) PFOA (py/m L) 196 550 <LLOQ <LLOQ <LLOQ <LLOQ River Sediments FOSA Ip g /in L ) 25 <LLOQ <LLOQ PFOS (pg/m L) 491 <LLOQ <LLOQ PFBS (pg/g) PFHS (pg/g) PFOA (pg/g) FOSA (pg/g) PFOS (pg/g) SL-1, RS 577 130 732 1440 3130 SL-2, RS 437 <LLOQ <LLOQ 141 457 SL-3, RS 452 <LLOQ 127 68 416 C = CatFish, LM Large mouth bass, SM = Small mouth bass, RW = River w ater, and RS * River Sediments. 1High triplicate value was statistically elim inated using Dixon's Q-Test. 2(Num ber o f Fish > LLOQ / Number o f Fish Analyzed). Only one River W ater and one River Sedim ent sample were collected from each sam pling location. 3M Environmental Laboratory Page 5 of 276 Report E02-0443 Tenn. River Valley Samples Purpose The purpose of this study is to perform quantitative screening for PFBS, PFHS, PFOA, FOSA, and PFOS in sport-caught fish, river water, and river sediments from three sampling locations of the Tennessee River near Decatur, Alabama. Test and Analytical Reference Substances Table 2: Characterization of the Test and Analytical Reference Substances. Testano Analytical Reference Substance PFHS FOSA PFOA Compound Source Storage Conditions 3M Laboratory Identification Number Physical Description Purity PFHS, Perfluorohexanesulfonate 3M Specialty Materials, Bldg. 236-2B-11 Frozen FOSA, Perfluorooctanesulfonamide 3M Specialty Materials, Bldg. 236-1B-10 Frozen PFOA, Perfluorooctanoate Ammonium 3M Specialty Materials, Bldg. 236-1 B-10 Frozen TCR-083 TCR-029 TCR-123 White Powder 98.6% Light yellow waxy solid Undetermined White Powder 95.0% Testano Analytical Reference Substance PFBS PFOS Compound Source Storage Conditions 3M Laboratory Identification Number Physical Description Purity PFBS, Potassium Perfluorobutane Sulfonate Wildlife International Frozen TCR-359 White crystals 97.3% PFOS, Potassium Perfluorooctanesulfonate 3M Specialty Materials, Bldg. 236-1 B-10 Frozen TCR-129 White Powder Undetermined 3M Environmental Laboratory Page 6 of 276 Report E02-0443 Tenn. River Valley Samples T est Systems Table 3a. Description of Fish Tissue Analyzed in this Study Source Types Storage Conditions Location 1 Location 2 Location 3 F is h Tissue Tennessee River Catfish Large Mouth Bass Small Mouth Bass Frozen Downstream from the 3M facility near Fox Creek (river mile 296) Across the river from the 3M facility (river mile 301) Upstream of the 3M facility (river mile 307.5) * The fish were filleted and representative aliquots of the fillets were analyzed. Table 3b. Description of River Water Analyzed in this Study River Water Source Storage Conditions Location 1 Location 2 Location 3 Tennessee River Chilled (approximately 4 C.) Downstream from the 3M facility near Fox Creek (river mile 296) Across the river from the 3M facility (river mile 301) Upstream of the 3M facility (river mile 307.5) Table 3c. Description of River Sediments Analyzed in this Study Source Storage Conditions Location 1 Location 2 Location3 R iv e r S EDI M ENTS Tennessee River Chilled (approximately 4 C.) Downstream from the 3M facility near Fox Creek (river mile 296) Across the river from the 3M facility (river mile 301) Upstream of the 3M facility (river mile 307.5) 3M Environmental Laboratory Page 7 of 276 Report E02-0443 Tenn. River Valley Samples M ethod Summaries The concentrations of PFBS, PFHS, PFOA, FOSA, and PFOS in Fish Tissue, River Water, and River Sediments were determined by using Solid Phase Extraction (SPE) and High Performance Liquid Chromatography-Electrospray/Mass Spectrometry (HPLC/ES/MS). Preparatory Methods The following tables describe the sample preparation methods for the Fish Tissue, River Water, and River Sediment samples. Data Quality Objectives (DQO) are also given for each sample preparation method. Fish Tissue Sample Preparation Method Table 4a. Fish Tissue Sample Preparation Method Step Fish Tissue Sample Preparation Method 1 Approximately 2 g of FishTissue and 8 mLofASTM Type 1 Water were homogenized. 2 The homogenate was centrifuged to eliminate thefoam and then shaken/vortexed to re suspend the homogenate. 3 Each homogenate was aiiquoted intotriplicate samples. This was accomplished by transferring 1.0 mLof homogenate to 3 separate 15 mL centrifuge tubes. Matrixspikes (MS) were prepared forevery other homogenate. In this case, an additional 4 (4th) 1.0 mLof homogenate was transferred to another 15 mL centrifuge tube. The MS's were spiked with 100 uL of a 100 ug/mL spike solution containing each ofthe test substances. 5 5.0 mL of acetonitrile was then added to the centrifuge tubes. The tubes were capped and shaken for20 min at 300 rpm. 6 After mixing, the sampleswere centrifuged at 3000 reffor 10 minutes to clarifythe supernatant. 7 The supernatantwas decanted into new 50 mL centrifugetubes and diluted with 40 mL of water. Waters C-18 Tri-funcflonal, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned inthe following manner. Approximately 10 mLof methanol was added to the columns and the vacuum was applied. 8 Once mostofthe methanol had been pulledthrough, ASTM Type 1Water was added (5-10 mL). When mostofthiswas pulledthrough, more waterwas added (5-1OmL). When there was only a small amount ofwater left inthe reservoir, the stopcockwas turned to stop the vacuum to the column. The columnswere not allowed to go dry. 9 The supematesfromstep 7 were passed through the pre-conditioned SPE columns. The aqueous eluentwas not collected. The columns were allowed to dryfor at least 3 minutes. 10 The analytes were eluted from the SPE columnswith2.0 mL of methanol into autovials. See the preparationworksheets for other exact amounts, times, speeds, etc. 3M Environmental Laboratory Page 8 of 276 Report E02-0443 Tenn. River Valley Samples Table 4b. Preparation of Extracted Calibration Curves for the Fish Tissue. Step Preparation of Extracted C a l i b r a t i o n Curves f o r the F i s h Tissue There were two extracted Fish Tissue calibration curves: Large Mouth Bass and CatFish. Rangefinding experiments were doneto determinewhich Fish Tissues had the lowest endogenous levels of the analytes. Then, one Large Mouth Bass and one CatFish sample containingthe least amount of endogenous test substances were selected as the matrixto construct the calibration curves. The Small Mouth Bass was analyzed using the Large Mouth Bass calibration curve. The procedure for preparingthe extracted calibration curves is the same as the Fish Tissue sample preparation, except the volumes were scaled-upto provide a homogeneous batch of fish tissue matrix. The differences are as follows: 1 Approximately 10 g of Fish Tissue and 40 mL ofASTM Type 1Water were combined and homogenized. 2 1.0 mL of homogenate was transferredto the appropriate numberoftubes. 3 Each tube was spikedwith the predetermined amountof spike solution. Table 4c. Fish Tissue Analytical Data Quality Objectives. Step Fish T issue: A n a l y t i c a l Data Qual ity O b j e c t i v e s 1 All samples were prepared intriplicate. The %RSD should be s 25% Matrixspikes were performedon half ofthe fish of each type from each sampling location. 2 Recovery should bewithin 30% from expected values. A total of 18 matrix spikes were prepared forthe Fish Tissue samples. Water blanks, consisting of an aliquotofwater runthroughthe entire sample preparation and 3 extraction process were prepared with samples fromeach sampling location. Water blanks containing < % LLOQ of each analyte for the data set in which they were run were considered acceptable. Extraction blanks, consisting ofan aliquotof methanol runthough a pre-conditioned SPE 4 cartridge, were prepared for each sampling location. Extraction blanks containing < % LLOQ of each analyteforthe data set inwhich they were runwere considered acceptable. 5 I Mid-level calibration curve pointswere used as CCVs. River W ater Sample Preparation Method Table 4d. River Water Sample Preparation Method Step River Water Sample Preparation Method 1 Waters C-18 Tri-functional, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned Inthe following manner. Approximately 10 mL of methanol was added to the columns and the vacuumwas applied. Once mostof the methanol had been pulled through, ASTM Type 1 Water was added (5-10 mL). When mostofthiswas pulled through, more waterwas added (5-1OmL). When there was only a small amount ofwater left inthe reservoir, the stopcockwas turned to stopthe vacuumto the column. The columnswere notallowed to go dry. 2 40 mL ofthe RiverWater was passed through a pre-conditioned SPE column. The columns were allowed to dryfor at least 3 minutes. 3M Environmental Laboratory Page 9 of 276 Report E02-0443 Tenn. River Valley Samples Table 4d. River Water S a rn ie Preparation Method Step River Water Sample Preparation Method | The analytes were eluted from the columnswith 2.0 mL of methanol into autovials. Table 4e. River Water Sample Data Quality Objectives Step 1 2 3 R ver Water Sample Data Quality Objectives Water blanks, consisting ofan aliquotofwater run through the entire preparation and extraction process, were prepared with samples each day sampleswere extracted. Water blanks containing < J4LLOQ of each analyte forthe data set inwhich theywere run were considered acceptable. A non-extracted solventcalibration curve was used to quantitate the River Water samples. No extracted CCVs were prepared, a mid-level calibration curve pointwas used for this purpose. No matrix spikes were preformed during the sample preparation ofthe River Water samples. River Sediment Sample Preparation Method Table 4f. River Sediment Sample Preparation Method Step 1 2 3 4 5 6 7 8 9 10 11 12 River Sediment Sample Preparation Me ihod There were 3 River Sediment samples, one from each sampHng location. Triplicate samples plus a matrixspikewere prepared for each location. Initially, sedimentwas transferredto 50 mL centrifuge tubes and centrifuged at 6000 RCF for 20 min. The liquidwas decanted off and the remaining sedimentwas used forthe sample preparation Approximately20g ofsediment and 35mLof 1% Acetic Acid (aqueous) were combined into 50mL centrifuge tubes. Matrixspikeswere prepared by adding 100 uLof 100 ug/mL spike solution tothe predetermined MS tubes. The tubeswere capped, vortexed, and teen shakenfor60 min at 300 RPM. They were then centrifuged at 6000 RCF for 20 minutes. Waters 0 18 Tri-functional, Sep-Pak 1g, 6cc SPE columnswith attached 70 mL reservoirs were placed ontovacuum manifolds and pre-conditioned inthe following manner. Approximately 10 mLof methanol was added to the columns and the vacuum was applied. Once most ofthe methanol had been pulled through, ASTM Type 1 Waterwas added (5-10 mL). When mostofthiswas pulled through, more waterwas added (5-1OmL). When there was only a small amountofwater left inthe reservoir, the stopcockwas turned to stopthe vacuum to the column. The columnswere not altowed to go dry. The aqueous solutionsfrom step #5 were decanted from the samples and passed through pre-conditioned SPE cartridges. The aqueous eluates were discarded. 20 mLof methanol was then added tothe sediment samples. The samples were vortexed, shaken for 30 min at 300 RPM, and then centrifuged at 6000 RCF for20 minutes. The methanol was decanted, passed through the SPE cartridge and collected. An additional 4 mLof methanol was usedto washthe reservoir and the column. The collected methanol was then added to approximately 200mL ofASTM Type 1 Water. This solutionwas then passed through a new pre-conditioned SPE cartridge. The aqueous eluatewas discarded. The analytes were eluted fromthe SPE cartridges with 2.0 mLof methanol into autovials. 3M Environmental Laboratory Page 10 of 276 Report E02-0443 Tenn. River Valley Samples Table 4g. River Sediment Sample Data Quality Objectives S f'EP River Sediment Sample Data Quality Objectives 1 All sampleswere prepared intriplicate. The %RSD should be s 25% 2 Matrixspikes were performed on each sample. Recovery should be within30% of expected values. Two lab control samples, consisting of spiked water carried through the entire extraction 3 process and analyzed with the samples, were prepared. However, the informationwas not used because the data suggested itwas impossible to recoverspiked analytes from acidified water when riversediment was not present Water blanks, consisting of an aliquotofwater run through the entire preparation and 4 extraction process, were prepared. Acceptable valueswere < % LLOQ forthe data set in which they were run. 5 The River Sediment samples were quantitated using a non-extracted solvent calibration curve. Mid-level calibration curve pointswere used as COV's. Sample Analysis The samples were analyzed using HPLC/ES/MS. The analytical method was based on the 3M Environmental Laboratory Method ETS-8-155.1 "Analysis of Waste Stream, Water Extracts or Other Systems Using HPLC-Electrospray/Mass Spectrometry". The following table details sample run information, including the sequence and the run start date of each sample. Table 5. Sample Analysis Information. Sample ' 1 Catfish 2 Large Mouth Bass 3 Small Mouth Bass 4 River Water 5 River Sediments Loca don SL-1 SL-2 SL-3 SL-1 SL-2 SL-3 SL-3 SL-1 SL-2 SL-3 SL-1 SL-2 SL-3 St UULNU:: D020629 D020629 D020702 D020626 D020628 D020628 D020628 D020812 D020812 D020812 1021112 1021112 1021112 Date Sequence Was Started 29 Jun 02 29 Jun 02 02 Jul 02 26 Jun 02 28 Jun 02 28 Jun 02 28 Jun 02 12 Aug 02 12 Aug 02 12 Aug 02 12 Nov 02 12 Nov 02 12 Nov 02 3M Environmental Laboratory Page 11 of 276 Report E02-0443 Tenn. River Valley Samples A nalytical Method Sample analysis was based on ETS-8-155.1 "Analysis of Waste Stream, Water Extracts Or Other Systems Using HPLC-Electrospray/Mass Spectrometry". Methanol extracts were analyzed using HPLC/ES/MS in the negative ion mode. PFBS, PFHS, PFOA, FOSA and PFOS levels were evaluated versus calibration standards ranging in concentration from 11000 ng analyte/mL. The target ions were as follows: m/z = 299 (PFBS), m/z = 399 (PFHS), m/z = 413 (PFOA), m/z = 498 (FOSA), and m/z = 499 (PFOS). The analytical method used for analysis is presented below; modifications may be necessary to optimize the method for individual instruments. Analytical Equipment Liquid Chromatograph; Agilent/Hewlett-Packard Series 1100 Liquid Chromatograph system Analytical column: Keystone BetasilTM CiB2x50mm, 5pm particle size Column temperature: 30 C Cycle Time: 9.5 minutes Flow rate: 300pL/min Injection volume: 4 to 20pL Mobile phase components: Solvent A: 2.0 mM ammonium acetate in water Solvent B: HPLC Grade Methanol Solvent Gradient: T0.i0m0e 0.50 0.80 3.50 5.50 6.50 9.50 %10 B % 10 % 60 % 100 % 100% 10 % 10% Mass Spectrometer: Agilent/Hewlett-Packard Series 1100 API/Mass Spectrometer Detector Software: Agilent ChemStationTM A.08.03 Fragmentor Voltage: m/z 299 = 100V m/z 399 = 120V m/z 413 = 100V m/z 498 = 80V m/z 499 = 140V Capillary Voltage: 4000 V Gain = 1.0 EMV Mode: Electrospray Negative Gas Temperature: 350 C Drying Gas: 8.0 L /min. Nebulizer Pressure: 30 psig Analysis Type: Single Ion Monitoring (SIM) 3M Environmental Laboratory Page 12 of 276 Report E02-0443 Tenn. River Valley Samples Analytical Results Data quality objectives outlined in the Preparation Methods section were met. Regressions. Quadratic curve fit was applied to calibration standards and sample data to improve quantitation over the concentration range appropriate to the data. All calibration curves had least-square fits of 0.990 or greater. Calibration Standards. Standards ranging in concentration from approximately 1.0 to 1000 ng/m l were used for the calibration curves. The standard curve points had an injection volume of 10 uL. In some instances, the 1.0 ng/mL standard was injected at smaller volumes (1 ,2 , and 5 uL), this was done to extend the low end of the calibration curve. Calibration curves were run before every analytical sequence. Percent deviations of each calibration standard were calculated. High-end curve points that were outside the 20% criteria of the target concentration were excluded from the curve calculations. Low-end curve points that were outside the 20% criteria were included in the curve calculations but excluded from the Lower Limit of Quantitation (LLOQ). Continuing Calibration Verification (CCV). For quantitative determinations, a mid-level matrix calibration check was analyzed at least every ten samples to monitor instrumental drift, with a limit of 20% deviation of the target concentrations. Lower Limit of Quantitation (LLOQ). The LLOQ was equal to the lowest standard in the calibration curve, with a level of accuracy within 20%, that demonstrated a response greater than two times the response of analyte in the blank samples. System Suitability. Five system-suitability standards were analyzed before each initial calibration curve to measure the precision of the retention times and peak area. The precision criterion of 5% for the mean area recovery was achieved. Lab Control Spikes (LCS). LCSs were performed for the River Sediments. However, the information was not used because the data suggested it was impossible to recover spiked analytes from acidified water when river sediment was not present. Matrix Spikes (MS). Matrix spikes were performed for the Fish Tissue and the River Sediment samples. Desirable matrix spike recoveries are 30%. Not all matrix spikes met this criteria. The Fish Tissue data was quantitated using an extracted calibration curve while the River Water and River Sediment samples were quantitated using unextracted calibration curves. The calibration curve range that was injected was from 1 ng/mL to 1000 ng/mL, but the range used differed. The tables that follow contain either the calibration standard or the sample preparation method Lower Limit of Quantitation (LLOQ) for the analytes for each sample at each location along with batch used and the analysis date. The sample preparation method LLOQs will be annotated in the tables. 3M Environmental Laboratory Page 13 of 276 Report E02-0443 Tenn. River Valley Samples Table 6a. PFOS Calibration Standard Reprocessing Summary PFOS CONCENTRATION Sample T ype and Location Catfish, SL-1 Catfish, SL-2 Catfish, SL-3 Batch and A nalysis Date D020629,29 Jun 02 D020629,29 Jun 02 D020702,02 Jul 02 Lower Limitcf Q uantitation (LLOQ) 2.5ng/g 2.5 ng/g 1.0 ng/g Large Mouth Bass, SL-1 Large Mouth Bass, SL-2 Large Mouth Bass, SL-3 D020626,26 Jun 02 D020628,28 Jun 02 D020628,28 Jun 02 1.0 ng/g 2.5 ng/g 2.5 ng/g Small Mouth Bass, SL-3 D020628,28 Jun 02 2.5 ng/g RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 D020812A, 12 Aug 02 D020812A, 12 Aug 02 D020812A, 12 Aug 02 125 pg/mL* 125 pg/mL* 125 pg/mL* RiverWater, SL-1 D020812B, 12 Aug 02 1.25ng/mL* RiverWater, SL-2 D020812B, 12 Aug 02 1.25 ng/mL* RiverWater, SL-3 River Sediment, SL-1 RiverSediment, SL-2 RiverSediment, SL-3 D020812B, 12 Aug 02 1021112,12 Nov 02 1021112,12 Nov02 1021112,12 Nov 02 1.25ng/mL* 250pg/g* 250pg/g* 250pg/g* * Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 3M Environmental Laboratory Page 14 of 276 Report E02-0443 Tenn. River Valley Samples Table 6b. FOSA Calibration Standard Reprocessing Summary FOSA CONCENTRATION Sample Type and Location Batch and Analysis Da t Catfish, SL-1 D020629,29 Jun02 Catfish, SL-2 Catfish, SL-3 D020629,29 Jun 02 D020702,02 Jul 02 Large Mouth Bass, SL-1 D020626,26 Jun 02 Large Mouth Bass, SL-2 Large Mouth Bass, SL-3 D020628, 28 Jun 02 D020628, 28 Jun02 Small Mouth Bass, SL-3 D020628,28 Jun 02 RiverWater, SL-1 D020812A, 12Aug 02 RiverWater, SL-2 D020812A, 12Aug 02 RiverWater, SL-3 D020812A, 12 Aug 02 RiverWater, SL-1 D020812B, 12Aug 02 RiverWater, SL-2 D020812B, 12 Aug 02 RiverWater, SL-3 D020812B, 12Aug 02 RiverSediment, SL-1 1021112,12 Nov 02 River Sediment, SL-2 1021112,12 Nov02 River Sediment SL-3 1021112,12 Nov 02 l. o w r RLimit of Quantitation (LLOQ) 2.5ng/g 2.5 ng/g 2.5ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 5.0 ng/g 25 pg/mL* 25 pg/mL* 25pg/mL* 12 5 ng/mL* 1.25 ng/mL* 1.25 ng/mL* 50pg/g* 50 pg/g* 50pg/g* * Denotes sample preparation method LLOQ. Method LLOQ 3 instrument LLOQ/Method Concentration Factor. 3M Environmental Laboratory Page 15 of 276 Report E02-0443 Tenn. River Valley Samples Table 6c. PFOA Calibration Standard Reprocessing Summary PFOA CONCENTRATION Sample Type and Location BArCH and A nalysis Date Catfish, SL-1 D020629,29 Jun02 Catfish, SL-2 D020629,29 Jun 02 Catfish, SL-3 D020702,02 Jul 02 Large Mouth Bass, SL-1 D020626,26 Jun 02 Large Mouth Bass, SL-2 0020628,28 Jun 02 Large Mouth Bass, SL-3 020628,28 Jun 02 Small Mouth Bass, SL-3 D020628,28Jun02 RiverWater, SL-1 D020812A, 12 Aug 02 RiverWater, SL-2 D020812A, 12 Aug 02 RiverWater, SL-3 D020812A, 12Aug 02 RiverWater, SL-1 D020812B, 12 Aug 02 RiverWater, SL-2 D020812B, 12 Aug02 RiverWater, SL-3 D020812B, 12 Aug 02 River Sediment, SL-1 1021112,12 Nov 02 River Sediment, SL-2 1021112,12 Nov02 River Sediment SL-3 1021112,12 Nov02 Q uantitation (LLOQ) 5.0 ng/g 5.0ng/g 5.0 ng/g 2.5 ng/g 5.0ng/g 5.0 ng/g 5.0 ng/g 50 pg/mL* 50 pg/mL* 50 pg/mL* 1.25ng/mL* 1.25ng/mL* 1.25ng/mL* 250pg/g* 250pg/g* 250 pg/g* * Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 3M Environmental Laboratory Page 16 of 276 Report E02-0443 Tenn. River Valley Samples Table 6d. PFHS Calibration Standard Reprocessing Summary PFHS CONCENTRATION Sample Type and Location Catfish, SL-1 Batch and Analysis Da i t D020629,29 Jun 02 Lower Limit of Quantitation (LLOQ) 2.5 ng/g Catfish, SL-2 D020629,29 Jun 02 2.5 ng/g Catfish, SL-3 D020702, 02 Jul 02 2.5 ng/g Large Mouth Bass, SL-1 Large Mouth Bass, SL-2 Large Mouth Bass, SL-3 Small Mouth Bass, SL-3 RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 D020626,26 Jun 02 D020628,28 Jun 02 020628,28 Jun 02 D020628,28 Jun 02 D020812A, 12Aug 02 D020812A, 12Aug 02 D020812A, 12Aug 02 1.0ng/g 1.0 ng/g 1.0 ng/g 1.0 ng/g 25pg/mL* 25 pg/mL* 25 pg/mL* RiverWater, SL-1 RiverWater, SL-2 D020812B, 12Aug 02 D020812B, 12 Aug 02 1.25ng/mL* 1.25ng/mL* RiverWater, SL-3 RiverSediment, SL-1 River Sediment, SL-2 River Sediment, SL-3 D020612B, 12 Aug 02 1021112,12 Nov 02 1021112,12 Nov02 1021112,12Nov02 1.25 ng/mL* 100pg/g* 100 pg/g* 100pg/g* * Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 3M Environmental Laboratory Page 17 of 276 Report E02-0443 Tenn. River Valley Samples Table 6e. PFBS Calibration Standard Reprocessing Summary PFBS CONCENTRATION Sample Type and Loca i on Catfish, SL-1 Batch and Analysis Date D020629,29 Jun 02 Lower Lhvlt ot Quantithon (LLOQ) 5.0 ng/g Catfish, SL-2 D020629,29 Jun 02 5.0 ng/g Catfish, SL-3 D020702,02 Jul 02 5.0 ng/g Large Mouth Bass, SL-1 D020626,26 Jun 02 1.0 ng/g Large Mouth Bass, SL-2 D020628,28 Jun 02 2.5 ng/g Large Mouth Bass, SL-3 D020628,28 Jun 02 2.5 ng/g Small Mouth Bass, SL-3 D020628,28 Jun 02 2.5 ng/g RiverWater, SL-1 D020812A, 12 Aug 02 SOpg/mL* RiverWater, SL-2 D020812A, 12 Aug 02 50pg/mL* RiverWater, SL-3 D020812A, 12 Aug 02 50pg/mL* RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 RiverSediment, SL-1 River Sediment, SL-2 RiverSediment, SL-3 D020812B, 12Aug 02 D020812B, 12 Aug 02 D0208128,12Aug 02 1021112,12 Nov02 1021112,12 Nov 02 1021112,12 Nov 02 1.25ng/mL* 1.25ng/mL* 1.25 ng/mL* 100pg/g* 100pg/g* 100pg/g* * Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 3M Environmental Laboratory Page 18 of 276 Report E02-0443 Tenn. River Valley Samples Blanks. Method blanks, Milli-Q water taken through the solid phase extraction process, provided a measure of method background. In this experiment, they were labeled as "WB". One set was prepared for each location. In the Fish Tissue portion of the experiment, they were run with the Catfish samples. Acceptable values for the blanks were less than 50% of the Lower Limit Of Quantitation (LLOQ). All method blanks in this study met this criterion. The Fish Tissue segment of the experiment also contained method blanks for the SPE cartridges. These were labeled as "SB" and consisted of methanol that was used to extract pre-conditioned columns that did not have any sample added. All of these method blanks met the previous criterion. Solvent blanks/Methanol blanks (methanol injections) provided a measure of instrument contamination. Acceptable solvent blanks must contain levels of target analyte less than 50% of the Lower Limit Of Quantitation (LLOQ). All of the solvent blanks in this study met this criterion except the following: Note - Solvent Blanks that were before the System Suitability injections and did not pass the criteria am not recorded below. D020626 extracted samples 0050 (PFBS, PFHS, and PFOA) and 0051 (PFHS). These were caused by carryover from higher level standard curve points. The solvent blanks that were run after these points showed minimal carryover. D020628 sample 0051 (PFBS, PFHS, and PFOA), 0052 (PFHS), and 0053 (PFHS). This was caused by carryover from the high-level standard curve point. The solvent blanks that were run after showed minimal carryover. D020629 samples 0059 (PFHS, PFOA, FOSA, and PFOS), 0060 (PFOS), and 0061 (PFHS, PFOA, and PFOS). This was caused by carryover from high-level standard curve points. The 0061 Methanol Blank had a significant level of analytes but this had no effect on the quality of the data. The next sample had trace amounts of analyte and was below the LLOQ for all analytes. Therefore, the 0061 Methanol Blank did not influence the sample. The next solvent blank (0067) had nominal analyte concentration. D020702 samples 0042 (PFOS), 0059 (PFHS and PFOS), 0060 (PFOS), and 0061 (PFOS). This was caused by carryover from the high-level standard curve point. The solvent blanks that were run after showed minimal carryover. D020812(A) samples 0016 (PFOA and FOSA) and 0031 (PFOA). These were caused by carryover from higher level standard curve points or system suitability points. The solvent blanks that were run after these points showed minimal carryover. Samples 0037 (PFOA) and 0039 (PFBS, PFHS, and PFOA) had carry-over from samples. Subsequent blanks showed minimal contamination. 1021112 samples 012 (PFBS, PFOA, and FOSA), 027 (PFBS, PFOA, and FOSA), 039(FOSA), 066, (PFOA and FOSA), 068 (FOSA), and 071 (FOSA). All of these can be attributed to carryover from high-level standards or samples. 3M Environmental Laboratory Page 19 of 276 Report E02-0443 Tenn. River Valley Samples Data Summary Tables 7a, 7b, 7c, and 7d present the data for individual samples. Table 8 summarizes the average data for sample groups. Representative chromatograms are presented in Attachment C. Tables 7a, 7b, 7c, and 7d display the on-column and corrected concentrations for individual samples. Also included are the average concentrations for each set of samples standard deviation, and % Coefficient of Variation, when applicable. The final values reported are corrected for dilution/concentration factors introduced during sample preparation and by injection volume differences. The reported values were not adjusted for Matrix Spike Recoveries. When some of the samples within a group were < LLOQ, the average value for the group was calculated using the reported analytical value for samples > LLOQ and the LLOQ value for samples < LLOQ. The abbreviations are as follows: SL - Sample Location, C - Catfish, LM - Large mouth bass, SM - Small mouth bass, RW - River Water, and RS - River Sediment. 3M Environmental Laboratory Page 20 of 276 Report E02-0443 Tenn. River Valley Samples Table 7a. Catfish Analytical Data. LIMS U S a m p le Name PFBS ij/g) 42777 42778 42779 42780 42781 42782 42783 42784 42785 42786 42789 42790 42791 42792 42793 42794 42795 42796 42797 SL-1; C-1-1 SL-1 ; C-1-2 SL-1.C-1-3 SL-1. C-2-1 SL-1. C-2-2 SL-1. C-2-3 SL-1. C-3-1 SL-1. C-3-2 SL-1. C-3-3 SL-1. C-4-1 SL-1. C-4-2 SL-1. C-4-3 SL-1. C-5-1 SL-1. C-5-2 SL-1. C-5-3 SL-1. C-6-1 SL-1. C-6-2 SL-1. C-6-3 SL-2; C-1-1 SL-2; C-1-2 SL-2. C-1-3 SL-2. C-2-1 SL-2. C-2-2 SL-2. C-2-3 SL-2. C-3-1 SL-2. C-3-2 SL-2. C-3-3 SL-2. C-4-1 SL-2. C-4-2 SL-2. C-4-3 SL-2. C-5-1 SL-2. C-5-2 SL-2. C-5-3 SL-2. C-6-1 SL-2. C-6-2 SL-2. C-6-3 SL-2. C-7-1 SL-2. C-7-2 SL-2. C-7-3 SL-3; C-1-1 SL-3; C-1-2 SL-3. C-1-3 SL-3. C-2-1 SL-3. C-2-2 SL-3. C-2-3 SL-3. C-3-1 SL-3. C-3-2 SL-3. C-3-3 SL-3. C-4-1 SL-3. C-4-2 SL-3. C-4-3 SL-3. C-5-1 SL-3. C-5-2 SL-3. C-5-3 SL-3. C-6-1 SL-3. C-6-2 SL-3. C-6-3 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ PFHS (ng/gi <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ cLLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ PFA (iKj/y) <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ FOSA On colum n (ng/gl 5.9 5.3 5.2 4.4 4.2 3.9 7.0 7.1 7.4 3.9 3.7 3.8 9.1 9.1 8.8 7.0 6.9 7.0 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ FOSA Cc t for Smpl Prep O'g/g) 58.7 53.5 52.0 44.5 41.7 39.1 70.5 70.8 73.8 39.3 36.7 38.2 91.0 90.7 87.5 69.6 69.1 69.8 A 70. Sind D and %C.V 54.7 3.49 6.4% 41.8 2.67 6.4% 71.7 1.85 2.6% 38.1 1.30 3.4% 89.8 1.95 2.2% 69.5 0.41 0.6% PFOS On colum n (ng/g) 11.2 10.5 10.0 9.8 9.2 8.6 16.1 17.9 19.2 17.1 16.2 16.6 8.1 8.0 7.8 5.9 6.0 5.9 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 1.9 1.9 1.4 1.2 1.1 1.2 <LLOQ <LLOQ <LLOQ 3.7 3.5 4.0 <LLOQ <LLOQ <LLOQ <LLOQ 2.3 2.3 PFOS C o ir for am pi Prep 0>g/g) 112.1 104.7 100.3 97.6 91.8 86.1 161.2 179.4 192.4 171.5 161.9 165.8 80.8 80.2 77.5 58.8 59.7 58.7 Avo. Stud. O and %C V. 106 6.00 5.7% 91.8 5.77 6.3% 178 15.67 8.8% 166 4.82 2.9% 79.5 1.74 2.2% 59.1 0.57 1.0% 18.8 17 18.7 2.75 14.0 16.0% 11.5 11.7 11.5 0.44 12.2 3.7% 36.9 37.4 35.1 2.72 40.4 7.3% 23.3 23.5 23.2 3M Environmental Laboratory Page 21 of 276 Report E02-0443 Tenn. River Valley Samples Table 7b. Large mouth and Small mouth Bass Analytical Data. Sample Name PFOA Corrected for Smpi Prep FOSA Cot reeled 42798 42799 42800 42801 42802 42803 42804 42805 42806 42807 42808 42809 42810 42811 42812 42813 42814 42815 SL-1; LM-1-1 SL-1; LM-1-2 SL-1. LM-1-3 SL-1. LM-2-1 SL-1. LM-2-2 SL-1. LM-2-3 SL-1. LM-3-1 SL-1. LM-3-2 SL-1. LM-3-3 SL-1. LM-4-1 SL-1. LM-4-2 SL-1. LM-4-3 SL-1. LM-5-1 SL-1. LM-5-2 SL-1. LM-5-3 SL-1. LM-6-1 SL-1. LM-6-2 SL-1. LM-6-3 SL-2; LM-1-1 SL-2; LM-1-2 SL-2. LM-1-3 SL-2. LM-2-1 SL-2. LM-2-2 SL-2. LM-2-3 SL-2. LM-3-1 SL-2. LM-3-2 SL-2. LM-3-3 SL-2. LM-4-1 SL-2. LM-4-2 SL-2. LM-4-3 SL-3; LM-1-1 SL-3; LM-1-2 SL-3. LM-1-3 SL-3. LM-2-1 SL-3. LM-2-2 SL-3. LM-2-3 SL-3. LM-3-1 SL-3. LM-3-2 SL-3. LM-3-3 SL-3. LM-4-1 SL-3. LM-4-2 SL-3. LM-4-3 SL-3. LM-5-1 SL-3. LM-5-2 SL-3. LM-5-3 SL-3. LM-6-1 SL-3. LM-6-2 SL-3. LM-6-3 SL-3. LM-7-1 SL-3. LM-7-2 SL-3. LM-7-3 SL-3. SM-1-1 SL-3. SM-1-2 SL-3. SM-1-3 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LL0Q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LL0Q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 6.4 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 64.3 (Eliminated via Q-Test) <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ (ny/g) 18.5 13.0 14.0 63.6 61.4 57.2 73.2 80.8 82.4 68.8 75.7 65.3 46.6 41.5 38.9 69.3 59.9 66.0 <LLOQ <LLOQ <LLOQ 2.6 <LLOQ <LLOQ 9.7 11.8 8.5 53.1 54.1 56.9 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LL0Q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ cLLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ PFOS Corrected for Smpi Prep ng/y) 185.5 130.0 139.7 635.5 614.0 571.7 732.1 807.7 824.4 688.4 757.0 Average, Std. Dev., and %C V (ny/g) 152 29.61 19.5% 607 32.49 5.4% 788 49.18 6.2% 700 52.70 653.3 465.5 415.0 388.7 693.2 599.1 660.2 7.5% 423 39.03 9.2% 651 47.78 7.3% 25.6 96.7 117.6 84.7 530.8 540.9 569.4 100 16.68 16.7% 2504.072 3.7% 3M Environmental Laboratory Page 22 of 276 Report 02-0443 Tenn. River Valley Samples Table 7c. River Water Analytical Data. LIMS # 38025 38026 38033 38034 38037 38038 LIMS U Sample Name SW01 SW01-Dup SW03 SW03-Dup SW02 SW02-Dup Sample Name PFBS , (' n , q/m L ) ' 3.0 3.7 <LLOQ <LLOQ <LLOQ <LLOQ , rP.rF~,H, .Sr-- 38025 38026 38033 38034 38037 36036 LIMS n 38025 38026 38033 38034 38037 36038 SW01 SWOl-Dup SW03 SW03-Dup SW02 SW02-DUP Sample Name SW01 SWOl-Dup SW03 SW03-DUP SW02 SW02-Dup 7.7 8.0 <LLOQ <LLOQ <LLOQ <LLO Q PFOA rnn/,ni i (ng/mL) 21.3 22.7 LLOQ <LLOQ <LLOQ <LLOQ LIMS n 38025 38026 38033 38034 38037 38038 LIMS ft 38025 38026 38033 38034 38037 38038 Sample Name SW01 SWOl-Dup SW03 SW03-DUP SW02 SW02-DUP Sample Name SW01 SWOl-Dup SW03 SW03-DUP SW02 SW02-Dup (,nq/,mL, ,) 'J 1.0 1.0 <LLOQ <LLOQ <LLOQ <LLOQ PFOS , , ,, (,uJ,m L) 18.5 20.8 <LLOQ <LLOQ <LLOQ <LLOQ Adjusted l.o r I,nj.. V.,oi. ,rig ;rn ,L . 1.50 1.85 t,oArdm,juis. t.Ve.od.i (ng/mL) 3.86 3.98 Adjusted for lnF Vo1 (ng/mL) 10.66 11.33 Adjusted fo.r mj Voi (ng/mL) 0.48 0.51 , AC'/I,5t^ ,l tor Inj Voi (ng/mL) 9.25 10.40 Admsted for Dannile Prep ,pcj,/mL. ) ' 75 93 s_Aadmjupsl,ete dPr ,rfeopr (pg/mL) 193 199 Adjusted for 3 an,P|e Prep (pg/mL) 533 566 Adjusted for Sam, ple. Pr,ep (pq/mL) 24 26 A d ju s te d for Sample Prep. (pg/mL) 462 520 A, ver.ag..e pq- /m L 84 <LLOQ <LLOQ A, ver.a.g.e ' pg,m L> 196 <LLOQ <LLOQ Avene e 2 (pg/mL) 550 <LLOQ <LLOQ A , p g /.m 7 L , 25 <LLOQ <LLOQ Aver ,, l P 9 ' ,nL) 491 <LLOQ <LLOQ The sample extracts were analyzed several times using different sized injection volumes in order to match the appropriate analytical ranges for extracted samples, matrix spikes, and calibration curves. Table 7c incorporates data using 20 uL extracted sample injection volumes, 2 uL matrix spike injection volumes, and 10 uL calibration curve injection volumes. 3M Environmental Laboratory Page 23 of 276 Report E02-0443 Tenn. River Valley Samples Table 7d. River Sediment Analytical Data. L. H V 1O FF 38044 38044 38044 38045 38045 38045 38046 38046 38046 1 IM Q H 38044 38044 38044 38045 38045 38045 38046 38046 38046 38044 38044 38044 38045 38045 38045 38046 38046 38046 L.IIVIO TT 38044 38044 38044 38045 38045 38045 38046 38046 38046 38044 38044 38044 38045 38045 38045 38046 38046 38046 S a m p le Name 38044-1. SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 S a m p le Name 38044-1, SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 Sam ple Name 38044-1, SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 S am ple Name 38044-1, SL-1 38044-2, SL-1 38044-3. SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 S a m p le Name 38044-1, SL-1 38044-2, SL-1 38044-3, SL-1 38045-1, SL-3 38045-2, SL-3 38045-3, SL-3 38046-1, SL-2 38046-2, SL-2 38046-3, SL-2 On C olum n PFBS (ng/g) 10.6 10.6 13.5 8.9 8.3 10.0 8.9 6.2 11.7 On Colum n PFHS (ng/g) 2.7 2.6 2.5 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ On Colum n PFOA (ng/g) 16.2 14.1 13.7 CLLOQ 2.6 <LLOQ <LLOQ CLLOQ CLLOQ On Colum n F O S A (ritj/g) 29.7 32.4 24.5 1.2 1.2 1.7 2.9 2.5 3.2 On Colum n PFOS (ng/g) 67.7 70.3 50.4 9.1 6.8 9.1 9.0 8.5 10.5 A d |iiste d for lnj Vol. (ng/g) 5.3 5.3 6.7 4.4 4.1 5.0 4.5 3.1 5.8 A d ju s te d fo r Inj Vol. (ng/g) 1.4 1.3 1.2 CLLOQ CLLOQ cLLOQ CLLOQ cLLOQ cLLOQ A d ju s te d fo r Inj. Vol. (ng/g) 8.1 7.1 6.9 cLLOQ 1.3 cLLOQ cLLOQ cLLOQ cLLOQ A d ju s te d to r in; Vol (IKJ/<J) 14.8 16.2 12.2 0.6 0.6 0.8 1.5 1.3 1.6 A d ju s te d fo r Inj. Vol. (ng/g) 33.8 35.1 25.2 4.5 3.4 4.6 4.5 4.2 5.3 A djusted for Sam ple Prep (pgej) 530 530 674 444 415 502 447 309 583 A djusted for Sam ple Prep, (pg/g) 136 132 124 cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ A djusted for Sam ple Prep, (pg/g) 810 705 686 cLLOQ 131 cLLOQ cLLOQ cLLOQ cLLOQ A djusted for Sam ple Prep, (pg/g) 1484 1618 1223 62 60 83 146 126 161 A djusted for Sam ple Prep, (pg/g) 3383 3513 2518 454 342 456 452 425 525 A verage Std Dev., and %C.V. (pg/g) 577 84 14% 452 44 10% 437 137 31% Average, Std Dev., and %C.V. (pg/g) 130 6 5% cLLOQ cLLOQ CLLOQ cLLOQ cLLOQ cLLOQ A verage. Std. Dev., and : C V (pg/g) 732 67 9% 131 cLLOQ cLLOQ cLLOQ cLLOQ cLLOQ Average, Std. Dev., and %C.V. (pg/g) 1439 201 14% 68 12 18% 141 17 12% A verage, Std. Dev., a n d %C.V. ( p g /g ) 3132 541 17% 416 65 16% 457 52 11% Summaries for the average analyte concentration per sampling group and location are given below. 3M Environmental Laboratory Page 24 of 276 Report E02-0443 Tenn. River Valley Samples Table 8. Sample Location, Sample Type, and Analytical Data Summary. Fish Tissue Sampling Location & Species Sampled SL-1. C (n=6) SL-2. C (n=7) SL-3. C (n=6 SL-1, LM {n --6) SL-2, LM (n=4) SL-3. LM (n=7) SL-3, SM (n=1) PFBS (ncj/g <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ PFHS (ng/g) RFC) A (ng/g) <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ1 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ River Water FOSA i rg'i!i 60.9 (6/6)2 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ PFOS (ng/g) 113 (6/6)2 <LLOQ 15.2 (4/6)2 553 (6/6)2 169 (2/4)2 <LLOQ <LLOQ SL-1, RW SL-2, RW SL-3, RW PFBS (pg/m L) 84 <LLOQ <LLOQ PFHS (Pg/mL) PFOA (pg/mL) 196 550 <LLOQ <LLOQ <LLOQ <LLOQ River Sediments FOSA (pg/m L) 25 <LLOQ <LLOQ PFOS (pg/mL) 491 <LLOQ <LLOQ PFBS PFHS PFOA FOSA PFOS (pg/g) (pg/g) (pg/g) (pg/g) (pg/g) SL-1, RS 577 130 732 1440 3130 SL-2, RS 437 <LLOQ <LLOQ 141 457 SL-3, RS 452 <LLOQ 127 68 416 C = CatFish, LM Large mouth bass, SM Small mouth bass, RW River w ater, and RS River Sediments. 'H igh triplicate value was statistically elim inated using Dixon's Q-Test. ^(Number of Fish > LLOQ / Number of Fish Analyzed). Only one River Water and one River Sediment sample were collected from each sampling location. Attachment B contains additional data summary tables. Statistical Methods Statistical methods were limited to calculating averages, standard deviations, % coefficient of variation and statistical examination of outlying data points using Dixon's Q-Test. 3M Environmental Laboratory Page 25 of 276 Report E02-0443 Tenn. River Valley Samples Statement of Conclusion Fish Tissue: Fish tissue obtained from Sample Location 1 contained quantifiable levels of FOSA and PFOS. Fish tissue obtained from Sample Locations 2 and 3 contained quantifiable levels of PFOS only. River Water: Water from Sampling Location 1 contained quantifiable levels of PFBS, PFHS, PFOA, FOSA, and PFOS. Water obtained from sample Locations 2 and 3 did not contain quantifiable levels of analytes. River Sediments: River Sediment obtained at Sample Location 1 contained quantifiable levels of PFBS, PFHS, PFOA, FOSA, and PFOS. River Sediment obtained at sample Location 2 contained quantifiable levels of PFBS, FOSA, and PFOS. River Sediment obtained at sample Location 3 contained quantifiable levels of PFBS, PFOA, FOSA, and PFOS. References 1. 3M Environmental Method ETS-8-155.1 "Analysis of Waste Stream, Water Extracts Or Other Systems Using HPLC-Electrospray/Mass Spectrometry". List of Attachments Attachment A: Analytical Method and SOP Deviations AttachmentB: Data Summary Tables Attachment C: Sample Chromatograms Attachment D: Sample Prep Sheets, Test Substance, and Test System Information Attachment E: Notes to File Report Revisions Typographical errors for the unit designators for Tables 1, 6a-e, 7a, 7b, 7d, and 8 were corrected. The number of fish sampled at each location was also added to Tables 1 and 8. The descriptions of the sampling locations were adjusted in the summary and in tables 3a, 3b, and 3c to reflect those reported in the Entrlx report, July, 2003 (project #178401). Removed two values for PFHS in river water in tables 1 and 8 because they were <LLOQ. Re-calculated average values for PFOS in fish at sampling locations 2 and 3 and PFOA in sediment at sampling location 3 in tables 1 and 8 using LLOQ values for samples < LLOQ. 3M Environmental Laboratory Page 26 of 276 Report E02-0443 Tenn. River Valley Samples Signature Page W e certify that this report is a true and complete representation of the data for this study: William K. Reagen, Testing Facility Management Date 3M Environmental Laboratory Page 27 of 276 Report E02-0443 Tenn. River Valley Samples A: SOPAttachment A nalytical Method and Deviations 3M Environmental Laboratory Page 28 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, i f current, for 14 days from 11/21/2002 3M Environmental Laboratory M ethod An a ly sis o f W aste Stream , W a ter E xtracts or Oth er Sy stem s U sin g H PL C -E leciro spra y /M ass Spectro m etry M ethod Number: ETS-8-155.1 Author. Mark L. Anderson, Mark E. Ellefson Approved By: Adoption Date: H / & / 00 Revision Date: 3M Environmental Laboratory Page 29 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 1.0 Scope and Application__________________________ 1.1 Ss1y.c1so.t1peme:sspSTturpaehsnepiicndsaigafrmriacHdtei(aotPshnn)LoaawCdlny-dodteeerloskes,tccshirthoreieobnresesppts,asrmt)rah.ayaem/tmraeinctaeaesrlsssy,sswspioseillocvltefbrnowetmsad,seetsfteroinylsu.etrdteioainnmst,,hwqeuapatreloirttyosaccmoolnpotlrreostlhsoe,risnoattmehrepnrlael 1.2 Applicable Compounds: Electrospray ionizable compounds. 1.3 Matrices: 13.1 Wsysatsetme Ss toreraams dseasnidgnoattheedrisnytshteempsromtoacyocloonrssiasmt opfleaqpureepoaursaatinodn/owroorrkgsahneicetsso)l.vent 1.3.2 wWsoolaurtkteisrohSnesae.mt(Tsp)hl.eesminactlruixdewtailpl bweadteerf,ingerdoubnydtwheapterro,twocaoslteowrastaemr apnledportehpearraaqtiuoenous 2.0 Summary of Method___________________________________________________ 2.1 This method describes the analysis of electrospray ionizable compounds, using HPLC- seelelecctrtoiosnproayf amsainsgslsepieocntrochmaeratrcyte(rHisPtiLcCo-fEaSp/MartSic).ulTarhceoamnaployusnisdi.s performed by the mass 3.0 Definitions________________________________________________________________ 3.1 AqsIooutnumairdzcoraeustspip,oohpnlereor(EisbcySesPsIt),er,ameAnsssdtumairnloletoseIwprofhanfecoirzeircasv.tPaioTrreinohsuse(usAsermPeinIec)cth:hleuoCmddoeismcboamulftIieooarnncreiiizaznalalottyiitooalnnivma(bAiiyltaePubdctliIetl)oi,Hz:TiEnPhgLleeCracmt-vrEooaSssrppi/eMrrtaayyyS,osefitncg. le vTahceuiuomni)z.ation in these processes occurs at atmospheric pressure (i.e., not under a 3.2 Epdrrleoescpstlureortses.,pTwrhaheyesreIeobdnyriozipoalnteistosinnar(seEopSlur,otEidoSunIca)e:rdeAbtrymantehstefheoardrpepodlfitcoiaottnihoieznagotiaofsnappshtearrosfenogrvmiealeetdicntaryticacathmlafroigeselpddh.eric 3.3 MscihnaagsrlgseeSqrpuaeaticdotrru(ompmo/zlee)tmearnad(sMssusSeb)ls:eeCcqtouivmeenmtdlyeetrdecceiattoellcryste.mdI.aonnusfaarcetusreeldecMteSd soynsttehme bsaasrieseoqfumipapsesdtowith 3.4 MisnpseitccrruifomimceoanpstsesroMafttiawosnasLroey.fnaxn /HHPLPCC-EheSm/MSSta.tiPolneaSsoefrtewfearreto: Sthyestmemansuoafltwfoarrtehdeesspigecniefdicfor the 3MEnvironmental Laboratory AnalysisUsingHPLCE-TESl-eSc-t1roSs5p.1ray/Mass Spectrometry 3M Environmental Laboratory Page 2 o f10 Page 30 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 4.0 Warnings and Cautions___________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 tUhseepcraoubteioenmwpliothytshaevvoollttaaggeeocfabaplepsrofoxrimthaeteellyec5t0ro0s0pVraoyltpsr.obe. When engaged, 4.1.2 aWndheenyhewanedalri.ng samples or solvents wear appropriate protective clothing, gloves, 4 2 Cautions: 4.2.1 bOapcekrparteesssoulrveeenxtcpeuemdsp4s0b0elboawr,athbeacHkPp1re1s0s0urweiollfi4n0it0iabtearau(5to8m00atpicsi)s.huItfdtohwe n. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences_______ 5.1 Tstoormagineiomriazneyinptearrfteorefnincsetsruwmheenntaatnioanlytzhinatgcsoammepsleins,cToenftlaocnt swhiothultdhenostabmepuleseodr feoxrtrsaacmt.ple 6.0 Equipment_________________________________________________________________ 6.1 mEqoudiipfmicaetniot nlisstiendthbeelroawwmdaatyabaes mmoetdhiofideddienvioartdioenrst.o optimize the system. Document any 6.1.1 MeleiccrtroomsparsasyPiloantfiozramtioLnCsZouMrcaes.s Spectrometer (or equivalent) equipped with an 6.1.2 HP1100 low pulse solvent pump, solvent degasser, column compartment, and autosampler or equivalent HPLC system. 7.0 Supplies and M aterials________________________________________________________ 7.1 Supplies 7.1.1 Hsyisgtehmpu.)r.ity grade nitrogen gas regulated to approximately 100 psi (or house air 7.1.2 HsiPzeL)Coraneqaluyivtiaclaelncto. lumn, such as a Betasil C l8 column (50x2mm, 5 pm particle 7.13 Capped autovials or capped 15 mL centrifuge tubes. 8.0 Reagents and Standards___________________________________________________ 8.1 Reagents: 8.1.1 Methanol, HPLC grade or equivalent. 3M Environments] laboratory Analysis Using HPLCE-TESl-e8c-t1ro5s5p.1ray/Msu Spectrometry Page 3 of10 3M Environmental Laboratory Page 31 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 8.1.2 wManaioltletih-rQeorTMrveeqnwudaiovtrea.rle(nAt,SaTnMd mtyapyebI)e, parllovwidateedr buyseadMinitllhi-isQmTeOthCodPlsuhsosuyldstebme Morilli-QTM 8.1.3 Ammonium acetate, reagent grade or equivalent. 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.13.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g aaSpmtopmrreoopanrtiiuraomteomvaocteleutmamtepe.eorPafotMuurreil.ilni-tQo aw2a0te0r0, mL ivxoulunmtileatrlilcsfollaisdks,aardeddtihsseolved. 8.1.4 pOrtehpearrsaotilovnenwtsoraknsdhesoetl.utions may be used as stated in the protocol or the sample 8.2 Calibration Standards: 8.2.1 Toyf p5iscoallvlyentwt sotamndetahrodds abrleanaknsal(yMzeildliw-Qithweaatecrh),gtwrooupmoaftrsiaxmbplalensk.s, and a minimum 9.0 Sample Handling___________________________________________________________ 9.1 cSetanntrdifaurdgse atunbdepsroepraortehdersasumitpalbelsemcoayntbaiensetrosruedntiinl acnaaplpyesdis.autovials, capped 15 mL 9.2 Iaafpdapenrtoarixlmyimseinsattwealliylalf4bfeecCdteoulnanyttiheldea,nssaotlalyunsbdeiaslirtcdyasnoafbnsedaptpuerrerafpotaerrdmedseodslau(mrtieopfnrliesg)se.mraatoyrbteemrepferirgaeturaretesdmaaty have 10.0 Quality Control__________________________________________________________ 10.1 Blanks: 10.1.1 Seaoclvhesnatmbplalneksse,tmtoedtheotedrmbliannekcso, nantadmminaattriioxnbolarnckasrrayroevperre.pared and analyzed with 10.1.1.1 Wwahteenr othreHsPtuLdCygmraadtreicoersgcaonnicsissotlovfenhtisg,htlhyepmureitfhieodd saonldvemnatstrsiuxcbhlaanskTsympaey1 be represented by a single solvent blank. 10.1.2 tSahnoedlvsmetunadttyrbilxsaanbmklaspnlsekhsso.suhIlfodcubaledrrabynoeavaleynrzaielsydzapepdrirooarbfttleoermetha,ecchoinncisateilaicblurctaiavtlieiobnsroacltuviorevnnetc.buMlravneekthbsoumdt pabryliaobnrektos necessary. 10.2 Matrix Spikes: 103.1 thMeasttruixdys)piakneds amnaaylybzeedptroepdaerteedrmfoinr eeaecxhtrsaecttioofneexftfriaccietendcysa.mples (if applicable to 3MEnvironmental Laboratory Analysis UsingHPLECT-ESl-e8d-1ro5sp.rIay/MassSpectrometry Page 4 of 10 3M Environmental Laboratory Page 32 of 276 Report E02-Q443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 10.2.2 Massaotrciixatsepdikweidthupthliecaanteaslymsiasy. be prepared periodically to measure the precision 10.2.3 aAsntahleyzoeritghienaml asatrmixpslpe.ike and matrix spike duplicate (ifprepared) in the same run 10.2.4 Mreloannwadgto-rergiaxeonnsfgpotehiukeoseficnatohnintedicaiemlnnciattaritaalriitlbxiocrasanptliioiobkfnreathctdiueourpnavnleciacuolaryrtvteseehc.ioofSuneplcxdietkrnbeetemrcapoterinleoycpnealsnorsetwrhdaoltaeiuotvlnde1sl.fs5as-ahl5lroeitunimeldtxhepfesaemltchlteeiindd.the 10.3 Continuing Calibration Verifications: 10.3.1 aCcocnutriancuyinogfcthaelibcraaltiibornatvioenrifciucravteio.ns (CCV) are analyzed to verify the continued 10.3.2 mAninailmyzuema omfiodn-reapngerescaamlibprleatsioetn. standard after every tenth sample, with a 10.4 Internal Standard/Surrogate Standard: 10.4.1 An internal standard (IS) may be used to quantify the target analytes by establishing a relationship between the ratio of analyte response to IS response aanndama konuonwt tnhactowncilelnftaralltiwonithoifnththeeamnaidly-treanogfeinotefrtheset.caTlihberaItSiosnhcouurlvdeb.eTshpeikIeSd at should be added after the extraction process and before analysis. 10.4.2 pAqscauruemrsapvunpaertlrr.ieotaatgptiioarvetneeplaasynrtaaedntviadoananluardalayntmesditsahs.yheTobeuehnleudtissrfeeuadrlarlfnowoagrliaytqthteuiicnasahltlihotpyuerlcoldoocwbneedtrtuosorple.mikiTinedhdc-leruaastdnutighnreregoobgsfaeatmgtheienpislnceiuanlsgiebdorafttotihoen 11.0 Calibration and Standardization_________________________________________ 11.1 Analyze the standard curves prior to and following each set of samples. The average of tqcwauloaibdsrrtaaattniicodnafrictdu(cyruv=revsaexssh2mo+uablydxbn+eopct )blouetstfeiondrgcbeMydlatihsnsreLoauyrgnrhexgzoreerrsoost.ihoenr(syui=tamblxe +sobft)wwaereig.hTtehde 1/x, or 11.1.1 cTrhiteercilao.sinIfgocnallyibtrhaetifoinrsctucruvrevemiasyubseede,xthcleucdaeldibirfatthioenCaCnVd 'sstamndeaertdaiczcaetipotnable parameters are the same. 11.2 mIfathineteinnaitniaclecoarlipbrreaptiaorne caunrvewe dsotaensdnaortdmcuerevteac(cifenpetacnecsesacrryi)tearniadpreearfnoarlmyzreo.utine 11.3 Fusoer tphuerploowsesenodf aocfcthueraccayliwbhraetnioqnucaunrtviteatriantghelorwthalenvtehles ofuflalnraanlygtee., iEt xmaamypblee:newcheesnsary to 3MEnvironmental Laboratory Analysis Using HPLECT-ESl-eSc-t1r5oJs.pIray/Mass Spectrometry Page 5 o f10 3M Environmental Laboratory Page 33 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 aco(5toftenhpmspigibsphttitinocngog1no0tcof0et0nqhtuperaapstnbtiaot)i.nntadTstaetharadinspsdpwfarrroiodlxmls.irme5daputepcelbyitno1a0c1pc0pu0brpaopcybf aarnattatrhliybeturett,ehgdaentnotehlrieantfeeuaalrlcrreaaglnirbgeresasotiioofntnhwceuecriuvgrehvteing 11.4 Hovigerhtahnedl/ionrealorwranpgoeinatsppmroayprbiaeteextocltuhdeeddaftraoomr tbheecacualsiebtrhateiyondicdurnvoetsmtoeeptrtohveidpereabetter fit determined acceptance criteria. Low-level curve points should also be excluded if their acraeliabcraotuionntscaurrevneoptoaitnltesawstiltlwbiecentohteadt oinf tthheemraewthdoadtab.lanks. Justification for exclusion of 11.4.1 A minimum of 5 points will be used to construct the calibration curve. 12.0 Procedures________________________________________________________________ 12.1 Aincsqtruuimsiteionnt. sAet-cutupa-l ppaleraamseerteefresrewnicllebtehereScOorPdethdaotnpethrteaiinnsstrtoumtheenstpperciinfitcouts. 12.1.1 Set up the sample list. 12.1.1.1 Assign a sample list filename using the first letter ofthe name o fthe instrument (T for Tucker), the year (00 for 2000), the month (04 for April), alinsdt itshme dadaye o(Tn0t0h1e0s1a2mfeodraOyc,tuosbeeirn1c2re,2as0i0n0g olenttTeruscokefrt)h.eIaflpmhoarbeetthsatnarotinneg with A at the end ofthe list. 12.1.12 Assign a method (MS) file. 12.1.1.3 Assign an HPLC program (Inlet file). 12.1.1.4 Type in sample descriptions and vial position numbers. 12.1.2 Tspoecctrreoamteeatemr heethaoddin, gcslicakndonsemleectthSoIdRi.nStheet iAonciqzuaitsioitniomn coodnetaroslappapnreolptrhiaetne manadss maGdUadsIistDitooEn4Tto9O9thDoerASoTtIhRAesrA. aCSpaQpvrUoepIaSrciIaqTtueIiOsmiNtaiosfsnoermsa.edAtdhioftiudo.lnl SascleaeinntfhoisermuMsauitcaiorllonym. caoslsleMctaesdsLinynx 12.1.3 Tstyanpdicaarldlys.the analytical batch run sequence begins and ends with a set of solvent 12.1.4 Safatmerpelveserayreteanntahlysazmedpwle.ithSaolcvoennttinbulainngkscsahlioburaldtiobne vanearilfyiczaetdiopner(iCodCiVca)lliynjteocted monitor for possible analyte carryover. 12.2 Using the Autosampler/Column H eater 12.2.1 Place sample vials into the sample tray according to the sample list prepared in Section 12.1.1. 3M Environmental Laboratory Analysis Using HPLCE-TESle-8c-t1ro5s5p.1ray/MassSpectrometry Page 6 o f 10 3M Environmental Laboratory Page 34 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 12.2.2 thAettsawchitcthheinpgrovpalevrea,neanlsyutirceatlhcaotltuhme ntuibninthgeiscorulunmton thheeataeprpcroomprpiaatretmpoenrtts.. If using 12.3 Using the Inlet Editor 12.3.1 cSoents-iudpertsheapHpPro1p1r0ia0teusfionrgotphteimfoalllorewspinogncseo.ndRiteicoonrsdoarcatutaclocnodnitdioitniosnthseinatnhaelyst . instrument logbook: 123.1.1 Sample size = 10 pL injection 123.1.2 Flow rate = 300 pL/min. 123.13 Cycle time = 10.0 minutes 123.1.4 Mobile phase components: SSoollvveenntt AB:: 2M.0emthManoAlm(MmeoOnHiu)m Acetate in Water Solvent Gradient: T0481....i0500m0000e (min.1 5%995.55.00B..0000%%%% 8.50 5.00% 10.0 Stop 12.4 Instrument Set-up 12.4.1 RETefSe-r9to-3t6h,e"POlpatefroartmionLaCnZd UMsaeirn'tseGnaunicdee,othftehMe MasiscLroymnxaNssTPUlatsfeorr'ms GLuCidZe, the Einlsetcrturmosepnraty/Mass Spectrometer", or the SOP that pertains to the specific 12.4.2 Check the solvent level in reservoirs and refill if necessary. 12.43 Ceuynhesepactikiesctfhea.ecttToiprhyeo,tdfipitshaseshssoetuamilndbllbeesesthfsleatetpewrloicbtahepnailonladjaryrgegapetladthceeedteghneedss.otaIfiftnhtlheeespstriosptbeieselwfcoiautphnidallnatoryb.e 12.4.4 Turn on the nebulizing gas. 12.4.5 Open the tune page. Click on `Operate' to initiate the desolvation heaters. 12.4.6 Open the Inlet Editor. 12.4.6.1 Set HPLC pump to "On". 12.4.6.2 Set the solvent flow to the desired flow rate. 12.4.6.3 eOxbpseelrlvede dwriothplnetosnceobmuilnizginogutgoasftlheeaktiinpgoafrtohuenpdrothbee.tipAoffintheempirsotbseh.ould be Readjust the tip ofthe probe if no mist is observed. 3M Environmental Laboratory ETS-8-155.1 Analysis Using HPLC-Electrospray/Mass Spectrometry Page 7 o f10 3M Environmental Laboratory Page 35 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 12.4.6.4 Allow to equilibrate for at least 10 minutes. 12.4.7 mTonhaeythicenhsiatnrnsugtmreueminnetonurtsdepesrritnthoteoosueptstpi.mariazme ethteersreastptohnesfeo.llAowctiunagl pseatrtainmgest.erTshwesilel bseettriencgosrded 12.4.7.1 Drying gas 250-425 liters/hour 12.4.7.2 ESI nebulizing gas 10-15 liters/hour 12.4.73 HPLC constant flow mode, flow rate 10 - 500 pL/min 12.4.7.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.4.7.5 Source Block temperature 150. 12.4.7.6 Desolvation temperature 250". 12.4.8 Print the tune page with its parameters, the Inlet page, sample list, mass ssptuedcytrobminedteerrwiniftohrcmoaptiieosnt,aapneddainlltootthheerianpsptrluicmabelnetirnufnorlmogabtoioonk.and store it in the 12.4.8.1 All copies must be initialed and dated. 12.4.9 Click on start button on the MassLynx toolbar. Ensure beginning and ending sample numbers encompass all samples to be analyzed. 13.0 Data Analysis and Calculations___________________________________________ 13.1 Calculations (including, but not limited to): 13.1.1 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Background Result x 100 Expected Result 13.1.2 Calculate percent difference using the following equation: % Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 13.13 Calculate actual concentration of analyte in matrix (pg/mL): On-Column Concentration (pg/mL) x Dilution Factors = Calculated Concentration 14.0 Method Performance______________________________________________________ 14.1 The Limit of Quantitation (LOQ) is method, analyte, and matrix specific. For many analytes, the LOQ concentration is selected as the lowest acceptable non-zero standard in the calibration curve. 3MEnvironmental Laboratory Analysis Using HPLCE-TESle-8et-rIo5sSp.rIay/Mass Spectrometry Page * of 10 3M Environmental Laboratory Page 36 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 14.2 cSaollivberanttioanndcumrveteh.od blank area counts must be < 54that of the lowest standard used in the 143 oTrheeqcuoaelftfoic0ie.9n8t0o.f determination (r2) value for the calibration curve must be greater than 14.4 CstaonndtianrudincgonCcaelnibtrraattiioonn. Verification (CCV) percent recoveries must be 30% o f the 14.5 Internal Standard recoveries should be within 50% ofthe spiked concentration. 14.6 If criteria listed in this method performance section are not met, maintenance may be panerafloyrsmt. eDd oocnutmheenstyastlelmactainodnssainmtphleesrarweandaatlay.zed or other actions as determined by the 14.7 fIofodtantoatiesdtoonbetarbelpeosratnedd wdihsceunspseerdfoinrmthaencteexctroitfetrhiaehreapveornt.ot been met, the data must be 15.0 Pollution Prevention and Waste Management______________________________ 15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 16.0 Records________________________________________ __________ 16.1 Each page generated for a study must have the following information included either in tihnetehgeraatdioernomr hetahnodd,wsraimttepnleonnatmhee,peaxgter:ascttuiodnydoartep,rodjielucttinounmfabcetro,ra(ciqfuapispitliiocnabmlee)t,haondd, analyst 163 rPtourniinnltcotlghubedoetouiknn.ethpeagaep,psraomprpialetelissttu,daycqfuoilsdietiro. nCmopetyhtohdesaendpaaglleostahnedr atapppeliicnatbolethienfionrsmtruamtioennt 163 Plot the calibration curve then print these graphs and store in the study folder. 16.4 Pstruidnyt dbaintadienrt.egration summary, integration method, and chromatograms and file in the 16.5 Summarize data using suitable software and store in the study binder. 16.6 Bbaacckke-du-puepleecletrcotrnoicnidcadtaattaoianptphreosptruiadtyebmineddeiur.m. Record the file names and location of 16.7 Documentation of analyte(s) and all reference substances will include trace numbers, lot #'s, purity, expiration, and storage conditions. 17.0 Attachments_______________________________________________________________ 17.1 None 3MEnvironmental Laboratory Analysis Using HPLCE-TESle-8c-t1ro5s5p.1ray/Mass Spectrometry Page 9 o f tO 3M Environmental Laboratory Page 37 of 276 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 18.0 References 18.1 5PRlaZtf;oormr FLloCaZtsURsoeard's, WGuyitdhee,nMshiacwroemMas2s3U9KLZL;imUnitietedd, TKuidnogrdRomoa.d, Altrincham, WA14 18.2 M5RaZss;LoyrnFxloNaTts URsoeard',sWGuyitdhee,nMshaicwroemMa2ss3U9KLZL;iUmnitietedd, TKuindgodroRmo.ad, Altrincham, WA14 18.3 MassLynx NT Guide To Data Acquisition, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.4 ETS-9-34.0, "Operation and Maintenance ofHewlett Packard HPLC1100 System Equipped with a Mass Spectrometer Detector and/or a Photo Diode Array Detector". 18.5 EETleSct-r9o-s3p6r.a0y,/"MOapsesraStpioenctarnomd Meteari"n.tenance of the Micromass Platform LCZ 19.0 Affected Documents 19.1 None 20.0 Revisions Revision Number Reason For Revision RDevaitseion 1 Section 1:coEmnlmaregnetds tahbeousctosppeecoiffiTtchiptelaemrGaemtrhaeontedgrebsywiinllcblueddinegfinaedddiitniotnhaelpmroattroiccoels.orAplrseopasdhdeeedts. 09 May 01 Sections 1 and 2: Removed references to specific compounds. SSeeccttiioonn 33:: CRehmanogveeddtpoaarlalgorwapdhifofenreCnotnsvyesntetimonsaalnvdss.oZf-tSwparraey. probe interface. SSeeccttiioonn S9:: ABdrodaeddepneadratghreaptyhpaelsloowfisntgorfaogrethcoenutsaeinoerfsalatenrdncaotinvdeistioolnvse.nts and solutions. Section 10: Added comments to allow for flexibility in quality controls for different types of studies and applicability. Section 11: Added a paragraph allowing for the excluding of the second curve. Section 11: Added a paragraph (11.4) allowing for the dropping of curve points and minimum number of curve points needed. Section 12: Added comments to reference the specific SOP's for set-up. Section 12: Corrected numbering. Section 16: Added paragraph on records of analytes and substances. Section 18: Added reference to the method for the Hewlett-Packard LC/MS. 3MEnvironmental Laboratory AnalysisUsingHPLCE-TESic-8c-tr1oSs5p.r1ayrMiss Spectrometry 3M Environmental Laboratory Page 10 o f 10 Page 38 of 276 Report EQ2-0443 Tenn. River Valley Samples Record of Deviation I. Identification Study / Project No. TN River Valley E02-0443 Deviation Type: SOP ^M ethod Equipment Procedure (Check one) Protocol Other: Document Number: ETS-4-04.0 Date(s) o f occurrence: _____________________________________________ H Tlv fco 3- - ) O r f ,900 II. Description: Required Procedure/process:ETS-4-04.0 section 4 states, "It is the responsibility o f anyone handling samples to record the movement o f those samples on the internal chain o f custody form." ..................................... ................. Actual Procedure/process: The internal chain o f custody forms were not generated or used in the course o f this study. (such as ameInIId.meAntcitsisouneds, TSOakPerne:vision, etc.) No additional action will be taken, as the information cannot be recalled so long after the fact. Recorded By: ' 'i ' \ r, ) j ^ " IV. Impact on Study / Project This deviation does not adversely affect the quality o f the data. Date: I 1 !) r r (71 3M Environmental Laboratory 3M Environmental Laboratory Deviation No. I _________ (assigned by Study Director or Project Lead at the end o f study or project) Page 39 of 276 Report E02-0443 Attachment B: Data S ummary Tables Tenn. River Valley Samples 3M Environmental Laboratory Page 40 of 276 Report E02-0443 Tenn. River Valley Samples S^ Copy of Original I* l? O e c 0 l 3M Environmental Laboratory Pane 41 nf?7fi D020628 P0*2ef2l Report E02-0443 Tenn. River Valley Samples S5H$I rnrnmSS S'8B8a88a!s'l:"; ^5'5,' 5^c8i8a8l8ai88aS8a8*.*23-S2'5il*0838al?a m nte Ssss 88888 3ig 3SSSaSSal 88 ^ '||S P ||||||||||||||||||||| S*5g! mn o n n tto S338S ^1l a1s1s St ?3 *SS* f i f SS U at b! ^ 8s 3 Eg I sg I; ?s. 8s8 3* * * * U SS s 3 SSiS2a B S S is s s lIII ISaiis "S f i t U g SS a1s_ O9t 5 i IS 3 8 11i i i I n lifM a n ' lai M um H ?asaja^aa33ssfaa|iaaa fff* ssl 3M Environmental Laboratory Page 42 of 276 D020628 Large Mouth, Extracted Curve Sam ple Lo ca tio n a 2 and 3 Pa99e<21 Report E02-0443 Tenn. River Valley Samples I 5 3M Environmental Laboratory Page 43 of 276 Report E02-0443 Tenn. River Valley Samples 0020629 3M Environmental Laboratory Page 44 of 276 Report E02-0443 Tenn. River Valley Samples D020629 3M Environmental Laboratory Page 45 of 276 Report E02-0443 Tenn. River Valley Samples sis p l s s s i g s g l s I l l I s S Sm l im ? f* ss s j ; III fif* esc: III ||S ~8 a i l l ! ' 11MO a wOo UiJ. |933aaa33SgaaS899a3aa9aa5aiassaS33 88SS8 t i l ! | l l l B | i l l | l i l ! l i i i i i i | | l i f a sn d As M3 : im s 23^5^o iss i | S 3 ss 9 88383 salassa* RR"IRRSJj~ " nm ss !Sl aPsis ! 3M Environmental Laboratory Page 46 of 276 Report E02-0443 Tenn. River Valley Samples D020702 CatFIsh, Extracted Curva IM Fnutfftnm ntal I ahnratnn/ as4*V7C i i I 1 1 Ui Page 48 of 276 3M Environmental Laboratory E02-0443 RIvDr0W2a0t8er1S2aAmples Stm pU Loca tion* 1 ,2 , and S. Low and o f u v * . Sam pTyp* F ite S sm p te W *" * $ M ip ta tn fe H V bL (M J A raa Am ount flg ftB L % s a m p l e D U O E 001.0 M aO H S a n k M aO H B tenk: tN J k -0 6 1 1 5 :0 5 JiUT Q 2 (ip i|; U L M E t 10 40981 -- E 55 SA M PLE DUDEOOOZD M aO H B lank M aO H S K n k T N J W I15; OS Ju rt 0 2 (ip j|: U tA S E 10 370 BLOQ SA M PLE OUOEOOOS.O 020G 3-5Q G 6 02001-K W 1, 2 5 0 .0 * F u t C u rv a * C M C : 2 0 Jun 02 10 4785132 0 .0 SA M PLE 0U OE Q 0 4 .0 0 2 0 0 3 -5 0 0 2 0 0 1 -5 0 ^ 9 .5 0 0 .0 * F h C u rv a * C M C ; 2 0 Juno? 10 8128442 0 .0 SA M PLE OUOEOOOS.O 0 2 0 0 3 -8 0 -1 0 0 2 0 0 3 -5 0 -1 0 ; 7S 0.0p p b Fish C urvas; C M C ; 2 0 Jun 02 10 11184848 0 .0 SA M PLE D U D E 0006.D M aO H Blank M aO H B iantc T N -A 4 8 1 1 5 ; 0 8 J u i 02(rp s); M LA M EE 10 72835 2 .1 SA M PLE D U D 6O O 07.D M e O H B ia rt U O H B an k : T N Jk -0 6115; OS Ju n O lin )-. M LA/M EE 10 30181 BLOQ SA M PLE D U D E 0006.D M a O H B te rt M aO H B lanA T N -A 236115:0 5 Jun 0 2 (ip t); U L A /U E 10 20138 BLOQ SA M PLE OUOEOOOS.O B M k iry a a B lan kin iact 10 12094 BLOQ S A M PLE O U OE 0 0 1 0 D B lank Jntect B ian kin tect 10 12035 BLOQ A va: SA M PLE D U O EO O H.O 0 2 0 0 3 -5 0 -0 7 0 2 0 0 3 -5 0 4 7 ; lOO.Oppb R *h C u rv a r. C M C ; 2 0 J in 02 10 2328587 10 1.7 10 3.2 SA M PLE O U O E Q 012O 0 2 00 3-5 0-07 0 2 0 0 3 -5 0 -0 7 ; m o p p b F tsft C urvas; C M C : 2 0 J w tf i 10 2346180 10 2.8 *8 % SAM PLE D U D E 013D 0 2 0 0 3 -5 0 -0 7 0 2 0 0 3 -5 0 4 7 ; lOO.Oppb F ia ti C urvas; C M C : 2 0 Ju n 02 10 2316113 10 1.1 10 8.4 S A M PLE o u d b x m 4 .o 0 2 0 8 3 4 0 4 7 0 2 0 0 3 8 0 4 7 ; m O p p b F n h C u rva *. C M C ; 2 0 Jun 02 1 0 23 92 40 9 1 0 5 .8 -8 % SA M PLE O U O E Q 015D 0XU-SO -O 7 0 2 0 0 3 -9 0 4 7 ; lOO.Oppb R s fl C a v a s : C M C J ta i 02 10 2380996 10 4.9 98 .1 SA M PLE O UDEDQ 16.D M aO H Stank M aO H a n k : T N A -0 6 1 1 5 ; OS Jun Q2{rp>; l& A JM B E 10 15495 BLOQ SA M PLE O U O E 0017.O M aO H B lank M aO H S a r t; T N A G 8 1 1 5 ; 05 Ju n Q 2(rps); U L A A J & 10 13883 BLOQ SA M PLE O U O E 0018.O M aO H S a n k M aO H B Isnk: T N -A -06 11 5; 0 5 Jun 02 (ip s ); M LA/M EE 10 13734 BLOQ SA M PLE D U 0 0 1 9 D M aO H B lank M aO H B ard e T N -A -06115; OS Ju n 0 2 (rp sj; M L A /M K 10 12581 BLOQ SA M PLE D U O E 0Q 20O S tank if^ a a S lv k ln M O 10 11213 BLOQ SAMPLE D U D E 0021D B ***ttK t 10 11139 BLOQ C A B 1 D U 0E 0Q 22.O Q 2 0 Q 3 -5 K )1 : l 0 2 0 0 3 -9 )4 1 :1uL <1OOpp0; t.O p j F o fl C urvas: C M C : 20 Jun ffi 1 18287 0 .0 9 89% C A U 8 2 D U D E 0023 D G 2 00 3-50 01 ;2 u L 0 2 0 0 3 -5 0 4 1 ; 2u L W OpoO; 1.0ppb Fish C a v a s : C M C 2 0 Jun 2 193 0 .2 0 98% C A U 8 3 D U D E 0 0 2 4 D G 2003-50-01;5uL 0 2 0 0 3 -5 0 4 1 ; 5u L (SOOppt); 1-Oppb Fteh C urvas; C M C 2 0 Jun t t 5 28774 0 .5 3 105% C A U B 4 D U D E 002S D 0 2 00 3-5 0-01 0 2 0 0 3 -5 0 G 1 :1 .0 p p b F ish C u n as; C M C 20 J u n 10 44778 1.0 9 109% C A LIB 5 D U 0 e 0 0 2 6 D 0 2 0 0 3 -5 0 -0 2 0 2 0 0 3 -S W 2 2 .5 p )> i> F iU > C u r*M :C U C ;2 0 J u n a 2 10 82135 241 96% C A L d u d e t o 0 2 0 0 3 -6 0 4 3 0 2 0 0 3 -5 0 4 3 ; S.Oppb F a h C u rv a r. C M C ; 2 0 Jw > 00 10 15370 4 .9 6 9% C A LiB 7 O U D E 0028.O aC A u a 0U Q 029D 0 2 0 0 3 -5 0 -0 4 0 2 0 0 3 -5 0 4 $ 0 2 0 0 3 -5 4 0 4 .10-Qppb Fish C urvas; C M C ; 2 0 Ju n 03 0 2 0 0 1 -5 0 0 5 : JS O ootr F n C u rv a * C M C ; 20 Jw iO J 10 293680 10 691296 10 .0 2 5 .0 100% 100% C A U 8 9 O U O E 0030 0 0 2 0 0 3 -9 0 4 8 Q2O3-50-O6; SQ.Oppb F s h C urvas; C M C ; 2 ) J u iQ 2 10 1297324 5 0 .0 100% SA M PLE D U D E 0 31D M aO H S M ftk M aO H B ta n t T tM -0 6 1 1 3 ; OS Ju n 02 (rp sn M L A A ttE 10 14526 BLOQ SA M PLE O U D S S 3 2 .D M aO H Stank M aO H S ir te T N -A 4 6 1 1 5 ; OS Jun Q 2(rps); M LA M EE 10 13362 BLOQ SA M PLE D U O 0O 33.D M aO H B lank M aO H B tank: T N -A -06 11 5; 05 Ju n 02<ip$fc M O M E E 10 11891 BLOQ SA M PLE D U 0E 0 34.O W ater B tenk-1 0 2 -0 4 4 3 W ater B tenk W ater Sam ptes; non-G LP; 6 0 0 4 2 ; O K 10 19474 BLOQ SA M PLE OUOECOS5.D W a t * O m * # E 0 2 4 4 4 3 W a m B a n k W M ar S am pias; norvG LP; 7/1 7 /0 2 ; O H 10 31338 B LO Q SA M PLE D U O Q 036.D 38029 E Q 2-0443-38025; W U a r S am ptet; non-G LP ; 6/20X22; OK 10 77613 2 .3 SA M PLE D U DE 37.D M aO H BJank M aO H B ianic T N -A 4 6 1 15; OS Jun 2 (n ); M J J H B B 10 16520 BLOQ SAMPLE D U OE 0038D 38028 & J 2 4 4 4 3 -3 8 0 2 8 ; W atar Sam ptes; no rvG LP ; 7 /l7 /Q 2 ;O K 10 76373 2 SA M PLE D U 0EO O 38.O M aO H Staik M aO H atante T N *4 8 1 1 S ; OS Ju n 02 ^ p s); M L A M S 10 26629 BLOQ SAMPLE DU D040D 38027 E 0 2 -0 4 4 3 -3 8 0 2 7 : VUMsr S a o # * : n o rvG LP . 7 /1 7 4 2 OK 10 61166 1 .7 SA M PLE 0U D E 041.D M aO H B an k M O H B lantc T N -A -06115; 05 J u n 0 2 (rp ^ ; M LA/M EE 10 14829 BLOQ SA M PLE O U 0E 00 42 .O 3 8 (0 9 2 4 * 4 3 4 8 0 ; W a w S a n ates : H W H 3LP; a Q O ro t OK 10 59420 1 .9 SA M PLE O U OE 0 0 4 3 D M aO H Stank kteO H B an k: T N J L 4 6 1 1 5 :0 5 J u i O Sfrps); IftA M E E 10 17103 BLOQ S A M PLE O U D E Q 044.0 0 2 -0 4 ^ -3 8 0 3 2 ; W ater Sam ptes; norvO LP ; 6 /2 0 4 2 ; OK 10 21417 BLOQ S A M PLE O U D E 004S .D D U OE 04 .0 M aO H Stank 38033 M aO H a r t e T N -A 4 8 1 1 5 ; ffl Jun 2(rps): M LA/M EE B Q 4 4 4 3 -3 8 0 3 3 . W ater S ra -. n o n C L P . 6 0 0 4 2 ; OK 10 11961 BLOQ 10 tS 8 1 6 BLOQ SA M PLE 0 U 0 E 0 4 7 .0 M aO H S a n k SAMPLE ouoOOAaD 38034 M aO H B iante T *A 4 6 1 1 5 ; 0 5 Jun 02<rpfc U L k/M E E 0 2 4 4 4 3 -3 8 0 3 4 : W a ta r Sam ptes; non-G LP : 8 0 0 /0 2 ; OK 10 12266 BLOQ 10 20207 BLOQ SAM PLE " D u x a x -D SA M PLE o u o e 0 0 9 0 .0 SAMPLE D u o e o o s ro M aO H 6 M f* 38039 M aO H Blank M aO H S ta rtc T N ^ -0 8 1 1 5 ; 0 5 Jun O 2 0p ^ ; M U M S 0 2 4 4 4 3 -3 9 )3 3 ; W teter Sam ptes; non-G LP ; 8 /2 0 4 2 : OK M aO H B lr te T M A 4 8 1 15; 0 9 Ju n 0 2 ip ^ ; M LA/M EE 10 11980 BLOQ 10 20954 BLOQ 10 12415 BLOQ S a m p l e D U D C 0052. ' 38037 D U D E 0053.D 0 2 0 0 3 -5 0 4 9 E 0 2 4 4 4 3 -3 8 0 3 7 ; W a tm t S a n ^ r t; nOTVGLP; 6 /2 0 /0 2 ; OK Q 2(K )3-S 04S ; 25 .0 p p p F M i C urves; C M C 2 0 Jw 02 10 22352 BLOQ 10 718526 28 .1 104% SA M PLE O U 0E 054.D M aO H Stank SA M PLE OUDEOQ 5SO 38038 M aO H B te rte T N ^ f4 6 1 1 5 ; 0 5 J w 0 2 (n ): U L A A IE E E 0 2 -0 4 4 3 -3 8 0 3 8 ; W a ta r Sam ptes; rteM S L P : 6 /2 0 /0 2 ; 0 * 10 13214 BLOQ 10 24604 BLOQ SA M PLE OUDEOOSB.O M aO H Blank D U O E0Q S7O 38038 M aO H B ir te T N -A -06 11 5; 05 Jun 02{rp s): M LA A IE E 10 12375 BLOQ 10 26143 BLOQ SA M PLE D U D E 0058.D M aO H B lank M aO H M a rt: T N -A 4 6 1 1 5 ; 05 Jun 02(rp s}; M L A M S 10 13377 BLOQ SAM PLE DUO EO Q 590 38041 E IQ -0 4 4 3 -38 04 1; W ater S a n r t : no tvG L P ; 2 0 X 0 ; OK 10 25881 BLOQ SA M PLE D U D 0060.D M aO H S ta rt M aO H B ir te T A 4 6 rS ; 0 5 Ju n 0 2{rp s ); M LAAOE E 10 12381 BLOQ SA M PLE o u o e o o o to 38043 S S 4 4 4 3 -3 8 0 4 3 ; W M f S a n fte s ; nW VG LP; 6 m K a . OK 10 21507 BLOQ S A M P L E " D U D E 0 62.D SA M PLE OUOEOOS3JO M aO H Stank 38047 M aO H B r t c 7 N -A 4 s fl5 ; 0 5 Jun 0 2 (rp ^ ; M LA/M EE E 0 2 -0 4 4 3 3 8 0 4 7 ; w a te r S am ples: non-G LP ; 6 /2 0 /0 2 ; OK 10 11663 BLOQ 10 23124 BLOQ SA M PLE C K 0 640 M aO H Stank U a O H B tantc T N -A 4 6 1 1 5 :0 5 Jun ftp s ); M LAA E 10 13994 BLOQ SA M PLE D U O E O 065.6 W ater Btank-1 E 2 4 4 4 3 W atsr B lank W ater Sam ptes; norvG LP ; S /0M J2; O K 20 29174 BLOQ SA M PLE SA M PLE SA M PLE SA M PLE D U O E o o ee.o D U O E 0067.D D U D E Q 068.D D U D E 0069.D D x o d i . W alarB tan k-2 3802$ M aO H B lank 38026 U e O H B te f* E 0 2 *M 3 W U lf B U nk W f S n p H i. nw vG LP ; 7 /1 7 /0 2 , OK E 0 2 4 4 4 3 -3 8 0 2 5 ; W ater Sam otes; norvG LP ; 6 /2 0 4 2 : OK U tO H B W T O J : 0 6 1 1 5 : OS Jun 0 2 (il |: M A A IB 0 2 -0 4 4 3 -3 0 0 2 6 : W ater S a m ste i: norvG LP : 7 /1 7 /0 2 : OK M aO H StwUu T N -A -06 11 & 0 5 Jun 02(rp s); IA A A IE E 20 54510 20 98531 10 18086 20 118567 10 12416 1 .4 3 .0 BLOQ 3 .7 BLOQ auara A na t e a s 0 9434014 11641429 60006 22991 11164 274 2146 2517190 2533016 2512307 2579744 2536146 7469 3571 2295 1483 1223 0 4867 7662 17073 33124 78398 159905 320769 766758 1427363 5446 2301 0 3537 1117 131130 7594 134719 10424 202744 3071 131319 6360 65594 2476 5944 1827 4678 1063 94878 0 7184 797390 3059 5490 1483 81597 0 83128 0 8876 0 3999 0 5192 4219 247750 3257 255868 0 Am ount n p fe tL BLOQ BLOQ 0 .0 0 -0 0 .0 2 .5 0 .7 BLOQ BLOQ BLOQ 1 0 5 .4 1 0 6 .5 10 S .1 1 0 9 .9 106 8 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 0 .1 5 0 .2 3 0 .5 2 1.01 2 .4 0 4 .9 4 100 2 5 .0 5 0 .0 BLOQ BLOQ BLOQ BLOQ BLOQ 4 .0 BLOQ 4 .2 BLOQ 6 .3 BLOQ 4 JO BLOQ 2 .1 BLOQ BLOQ BLOQ BLOQ BLOQ 2 .9 BLOQ BLOQ 2 6 .1 BLOQ BLOQ BLOQ 2J BLOQ 2 .6 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 7 .7 BLOQ 8 .0 BLOQ Am ount % Ana nghaL A im : 1 0 8 .7 5% 1 1 2.0 4% 1 0 1.4 145% 115% 104% 101% 96% 99% 100% 100% 100% 104% "S S E T 15700 2222061 3961548 5462222 45568 232 16017 6745 6821 1159473 1175609 117903 11B 7272 1187119 12509 10727 10506 9167 6534 7056 10608 11563 16208 24216 45920 64652 159993 372294 667569 12766 11351 10656 9173 9700 16112$ 12473 171533 13964 206265 11264 171670 11619 46142 110 9620 10532 12092 10121 49413 10336 113 392926 11362 12087 10830 464 10738 47821 10096 10 8656 9531 10770 91 11746 321648 11340 31410001611 1 9 .3 BLOQ 6 .0 0 .0 0 .0 2 -4 BLOQ BLOQ BLOQ BLOQ 96 .1 1 0 0 .3 1 0 0.6 1 0 1 .6 10 1.8 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 0 .1 4 0 .2 0 0 .5 0 1 ,0 2 2 .4 3 4 .8 8 1 0 .0 2 5 .0 5 0 .0 BLOQ BLOQ BLOQ BLOQ B LO Q 16 .1 BLOQ 1 8 .8 BLOQ 112 BLOQ 10J BLOQ 2J BLOQ BLOQ BLOQ BLOQ BLOQ 2 .7 BLOQ BLOQ 2 6 .5 BLOQ BLOQ BLOQ 2J BLOQ 2 .8 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOO 214 BLOQ 227 BLOO % A va 10 0.5 +5% 1056 -5 % 9 5 .5 141% 101% 101% 102% 97% 100% 100% 100% 100% 106% T B s n ra r Am t Am ount n e/m L % 88388 7554 6079195 11100827 15609912 59639 23381 16560 11181 9635 2864799 2863989 2874831 2117264 2683854 10447 7611 04 4355 3221 3444 5642 8628 17101 29673 7307 150031 296779 749438 1461610 5723 3628 3577 3902 3405 15910 2655 16662 2215 57230 0 17294 2129 66397 2759 3598 2558 4607 2048 53098 2B 59 5073 7726 3719 3274 2764 71897 3153 70849 2080 4395 2404 3387 2178 3371 29388 2474 31162 2164 2 .9 6LO 2 4 4 .3 00 0 .0 2 .0 Q .6 BLOQ BLOQ BLOQ 10 2.0 10 2.0 10 2.4 10 0.2 1 0 2 . BLOO BLOQ BLOQ BLOQ BLOQ BLOQ 0 .1 9 0 .2 6 0 .5 6 197 2 .4 0 4 .9 5 9 .6 4 2 5 .1 5 0 .0 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1 .9 BLOQ 0 .6 BLOQ 2 BLOQ BLOQ BLOQ BLOQ BLOQ 1 .7 BLOQ BLOQ 259 BLOQ BLOQ BLOQ 14 BLOQ 2 .3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ B1L.O0Q BLOQ Avat 1 0 1.9 4-5% 1 0 7 .0 -$ % 9 6 .9 186% 139% 111% 97% 98% 88% 96% 101% 100% 104% P W S tfW ) A ras Am ount n g /m L 9 0 4 4 34456 68910 8575576 11897063 95548 51276 36123 29189 28814 2521536 2531747 2548168 2504346 2546185 34400 31640 30933 29010 26149 26205 32546 34279 44403 60834 105750 184464 336343 765247 1398166 32297 30337 26614 320 31254 294975 3581? 334613 35687 403737 32700 1315 32843 111790 31103 32811 29748 39153 594 102435 29657 180 795740 31386 38088 30464 99019 29732 114326 29451 30794 28614 31233 29474 34010 33607 S83655 30917 648655 30542 3 1 .9 BLOQ 0 .0 0 .0 BLOQ BLOQ BLOQ BLOQ BLOQ 1 1 2 .3 1 1 3 .1 110 1142 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 0 .1 2 0 .1 5 0 .5 0 1.0 2 248 500 1 0 .0 2 5 .0 5 0 .0 BLOQ BLOQ BLOQ BLOQ BLOQ sc BLOQ 1 0 .0 BLOQ 113 BLOQ 8 .8 BLOQ 2 .7 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 261 BLOQ BLOQ BLOQ BLOQ BLOQ 2 .7 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1 5 .5 BLOQ 2 6 . BLOQ % A ve: 1130 11 8.6 124% 89% 100% 102% 96% 100% 100% 100% 100% ; 104% - - Tenn. River Valley Samples Report E02-0443 D020812A River Water Sample Sample L o ca tio n * 1 ,2 , end 3. Low end o f curve. Pag*34 Report E02-0443 3S3SSSS 5 mi "3 si 5 * SA' i i f i i i i i i ! I 2 n BRn u n h S: aia I n 33 5 1! E ?a SI Jo 88 88 as 88 88 8 8 8 8 8 8*8 ! i* u>I8i[S<o :-e is iliiiiiliiii IIIi.s l l llil 1iM il i f I 5I OQQ sie si Sfc si 5I 5 ip if Tenn. River Valley Samples I S 3 t-K)-Z03 JJOday saiduies te||BAJawy uusi **o " IS ?S ff S 3 CS ijQ jpsn*fuogs9fti!*]n?*M lAluO 'T fr P08'S 'I *1^*1 m as J* P*M * *}dujes sm Report E02-0443 1021112 Riva; Sediments Sam ple L o c a tio n * 1 ,2 , and 3. -----------P fB 5 |H iT SimpTypc Fttc InJ.Vof Sample Name (U Sim ple info Ar" SAMPLE ITCHY01.D 10 MaOH Blank- MaOH BUnk: TN-A-06264; 12 Sapttoppa* MIA/Ufc 50959 SAMPLE ITCHY002.0 10 MaOHBlank MaOH BUnk TN-/L062M; 12 Sept02(cpv, MLA/MEE 21360 SAMPLE ITCHY003.0 10 MaOH Blank MaOH BUnk TN.A-06264; 12 Sapt02(ip); MIAAIEE 19017 SAMPLE ITCHY004.D 10 MaOH Bank MaOH Blank: TN-A-062M; 12 Sapt 02(ipi): MLAAIEE 19616 SAMPLE ITCHY005.D 10 Blarfcifliact Blank inject 15214 SAMPLE ITCHY006.D 10 Blank intact 15582 SAMPLE ICHY007.0 10 02003-50-07 02003-50-07; lOOOppb Fish Cuva; 20Jun02: CMC 3116944 SAMPLE ITCHY006.0 10 02003-50-07 02003-5007; 100.0ppb Futi Cuva; 20JU102;CMC 3226292 SAMPLE ITCHY009.0 10 02003-50-07 0200350-07; 100.0ppb Fish Cuva; 20Jun02: CMC 3290155 SAMPLE ITCHY01QO 10 Q2003WS7 020034047; lOOOppbF in i Cuva; 203UI2; CMC 3264394 SAMPLE ITCHY011.0 10 02003-50-07 02003-50-07:lOOOppb Fish Cuve: 20Jun02 CMC 3265467 SAMPLE ITCHY012.0 10 MaOHBlank MaOH Bank TN-A-06264; 12 Sapi02(rps); MLA/MEE 28625 SAMPLE ITCHY013.0 10 MaOHBank MaOH Bank TNJP062S4; 12 Septtappe* MLA/MEE 19985 SAMPLE rrcH Y0i4.o 10 MaOHBank MaOH Bank TN-A-06264; 12 Sapt02(ipa): MLA/MEE 20057 SAMPLE ITCHY015.D 10 Blank na ci Blank injact 15091 SAMPLE ITCHY016.0 10 Hank Intact 14788 CAua i ITCHY017.D 02003-50-01 020035041:1-OpppFish Cuva: 20Jun02; CMC 22011 CAUB 2 rrCHYOIB.O 2 02003-504)1 020034041:1.OpohFish Cuva; 20Jun02: CMC 25188 CALIB 3 ITCHY019.D 5 02003-5001 020034041:1-OppDFish Cuna; 20Jun02: CMC CALIB 4 ITCHY020D 10 02003-50-01 02003-50-01:1.OppbFish Curva; 20Jun02; CMC 54827 CALIB $ 1TCHY021.0 10 02003-50-02 020035002:25ppb Fish Curva; 20JU1B2; CMC 105679 CALIB 6 ITCHY082.O 10 02003-504 0200350-03:5 .0 * Fish Curva: 20Jun2; CMC 195112 CALIB 7 ITCHYQ23.0 10 02003-50-04 020034044; lO.OppbFish Cuna; 20Jun02; CMC 366155 CALIB 8 ITCHY024.D 10 02003-5005 020034045; 25.0ppb Fish Curve: 20JunO2. CMC 852340 CALIB 9 [TCHY025D 10 02003-50-06 02003-50-06:50.0* Rsh Gave; 2Jun02: CMC 1677041 II1 I 8 i CALIB 10 ITCHY026.0 10 02003-50-07 3128959 SAMPLE ITCHY027.D 10 MaOH Bank MaOH BUnk TN-A-052S4; 12 Sapt02(ip>): MLA/MEE 30131 SAMPLE ICHY028D 10 MaOHBank MaOH Bi4c TI^A-06264; 12 SapttBfa): MLA/MEE 24605 SAMPLE ITCHY029D 10 MaOHBank MaOH BUnk TH-A462M. 12 Sapt02(fp* MLAAIEE 19172 SAMPLE ITCHY0300 10 MaOH Bank MaOH Blank: TN-A-06264; 12 Sept Q2(ips); MLAAIEE 18797 SAMPLE (TCHY031.D 10 Hank intact Blank aje d 14468 SAMPLE ITCHY032.D 10 Bank intact Blank irject 14928 SAMPLE (TCHY033.D 10 MaOH Blank MaOH Blank: TN-A-06284; 12 Sapt 02(rps); MtA/MEE 19375 SAMPLE ITCHYQ34.D 10 0443-WB-1 02-044iwvB-1;Water Blank; MaOH Extract; 21Oct 02, MLA 37874 SAMPLE ITCHY035.D 10 0443-WB-2 E02-0443WB-2; Water BlanK MaOH Extract 21 Oct02; M IA 32544 SAMPLE ITCHY036.D 10 0443-LCS-1 E024443-LCS-1; Lap Control Spike; MaOH ExtnO; 21 Oct 02; 1 263855 SAMPLE ITCHY037.D 10 0443-LCSO E02-0443-LCS-2; LapControl Spfee; MaOH Exffa 21 Oct 02; 4 482168 SAMPLE ITCHY038.D 20 SAMPLE ITCHY039.D 10 SAMPLE ITCHY04O.D 20 0443-36044-1 E02-0443-36044-1: SL-1; MaOH Extract: 21 Oct02: MLA MaOH Bank MaOH Blank: TN-A-06264; 12 Sapt02(rps}; MLAAIEE 0443-36044-2 E02444338044-2: SL-1; MaOH Expact 21 o a 02: MLA 383859 20291 383808 SAMPLE ITCHY041 0 10 MaOH Blank MaOH Blank: TNA-06264; 12 Sapt 02{/ps): MLAAIEE 19921 ITCHY042.0 20 0443-36044-3 ED2-0443-38044-3; SL-1. MaOH Extract 21 Oct02; MLA 482034 SAMPLE ITCHY043.0 10 MaOHBank MQH Blank: TN-A-06284; 12 Sapt02{ip*}; MLAAIEE 21235 SAMPLE rrCHY044O 10 01 M M I-M SHI E02-04-ja0<4-MS(J); SL-1; MaOH Extract; 21 Oct 02: MU 1373477 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE ITCHY045.0 rrcHY04d.0 ITCHY047.D ITCHYO40.O ITCHY049.D 10 20 10 20 10 MaOH Bank 0453-38045-1 MaOH Bank 0453-38045-2 02003-50-06 MaOH Biarfc TN-A-06264; 12Sept02(fp*); MLAAIEE E02-0443-38045-1: SL-3; MaOH Extract 21 Oci02: MLA MaOH Blank: TN-A-06264; 12 SeptQ2(rp*); MLAAIEE 02-0443-36045-2: SL-3; MaOH Extract 21 0002; MLA 020(04048; MOppb Fish Curve: 20Jun02; CMC 23305 325254 21014 305101 1647938 sam ple ITCHYOS.D 10 MaOH Bank MaOH B ank TN-A-06264; 12 Sept02(rps); MLAAIEE 23146 SAMPLE ITCHY051.0 20 0453-38045-3 E02-044338045-3. SL-3; MaOH Extract:21 Od02; MLA 364668 SAMPLE ITCHY062.D 10 MaOHa * MaOH Bank: TN-A-06264:12 Sept ((6); MLA/MEE 19743 SAMPLE 1TCHYS3.D 10 04534804S-USC 02 0443 3604S MS(3); SL-3; MaOH Extract; M Oct 62; MLA 1648788 SAMPLE ITCHY054.D 10 SAMPLE ITCHYQ55.D 20 MaOH Bank MaOH Bank: TN-A-06264:12 Sept02(rw); MLA/MEE 0463-36046-1 E02-044338046-1: SL-2; MaOH E x n c t 21 OU02; MLA 20665 327380 Sam ple TCHYQ56D 10 MaOH Bank MaOH Bank: TNA-06264; 12 Sapt Q2(ipt); MU/MEE 18866 SAMPLE ITCHY057. 20 SAMPLE ITCHY05O 10 0463-38046-2 E02-0443-38046-2; SL-2: MaOH Exbct 21 ct2; MLA MaOH Bank MaOH Bai4c TNA-06264; 12 Sept 02(rpa); MLAA4EE 232749 1B641 SAMPLE YfCHYW' D* 20 0463-36046-3 E02-044338046-3; SL-2; MaOH Extract 21 Od 02; MLA 420079 10 MaOH Blank MaOH Bank: TN-A-06264:12Saot02ffM): MLAAIEE 18094 `sam ple* ITCHY601D 10 0463-3S646-MS3} 820443 3B04SMS3); SL-3; MaOH E xtract; O ct62; MUI 132S951 SAMPLE 1TCHY062D 10 MaOH Bank MaOH BUnk TN-A-06264; 12 Sapt 02frp>): MLAAIEE 21141 SAMPLE ITCHY063D 10 0443-WB-3 E02-0443-WB-3; Water Bank; MaOH Exkact 21Oct02; MLA 33516 SAMPLE ITCHY064.D 10 MaOH Blank MaOH BUnk TN-A-06264; 12 Sapt 02(ips); MLAAIEE 17365 SAMPLE ITCHY065 D 10 ITCHYQ6.0 10 0443-LCS-3 24443-LCS4: Lab Control Spike; MaOH E ttact 21 O d K 1 37815 MaOH Blank MaOH Blank: m A-06264; 12 Seot02<fMi: MUAIEE 17738 SAMPLE ITCHY067.O 20 0443-38044-4 E02-O443-38O44-4; SL-1; MaOH Extra 21 Oct02; MLA 452851 Amount ngtmL BLQ BLQQ BLOQ BLOQ BLOQ BLOQ 99.5 103 105.9 105.7 105.7 BLOQ BLOQ BLOQ BLOQ BLOQ 0.1 02 OJ 1.0 2.5 5.1 10.1 24.6 50.3 99.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 7.1 13.5 10.6 BLOQ 10.6 BLOQ 13.5 BLOQ 40.6 BLOQ 89 BLOQ 8.3 49.4 BLOQ 10.0 BLOQ 4M BLOQ 8-9 BLOQ 6.2 BLOQ 11.7 BLOQ 39J BLOQ BLOQ BLOQ BLOQ BLOQ 12.6 ----------- 0FWS(SU) % Ava: 104.1 +5% 106.3 4% 98.9 95% 63% 101% 104% 100% 102% 101% 96% 101% 100% 14% 27% 81% 99% 82% 78% . *" 169862 1830 1350 1432 1460 1317 4263993 4325829 4377377 4351068 4330657 20656 3600 1293 1571 1312 628? 10753 24660 47829 110003 222096 448963 1115227 2235317 4223532 21365 5759 3655 1446 1306 1147 1961 2541 3628 71410 240625 122635 2099 118901 2000 111724 1660 1385185 2067 13341 2114 11469 2185430 1745 12125 1694 1885858 6058 17353 1682 18434 1723 25494 1664 1546883 6932 1745 1485 2065437 4071 126160 Am our* ngM . 3.7 BLOQ BLOQ BLOQ BLOQ BLOQ 101.0 102-6 104.0 103.3 102.7 BLOQ BLOQ BLOQ BLOQ BLOQ 02 0.3 0.6 1.1 2.4 4.9 98 24.0 50.4 69.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1.6 5.3 2.7 BLOQ 26 BLOQ 2.5 BLOQ 30.7 BLOQ BLOQ BLOQ BLOQ 49.2 BLOQ BLOQ BLOQ 373 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 30.7 BLOQ BLOQ BLOQ 46.4 BLOQ 2.8 ---------- P R jjrp n r ----------- FOSAM W % *"* Amount itg/m L % Amount nflftnL 1291736 34022 27981 80.6 BLOQ BLOQ 15342 0 0 BLOQ BLOQ BLOQ 23447 BLOQ 0 BLOQ Ava: 102.7 +5% 107.9 8% 97.6 13605 14484 1567803 1565427 1583410 1582946 1576615 33094 21962 21600 BLOQ BLOQ 101.1 102,5 102.3 102.3 101.9 BLOQ BLOQ BLOQ Ava: 102.0 5% 107.1 *8% 96.9 0 0 4014481 3990495 4059608 4064888 4041973 43396 0 0 BLOQ BLOQ 99.9 99.2 101.1 101.2 100.6 1.1 BLOQ BLOQ 214% 155% 123% 111% 98% 97% 98% 98% 13817 13047 16607 17924 23492 32917 58279 101209 188013 436156 BLOQ BLOQ 0.2 Q 05 1.1 2.5 4.9 9.9 24.7 157% 115% 109% 108% 100% 99% 99% 99% 0 0 3903 7866 19922 41430 99625 205416 414854 1043141 BLOQ BLOQ 0.2 0.3 0.6 1.1 2.4 4.9 9.8 24.7 101% 100% 847970 1552778 30743 24724 21388 22776 50.3 99.9 BLOQ BLOQ BLOQ BLOQ 101% 100% 2094504 4016583 12135 3012 0 0 50.3 999 BLOQ BLOQ BLOQ BLOQ 14388 13634 22413 13412 BLOQ BLOQ BLOQ BLOQ 0 0 0 1927 BLOQ BLOQ BLOQ BLOQ 3% 11% 81% 96% 76% 14592 22317 S24B9 295590 21843 260003 22126 253343 21251 860980 23125 48048 22078 60231 820358 21007 54999 20675 101398 20620 53375 22309 BLOQ BLOQ BLOQ 16.2 BLOQ 14.1 BLOQ 13.7 BLOQ 384 BLOQ BLOQ BLOQ 2.5 48.5 BLOQ BLOQ BLOQ 4M BLOQ BLOQ BLOQ 2453 1647305 1645867 1250415 11137 1361450 842 1033771 1205 77% 1344881 1547 48310 1569 46172 97% 1974681 488 65768 0 81% 1092818 0 120467 0 BLOQ 393 39.3 29.7 BLOQ 32.4 BLOQ 24.5 BLOQ 32.0 BLOQ 1.2 BLOQ 1.2 47.4 BLOQ 1.7 BLOQ 28.8 BLOQ 2.9 BLOQ 35197 22164 BLOQ BLOQ 103503 0 2J BLOQ 40917 21433 73% 793883 24278 BLOQ BLOQ 41.1 BLOQ 133252 0 82% 1207789 590 3.2 BLOQ 28.6 BLOQ 14415 24428 93% 971952 29767 BLOQ BLOQ 58.5 BLOQ 117% 4119 0 1668270 12836 BLOQ BLOQ 398 BLOQ 283636 15.5 1275839 30.3 ----------- FFOMH) " %. Amount np/mL % Ava: 100.4 5% 105.4 4% 95.4 218% 155% 118% 109% 98% 98% 98% 99% 101% 100% 79% 79% 64% 95% 3153698 70106 43674 38465 32286 32248 3978456 3995743 4030623 4037322 3980654 60157 36204 35701 32683 31853 41060 43918 57596 78063 138044 241208 449202 1072829 2106206 3996955 51755 40561 37317 37240 33624 33353 36645 78922 42341 49479 67159 2785277 45742 2885124 54997 210910$ 46050 2171911 40110 416454 40543 323943 2012855 420485 35793 62% 1285365 34458 417236 35976 383650 36976 478587 57% 80% 1324578 37316 44719 36786 2060664 44151 3179373 77.3 BLOQ BLOQ BLOQ BLOQ BLOQ 994 99.9 100.9 101.0 99$ BLOQ BLOQ BLOQ BLOQ BLOQ 02 0.3 08 1.1 2.5 9.8 247 503 99.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 67.7 BLOQ 70.3 BLOQ $0.4 BLOQ 51J BLOQ 9.1 BLOQ 6.8 47.9 BLOQ 9.1 BLOQ 28.9 BLOQ 9.0 BLOQ 8.5 BLOQ 105 BLOQ 38J BLOQ BLOQ BLOQ 496 BLOQ 78.0 Ava: 1002 5% 105.2 5% 95.1 206% 137% 119% 99% 96% 98% 99% 101% 100% 104% 96% 80% 52% 99% - - Tenn. River Valley Samples Ml CortdwitH 13/170002 Pspalfef}* 1021112 Rlvar Sediments S am pla L o ca tio n s 1 ,2 , and 3. Report E02-0443 Term. River Valley Samples Report EQ2-0443 Tenn. River Valley Samples 1021112 River Sediments Sample Locations 1,2, and 3. in . Vol Sam ple Nam * lu t) Sam ple In fo A re a PFBS (29) O n-C olum n O n-C olum n C o m cto d C orractad fo r Average, Am ount A v a ra g o fo r In). Vol Sam pfoP rop. Stnd O and %CV (n g ta iL ) Ingfm L.) (ngnL) (P flftnL) 20 0443-38044-1 E02-0443-38044-1 ; SL-1; 383859 10.8 11.6 20 0443-38044-2 E02-0443-3M 44-2; SL-1; 383608 10.6 20 0443-3* 044-3 E02-0443-36044-3; SL-1; 4 462034 20 0453-38045-1 E02-0443-38045-1; S t-3 ; 4 325254 13.5 8.9 9.1 20 0453-38045-2 E02-0443-38045-2; SL-3; 1 305101 8.3 20 0453-38045-3 E02-0443-38045-3; SL-3; 4 364688 10.0 20 0463-38045-1 E02-0443-38046-1; SL-2; 4 327380 20 0463-38048-2 E02-0443-3W 46-2; SL-2; 4 232749 8.9 6.2 6.9 20 0463-38046-3 E02-0443-38046-3; SL-2; 4 420079 11.7 PFHS (399) 20 0443-38044-1 E02-0443-3B044-1; S t-1 ; 4 122635 2.7 2.6 20 0443-38044-2 E02-0443-38044-2! SL-1; 4 118901 20 0443-38044-3 E02-0443-38044-3; SL-1; 4 111724 2.6 2.5 20 0453-38045-1 EO2-O443-30O45-1; SL-3; 4 13341 20 0453-38045-2 E02-0443-38045-2; SL-3; 4 11469 20 0453-38045-3 E02-0443-38045-3; SL-3; 4 12125 20 0463-38046-1 E02-0443-38046-1 ; SL-2; 4 173S3 BLO BLOQ BLOQ BLOQ BLOQ BLOQ 20 0463-38046-2 02-0443-3*046-2; SL-2; 4 18434 BLOQ 20 0463-38046-3 E02-0443-38046-3; S t-2 ; 4 25494 BLOQ PFOA (413) 20 0443-38044-1 E02-0443-38044-1 ; SL-1; 1 295590 16.2 14.7 20 0443-38044-2 02-0443-3*044-2; SL-1; 4 280003 14.1 20 0443-38044-3 E02-443-36044-3; SL-1; 4 253343 13.7 20 0453-38045-1 E02-0443-36045-1 ; SL-3; 4 46048 20 0453-38045-2 E02-0443-3604S-2; S t-3 ; 4 60231 BLOQ 2.6 2.6 20 0453-38045-3 E02-0443-38045-3; S t-3 ; 4 54999 BLOQ 20 0463-38046-1 E02-0443-38046-1; SL-2; 1 53375 BLOQ BLOQ 20 0463-38046-2 E02-0443-36046-2; SL-2; 4 35197 BLOQ 20 0463-38046-3 E02-0443-38046-3; SL-2; 4 40917 BLOQ FOSA (498) 20 0443-38044-1 E02-0443-38044-1 ; SL-1; 4 1250415 29.7 28.6 20 0443-38044-2 E02-0443-38044-2: SL-1; 41361450 20 0443-38044-3 E02-0443-3M 44-3; SL-1; 41033771 20 0453-38045-1 E02-0443-38045-1 ; SL-3; 4 48310 20 0453-38045-2 E02-0443-38045-2; SL-3; 4 46172 32.4 24.5 1.2 1.2 1.4 20 0453-38045-3 E02-0443-36045-3; SL-3; 4 65768 20 0463-38046-1 024)443-3*040-1; SL-2; 4 120467 1.7 2.9 2.9 20 0463-38046-2 E02-0443-36046-2; SL-2; 103503 2.5 p r o s (493)20 0463-38046-3 E02-0443-38046-3; SL-2; 4 133252 3.2 20 0443-38044-1 E02-0443-3B044-1; SL-1; 42785277 20 0443-36044-2 E02-0443-38044-2; S t-1 ; 12885124 20 0443-38044-3 E02-0443-38044-3; SL-1; 12109105 67.7 70.3 50.4 62.0 20 0453-38045-1 E02-0443-3804S-1; SL-3; 4 418454 20 0453-30045-2 02-0443-3*043-2; SL-3; 4 323943 9.1 6.8 8.3 20 0453-38045-3 E02-0443-38045-3; SL-3; 4 420485 9.1 20 0463-38046-1 02-0443-36046-1; SL-2; 4 417236 9.0 9.3 20 0463-38046-2 02-0443-38046-2; SL-2; 4 393650 20 0463-38046-3 E02-0443-3B046-3; SL-2; 4 478587 8.5 10.5 5.3 5.3 6.7 4.4 4.1 5.0 4.5 3.1 5.B 1.4 1.3 1.2 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 8.1 7.1 6.9 BLOQ 1.3 BLOQ BLOQ BLOQ BLOQ 14.8 16.2 12.2 0.6 0.6 0.8 1.5 1.3 1.6 33.6 35.1 25.2 4.5 3.4 4.6 4.5 4.2 5.3 529 529 673 443 413 500 438 302 571 136 132 124 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 808 704 665 BLOQ 131 BLOQ BLOQ BLOQ BLOQ 1481 1615 1221 62 60 82 143 124 157 3377 3506 2514 452 341 455 443 415 514 577 83 14% 452 44 10% 437 134 31% 130 6 5% BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 732 66 9% 131 BLOQ BLOQ BLOQ BLOQ BLOQ 1439 200 14% 68 12 18% 141 17 12% 3132 540 17% 416 65 16% 457 51 11% Sam ple W L (g) 38044 20.0 38044-M S 38045 20.01 20.1 3804S-MS 3*04* 20.30 20.4 36046-MS 19.98 fU u u ttr u m p lM m <n m s m o f a m M io tw . O n-C olum n A verage * Average of triplicate * C o rractad fo r In i. V ol. O n-Col am ount * 0.5 C o rractad fo r Sam el Prop On-Col Am ount * 0.5 2 1000 Sample W eight (Ave) "2" is the Final Vol of the Extract (m t) a M C o n M a n tia l 3M Environmental Laboratory 1 2 /1 7 /2 0 0 2 P a tf* 1 3 o f 2> Page 53 of 276 Report E02-0443 Tenn. River Valley Samples E02-0443 Combined Large Mouth Bass Data Table UMS# 42798 42799 42800 42801 42802 42808 42804 42805 42806 42807 42608 42809 42810 42811 42812 42813 42814 42815 PFBS (299) PFHS (399) T fcSA (413) Sample Name Amount ng/mL Amount ng/mL Amount ng/mL Corrected for Smpl Prep __________ (ng/mL) SL-1; LM-1-1 BLOQ BLOQ BLOQ SL-1; LM-1-2 BLOQ SL-1. LM-1-3 BLOQ BLOQ BLOQ BLOQ BLOQ SL-1. LM-2-1 BLOQ BLOQ BLOQ SL-1. LM-2-2 BLOQ SL-1. LM-2-3 BLOQ BLOQ BLOQ BLOQ BLOQ SL-1. LM-3-1 BLOQ SL-1. LM-3-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-1. LM-3-3 BLOQ BLOQ BLOQ SL-1. LM-4-1 SL-1. LM-4-2 SL-1. LM-4-3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 8.4 BLOQ 64.3 SL-1. LM-5-1 SL-1. LM-5-2 SL-1. LM-5-3 SL-1.LM-6-1 SL-1. LM-6-2 SL-1, LM-6-3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-2; LM-1-1 BLOQ BLOQ BLOQ SL-2; LM-1-2 BLOQ BLOQ BLOQ SL-2. LM-1-3 BLOQ BLOQ BLOQ SL-2. LM-2-1 BLOQ SL-2. LM-2-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-2. LM-2-3 BLOQ BLOQ BLOQ SL-2. LM-3-1 BLOQ BLOQ BLOQ SL-2. LM-32 BLOQ BLOQ BLOQ SL-2. LM-3-3 BLOQ BLOQ BLOQ SL-2. LM-4-1 SL-2. LM-4-2 SL-2. LM-4-3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-3; LM-1-1 SL-3; LM-1-2 SL-3. LM-1-3 SL-3. LM-2-1 SL-3. LM-2-2 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-2-3 BLOQ BLOQ BLOQ S L -3 . LM -3 -1 SL-3. LM-3-2 BLOQ BLOQ BLOQ BLOQ BLO Q BLOQ S L -3 . L M -3 -3 B LO Q BLOQ BLOQ SL-3. LM-4-1 SL-3. LM-4-2 SL-3. LM-4-3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-5-1 SL-3. LM-5-2 SL-3. LM-5-3 SL-3. LM-6-1 SL-3. LM-6-2 SL-3. LM-6-3 SL-3. LM-7-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-7-2 BLOQ SL-3. LM-7-3 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. SM-1-1 SL-3. SM-1-2 SL-3. SM-1-3 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ FOSA (498) Amount ng/mL BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ "PFOS (499) Amount ng/mL 18.5 13.0 14.0 83.6 61.4 57.2 73.2 80.8 82.4 68.8 75.7 65.3 46.6 41.5 38.9 69.3 6569..09 Corrected fo r Smpl Prep (ng/mL) 185.5 130.0 139.7 635.5 614.0 571.7 732.1 807.7 824.4 688.4 757.0 653.3 465.5 415.0 388.7 693.2 599.1 660.2 BLOQ BLOQ BLOQ 2.6 BLOQ BLOQ 9.7 11.8 8.5 53.1 54.1 56.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 25.6 96.7 117.6 84.7 530.8 540.9 569.4 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ Ave, Stnd Dev, and %CV 152 29.61 19.5% 607 32.49 5.4% 788 6 249.18 .% 700 52.70 7.5% 423 39.03 9.2% 651 47.78 7.3% 100 16.68 16.7% 547 20.02 3.7% Corrected fo rs a m D le D re n . Amount (ng/mL) * 10 3M Confidential Average (ppb) : Stnd. D.: SL-1, LM PFOA 64.3 NA PFOS 553.4 220 12/17/2002 SL-2, LM PFOS Average (pp"b) : 28.8 Stnd. D.: 251 Pag* 14 of 21 3M Environmental Laboratory Page 54 of 276 Report E02-0443 Tenn. River Valley Samples E02-0443 Combined CatFish Data Table UM S# 42777 42778 42779 42780 42781 42782 42783 42784 42785 42786 42780 42790 42791 42792 42793 42794 42795 42796 42797 PFBS (2991 PFHS (399) S a m p le Nam a Am ount n g /m L Am ount ng/m L. S L-1; C-1-1 S L-1; C -1-2 S L-1. C -1-3 S L-1. C -2-1 S L-1. C -2-2 S L-1. C -2-3 S L-1. C -3-1 S L-1. C -3-2 S L -1. C -3-3 S L -1. C -4-1 S L -1. C -4-2 S L-1. C -4-3 S L-1. C-5-1 S L-1. C -5-2 S L-1. C -5-3 S L-1. C-8-1 S L-1. C -8-2 S L -1. C -6-3 S L-2; C-1-1 S L -2; C -1-2 S L -2. C -1-3 S L-2. C-2-1 S L-2. C -2-2 S L-2. C -2-3 S L-2. C-3-1 S L-2. C -3-2 S L-2. C -3-3 S L-2. C-4-1 S L-2. C -4-2 S L-2. C -1-3 S L-2. C-5-1 S L -2. C -5-2 S L-2. C -5-3 S L-2. C-8-1 S L-2. C -6-2 S L-2. C -6-3 S L-2. C -7-1 S L-2. C -7-2 S L-2. C -7-3 S L-3; C -1-1 S L -3; C -1-2 S L-3. C -1-3 S L-3. C-2-1 S L-3. C -2-2 S L-3. C -2-3 S L-3. C-3-1 S L -3. C -3-2 S L-3. C -3-3 S L-3. C-4-1 S L-3. C -4-2 S L-3. C -4-3 S L -3. C-5-1 S L-3. C -5-2 S L -3. C -5-3 S L-3. C-8-1 S L-3. C -6-2 S L-3. C -8-3 BLOQ blo q BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ PFO A (413) Am ount n g /m L BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ --------------------- F 5 5 X 4 9 5 )--------------------- --------------------- T O S (499)--------------------- Am ount n g /m L 5 .9 5 .3 5 .2 4 .4 4 .2 3 .9 7 .0 7.1 7 .4 3 .9 3 .7 3 .8 9.1 9.1 8 .8 7 .0 6 .9 7 .0 BLOQ BLOQ BLOQ C o rra cta d fo rS m p l P r*p (n g /m L ) 5 8 .7 535 5 2 .0 4 4 .5 4 1 .7 39.1 7 0 .5 7 0 .8 7 3 .8 3 9 .3 3 6 .7 3 8 .2 9 1 .0 9 0 .7 8 7 .5 6 9 .8 69.1 698 A va , S tn d Dev, and %CV 5 4 .7 3 .4 9 6.4% 4 1 .8 2 .6 7 8.4% 71.7 1.85 2.6% 38.1 1.30 3.4% 8 9 .6 1.95 2.2% 6 9 .5 0.41 0.5% Am ount ng /m L 11.2 10.5 10.0 9.8 9 .2 8 .8 16.1 17.9 19.2 17.1 16.2 16.6 8.1 8.0 7.8 5 .9 6 .0 5 .9 BLOQ BLOQ BLOQ C o rra c ta d (o r Sm pl P rep (n g /m L ) 112.1 1 0 4 .7 1 0 0 .3 9 7 .6 9 1 .8 86.1 161.2 179.4 1 9 2 .4 171.5 1 6 1 .9 1 6 5 .8 8 0 .8 8 0 .2 7 7 .5 5 8 .8 5 9 .7 5 8 .7 A va , S tn d Dev, and %CV 106 6 .0 0 5.7% 91.3 5.77 6.3% 178 15.67 8.8% 166 4 .8 2 2.9% 79.5 1.74 22% 59.1 0.57 . 1.0% BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ ' BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1.9 1 8 .8 17.21 1.9 18.7 2 .7 5 1.4 14.0 18.0% BLOQ BLOQ BLOQ BLOQ 1.2 1.1 1.2 BLOQ 11.5 1 1 .5 1 2 .2 11.73 0 .4 4 3.7% BLOQ BLOQ BLOQ BLOQ BLOQ 3.7 3 8 .9 3 7 .4 5 BLOQ BLOQ BLOQ 3.5 4 .0 BLOQ 35.1 4 0 .4 2 .7 2 7.3% BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 2,3 2 .3 2 3 .5 2 3 .2 2 3 .3 2 0 .1 9 0.6% g rre c to d fo r ie m a le nra. A m ount (ng/m L) * 10 ________________S L -1. C____________ POSA PFOS A ve ra g e (p p b ) : 6 0 .9 113.4 S in d . D .: 18.6 4 5 .6 ______su-a, c PFOS A va ra g * (p p b ) : 22.3 S tn d . D .: 10.8 3M Environm ental Laboratory 1 2 /1 7 /2 0 0 2 Pag 1 5 0 /2 1 3M Environmental Laboratory Page 55 of 276 Report E02-0443 Tenn. River Valley Samples Fi*h Tissu* MEat0ri2x-S0p4l4ka3% Recovara P*#*lCrf2t 11 f< sI s III I S I 1 1 l^11lf!n'|lifrll.|oi|5lfiff|P. y -M . ilil iij ii!m tit K 1I1I i\ i1 !! IjlJiI . ! < i< _ 3; i m 7 iS 73 idhisi 3 i |a < 7&3.*33i' " m 5 3 ' i< 1 3M Environmental Laboratory P a n RR n f 07 1021112 Condensed River Sedim ents Data Table Sam ple Name m. D e scription O n- On-CoL C orrected Cone. C orrected fo r C one. C o rrected fo r S p lit o r MS - Endogenous Colum n fo r irtfe c t VoL 1 4 V ol. And in |, VoL, D ilu tio n , and M S *, * C orrected MS % Vol (ng/m L)* (ng/m L) D ilu tio n (ng/m L) Sam ple W t (pg/m L) R ecovery R ecovery PFBS (299) 0443-W B 0443-38044 0443-35044418(3) 0453-38045 04S3*38045483(3) 0463-38046 0483-38046M S(3) 10 20 10 20 10 20 10 W ater Blank SHe#1 SK IM S Site *3 S ite #3 MS Site #2 S ite 2 MS BLOQ 11.6 40.6 9.1 45.8 8.8 39.2 5.8 40.6 4.5 45.9 4.5 39.2 PFHS (399) 0443-W B 0443-38044 0443-3804448S(3] 0453-38045 0453-38045-M S(3} 0463-38046 0483-38046488(3) 10 20 10 20 10 20 10 W ater Blank S ite 81 S ite IM S Site 3 S ite #3 MS Site *2 S ite 82 MS BLOQ 2.6 30.7 BLOQ 37J BLOQ 36.7 BLOQ 1.3 30.7 BLOQ 37.8 BLOQ 38.7 PFOA (413) 0443-W B 0443-38044 0443-3804448S{3) 0453-38045 0453-35045-M S (3) 0463-38046 0463-38046-M S(3) 10 20 10 20 10 20 10 W ater Blank Site *1 S it* IM S Site 3 S ite 3 MS Site 2 S ite 2 MS BLOQ 14.7 38.4 2.6 49.3 BLOQ 41.1 BLOQ 7.3 38.4 1.3 40.3 BLOQ 41.1 FOSA (498) 0443-W B 0443-38044 0443-38044485(3} 0453-38045 0453-35045455(3) 0463-38046 0453-3504645S{3) 10 20 10 20 10 20 10 W ater Blank Ska #1 S ite IM S S ite 3 S ite 3 MS Site 2 S ite 2 MS BLOQ 28.8 32.0 1.4 25.8 2.9 28.6 BLOQ 14.4 32.0 0.7 25.9 1.4 28.8 PFOS (499) 0443-W B 10 W ater Blank 1.1 0443-38044 20 S ite ! 62.8 0443-38044485(3) 10 S ite IM S 61.9 0453*38045 0453-35045445(3) 0463*38046 20 10 20 Site 3 S ite 3 MS Site #2 8.3 .9 9.3 0463-38046-M S(3) 10 S ite 2 MS 30.9 * Are averages except fo r the MS unless noted. BLOQ * Below U n it o f Q uantitation 0453-38045. PFOA is a single po in t 1.1 31.4 51.9 4.2 29.9 4.7 30.9 11.6 81.3 9.1 91.9 8.9 78.3 BLOQ 2.6 61.4 BLOQ 75.6 BLOQ 73.4 BLOQ 14.7 76.7 2.6 80.6 BLOQ B2.1 BLOQ 28.8 63.9 1.4 51.8 2.9 57.3 22 62.8 103.9 6.3 59.8 9.3 61.8 577 4062 452 4591 437 3913 BLOQ 130 3068 BLOQ 3779 BLOQ 3687 BLOQ 732 3834 131 4026 BLOQ 4103 BLOQ 1439 3194 68 2557 141 2863 2182 3132 5193 416 2990 457 3086 81% 92% 75% 70% 83% 69% 81% 75% 73% 59% 77% 81% 52% 62% 78% 84% 52% 57% 35% 50% 54% 104% 60% 62% 41% 51% 52% SampleWt (fl) F in s) E xtra ct Volume (mL) 38044 20.0 38044-M S 20.01 35045 38045-M S 38046 20.1 20.30 20.4 38048-M S 19.98 R syjer senile s w ges ofthe tree weighls. 2.0 O n-C ol. C o rrected fo r In la c L V o l. (n a /m U = Orv-Cdumn * 0.5 The Inject V o l factor is only fo r the regular samples. 0.5 is the I r i Voi factor. Cone. C orrects^) fy r In i. V o l, A nd D ilu tio n (n o /m U - O n-Column ` 0 5 * Final E xtract Vol. C one. C orrected fo r In f. V o l.. D ilu tio n , end Sam ple W t (p o /m L l Otv Column * 0.5 * Final E xtract Vol. * 1000 Sample VM Spite o r M S % R .c o v trv = On-Column MS 50 MS - Endogao m C o rw cte d MS St R ecovery * On-Column MS - O n-C ol Corrected fo r In ie c t V ol. Smol. 50 F u ll Pet o f sam ple w t (g) 38044*1 20.04 36044*2 20.08 38044-3 38011 MS 20.00 20.01 38046-1 20.08 36046-2 20.04 38046*3 20.07 38045-M S 20.30 38046-1 20.13 38046-2 20.98 36046-3 38046-MS 20.21 19.98 A verage (g) 20.0 20.1 20.4 3MCcftfiemitW 12/17/2002 PS0> 17 of21 Tenn. River Valley Samples o73 TO3 Nom) t l E02-0443 River Sediments M atrix Spike % Recoveries PF8S(288) PFHS (3M ) PFOA (413) FOSA (468) PFOS (499) Sample Name Sample Info Amount Triplicate (ng/m L) Average (ng/m L) 0443*30044 Sample Location 1, River Sediments Average 0443-38044-MS(3) Sample Location 1, River Sediments 0453*38045 Sample location 3, River Segments Average 0453*36045*MS(3) Sample Location 3, River Sediment* 0463*38046 Sample Location 2, River Sediments Average 0463*36046-MS(3) Sample Location 2, River Sediment* 40.6 45.9 39.2 5.6 4.5 4.5 Corrected US % Recovery Am ount (ng/m L) T rip lic a te Average (ng/mL) 70 63% 69% 1.3 30.7 BLOQ 37.6 BLOQ 36.7 C orrected MS% Raeoveiy Amount (ngAiiL) Trip&cate Average (ng/m L) 7.3 59% 38.4 13 76% 40.3 BLOQ 73% 41.1 Confected US% Raeoveiy Am ount Triplicate (ng/m t) Average (ng/m L) 14.4 62% 32.0 0.7 76% 25.9 1.4 82% 28.6 Corrected US% Recovery Am ount (n g/m l) T rip lic a te Average (ng/m L) 31.4 35% 51.9 4.2 50% 29.9 4.7 64% 30.9 Corrected US% Recovery 41% 51% 52% Calculated final concentrations oiMSs targeted to 50 ng/mL. Triplicate average* ore from the Condensed RiverSediments Data Tables. Corrected US Recoveries If theT riplicate Average is BLOQ, then * Amount fn a ftn L l 50 ng/m l Final Cone. Spdta ehre: - Amount (notaiL) Trinftate A n trm ina/mLI 50 ng/mL Fired Cone. Spire Amount (ng/m l) has been corrected ter fra injection volume. These calculations are found on the Condensed River Sediments Date Tabta. I Tenn. River Valley Samples SMCer^teMM 12/17/2002 Pag*11 of21 Sequence F ile DO20812 0020612 0020812 0020812 D020812 0020812 0020812 0020812 0020812 DO20812 0020812 0020812 0020812 D020B12 D U D E 0067.D D U D E 0069.D D U D E 0071.D DU D E0073.0 DUDE078.D D U D E 0078.D D U D E 0080.D O UDE0082.0 DUDE00B4.D D U D E 0086.D DU DE0088.D D U D E 0090.D D U D E 0092.D D U D E 0094.D D020812 D020812 D020812 D020812 0020812 D U D E 0127.0 D U D E 0130.D DU 0E0133.D O U D E 0138.D DUDE01S9.D LIM S 38025 38028 38027 38029 38032 38033 38034 38035 38037 38038 38039 38041 38043 38047 38028 38030 38038 38040 38042 D e s c rip tio n SW01 SW O l-O up SW O l-Low FC SO I-Low FB02 SW 03 SW OJ-Dup SWO3-Low SW 02 SW 02-DUP SW02-LOW FSC02-LOW T rip Blank #1 T rip Blank #2 SW Q 1-M ed FSCO I-M ed SW 03-Med SW 02-Med FSC02-M ed In j. V o i. (u L ) 20 20 20 20 20 20 20 20 20 20 20 20 20 20 E02-0443 Combined River Water Data Table PFBS (iM| P #KS (399) ---------1* b k m --------- ---------m m & w -------- ---------PF5TPHS-------- Am ount On- Am ount On- A d ju s te d fo r A d ju s te d fo r Colum n In j. V o i. ng/m L C olum n In j. V o i. ng/m L ng/m L ng/m L A m ount OnA d ju s te d fo r C olum n In j. V o i. ng/m L ng/m L Am ount OnC olum n ng/m L A d ju s te d fo r In j. V oL ng /m L A m ount OnA d ju s te d fo r C o lum n In j. V o i. ng/m L ng/m L 3.0 3.7 3.1 2.7 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1.50 1 S 1.57 1.33 7.7 S i) 12.8 7.9 4 .9 BLOQ 0.3 5 .2 OA 0 .2 5.0 5.1 BLOQ BLOQ 3.86 3.98 6.40 3.83 2.43 0.13 2.60 CL29 0.12 2.48 253 21.3 22.7 28.0 21.8 4 .9 BLOQ BLOQ 5.8 BLOQ BLOQ 5.1 5.4 BLOQ BLOQ 10.56 11.33 13.98 10.92 2.47 2-80 2.54 2 .6 9 i1J.0> 4 .0 1.1 4 .6 BLOQ BLOQ 3.6 BLOQ BLOQ 4 .8 4.9 BLOQ BLOQ 0 .4 8 OAI 2 .0 0 0.58 2 .2 8 1.79 2 .4 2 2.43 18.5 20.8 28.6 20.2 5.2 BLOQ BLOQ 4 .9 BLOQ BLOQ 4 .6 5.5 BLOQ BLOQ 9.25 10.40 13.29 10.09 2.59 2.47 2.28 2.73 2 BLOQ 2 BLOQ 2 BLOQ 2 BLOQ 2 BLOQ 3 9 2 .6 4 2 4 .9 4 0 4 .9 4 1 5 .9 413.1 1963 2124 2024 2078 2068 388.4 4 2 7 .9 398.5 4 0 7 .6 4 1 8 .9 1942 2139 1992 2038 2085 302.1 3 0 0 .2 3 2 4 .5 299.2 3 0 8 .3 1511 1501 1623 1496 1542 361.8 423.7 365.3 358.0 4 2 6 .8 1809 2118 1826 1790 2134 Tenn. River Valley Samples 3M C onfidential 12/17/2002 Page 19 Report E02-0443 Tenn. River Valley Samples E 0 2 -0 4 4 3 Condensed River Water Data Table UM S* 38025 38026 38033 38034 38037 38038 38028 38030 38036 36040 38042 38025 38028 38033 38034 38037 38038 38028 38030 38036 38040 38042 38025 38028 38033 38034 38037 38038 38028 38030 38036 38040 38042 38025 36026 38033 38034 38037 38038 3802S 38030 38036 38040 38042 38025 38026 38033 38034 38037 38038 38028 38030 38036 36040 38042 S a m pt* N am * swot SW O l-Dup SW 03 SW 03-Dup SW 02 SW02-DUP SW 01-Mod FSC01-M ed SW 03-Med SW 02-Med F$C02-M ed SWD1 SW Ot-Oup SW 03 SW03-DUP SW 02 SWOZ-Dup SVV01-Med FSC01-M ed SW 03-Med SW 02-Med FSC02-M ed SW 01 SW 01-Oup SW 03 SW M -D up SW 02 SW 02-Dup SW O l-M ed FS C 01-M ed SW 03-Med SW 02-M ed FS C 02-M ed SW01 SW O l-Dup 8WQ3 SW03-DUP SWQZ SW02-DUP SW D1-M ed FSC01-M ad SW 03-Med SW 02-Med FS C 02-M ed swot SW O l-Dup SW 03 SW 03-Dup SW 02 SW 02-Oup SW 01-Med FSC01-M ed SW 03-Med SW 02-Med FSC02-M ed In). V o i. lu i-) 20 20 20 20 20 20 2 2 2 2 2 20 20 20 20 20 20 2 2 2 2 2 20 20 20 20 20 20 2 2 2 2 2 20 20 20 20 20 20 2 2 2 2 2 20 20 20 20 20 20 2 2 2 2 2 PFBS <299) Am ount On- . . . . . . * . A d justed fo r C olum n . . . . . . . . In n /m U In ). V o l. (n p /m t) 3.0 3.7 <LOQ <10Q <LOQ <LOQ <LQQ <LOQ <LOQ <LOQ <LOQ PFHS (399) 1.50 1.85 Ad) L ilte d fo r S am pln P rp. (p fl/m L ) 75 93 7.7 8.0 <LOQ 0.3 0.4 0.2 382.8 424.8 404.9 415.9 413.1 PFOA (413) 21.3 22.7 <Loa <LOQ <LOQ <LOQ 388.4 427.9 398.5 407.8 416.9 FOSA (498) 1.0 1.0 <LOQ <O Q <tO Q <10Q 302.1 300.2 324.5 299.2 306.3 PFOS (499) 3.86 3.98 0.13 0.20 0.12 1963 2124 2024 2079 2066 10.66 11.33 1942 2139 1992 2038 2085 0.48 0.51 1511 1501 1623 1496 1542 193 199 6.5 9.8 6.2 533 566 24 2e 16.5 20.8 <10Q <LOQ <LOQ *LO Q 361.8 423.7 365.3 356.0 428.8 9.25 10.40 1609 2118 1626 1790 2134 462 520 A verage Ipg/m L) 84 <LOQ <10Q 196 6.5 6.0 550 <LOQ <LOQ 25 <LOQ LOQ 491 <LOQ <LOQ ftfflMitwl tor Ini. Voi ImVmU For 20 u l injections * A m o u n t/2 For 2 uL injection Amount 5 Mta far Sample Prop fpg/mLl (Adjusted fo r InJ. Voi. / 20) * 1000 20 is the factor o f original concentration 1000 is the conversion from ng to pg. S M C o n ffO s n iM 12/17/2002 Pag*20O21 3M Environmental Laboratory Page 60 of 276 Report E02-0443 Tenn. River Valley Samples E02-0443 Tenn. River Valley Samples Summary Table Catfish, Sample Location 1 Catfish, Sample Location 2 Catfish, Sample Location 3 Large Mouth, Sample Location 1 Large Mouth, Sample Location 2 Large Mouth, Sample Location 3 Small Mouth, Sample Location 1 River W ater, Sample Location 1 River W ater, Sample Location 2 River W ater, Sample Location 3 River Sediments, Sample Location 1 River Sediments, Sample Location 2 River Sediments, Sample Location 3 PFBS (n g/m L j LOQ Location Averages PFHS (ng/m L) PFOA (ng/rnL) FOSA (ng/m L) <LOQ <LOQ 60.9 PFOS -- (ng/m L) 113 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 22.3 <LOQ <LOQ 64.3 <LOQ 553 <LOQ <LOQ <LOQ <LOQ 281 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ PFBS (p g /m L ) 84 <LOQ PFHS (pg/m L) 196 <LOQ PFOA (pg/m L) 550 <LOQ FOSA (p g/m L ) 25 <LOQ PFOS (pg/m L) 491 <LOQ 8 <LOQ <LOQ <LOQ <LOQ 7 PFBS PFHS (ng/mL): ; (ng/m L) 576.9 130.5 <LOQ PFOA (ng/m L) 732.4 <LOQ FOSA (n g/m L ) 1439.0 <LOQ PFOS (ng/m L) 3132.3 436.9 <LOQ <LOQ 141.4 457.3 452.0 <LOQ 130.5 68.0 416.2 The Fish Tissue results are calculated by taking the average o<the averages. Please refer to Combined Large Mouth and Catfish Data Tables for averages of samples. 3M Confidential 3M Environmental Laboratory 12/17/2002 Page 21 of 21 Page 61 of 276 Page 62 of 276 3M Environmental Laboratory Solvent Curve: 02003-50 Sequence: 0020626Extractod DUDE0015 DUDE0016 DUDE0017 DUDE0018 DUDE0019 DUDE0020 DUDE0021 DUDE0022 DUOE0023 10 25 15000 250 500 162283 313833 739433 1369316 2487273 5416418 8898793 D020626Extracted CCV Calculation PFBS 5.000 10.000* 25:000 : 15000.0.00000 250.0001 500.000 0.000 0.000 162283"! *313833* 7394331369316 72487273 (5416418: 8898793 4,65 . .-6,9 1^59# 27.51 ilOO 53.25 6.5 . 101.29 1.3 246:68 -1.3 50132 -1.65 -1.65 Q.0:# * 0.07 0.0 0.0 0. 4 M oe m DUDE0065 DUDE0078 DUDE0081 2483358 2451622 2445634 s iS S S lil S 101.11 99.70 99.44 -1.65 -1.65 -1.65 -1.65 -1.65 -1.65 -1.65 sB 100 100 . 100 101% 100% * 99% 0 00 O' 0 0 0 5M Confidential 12/12/2002 BeaciCopVotOrtg'^ r ) /4 S i/ Page 1 of5 Tenn. River Valley Samples Report E02-0443 Page 63 of 276 3M Environmental Laboratory Solvent Curve: 02003-50 Sequence: D020626Extracted D020626Extracted CCV Calculation PFHS i U) 1 8Ul 0 Ig :n0# s8 c 0 | DUDE00781| 3045749 i| 103.33 |1 100 | DUDE00811| 3008932 |I 10 1.9 5 | * s I I 102% | 1__________1 O0 0 0 0 OO s a. a 1t -1.56 -1.56 -1.56 | | | 3M Confidential 12/12/2002 Page2of s Tenn. River Valley Samples Report E02-0443 Page 54 0f 276 3M Environmental Laboratory Solvent Curve: 02003-50 Sequence: D020626Extracted DUDE0015 DUDE0016 DUDE0 0 1 7 0UDE0018 DUDE0019 OUDE0020 OUDE0021 DUDE0022 DUDE0023 10 25 50 100 250 500 94999 182546 422134 765880 1368745 2938643 4830576 D020626Extracted CCV Calculation PFOA 10.000 25.000 15000.0.00000 250.000 500.000 0.000 0.000 94999 162546 422134 765880 1368745 2938643 4830576 10.67 8.7 3 0.0 - 20.38 13.5 .-m~a ffirm 54,23 101.92 8.5 1.9 0.0 - ;:O,0:S' 245.43 - 1,8 0.0 501,83 - 2.21 -Z21 DUOE0065 1459295 DUDE0078 1486918 DUDE0081 1477410 109.37 111.66 110.87 -2.21 -2.21 -2.21 -2.21 -2.21 -2.21 -2.21 100 109% : 100 112%; 100 111% .: 0. 0. 0 . , 0 -y : ' 0 0 0 3M Confidential 12/12/2002 Page 3 of 5 Tenn. River Valley Samples Report E02-0443 3M Environmental Laboratory Solvent Curve: 02003-50 Sequence: P020626Extracted_______________ ________ D020626Extracted C C V C a lc u la tio n POSA _______ ____________________ DUDE0013 OUDE0014 DUDE0015 DUDE0016 DUD0017 DUDE0018 DUDE0019 DUDE0020 DUDE0021 DUDE0022 DUDE0023 1 2.5 5 10 25 50 100 250 500 .1 ..-1: : 1.000"#:. 1 71308 1 136118 1 .. 2.500 - 71308 5.000 136118 . 2.26 -9.4 0.0- 4.65 ' -7.0 1 1 275178 1 . . 10 .0 0 0 ; '>v- -275178: 9.79 . ; * . 1 \ OO 1 693598 1 25.000 693598 25.36 1.4; 0.0 1 1376588 .1 so.ooo; 1376588 ; 51.19 2.4 V"-"- 0.0 ' & j * 1 2665321 '1 100.000 2665321 101.39 1;4 :: .-iO.O-r-.f 1 6144958 1 250.000 6144958 248.44 -0.6 '--o.O ." r i 1 11083740 1 500.000 11083740 500.40. r 0.1 0.0 1 1 0.000 0 -0.36 - - 0.0 ' f 1 1 0.000 0 -0,36 o.o- 1 0 i . 0.00 x S iS S S E DUDE0065 2677359 DUDE0078 2644901 DUDE0081 2687949 101.87 100.58 102.29 -0.36 -0.36 -0.36 -0.36 -0.36 -0.36 -0.36 100100 100 . 102% ' 101% 102% .. 0 .. -o 0 0 0 0 0 Page 65 of 276 3M Confidenza/ 12/12/2002 Report E02-0443 Tenn. River Valley Samples Pag 4 of 5 Report E02-0443 Tenn. River Valley Samples Page 5 of 5 12/12/2002 1 114% I I %ZU'-I IMI P n u ir n n m A n t a l I a h rv ra to rv T$T"* Q o o o o o b | sT" U(VN") pmTC"Nl- fe oi ! 3038326 I| 113.59 i I 3004248 I 112.09 | I 2998564 || 111.84 | ! -12.57 ] -12.57 | -12.57 | -12.57 | 1 in so QDQ Noo8SZao) Uoza>J Page 66 of 276 3M C onfidential Report E02-0443 Attachment C: Sample Chromatograms Tenn. River Valley Samples 3M Environmental Laboratory Page 67 of 276 Report E02-0443 Tenn. River Valley Samples Data Fils: DUDE0056.D Report Date: 27-Aug-2002 13:27 Page 1 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f il e \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D020626Extracted.b\DUDE0056.D Lab Smp Id S L - 1 . L M -1-3 In j Date 2 6 - JUN-2002 2 3 :16 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method Meth Date \2\7E-t s tAaurgg-2e0t0\t2a r1g3e:2t2\c hdeumd \edjru.di e jr .Qi\uDa0n2t 0T6y2p6eE:x tErSaTcDte d .b \D 0 20 6 2 6 e x tra Cal Date 26-JUN-2002 22:00 C a l F i l e : DUDE0049.D A ls b o t t le 43 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 C o n ce n tra tio n Form ula: Amt * DF * Cp n d V ariab le Cpnd V a ria b le L o c a l Compound V a r ia b le Com pounds I t PFBS (2 9 5 ) 20 PFH3 (3 5 9 ) 2 1 PFQA (4 1 3 ) 2 2 POSA (4 9 5 ) 23 EPOS (4 9 9 ) QUANT S IG NASS 29 299 29 399 39 39 413 413 498 498 499 49 C O N C E N T R A T IO N S O N -C O LU M N P IN A L RT EX P R T D L T R T RESPONSE (n g /m L ) (n g /m L ) 3 .3 8 8 3 .1 7 3 .7 2 3 3 .8 0 S 3 .4 0 1 3 .9 7 4 .0 0 3 3 .8 7 3 4 .7 S S 4 .4 4 1 4 .1 7 4 4 .8 0 S 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .9 9 0 3 .9 9 0 4 .7 8 2 4 .7 8 2 4 .1 7 4 4 .1 7 4 0 .0 0 7 -0 .2 0 5 0 .3 4 2 0 .0 1 3 -0 .3 9 1 0 .1 8 4 0 .0 1 3 -0 .1 1 7 -0 .0 0 7 -0 .3 2 1 0.000 0 .4 3 1 11884 2064 1527 9981 4708 4267 15342 5385 85375 984 1903432 1907 5 5 3 .3 3 4 5 5 3 .8 9 5 5 5 3 .7 1 4 8 0 9 .3 5 5 8 0 9 .4 8 8 8 0 9 .4 9 9 8 3 7 .2 5 3 8 3 7 .7 5 0 0 .1 1 5 9 8 1 9 1 7 .3 1 1 3 .9 7 0 2 1 6 8 0 .2 8 5S3 554 554 809 809 809 837 838 0 .1 1 6 1920 1 4 .0 1680 Exist Cc.r/cr Original Initial Data 3M Environmental Laboratory Page 68 of 276 Report E02-0443 Tenn. River Valley Samples Sata F ila : S\Et*targatStargetSchaSdudajr.i\D020626Extracted.b\BtJDE0056.D Paga 2 Io n 399 .0 0 3 .0 2 ,8 2 .6 - 2 . 4 - ___ ? 2 .2 - w n 2 .0 1 .8 - T 1 . 6 - - r*> V0 * W > 1 .4 1 .2 - 1 .0 - 0 ,8 0 .6 - A /V _ ' 3 ,4 0 3 ,6 0 3 , 80 4 .0 0 _____ t U o _ 4.2 0 3M Environmental Laboratory Bract Copy of Origina! . i t . n i IA Iiq .'q j- Initial Date Page 69 of 276 Report E02-0443 Tenn. River Valley Samples Data F ilas \SEt*tars#tStap|;atSchenSdudaJr.iSD020626Extraotad.bSDUDE0086,D 21 PFOft <413) Paga 3 22 FOSA <49B> 23 PFOS <499) Exact Co? r . i 1-r Initial 3M Environmental Laboratory Page 70 of 276 Report E02-0443 Tenn. River Valley Samples Data File: DUDE0058.D Report Date: 27-Aug-2002 13:27 " Page 1 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D 0 2 0 6 2 6 E x tra cte d .b \D U D E 0 0 5 8 .D Lab Smp Id S L - 1 . LM -2-2 I n j Date 26 - JUN-2002 23:38 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\Etstarget\targ et\chem \dudejr . i\D020626Extracted.b\D020626extra Meth Date 27-A ug-2002 1 3 :2 2 d u d e jr .i Quant Type: ESTD Cal Date 26-JUN-2002 22:00 C a l F i l e : DUDE0049.D A ls b o t t le 45 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * CpndVariable Cpnd V a r ia b le L o ca l Compound V a r ia b le Com pounds IB p p b a (2 9 9 ) 20 P F H S ( 3 9 9 ) 21 P F O A ( 4 1 3 ) 23 POSA ( 4 9 23 PPOS (4 9 9 ) QUANT S IG NASS 299 299 299 299 3 99 399 413 413 49B 499 499 C O N C E N T R A T IO N S O N -C O LU M N P IN A L R T EXP R T D LT RT RESPONSE (n g /m L ) (n g /m L ) 3 .3 B B 3 .1 9 0 3 .3 0 4 3 .7 2 3 3 .B 0 5 3 .9 4 5 3 .8 6 7 4 .2 2 9 4 .7 6 2 4 .1 7 4 4 .6 0 5 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .7 9 2 3 .9 9 0 3 .9 9 0 4 .7 6 2 4 .1 7 4 4 .1 7 4 0 .0 0 7 -0 .1 9 1 -0 .0 7 5 0 .3 4 2 0 .0 1 3 -0 .2 4 7 -0 .1 2 3 0 .2 3 9 0.000 0.000 0 .4 3 1 11577 4980 5158 2027 13422 2338 47254 2483 142853 3385486 16466 5 5 3 .3 4 5 5 5 3 .5 8 8 5 5 3 .5 8 1 5 5 3 .6 9 6 8 0 9 .2 6 9 8 0 9 .5 4 8 0 .6 5 5 5 7 8 3 7 .8 9 4 1 .9 6 5 7 6 6 1 .4 0 0 6 1 6 8 0 .3 6 553 554 554 554 809 810 0 .6 5 6 838 1 .9 6 6 1 .4 1680 Bract Copy of Original Ci~n( ) d /'s o 'ji -- Initial Data 3M Environmental Laboratory Page 71 of 276 Report E02-0443 Tenn. River Valley Samples Data Fi Ir: SSEtstargtStarg*tSoh*n\dudejr.iSD020626ExtractedbSDUDE0058,D Pag* 2 20 PFHS <399> 3M Environmental Laboratory Exact Copy ni Origina! - W >X//a / s^- initia] Date Page 72 of 276 Report E02-0443 Tenn. River Valley Samples Data F ila \\EtstargatStarg#t\ch#i\dudaJr*i\D2<>626i;xtractecl.bVDlJD0058*D 21 PFOA <413> 22 FOSA <498> 23 PFOS <499> 3M Environmental Laboratory Exact Copy of Origina! #n< m / t o / a -- InitiaJ Date Page 73 of 276 Report E02-0443 Tenn. River Valley Samples Data File: DUDE0063.D Report Date: 27-Aug-2002 13:27 ' Page 1 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E tsta rg e t\ta rg e t\c h e m \d u d e jr. i\D020626Extracted.b\DUDE0063.D Lab Smp Id S L -1 . LM -3-2 I n j Date 2 7 - JTJN-2002 00:33 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method Meth Date \2\7E-At sutga-r2g0e0t2\t 1a3r:g2e2t \dc huedme j\rd.ui d e jQru.ia\Dnt0 2T0y6p2e6: EExStTraDcte d .b \D 0 20 6 2 6 e x tra C a l Date 2 6 -JUN-2002 22:00 C a l F i l e : DUDE0049.D A ls b o t t le 49 D il Factor 1.00000 In teg rator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tra tio n Form ula: Amt * DF * Cp n d V ariab le Cpnd V a r ia b le L o c a l Compound V a r ia b le Coapounda IB PPBS (2 9 9 ) 2 0 PPHS 139) 21 PPO* (413) 22 POSA (4 9 9 ) 23 PPOS (4 9 9 ) QUANT S IG NASS 299 299 299 299 399 399 399 413 413 499 499 499 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DLT RT RESPONSE (n g /n L ) (ng/m L) 3 .3 8 8 3 .1 7 6 3 .7 2 3 3 .9 1 2 3 .7 9 8 3 .5 4 5 3 .9 7 6 3 .9 9 7 3 .8 5 3 4 .7 6 2 4 .4 1 4 4 .1 7 4 4 .6 0 5 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .9 9 0 3 .9 9 0 4 .7 6 2 4 .7 6 2 4 .1 7 4 4 .1 7 4 0 .0 0 7 0 .2 0 5 0 .3 4 2 0 .4 3 1 0 .0 0 6 -0 .2 6 7 0 .1 8 4 0 .0 0 7 -0 .1 3 7 0 .0 0 0 -0 .3 4 8 0 .0 0 0 0 .4 3 1 11469 2575 1432 378 9750 3036 4357 15533 5478 236312 970 3964776 26340 5 5 3 .3 4 9 5 5 3 .6 7 6 5 5 3 .7 1 8 5 5 3 .7 5 6 8 0 9 .3 6 1 8 0 9 .5 3 0 8 0 9 .4 9 7 8 3 7 .2 4 3 8 3 7 .7 4 5 4 .9 8 1 1 5 1 9 1 7 .3 1 80.7677 1 6 8 0 .0 7 553 554 554 554 809 810 809 837 838 4 .9 8 1920 8 0 .8 1680 Exact Copy nf Origina! -6>W I i j / l i y x- Initial oats 3M Environmental Laboratory Page 74 of 276 Report E02-0443 Tenn. River Valley Samples Data F it ; SSEttarc*tStarst\ch*iSduet*jr.i\D020626ExtracteeUbMHJDE0063.D Pae* 2 20 PFHS <399) 3M Environmental Laboratory Exact Copy of Original X _ ja./ro/2_ initial Oats Page 75 of 276 Report E02-0443 Tenn. River Valley Samples Data F ila : SSEtstar(atStargatSchamSdudaJr,iSD020626Extractd.b\DUDE00S3,D 22 FOSTI <498> 23 PFOS C49 3M Environmental Laboratory Bract Copy o{ Qno!,-;a! initial Date Page 76 of 276 Report E02-0443 Tenn. River Valley Samples Deit File : DUDQ0068.D Report Date: 27-Aug-2002 13:27 page X 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020626Extracted.b\DUDE0068.D Lab Smp Id S L - 1 . LM -4-2 In j Date 27-JUN-2002 01:28 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\Etstarget\target\chem \dudejr.i\D020626Extracted.b\D020626extra Meth Date 27-A ug-2002 1 3 :2 2 d u d e jr .i Quant Type: ESTD Cal Date 2 6 -JUN-2002 22:00 C a l F i l e : DUDE0049.D A ls b o ttle 52 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * Cp ndVariable Cpnd V a r ia b le L o ca l Compound V a r ia b le Compound 1 PPBS (2 9 9 ) 20 PPHS (3 9 9 ) 21 PFOA < 3 ) 22 POSA ( 4 9 ) 23 PP03 (4 9 9 ) QUANT S IO HASS 399 299 299 399 399 399 413 496 499 49 499 CONCENTRATIONS ON-CQLUMN F IN A L RT BXP KT D LT RT RBflPONSB (n g /t*L ) (n g / L ) 3 .3 8 4 3 .1 8 3 3 .7 2 3 3 .7 9 8 3 .3 5 4 3 .5 5 9 3 .9 9 7 4 .7 6 3 4 .1 7 4 3 .8 6 7 4.605 3 .3 4 1 3 .3 4 1 3 .3 4 1 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .9 9 0 4 .7 6 2 4 .1 7 4 4 .3 7 4 4 .1 7 4 0 .0 0 7 -0 .1 9 8 0 .3 4 2 0 .0 0 6 -0 .4 3 4 -0.2 3 3 0 .0 0 7 0 .0 0 0 0 .0 0 0 -0 .3 0 7 0 .4 3 1 51072 2350 1509 49154 415 3064 161661 9787S 3014537 1628 16516 0.83331 5 5 3 .6 8 4 5 5 3 .7 1 5 0 .6 3 7 2 6 8 0 9 .6 9 6 4 0 9 .5 2 9 6 .4 2 6 4 9 0.51796 75.6964 3 6 8 0 .7 1 6 6 0 .3 5 0 .8 3 3 554 554 0 .6 3 7 810 610 6 .4 3 0 .5 1 8 7 5 .7 lc a o 1680 ExactCopy cf Original C i b ___ initial Date F n v im n m n n ta l I Report E02-0443 Tenn. River Valley Samples Data F ila t SSEtatarjatStartatSohanSctuolajr, iSD0202Extraotct.bSDUDE0068.D Page 2 20 PFHS <399) 3M Environmental Laboratory Exact Ccpy fjf Ort.-n?.' & IZnlLtiaLl -. 1 2A cJ oste ^ Page 78 of 276 Report E02-0443 Tenn. River Valley Samples Dta F11S SSEttargetStrgetScheiScludejr,iSD020626Extrctecl.b\DUDE0068.D 21 PFOA (413> Page 3 23 PFOS <499) 3M Environmental Laboratory Exact Copy of Origina) - Jjo / p initial Data Page 79 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0058.D Page 1 Report Date: 09-Dec-2002 13:07 3M Environm ental Lab o rato ry E02-0443 Tenn. R iv e r V a lle y Samples Data f i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D020628.b\DUDE0058.D Lab Smp Id : S L -2 . L M -2 -1 In j Date : 2 9 -JUN-2002 0 2 :15 Operator : mla In st ID: d u d e jr.i Smp In fo : Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr . i\D 020628.b\D 020628.m Meth Date : 09-D ec-2002 1 3 : 0 1 d u d e jr .i Quant Type: ESTD Cal Date : 2 9 -JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o t t le : 28 D il Factor: 1.00000 Integrator : Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 C o n ce n tra tio n Form ula: Amt * DF * CpndVariable Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounds 18 PFBS (2 9 9 ) 20 PFHS (3 9 9 ) 21 PPOA [4 1 3 ) 22 FOSA (4 9 9 ) 23 PFOS (4 9 9 ) QUANT SIG MASS 299 299 299 399 399 413 498 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE (ng/raL) (ng/m L) 3 .3 8 8 3 .1 8 3 3 .7 5 7 3 .8 0 S 3 .5 4 5 4 .0 0 4 4 .7 7 6 4 .1 8 1 4 .8 0 5 3 .3 8 8 3 .3 8 8 3 .3 8 8 3 .7 9 8 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0 .0 0 0 -0 .2 0 5 0 .3 6 9 0 .0 0 7 -0 .2 5 3 0 .0 0 7 0 .0 0 7 0 .0 0 7 0 .4 3 1 15144 2946 2208 10047 540 25432 65904 1348329 20726 5 6 9 .5 2 4 5 6 9 .9 9 6 5 7 0 .0 2 5 7 8 6 .2 2 9 7 8 6 .4 7 7 8 1 5 .2 7 7 1 8 8 5 .8 5 2.56372 1 6 5 9 .6 9 570 570 570 786 786 8 1 5 (M) 1880 2 .5 6 1660 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Origina! Initia! Date 3M Environmental Laboratory Page 80 of 276 Report E02-0443 Sata Filas SSEt*tarjatStaretSchaiSdi(aJr.iSB0Z0628.bSDUDE0058.D Tenn. River Valley Samples Pate 2 3M Environmental Laboratory Exact Copy of Origina! rr<s>{ , x Initia! Date Page 81 of 276 Report E02-0443 Data F ila : S\EtstarttNtar*tSchewSudeJr,iM2O620.bSDUDEOO58,D 21 PFOA <413) Tenn. River Valley Samples 2 2 FOSA <498) 3M Environmental Laboratory ExactCopyor Or'gT:--! initial Ogtg Page 82 of 276 Report E02-0443 Tenu. River Valley Samples Data File: \\Etstarget\target\chem\dudejr .i\D020628.b\DUDE0064.D Page 1 Report Date: 09-Dec-2002 13:07 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D020628.b\DUDE0064.D Lab Smp Id S L -2 . LM -3-2 In j Date 29-JUN-2002 0 3:21 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 8 .b\D020628.m Meth Date 09-Dec-2002 1 3 :0 1 d u d e jr .i Quant Type: ESTD C a l Date 29-JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o ttle 33 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * CpndVariable Cpnd V a r ia b le L o cal Compound V a r ia b le Compounds 18 PFBS (2 9 9 ) 20 PPHS 13991 21 PPOA 1413) 22 POSA (4 9 8 ) 23 PFOS (4 99) QUANT S IO MASS 299 299 299 399 413 498 499 499 CONCENTRATIONS ON-COLUMN PINAL RT EXP RT DLT RT RESPONSE tng/m L) (ng/m L) 3 .4 0 1 3 .2 1 0 3 .7 7 1 3 .8 1 8 4 .0 1 7 4 .7 8 9 4 .1 9 4 4 .6 2 5 3.388 3.388 3.38B 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0 .0 1 3 -0 .1 7 8 0 .3 8 3 0 .0 2 0 0 .0 2 0 0 .0 2 0 0 .0 2 0 0 .4 5 1 22037 3476 3793 17063 38939 98985 1627015 1774 5 6 9 .2 5 7 5 6 9 .9 7 6 5 6 9 .9 6 4 0 .0 8 8 5 0 8 1 4 .5 5 9 0.72476 11.7650 1 6 6 0 .2 8 569 570 570 0 .0 8 8 5 (M) 814 (M) 0 .7 2 5 1 1 .8 1660 QC Flag Legend M - Compound response m anually in te g ra te d . ElcfCo Orinai Opjd 3M Environmental Laboratory Page 83 of 276 Report E02-0443 Data F ile s \\E tstargtS targetScheSducjJr.t\D li2028.b\IXJDC>064.D Tenn. River Valley Samples Pag 2 2 0 PFHS <3991 3M Environmental Laboratory Copy OfOriginal initial u J m U -*-- Cals Page 84 of 276 Report E02-0443 Dta Fi U* SSEt*trt*tStarj*tSchiSdud#jr.iM2O628.bSDUDE00M,D 21 PFOfl <413) Tenn. River Valley Samples 3M Environmental Laboratory Exact Copi; of Qrigna; J r t ( l2 Ju U > ~ Initial Datd Page 85 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0070.D Page l Report Date: 09-Dec-2002 13:07 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f i l e \ \ E t s targ et\targ et\ch em \dudej r . i\D 020628. b\DUDE0070. D Lab Smp Xd S L -2 . LM -4-3 In j Date 2 9 -JUN-2002 04:26 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr. i\D020628.b\D020628.m Meth Date 09-Dec-2002 1 3 :0 1 d u d e jr .i Quant Type: ESTD C a l Date 2 9 -JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o ttle 37 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version : 4 .12 C o n ce n tratio n Form ula: Amt * DF * CpndVariable Cpnd V a ria b le L o ca l Compound V a r ia b le Compounds 18 PFBS (2 9 9 ) 20 PFH5 (3 9 9 ) 21 PFQA (4 1 3 ) 22 FOSA (4 9 8 ) 23 PFOS (4 9 9 ) QUANT S IG MASS 299 299 299 399 413 498 499 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE (n g /m L ) (ng/m L) 3 ,3 8 8 3.1B 3 3 .7 5 7 3 .8 0 5 4 .0 0 3 4 .7 7 6 4 .1 7 4 3 .805 4 .605 3 .3 8 8 3 .3 8 8 3 .3 8 8 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 4 .1 7 4 0 .0 0 0 -0.2 0 5 0 .3 6 9 0 .0 0 7 0 .0 0 6 0 .0 0 7 0 .0 0 0 -0 .3 6 9 0 .4 3 1 13695 1232 1592 10665 23745 120542 2949014 2773 32944 5 6 9 .5 8 0 5 7 0 .0 6 2 5 7 0 .0 4 9 7 8 6 .2 1 3 8 1 5 .3 6 6 1.45583 56.9432 1 6 6 0 .2 5 1 6 5 9 .3 1 570 570 570 7 8 6 (M) 8 1 5 (M) 1 .4 6 5 6 .9 1660 1660 QC F la g Legend M - Compound response m anually in te g ra te d . E::act Copy cf Original :h J L - initia! Date 3M Environmental Laboratory Page 86 of 276 Report E02-0443 Dt FU; SSEtstarget\fcargetSch*\dud*Jr.tSD020628.bM>Ut>E0070.D Tenn. River Valley Samples Page 2 1 8 PFBS <2997 2 0 PFHS <399> 3M Environmental Laboratory Exact Copy of Oriina! ^ yi(- initial Oats Page 87 of 276 Report E02-0443 Dfc F ile s \\EtstartefcStarset\chemSeludejr.i\JM2C628.bSDUDE007'l.D E l PFOft <413> Tenn. River Valley Samples 3M Environmental Laboratory Exact Co,]', f''V -'r .'n - .LAJlo/ oX - initial Oal--. Page 88 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudej r .i\D020628.b\DUDE0076.D Page 1 Report Date: 09-Dec~2002 13:08 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f il e \\E tstarg e t\targ et\ch em \d u d e j r . i\D02062B.b\DUDE0076. D Lab Smp Id S L - 3 . L M -1-3 In j Date 2 9 -JUN-2002 05:32 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D020628.b\D020628.m Meth Date 09-D ec-2002 1 3 :0 1 d u d e jr .i Quant Type: ESTD C a l Date 2 9 -JUN-2002 00:48 C a l F i l e : DUDE0050.D A l s b o t t le 42 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 t C o n ce n tra tio n Formula: Amt * DF * Cp ndVariable Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounds 18 PFBS (2 9 9 ) 20 PFttS (3 9 9 ) 21 PFOA (4 1 3 ) 22 POSA (4 9 8 ) 23 PFOS (4 99) QUANT S IG MASS 299 299 299 399 399 413 498 499 499 C O N C E N T R A T IO N S ON-COLUMN F IN A L RT EXP RT E LT RT RESPONSE (n g /m L ) (ng/m L) 3.388 3 .1 8 9 3 .7 6 4 3 .6 0 5 3 .5 5 9 3 .9 9 6 4 .8 9 9 4 .1 7 4 4 .6 1 1 3 .3 8 8 3 .3 8 8 3 .3 8 8 3 .7 9 8 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0.000 -0 .1 9 9 0 .3 7 6 0 .0 0 7 -0 .2 3 9 - 0.001 0 .1 3 0 0.000 0 .4 3 7 17998 3724 1836 16875 3229 60835 78316 716542 12 921 5 6 9 .4 1 4 5 6 9 .9 6 6 S 7 0 .0 3 9 0.08359 7 8 6 .4 0 7 0 .9 5 2 9 9 0 .0 2 4 3 3 1 6 3 7 .7 1 1 6 5 9 .9 4 569 570 570 0 .0 8 3 6 786 0 .9 5 3 (M) 0 .0 2 4 3 (M) 1640 1660 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Original toittal Data 3M Environmental Laboratory Page 89 of 276 Report E02-0443 D a ta F i l e ; S S E t t a r e t \ t a r K t S c h iS d u d * jr . IS IW 2 0 6 2 8 . to\DUDECi076, D Tenn. River Valley Samples PS 2 3M Environmental Laboratory Exact Copy of Origina! m al o,iif" Page 90 of 276 Report E02-0443 B at F il : SSEtstaretStar*atSch*S<Jueljr.l'J20628,bSD U D E0076.B 21 PFOA (4 1 3 ) Tenn. River Valley Samples 2 2 FOSA <498) 3M Environmental Laboratory Exact Co,;::' nf Oryn Initial Or.ir Page 91 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0089.D Page 1 Report Date: 09-Dec-2002 13:OS 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f i l e \\E tsta rg e t\ta rg e t\ch e m \d u d e jr. i\D020628.b\DUDE0089. D Lab Smp Id S L -3 . LM -4-3 In j Date 2 9 -JUN-2002 07:55 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020S28.b\D020628.m Meth Date 09-Dec-2002 1 3 : 0 1 d u d e jr .i Quant Type: ESTD Cal Date 2 9 -JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o t t le 52 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Formula: Amt * DF * CpndVariable Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounds 18 PFBS (2 3 9 ) 20 PFHS (3 9 9 ) 21 PFOA (4 1 3 ) 22 FOSA (4 9 8 ) 23 PFOS (4 9 9 ) QUAKT S I6 MASS 299 299 299 399 399 413 498 499 499 CONCENTRATIONS ON-COLUMN RT EXP RT DLT RT RESPONSE Ing/m L) F IN A L (ng/m L) 3 .3 9 5 3 .1 9 0 3 .7 5 7 3 .8 0 5 3 .S 5 2 4 .0 0 3 4 .7 6 9 4 .1 7 4 4 .6 0 5 3 .3 0 8 3.388 3 .3 8 8 3 .7 9 8 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0.007 -0 .1 9 8 0 .3 6 9 0 .0 0 7 -0.2 4 6 0 .0 0 6 0 .0 0 0 0 .0 0 0 0 .4 3 1 12936 3732 1991 7393 2451 24746 64726 1029081 18761 5 6 9 .6 1 0 5 6 9 .9 6 6 5 7 0 .0 3 3 7 8 6 .2 9 8 7 8 6 .4 2 7 8 1 5 .3 1 3 1 8 8 5 .8 9 1 6 2 7 ,6 4 1 6 5 9 .7 5 570 570 570 786 786 815 CM) 1880 1630 1660 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy ni Oriin^1__ LaJjLoJ initia! Qat>": 3M Environmental Laboratory Page 92 of 276 Report E 02-0443 Bat F ila r S S tsta reatStarstSchrSduclejr.iM 20628.b\DUBE0039.D Tenn. River Valley Samples Pasa 2 18 PFBS <299) 20 PFHS <399) 3NI Environmental Laboratory Exact Copy of Origins! initial Date Page 93 of 276 Report EQ2-0443 Dat F il* ; SSEtstare*tStarg*tSeh*iSdud*Jr.iSl>0628.bSIIUDE<IO8e.D 21 PFOA C413> Tenn. River Valley Samples 3M Environmental Laboratory Sxs* Copy of Origin ChU initiai Page 94 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0102.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f il e \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020628.b\DUDE0102.D Lab Snip Id S L -3 . LM -7-2 In j Date 2 9 -JUN-2002 10 :18 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Misc In fo Comment Method \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D020628.b\D020628.m Meth Date 09-D ec-2002 1 3 : 0 1 d u d e jr .i Quant Type: ESTD C a l Date 2 9 -JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o t t le 62 D il Factor 1.00000 Integrator Falcon Compound S u b lis t :a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * Cp ndVariable Cpnd V a ria b le L o ca l Compound V a r ia b le Compounds I d PFBS (2 9 9 ) 20 PFH3 (399) 21 PFQA (4 1 3 ) 22 F05A (98) 23 PFOS ( 9 9 ) QUANT S IG NASS 299 299 299 399 413 498 498 499 499 CONCENTRATIONS ON-COLUHN RT EXP RT DLT RT RESPONSE (ng/m LI FINAL* (ng/m L) 3.388 3 .1 7 6 3 .7 5 7 3 .7 9 9 3 .9 9 7 4 .7 6 9 4 .4 4 1 1 .175 4 .5 9 8 3 .3 8 8 3 .3 8 8 3 .3 3 8 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .7 6 9 4 .1 7 4 4 .1 7 4 0 .0 0 0 -0 .2 1 2 0 .3 6 9 0 .0 0 1 0 .0 0 0 0 .0 0 0 -0 .3 2 8 0 .0 0 1 Q .4 2 4 24706 1376 1023 9487 62864 23637 779 906705 29289 5 6 9 .1 5 4 5 7 0 .0 5 7 5 7 0 .0 7 1 7 8 6 .2 4 4 1.06124 1 8 8 7 .2 8 1 8 8 8 .0 5 1 6 3 1 .6 0 1 6 5 9 .4 3 569 570 570 786(H ) 1 .0 6 1690 1890 1630 1660 QC F la g Legend M - Compound response m anually in te g ra te d . -X3C Copy o' Oririn: 3M Environmental Laboratory Page 95 of 276 Report E02-0443 D ata F i l e j SSEts t a r je t S t a r j e t \cherVsdudejr.iSD02<>628,bSDUIiE0102*D Tenn. River Valley Samples P a je 2 3M Environmental Laboratory Exact Copy of Original C i t i ( ... t D Z / c / Crx^ Initial Data Page 96 of 276 Report E02-0443 r.D ata F i l e : N \E ts ta r g e tS ta r s e t\c h e n \c iu d e j iSD020629. bSDUEEOlOZ. D Tenn. River Valley Samples 22 FOSA (4 9 8 ) 23 PFOS (499) 3M Environmental Laboratory Exact Copyo f Origins: _C*yn / a / to / n_ initial oats Page 97 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0104.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f ile \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020628.b\DUDE0104.D Lab Smp Id S L -3 . S M -1-1 In j Date 2 9 -JUN-2002 10:40 Operator mla Inst ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020628.b\D020628.m Meth Date 09-Dec-2002 1 3 : 0 1 d u d e jr .i Quant Type: ESTD Cal Date 29-JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls bottle 65 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 C o n cen tratio n Form ula: Amt * DF * CpndVariable Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounds 18 PFBS (2 9 9 ) 20 PFHS (3 9 9 ) 21 PPQA (9 1 3 ) 22 FOSA (4 9 9 ) 23 PFOS (4 9 9 ) QUANT S IG MASS 299 299 299 399 399 399 413 498 499 499 CONCENTRATIONS OR-COLUMN PINAL RT EXP RT DLT RT RESPONSE Ing/tnL) (ng/roL) 3.368 3 .1 9 0 3 .7 5 7 3 .8 1 2 3.566 4 .1 7 4 3 .9 9 6 4 .7 6 9 4 .1 7 4 4 .6 0 5 3 .3 8 8 3 .3 8 8 3 .3 8 8 3 .798 3 . 79B 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0 .0 0 0 -0 .1 9 8 0 .3 6 9 0 .0 1 4 -0.2 3 2 0 .3 7 6 -0.0 0 1 0 .0 0 0 0 .0 0 0 0 .4 3 1 10955 2138 1256 11252 56B8 975 55673 41082 429027 15813 5 6 9 .6 8 6 5 7 0 .0 2 7 5 7 0 .0 6 2 7 8 6 .1 9 7 7 8 6 .3 4 3 7 8 6 .4 6 6 0.67774 1 8 8 6 .6 9 1 6 4 6 .8 6 1 6 5 9 .8 5 570 570 570 786 786 786 0 . 6 7 8 (M) 1B90(M) 1650 1660 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Original a J iz t- Initial Data 3M Environmental Laboratory Page 98 of 276 Report E02-0443 Tenn. River Valley Samples D ata F H : SSEt*targetStarget\cheiSdudeJr.i''>D 02062e.b\D U D E0104.D SSEtta rg e t StargetSchem SdutleJr. i \D020629.b\DUI0104. D Page 2 18 PFBS <299> 20 PFHS 3 M Environmental Laboratory Exact Copy of Origina; .LKH 2 /2~- Initia! Date Page 99 of 276 Report E02-0443 D ata F ile : S\EtstarstStarjetSohm Sdudejr.i\D )20628.bSD U D E0iO -*.D 21 PFOft (413 ) Tenn. River Valley Samples 3M Environmental Laboratory Etaci Copy of Origins] Lkkx._ Initia! Qai Page 100 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudej r .i\D020628.b\DUDE0105.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f il e \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D020628.b\DUDE0105.D Lab Smp Id S L -3 . S M -1-2 In j Date 2 9 -JUN-2002 1 0 :5 1 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020628.b\D020628.m Meth Date 09-Dec-2002 1 3 : 0 1 d u d e jr .i Quant Type: ESTD C a l Date 2 9 -JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o ttle 66 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * CpndVariable Cpnd V a ria b le L o c a l Compound V a r ia b le Compounds IB PFBS (2 9 9 ) 20 PFHS (3 9 9 ) 21 PPOA (4 1 3 ) 22 FOSA (4 9 8 ) 23 pros (499) QUANT 81Q MASS 299 299 299 399 399 399 413 498 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE (ng/m L) (ng/m L) 3 .3 8 0 3 .1 8 2 3 .7 6 4 3 .8 2 5 3 .5 5 2 4 .1 9 4 3 .9 9 6 4 .7 6 9 4 .1 7 4 4 .6 0 5 3.3SB 3 .3 8 8 3 .3 8 8 3 .7 9 8 3 .7 9 8 3 .7 9 8 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0 .0 0 0 0 .2 0 6 0 .3 7 6 0 .0 2 7 0 .2 4 6 0 .3 9 6 -0 .0 0 1 0 .0 0 0 0 .0 0 0 0 .4 3 1 11225 1896 1126 12780 6122 930 52802 40143 469574 14246 5 6 9 .6 7 6 5 7 0 .0 3 7 5 7 0 .0 6 7 7 8 6 .1 5 8 7 8 6 .3 3 1 7 8 6 .4 6 7 0.52474 1 8 8 6 .7 2 1 6 4 5 .5 8 1 6 5 9 .8 9 570 570 570 786 786 786 0 . 5 2 5 (M) 1 8 9 0 (M) 1640 1660 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy or Grinina! C it a i... 1,2.1(<?/!-- initia! Data 3M Environmental Laboratory Page 101 of 276 Report E02-0443 D ata F ila s SSEtstargetStargetSchenSdudejr,iSD ')20628.bSD U DE010S.D Tenn. River Valley Samples Page 2 i 18 PFBS <299) i 1 _3_._4__0____3__.6__0H in3 .8__0____4__.0__0____4__.2__0_ 3M Environmental Laboratory xa'jt Cu'y of Origina! C U L. L 2 ./( /o i-- Date Page 102 of 276 Report E02-0443 D ata F ila ? SSEttargat\taratSchaSdudajr*iM W 20628*bSDUBE0105*D 21 PFOA <413> Tenn. River Valley Samples Paca 3 22 FOSA <498> 23 PFOS <499> 3M Environmental Laboratory Etct Copy of Origina! -- /2/Va/oi- Wa! Date Page 103 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chera\dudejr.i\D020628.b\DUDE0108.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f il e \\E tsta rg e t\ta rg e t\ch e m \d u d e jr. i\D020628.b\DUDE0108.D Lab Smp Id S L -3 . SM-1 - 3 In j Date 2 9 -JUN-2002 1 1 :2 5 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr. i\D020628.b\D020628.m Meth Date 09-Dec-2002 1 3 : 0 1 d u d e jr .i Quant Type: ESTD C a l Date 29-JUN-2002 00:48 C a l F i l e : DUDE0050.D A ls b o t t le 67 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * CpndVariable Cpnd V a ria b le L o c a l Compound V a r ia b le Compounds 18 PFBS (2 9 9 ) 38 PFHS (3 9 9 ) 21 PFOA (4 1 3 ) 22 POSA (4 9 8 ) 22 PFOS (4 9 9 ) QUANT S IS MASS 299 299 299 399 413 498 499 499 CONCENTRATIONS ON-COLUMN PINAL RT EXP RT ULT RT RESPONSE (ng/m L) (ng/m L) 3 .3 8 8 3 .1 8 3 3 .7 6 4 3 .7 9 8 3 .9 9 6 4 .7 6 2 4 .1 7 4 4 .5 9 8 3 .3 8 8 3 .3 8 8 3 .3 8 8 3.798 3 .9 9 7 4 .7 6 9 4 .1 7 4 4 .1 7 4 0 .0 0 0 >0.205 0 .3 7 6 0.000 -0.0 0 1 -0 .0 0 7 0.000 0.424 16091 2727 1588 13195 54265 443BB 458983 15684 5 6 9 .4 8 8 5 7 0 .0 0 5 5 7 0 .0 4 9 7 8 6 .1 4 7 0.60270 1 8 8 6 .5 7 1 6 4 5 .9 1 1 6 5 9 .8 5 569 S70 570 786 (M) 0 . 6 0 3 fM) 1 8 9 0 (M) 1640 1660 QC Flag Legend M - Compound response m anually in te g ra te d . Exact Copy of Origina! L itU .-- _ initial Date 3M Environmental Laboratory Page 104 of 276 Report E02-0443 Tenn. River Valley Samples D ata F ila s SSEtstargetStarjetSchem Sciuelejr.iM 20fc28.bSBUDE01Q 8.D S S E t ta rs* tS t* rg * tS ch # n S d u d * jr. i SD020628,bSBUIEOXOS. B PS* 2 le PFBS <299) 20 PFHS <399) 3 M Environmental Laboratory Bfact Copy of Orrorn 'niii'ai y,: Page 105 of 276 Report E02-0443 D a ta F i l e t S S E ts ta rg e tS ta r^ e tS c h e a S d u d e jr ,iND020628*bSIMJDEOi08.D 21 PFOA <413) Tenn. River Valley Samples 3M Environmental Laboratory Exact Copy cf Original (j JjlJ - inial Dais Page 106 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0089.D Page 1 Report Date: 27-Aug-2002 10:06 3M Environm ental Laboratory E02-0443, Term. R iv e r V a lle y Samples Data f i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D020629.b\DUDE0089.D Lab Smp Id : S L - 1 . WB-1 In j Date : 0 1 -JUL-2002 04:25 Operator : mla In st ID: d u d e jr.i Smp In f o : Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 9 .b \D 0 2 0 6 2 9 .m Meth Date : 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD C a l Date : 3 0 -JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o t t le : 47 D il Factor: 1.00000 Integrator : Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * Cp n d V ariab le Cpnd V a ria b le L o ca l Compound V a r ia b le Compounds 18 PFBS |23> i 30 PPHS 399) 21 PFOA (4 1 3 ) 1 22 POSA 49) 23 PPOS (4 9 9 ) QUANT S IQ MASS 299 299 299 399 413 498 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE (ng/m L) (ng/m L) 3 .3 1 3 2 .9 4 4 3 .1 8 3 3 .7 9 8 4 .0 0 4 4 .7 7 4 .1 8 8 4 .6 0 5 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .9 9 0 4 .7 5 6 4 .1 6 8 4 .1 6 8 -0 .0 6 8 -0 .4 3 7 -0 .2 1 8 0 .0 0 6 0 .0 1 4 0 .0 2 0 0 .0 2 0 0 .4 3 7 23577 478 2981 8170 10932 7649 96922 22825 1 2 2 3 .2 2 1 2 2 4 .5 4 1 2 2 4 .3 9 0 .1 6 4 3 5 8 1 9 .1 4 4 2 7 4 4 .0 0 1 2 7 4 .9 1 1 2 7 7 .0 9 1220 1220 1220 0 .1 6 4 819 2740 1270 1280 Exact C o i : . : Cnfi'ii- fnitia! Oatf 3M Environmental Laboratory Page 107 of 276 Report E02-0443 Tenn. River Valley Samples Data F ila : SSEtstartet\trtetSch*rr>\dudjr,iSB020629.b\D UD EC >089,D S S E ta ta rte tS ta rfetScheSdudej r . i SD020629.b\IXJDE0089. B Pate 2 18 PFBS <299) 3M Environmental Laboratory Exact Copy ; L m u . L$ 02- initiai Oatt- Page 108 of 276 Report E02-0443 D ata F ile s SSEtstarcetStarcetSch*nSdueIejr.iSD 020629.bSD UD E0089.D 21 PFOA <413> Tenn. River Valley Samples Pa<e 3 22 FOSA <4981 3M Environmental Laboratory Exact Copy or Origina! ts U a J a x - 'nitiai Dato Page 109 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0127,D Page 1 Report Date: 27-Aug-2002 10:07 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 9 .b \D U D E 0 12 7 .D Lab Smp Id S L -2 . WB-1 In j Date 0 1 -JUL-2002 11:2 3 Oprtor mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 03 Mise In fo Comment Method \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 9 .b \D 0 2 0 6 2 9 .m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD Cal Date 30-JDN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o t t le 76 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tra tio n Form ula: Amt * DF * C p n d V ariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounds 18 P7BS ta) 20 PPHS (3 9 9 ) 21 PPOA (4 1 3 ) 22 POSA (4 9 9 ) 23 PF08 (499) QUANT S id MASS 299 299 399 399 413 498 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE (ng/m L) (ng/L> 3 .3 1 9 3 .1 7 3 .7 9 1 3 .9 8 2 3 .9 9 4 .7 7 4 .1 8 8 4 .5 9 8 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .7 9 2 3 .9 9 0 4 .7 5 4 .1 5 8 4 .1 6 8 -0 .0 6 2 -0 .2 0 5 -0 .0 0 1 0 .1 9 0 0 .0 0 0 .0 2 0 Q.03Q 0 .4 3 0 21873 3784 3614 1921 12881 3433 86874 12403 1223 .32 1324 .35 0 .0 3 4 7 8 7 9 7 .1 6 8 8 1 9 .0 3 5 2 7 4 4 .1 8 127S .20 1 2 7 7 .4 0 1220 1220 0 .0 3 4 8 797 819 3740 1280 1280 act Copy of Originai Date 3M Environmental Laboratory Paae 1 l0 o f2 7fi Report E02-0443 D a ta P U : V \E tita rs * t\ta rg e tS c h n i\c !u ti* jp ,i''.D 0 2 0 i,2 9 .b l\B U nE 0i27.D Tenn. River Valley Samples Pa* 2 20 PFHS <399) 3M Environmental Laboratory 4QJL / P r/j /o y ~ nfal P a g e lli o f276 Report E02-0443 D ata F ile s S \E tsta i* g e tS ta r getSchem V kidej r . i \D02O629. bSDUDE0127. D 21 PFOA <413) Tenn. River Valley Samples Page 3 23 PFOS <499) 3M Environmental Laboratory Copy x Origin:' fnffiai Data Paae 112 of 27S Report E02-0443 Tenn. River Valley Samples Data File: DUDE0089.D Report Date: 27-Aug-2002 11:06 Page 1 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 7 0 2 (D20702).b\DUDE0089.D Lab Smp Id : S L -3 . WB-1 In j Date : 03-JUL-2002 07:02 Operator : mla In st ID: d u d e jr.i Smp In fo : Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr .i\D 0 2 0 7 0 2 (D20702).b\D020702.m Meth Date : 2 7 -A u g -2002 1 1 : 0 1 d u d e jr .i Quant Type*. ESTD Cal Date : 03-JL-2002 0 1:2 1 C a l F i l e : DUDE0058.D A l s b o t t le : 72 D il Factor: 1.00000 Integrator: Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 C o n ce n tratio n Formula: Amt * DF * Cp n d V ariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le Cooipounda 1 * PPBS (2 9 9 ) 20 PFH8 (3 9 9 ) 21 PPOA (4 1 3 ) 22 POSA ( 4 9 * ) 23 PFOS (4 9 9 ) QUANT SX6 HASS 299 299 299 399 399 413 498 499 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DLT RT R8SPONSB (ng/m L) (n g /ttL ) 3 .3 2 6 3 .1 8 3 3 .7 7 7 3 .8 2 5 3 .5 4 5 4 .0 1 0 4 .8 0 3 4 .1 9 4 4 .5 9 1 3 .3 8 7 3 .3 8 7 3 .3 8 7 3 .7 9 1 3 .7 9 1 3 .9 8 9 4 .7 4 8 4 .1 4 7 4 .1 4 7 -0 .0 4 1 -0 .2 0 4 0 .3 9 0 0 .0 3 4 -0 .2 4 4 0 .0 2 1 0 .0 5 5 0 .0 2 7 0 .4 3 4 25327 3224 498 7877 937 14443 5535 82445 22937 1 2 1 9 .5 8 1 2 2 0 .4 7 1 2 2 0 .5 8 0 .2 5 8 4 5 0 .1 2 4 2 0 7 9 5 .1 0 3 2 8 5 4 .3 5 1 3 2 3 .0 2 1 3 2 4 .3 4 1220 1220 1220 0 .2 S 8 0 .1 2 4 795(H ) 28S0(N) 1320 1330 QC F la g Legend M - Compound response m anually in te g ra te d . ExactCopy of Origin C in C , initia! Dato 3M Environmental Laboratory Page 113 of 276 Report E02-0443 Tenn. River Valley Samples D ata F ila s W E t ta rg a t\ta rg e tS c h a n S * jd tJ r . iSD020702CS20702). bSDUDE0069. D Page Z 20 PFHS <399) uf iI 3M Environmental Laboratory Exact Copy of Original `initia! nnt0 Page 114 of 276 Report E02-0443 Tenn. River Valley Samples D ata F i l a i S \E ts ta reatStarsatSohamSdudeji-.iSD02070a<D20702>.bSDUDE089.D 21 PF0A <413) 22 FOSA <498) 23 PFOS <499) 3M Environmental Laboratory :acf C'JPV or riginai ^ A sJc i~ Unite] Page 115 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0064.D Page 1 Report Date: 27-Aug-2002 10:05 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D020629.b\DUDEQ064.D Lab Smp Id S L - 1 . C - l - 3 In j Date 30-JUN-2002 2 3 :5 1 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020629.b\D020629.m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD Cal Date 30-JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b ottle 28 D il Factor 1.00000 Integrator Falcon Compound S u b l i s t : a l l . sub Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * Cp n d V ariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le Compound* 19 m a (299) 20 PPHS (3 9 9 ) 21 PPOA (4 1 1 ) 22 POSA ( 4 S I ) 22 PPOJ3 (4 9 9 ) QUANT 8ZG MASS 299 299 299 399 413 49 499 499 499 COHCBHTRATIONS ON-COLUMN PINAL RT SXP RT DEiT RT RBSPONSB |ng/m L) (n g /*L ) 3 .3 8 3 .1 7 3 .7 5 1 3 .7 9 8 3 .9 9 7 4 .7 5 4 .1 7 5 4 .4 3 4 4 .6 0 5 3 .3 8 1 3 .3 6 1 3 .3 8 1 3 .7 9 3 3 .9 9 0 4 .7 5 4 .1 6 9 4 .1 6 4 .1 6 0 .0 0 7 -0 .2 0 5 0 .3 7 0 0 .0 0 6 0 .0 0 7 0 .0 0 0 0 .0 0 7 0 .2 6 0 .4 3 7 12710 3939 2555 7182 23937 140C2S 480864 577 16925 1 2 2 3 . 4 1 2 2 4 .3 4 1 2 3 4 .4 2 0.1362S 0 .3 8 2 5 9 5 .2 0 3 8 8 10.0262 1 2 7 7 .6 0 1 2 7 7 .2 7 1220 1220 1220 0.136(H ) 0 . 3 8 2 <M) 5.20(H ) 1 0 .0 1280 1280 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Or;TM;. LZliJ.o l itim i > lr 3M Environmental Laboratory Page 116 of 276 Report E02-0443 Tenn. River Valley Samples fiat* F l l S\Et.stargatN taret\chen\dudejr.iSD 020629.toSD U IiE<X X .4.D SSEtstar{kStar*t\chea\dudjr.iSD 020629,bSD U D E0064.I) Pas 2 ' 11 11 in J l A l U - l - 1 l_ 1 0 .5 1 .0 1 .5 2 .0 2 .5 3 .0 3 .5 4 .0 H4 .i5n 6 .0 6 ,5 6 .0 6 .5 7 .0 7 .5 8 .0 8 . 5 9 .0 18 PF8S <299> 20 PFHS <399) 3M Environmental Laboratory facr cvyy t-l-./j.p /a ju Jai. Page 117 of 276 Report E02-0443 D ata F i l a i S S E t* ta r Sa tS ta rte tS ch a a S d u d a jr.iS I)0 2 0 6 2 9 .b S D U D E 0 0 6 4 .D 21 PFOft (413> Tenn. River Valley Samples Pas 3 23 PFOS <499) I 1 Ii i 3M Environmental Laboratory BeaciCop teitial.Ck!L_ J .2 jio /0 2 ^ DV- Page 118 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0065.D Page 1 Report Date: 27-Aug-2002 10:05 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D020629.b\DUDE0065.D Lab Smp Id S L - 1 . C - 2 - 1 In j Date 01-JU L-2002 00:02 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E tsta rg e t\targ et\ch em \d u d e j r . i\D020629.b\D020629.m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD C a l Date 3 0 -JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o t t le 29 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tra tio n Form ula: Amt * DF * Cp n d V ariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le Compound I t PPBS (3 9 9 ) 30 FPH8 (3 9 9 ) 31 PPOA (4 1 3 ) 33 F03A (491) 13 PROS (4 9 9 ) QUANT S IS MASS 239 299 299 399 399 399 413 49ft 499 499 499 C O N C E N T R A T IO NS ON-COLUHN PXMAL RT EXP RT DLT RT RESPONSI (ng/m li) (n g /n L ) 3 .3 6 6 3 .1 6 9 3 .7 5 1 3 .7 9 ft 3 .4 0 2 3 .5 3 9 3 .9 9 7 4 .7 6 3 4 .1 7 5 3 .7 9 2 4 .6 0 5 3 .3 6 1 3 .3 6 1 3 .3 6 1 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .9 9 0 4 .7 5 6 4 .1 6 6 4 .1 6 6 4 .1 6 6 0 .0 0 7 -0 .2 1 2 0 .3 7 0 0 .0 0 6 -0 .3 9 0 -0 .2 5 3 0 .0 0 7 0 .0 0 7 0 .0 0 7 -0 .3 7 6 0 .4 3 7 13624 2606 1621 10531 1006 2533 26775 122304 472057 2335 21371 1 2 2 3 .7 9 1 2 2 4 .4 0 1 2 2 4 .4 7 0.23151 7 9 7 .1 9 4 0 .0 0 4 0 4 0.54153 4.44736 9.76111 1 2 7 7 .7 0 1 2 7 7 .1 4 1220 1220 2220 0 .2 3 2 797 0.00404 0 . 5 4 2 (M) 4 .4 5 9 .7 6 1260 1260 QC F la g Legend M - Compound response m anually in te g ra te d . Siaci Cr aitia' Osto 3M Environmental Laboratory Page 119 of 276 Report E02-0443 Tenn. River Valley Samples Data F i U : SSEtt-*tStretSchw iSduc(*Jr,iM K>20629.bSJD E0O 65.D S S E ts ta r f t S t a r gatScham Scluel*jr . i \D 02 062 9. bSDUSEOOS . 0 P*s* z iS PFBS <299> 20 PFHS <399) 3M Environmental Laboratory bcact Copy or O/iginai 1 3 - 1 / o f ai. !nitia! Dais Page 120 of 276 Report E02-0443 Data F ile t \S E tstargetS targetS chen\dudejr.iM )020629.bS D U D E 0065.D 21 PFOfl <413) Tenn. River Valley Samples Page 3 22 FOSA <498) 23 PFOS <499) 3M Environmental Laboratory wX2Ci Cc,jy 'te tu L illo is Initia! oaifj Pane 121 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629,b\DUDE0071.D Page 1 Report Date: 27-Aug-2002 10:05 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f i l e \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0071.D Lab Smp Id SL-1. C-3-2 In j Date 01-JUL-2002 01:08 Operator mia In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 9 .b \D 0 2 0 6 2 9 .m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD C a l Date 3 0 -JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o ttle 34 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . sub Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * Cp ndVariab le Cpnd V a ria b le L o ca l Compound V a r ia b le Compounds IS pres (2**1 ao PPHS {3 9 ) 21 PPOA (4 1 2 ) 33 POSA ) 33 PPOS (4 9 9 ) QUANT SIQ MASS 399 399 299 399 413 499 499 499 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DLT RT RESPONSE (ng/m L) (ng/m L) 3 .3 9 9 3 .1 7 3 .7 5 0 3 .7 9 9 3 .9 9 7 4 .7 6 2 5 .0 0 9 4 .1 7 4 4 .6 0 5 3 .3 9 1 3 .3 9 1 3 .3 9 1 3 .7 9 3 3 .9 9 0 4 .7 5 6 4 .7 5 6 4 .1 6 9 4 .1 6 8 0 .0 0 7 -0 .2 0 5 0 .3 6 9 0 .0 0 6 0 .0 0 7 0 .0 0 6 0 .3 5 3 0 .0 0 6 0 .4 3 7 15305 2054 1430 12499 20299 1959S9 9791 742237 20176 1 2 2 3 .6 9 1 2 2 4 .4 5 1 2 2 4 .4 9 0.29719 0.17934 7.07763 2 7 4 3 .9 2 17.9441 1 2 7 7 .1 7 1220 1220 1220 0 . 2 8 7 (M) 0 . 1 7 8 (M) 7 .0 8 2740 1 7 .9 1280 QC F la g Legend M - Compound response m anually in te g r a te d . exact Copre; CnsKi Enfia! Dote 3M Environmental Laboratory Page 122 of 276 Report E02-0443 D a ta F i l a i S S E ls ta r ta tS t a r ia tS c h a a S d u d a jr .SD020629.1ADUDE0071.D Tenn. River Valley Samples Page 2 18 PFBS (299) 20 PFHS <399) 3M Environmental Laboratory Exact CiJy Dali Page 123 of 276 Report E02-0443 D ata F ila s SSEt*tareatStartatSoham S(fcjdajr.lSD 20629.b\D UD E0071.D Tenn. River Valley Samples Paga 3 2 2 FOSA <498) 23 PFOS <499) 3M Environmental Laboratory Exact OopO.'(jiitici O z L - tU id s L - buia] oata Pape 124 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr .i\D020629.b\DUDE0076.D Page 1 Report Date: 27-Aug-2002 10:06 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D020629.b\DUDE0076.D Lab Smp Id S L - 1 . C -4 -2 In j Date 0 1 -JUL-2002 02:03 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E tsta rg e t\ta rg e t\c h e m \d u d e jr. i\D020629.b\D020629.m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD Cal Date 3 0 -JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o ttle 37 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 C o n ce n tra tio n Form ula: Amt * DF * C p n d V aria b le Cpnd V a r ia b le L o c a l Compound V a r ia b le Compound QUAKT S IG NASS CONCENTRATIONS ON-COLUMN F IN A L RT HXP RT DLT RT RBSFONSB (ng/m L) (n g /n L ) 1ft PPBS (2 9 ) ' 20 PFHS (3 9 9 ) 21 PPOA (4 1 3 ) ! 22 FOSA (4 9 9 ) 23 PPOS (4 9 9 ) 41 i 239 3.381 3.381 0.000 13243 1 2 2 3 .8 1 1220 299 3.224 3.381 -0 .1 5 7 2813 1 2 2 4 .4 0 1220 299 3 .7 5 0 3 . 3B1 0 .3 8 9 29 1224.53 1220 399 3.792 3.792 0.000 5712 0 .0 9 4 4 4 0 . 0 9 4 4 (M) 413 3.997 3.990 0.007 11767 8 1 9 .0 9 7 19(H ) 498 4.789 4.7 5 8 0.013 103527 3.6724S 3 .6 7 499 4.174 4.18ft 0.008 684549 16.187 1 8 .2 499 3.785 4.16S -0 .3 0 3 516 1277.75 1280 499 4.434 4.1 8 ft 0.268 11460 1 2 7 7 .4 3 1280 499 4 . OS 4 . IS 0.4 3 7 30424 1 3 7 7 .IS 1280 QC F la g Legend M - Compound response m anually in te g ra te d . .'Ttlui t 'v.' . t , 7 :it / 1~Pnit'31 3M Environmental Laboratory Page 125 of 276 Report E02-0443 D a ta F i l a : S S E ts ta r e a tS ta r e t\c h * '\d u d * jr . iSD 02062S. b\DUDE0<>76, D I Tenn. River Valley Samples Pate 2 I ") i i i t i I :i 3M Environmental Laboratory I E tac C t;> ..I. , ( d r iL jg . ( f fc Page 126 of 276 Report E02-0443 D ata F il t S S E ttart tStarttSchw >Sdudajr.iSD020629.bSD U D E0076,D 21 PFOft <413) Tenn. River Valley Samples 23 PFOS <499) 3M Environmental Laboratory Exact Cop C m c_ M ai Page 127 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0097.D Page 1 Report Date: 27-Aug-2002 10:06 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr .i\D 0 2 0 6 2 9 .b\DUDE0 097 . D Lab Smp Id S L -2 . C - 1 - 3 In j Date 0 1 -JUL-2002 05:53 Operator mla In s t ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 9 .b\D020629.m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD C a l Date 3 0 -JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o t t le 54 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l . sub Target Version.- 4 .12 C o n ce n tratio n Form ula: Amt * DF * C p n d V ariab le Cpnd V a r ia b le L o c a l Compound V a r ia b le Compounds 18 PPBS 119) 2 0 PFHS (3 9 ) 2 1 PPOA (4 1 3 ) 22 POSA (4 9 ) 23 PPOS ( 4 9 9 ) QUAKT S IO NASS 299 299 299 399 399 399 399 413 498 49 499 COMC8NTRATION8 ON-COLUHN F IN A L BT BXP RT DLT RT RESPONSE (ng/m L) (ng/m L) 3 .3 8 7 3 .1 6 9 3 .7 5 0 3 .7 9 8 3 .3 9 4 3.S5B 3 .9 8 2 3 .9 9 6 4 .7 6 2 4 .1 8 0 4 .6 1 1 3 .381 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .9 9 0 4 .7 5 6 4 .1 8 8 4 .1 6 8 0 .0 0 6 -0 .2 1 2 0 .3 6 9 0 .0 0 6 -0 .3 9 8 -0 .2 3 4 0 .1 9 0 0 .0 0 6 0 .0 0 6 0 .0 1 2 0 .4 4 3 11345 2189 1134 3692 1197 8611 1879 12700 149S4 126853 11361 1 2 2 3 .9 2 1 2 2 4 .4 4 1 2 2 4 .5 0 0 .0 3 7 0 0 7 9 7 .1 8 8 0.17689 7 9 7 .1 6 9 8 1 9 .0 4 5 0.02301 1 2 7 4 .0 2 1 2 7 7 .4 3 1220 1220 1220 0 .0 3 7 0 797 0 .1 7 7 797 19(H ) 0.0230(H ) 1270 1280 QC F la g Legend M - Compound response m anually in te g r a te d . Exact Cop; C h U IQ -M oJ gl*. irifja 3M Environmental Laboratory Page 128 of 276 Report E02-0443 Tenn. River Valley Samples D a ta F i l e t S S E tsta rg t.S ta rg e tS c h ii\* K t* ljr,iM )02062?.bSDUDEC>097.D S S E t b arg * tS targ etS o h * n S d u d eJr. iSB02029.bSDUBE0097.D Pag* 2 18 PFBS <299> 20 PFHS <399> 3M Environmental Laboratory --'l.'vt Oi.i!".' * ' p .C .... ! ,, x / f j 1U Page 129 of 276 Report E02-0443 S ata F ila : SSEt*tartatStartat\chanSdudejr.iSD 020629.bSD O D E0097.D 21 PFOA <4135 Tenn. River Valley Samples Paca 3 22 FOSA <4985 23 PFOS <4995 3M Environmental Laboratory Exact Copy of Original imm Osta Page 130 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0105.D Page 1 Report Date: 27-Aug-2002 10:06 3M Environm ental Laboratory E02-Q443, Tenn. R iv e r V a lle y Samples Data f i l e \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 6 2 9 .b \D U D E 0 10 5 .D Lab Smp Id S L -2 . C -3 -2 In j Date 01-JU L-2002 0 7 :2 1 Operator mla In st ID: d u d ejr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020629.b\D020629.m Meth Date 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD Cal Date 30-JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o t t le 60 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Formula: Amt * DF * p n d V ariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le uo Coapounda 18 PPBS (3 9 ) (399) 21 PPOA (4 1 3 ) 22 TOSA (4 9 ) 23 p r o s <4> QUANT S1G NASS 299 299 299 399 399 399 413 498 498 499 49 499 C O N C E N T R A T IO N S ON-COLUMN P IN A L RT EXP RT DLT RT RESPONSE (ng/.L ) (ng/aL) 3 .3 8 8 3 .1 8 2 3.7S 3 .7 9 8 3 .5 4 5 3 .9 7 8 3 .9 9 8 4.7S 8 4 .4 2 7 4 .1 7 4 4 .4 3 4 4 .4 0 8 3 .3 8 1 3 .3 8 1 3 .3 8 1 3 .7 9 2 3 .7 9 2 3 .7 9 2 3 .9 9 0 4 .7 5 8 4 .7 5 8 4 .1 8 8 4 .1 6 8 4 .1 6 8 0 .0 0 7 -0 .2 1 9 0 .3 8 9 0 .0 0 6 0 .2 4 7 0 .1 8 4 0 .0 0 6 0 .0 1 3 -0 .3 2 9 0 .0 0 6 0 .2 6 6 0 .4 3 7 9238 1696 2638 3298 4903 3370 8771 20531 1466 178402 85700 19S33 1 2 2 4 .0 4 1 2 2 4 .4 7 1 2 2 4 .4 1 0.02579 0.07143 0.02784 8 1 9 .2 6 4 0.25210 2 7 4 4 .2 6 0.98662 1 2 7 5 .2 4 1 2 7 7 .1 9 1220 1220 1220 0 .0 2 5 8 0 .0 7 1 4 0 .0 2 7 8 19(H ) 0 .2 5 2 2740 0 .9 8 7 1280 1280 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Orlr'rt- fniaJ oat,- 3M Environmental Laboratory Page 131 of 276 Report E02-0443 H a t F i l * : S S E ts t rt* tS t r * * t\c h * m S d u d j r . i\D 0 2 0 6 2 9 .bSDUBEOlOS. D Tenn. River Valley Samples Pg 2 20 PFHS <399) 3M Environmental Laboratory Copy . : , Mal oau Page 132 of 276 Report E02-0443 S s ta F i l a : S S E t ta r j* t\t r j;e t\o h e * i\d u d jr . i\D 020629.b\DU IlE0105.D 21 PFOA (4 1 3 ) Tenn. R iv e r V a lle y Samples pa( 3 22 POSA (4 9 8 ) 3M Environmental Laboratory actCp tiiO r Page 133 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629,b\DUDE0117.D Page 1 Report Date: 27-Aug-2002 10:07 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f il e : \\E tsta rg e t\ta rg e t\ch e m \dudejr.i\D020629.b\DUDE0117.D Lab Smp Id : S L -2 . C - 6 - 1 In j Date : 0 1 -JUL-2002 09:33 Operator : mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo : Comment : Method : \ \E t s ta r g e t\ta r g e t\c h e m \d u d e jr . i\D 0 2 0629.b\D02 062 9 .m Meth Date : 27-A ug-2002 09:59 d u d e jr .i Quant Type: ESTD Cal Date : 30-JUN-2002 22:46 C a l F i l e : DUDE0058.D A ls b o t t le : 69 D il Factor: 1.00000 Integrator : Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 C o n ce n tratio n Form ula: Amt * DF * Cp n d V ariab le Cpnd V a ria b le L o ca l Compound V a r ia b le Compounds 18 PPBS (2 9 9 ) 20 PFHS (3 9 9 ) 21 PPOA (4 1 3 ) 22 POSA (4 9 9 ) 23 pros (499) quant s iq HASS 299 299 299 399 413 49 499 499 COHCBHTRATIONS ON-COLUMN PINAL RT EXP RT DLT RT RBSPONSB {n g /*D (nsr/mL) 3 .3 1 8 3 ,1 7 6 3 .7 5 0 3 .7 9 6 3 .9 9 6 4 .7 6 9 4 .1 6 1 4 . #05 3 .3 8 1 3 .3 6 1 3 .3 8 1 3 .7 9 2 3 .9 9 0 4 .7 5 6 4 .1 6 8 4 .1 6 ft 0 .0 0 7 -0 .2 0 5 0 .3 6 9 0 .0 0 6 0 .0 0 6 0 .0 1 3 0 .0 1 3 0 .4 3 7 473 1416 545 2433 6100 22417 2212 63 22665 1 2 2 4 .0 2 1 2 2 4 .4 6 1 2 2 4 .5 3 0.00120 6 1 9 .3 0 2 0.33013 2.26035 1 3 7 7 .1 0 1220 1220 1220 0 .0 0 1 2 0 (N) 619(H ) 0 .3 3 0 2 .2 6 1290 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Orfani: initia' 3M Environmental Laboratory Page 134 of 276 Report E02-0443 D ata F ila s SSEttargetStargetScheiSdude4r,i\D 020i29.b\BU D E01.17.B Tenn. River Valley Samples Page 2 IS PFBS <299) 20 PFHS <399) 3M Environmental Laboratory Exact Copy of Origina! te iU y b jOa(v Page 135 of 276 Report E02-0443 D ata F i l e : \SEtstareet\targtScheSelu<*eJr.i\D020629.k>SDUDEC>117,D 21 PFOA <413) Tenn. River Valley Samples Psge 3 22 FOSfl <498) 23 PFOS (499 ) 3M Environmental Laboratory te t- ia d * '* - nit'a! Hpti Page 136 of 276 Report E02-Q443 Tenn. River Valley Samples Data File: DUDE0066.D Report Date: 27-Aug-2002 11:05 Page 1 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f il e \ \E t Starget\targe t\chem\dudej r.i\D020702{D20702).b\DUDE0066.D Lab Snip Id S L -3 . C -2 -2 In j Date 03-JUL-2002 02:49 Operator mla In st ID: d u d e jr.i Smp In fo Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020702(D20702).b\D020702.m Meth Date 27-A ug-2002 1 1 : 0 1 d u d e jr .i Quant Type: ESTD Cal Date 0 3-JUL-2002 0 1:2 1 C a l F i l e : DUDE0058.D A ls b o t t le 55 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 C o n ce n tratio n Formula: Amt * DF * Cp ndVariable Cpnd V a ria b le L o ca l Compound V a r ia b le Compound 1ft PFBS (J 9 9 ) 30 PPH5 <399) 31 PPOA (4 1 3 ) 33 POSA (4 9 9 ) 33 PROS (4 9 9 ) QUANT SIO HASS 39 299 399 399 413 49B 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT BXP RT DLT RT RBSPONSB (n g / L ) < n g /m L ) 3 .3 9 5 3 .1 9 3 3 .7 5 7 3 .1 1 9 4 .0 0 3 4 .8 0 3 4 .1 8 1 4 .5 9 1 3 .3 8 7 3 .3 8 7 3 .3 8 7 3 .7 9 1 3 .9 8 9 4 .7 4 8 4 .1 0 7 4 .1 0 7 0 .0 0 8 **0.304 0 .3 7 0 0 .0 3 8 0 .0 1 4 0.055 0.014 0 .4 3 4 14873 3040 3330 5059 22949 33838 193814 33954 1 2 3 0 .0 0 1 2 2 0 .4 8 1 3 2 0 .5 1 0.30394 0.27074 0.43108 1.14537 1 3 3 4 .2 2 1220 1220 1220 0 . 2 0 4 (N) 0 . 2 7 1 W) 0 .4 3 1 1 .1 4 1320 QC F la g Legend M - Compound response m anually in te g ra te d . ^ act Copy of origina] 3M Environmental Laboratory Page 137 of 276 Report E02-0443 Tenn. River Valley Samples 18 PFBS <299> 3M Environmental Laboratory Exact Copy of Originai !2 h / o initia! Oats Page 138 of 276 Report E02-0443 Tenn. River Valley Samples S ata F i l a : W E ts t r * e t\t a r e a t\ c h e n \d u d e jr , i \D020702<D20702),b\DUDE0066. D 2 1 PFOA <413> 2 2 FOSA < 4 9 8 ) 23 PFOS <499) 3M Environmental Laboratory Bfact Copy of Original IS rJ lA p 1- `nife) fe r Page 139 of 276 Report E02-0443 Tenn. River Valley Samples Data File: DUDE0076.D Report Date: 27-Aug-2002 11:06 Page 1 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 7 0 2 (D20702),b\DUDE0O76.D Lab Smp Id : S L -3 . C -4 -2 In j Date : 0 3 -JUL-2002 04:39 Operator : mla In st ID: d u d e jr.i Smp In fo : Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo : Comment : Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr. i\D020702(D20702).b\D020702.m Meth Date : 27-A ug-2002 1 1 : 0 1 d u d e jr .i Quant Type: ESTD Cal Date 0 3-JUL-2002 0 1:2 1 C a l F i l e : DUDE0058.D A ls b o t t le : 62 D il Factor: 1.00000 In teg rato r: Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 C o n ce n tratio n Form ula: Amt * DF * Cp ndVariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounds 1 PPBS ( 2 9 20 PPHS (3 9 9 ) 21 PFOA (4 X 3 ) 22 POSA ( 4 9 9 ) 23 PROS (4 9 9 ) QUANT SXO HASS 39 29 299 399 399 399 413 498 499 49 49 CONCENTRATIONS ON-COLUMN FINAL RT HXP RT DLT RT RESPONSE (ng/m L) (n g /m L ) 3 .3 9 4 3 .1 8 2 3 .7 7 0 3 .8 2 5 3 .5 7 2 4 .0 1 0 4 .0 1 0 4 .7 5 9 4 .1 8 7 3 .8 1 1 4 .5 9 1 3 .3 8 7 3 .3 8 7 3.3B 7 3 .7 9 1 3 .7 9 1 3 .7 9 1 3 .9 8 9 4 .7 4 8 4 .1 6 7 4 .1 6 7 4 .1 6 7 0 .0 0 7 -0 .2 0 5 0 .3 8 3 0 .0 3 4 -0 .2 1 9 0 .2 1 9 0 .0 2 1 0 .0 2 1 0 .0 2 0 -0.3S C 0 .4 2 4 21375 2087 1284 3965 3286 3291 9130 20987 307947 1347 20381 1 2 1 9 .7 4 1 2 2 0 .5 2 1 2 2 0 .5 5 0.18277 0 .1 6 9 6 4 0.16973 7 9 5 .3 1 0 0.3S23S 3.50667 1 3 2 4 .6 9 1 3 2 4 .2 9 1220 1220 1220 0.183 0.170 0 .1 7 0 795 (M) 0 .3 5 2 3 .5 1 1320 1320 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copy of Original C k n i... /9 -J j^ L o 'i- 3M Environmental Laboratory Page 140 of 276 Report E02-0443 Tenn. River Valley Samples S a t* F i l t S \E t t a r g t\ta rg e tS c h e n S d u d j r , iSD020702<D20702).bSDUBE0076.D pe* 2 20 PFHS < 3 > 3M Environmental Laboratoiy Exact Copy of Original {nitiaJ oai,; Page 141 of 276 Report E02-0443 Tenn. River Valley Samples D ata F ila s S S E ttarj#tStarcatSchaKi\dudajr.iM )e20702<D 20702>.bSBllD E0076.D 21 PFDA <413) pas, 3 23 PFOS <49S) 3M Environmental Laboratory ' Copy of Origina! Date Page 142 of 276 Report E02-0443 Tenn. River Valley Samples Data F i l e : DUDE0083.D Report Date: 27-Aug-2002 11:0 6 Page 1 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 7 0 2 (D20702).b\DUDE0083 D Lab Smp Id : S L - 3 . C - 6 - 1 In j Date : 03-JUL-2002 05:56 Operator : mla In st ID: d u d e jr.i Smp In fo : Tenn. R iv e r V a lle y F is h . P r e p -17 Jun 02. CMC/MLA. 20 Jun 02 Mise In fo : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr .i\D 0 2 0 7 0 2 (D20702).b\D020702.m Meth Date : 27-A ug-2002 1 1 : 0 1 d u d e jr .i Quant Type: ESTD Cal Date : 03-JUL-2002 0 1:2 1 C a l F i l e : DDDE0058.D A ls b o ttle : 68 D ii Factor: 1.00000 In teg rator: Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 C o n ce n tratio n Formula: Amt * DF * Cp ndVariab le Cpnd V a r ia b le L o ca l Compound V a r ia b le Compounde la a K B sa a a a i 18 PPBS ( a s s i 20 PPHa <399) 21 PPOA (9 1 3 ) 22 POSA (9 9 8 ) 23 PPOS <999) QUANT S IO MASS aia a 299 399 413 498 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE (n g /n L ) (ng/niL> Compound N o t D e te c te d . Compound M ot D e te c te d . Compound N o t D e te c te d . Compound N o t D e te c te d . Compound N o t D e te c te d . 3M Environmental Laboratory !?xact Copy of Original i'tllC.-. iZU sl&j- Dsto Page 143 of 276 Report E02-0443 Tenn. River Valley Samples Dat F i l * ; S \E tstar*tS t*r*tS chem S dud*jr.iS l20702(D 20702).bM X JD E 0083.D Pa* 2 20 PFHS <399) <Undt*et*d> 3M Environmental Laboratory Exact Copy of Original D a n a 1 A j4 rs4 0 7 C Report E02-0443 Tenn. River Valley Samples D ata F ile s SSEt*tartlStaretSchnSdudejp.i\D020702<D 20702>.bSDU BE0083.D 21 PFOA <413) <U n d e te c te d ) Pace 3 22 FOSA <498) <U n d e te c te d ) 2 3 PFOS < 4 9 9 ) <U n d e te c te d ) 3M Environmental Laboratory .'. 'ci. Copy of Original C J L- a ///s /o 3- '.nitia! oats Page 145 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chetn\dudejr.i\D02082A.b\DUDE0065.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environm ental Laboratory E02-0443 Tenn. R iv e r V a lle y Samples Data f ile \\Etstarget\target\chem \dudejr.i\D020812A.b\DUDE0065.D Lab Smp Id Water B la n k -l In j Date 1 2 -AUG-2002 2 3 :1 1 Operator mla In st ID: d u d e jr.i Smp In fo E02-0443 Water B lan k Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Misc In fo Comment Method \\Etstarget\target\chem \dudejr.i\D0208l2A .b\D020812A .m Meth Date 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD C a l Date 1 2 -AUG-2002 1 6 :1 3 C a l F i l e : DUDE0027.D A ls b o ttle 20 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compounds ..... a .a X PFBS (2 9 9 ) a PFHS (3 9 9 ) a PPOA (9 1 3 ) 4 POSA (9 9 9 ) 5 PROS (9 9 9 ) QUAKT S IG HASS BS* 299 299 299 299 299 413 498 499 RT 3 .3 S 3 3 .2 0 9 4 .2 0 1 3 .8 0 4 3 .5 6 5 4 .0 1 4 4 .8 0 9 4 .2 0 1 1Btt 1 1 B R BXF RT 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .791 3 .7 9 1 3.9B 2 4 .7 6 8 4 .1 4 0 R R > R RI R i >B 1 N R R R DLT RT R8SPOKSS -0 .0 4 1 '0 .1 8 5 0 .8 0 7 0 .0 1 3 -0 .2 2 6 0 .0 3 4 0 .0 4 1 0 .0 4 1 29174 5546 1904 5192 1012 9179 3390 34010 CONCBWTRAT20H8 ON-COLUWN 72NAU (ng/m L) (ng/m L) .* . 0 .5 4 1 4 1 5 0 3 .6 6 0 5 0 3 .7 8 8 0 .5 4 1 504 504 0.15468 0.02703 0.04921 0 .1 0 5 4 9 0 .1 5 5 0.0270 0.0492 0 .1 0 5 0.16998 0 .1 7 0 3M Environmental Laboratory traci Ccuy er Ongina: i.A / r o i ox - Initial Date Page 146 of 276 Report E02-0443 Tenn. River Valley Samples 1 PFBS <299 3M Environmental Laboratory Exact Copy & Ltnltia! Dato Page 147 of 276 Report E02-0443 D ata F ila s S S E tita rte tS ta rte tS c h a n S d u d e J r. ISD020812A. b\DUDE0065,D 3 PFOA <4135 Tenn. River Valley Samples B PFOS < 4 9 9 ) 3M Environmental Laboratory Exact Copy (if Or;c:;i initia! bai Page 148 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0066.D Page l Report Date: 27-Aug-2002 14:11 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e : \\E ts ta r g e t \t a r g e t \ch em \d u d ejr.i\D020812A.b\DUDE0066.D Lab Smp I d : Water B la n k -2 In j Date : 12-AUG-2002 23:22 Operator : mla In st ID: d u d e jr.i Smp In f o : E02-0443 Water B lan k Water Sam ples; non-GLP; 7 / 1 7 / 0 2 ; OK Misc Info : Comment : Method : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 8 l2 A .b \D 0 2 0 8 12 A .m Meth Date : 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date : 12-AUG-2002 16 :13 C a l F i l e : DDDE0027.D A ls b o ttle : 21 D il Facto r: 1.00000 In teg rato r: Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compound 1 PFBS (2 ) 2 PPHS (3 9 9 ) 3 PFOA ( 4 1 3 ) 4 POSA (4 9 B ) 5 PPOS ( 4 9 9 ) QUANT SIQ HASS 299 299 299 299 399 413 413 498 499 CONCENTRATIONS ON-COLUMN P IN A L RT EXP RT D LT RT RESPONSE (n g / L ) < n g / L ) 3 .3 5 4 3 .2 1 0 3 .7 4 3 4 .1 9 5 3 .8 0 5 4 .0 1 0 4 .3 5 9 4 .8 1 0 4 .2 0 1 3 .3 9 4 3 .3 9 4 3 .394 3 .3 9 4 3 .7 9 1 3 .9 8 2 3 .982 4 .7 6 8 4 .1 6 0 -0 .0 4 0 -0 .1 8 4 0 .3 4 9 0 .8 0 1 0 .0 1 4 0 .0 2 8 0 .3 7 7 0 .0 4 2 0 .0 4 1 S4510 10619 1176 3650 4219 11746 1069 3371 33507 1 .4 3 3 7 6 5 0 3 .4 8 2 5 0 3 .8 1 3 5 0 3 .7 2 7 0.12496 0.21476 4 0 1 .9 7 6 0.10487 0 .1 S 7 2 0 1 .4 3 503 504 504 0 .1 2 5 0 .2 1 5 402 0 .1 0 5 0 .1 5 7 Exact Copy of Grig-. L y t u ... J U d o " in itia ! Date 3M Environmental Laboratory Page 149 of 276 Report E02-0443 Bfca F i l t \S E ts ta rj tS ta rg tS c h i*S e tu d jr.iS B 0 2 0 8 1 2 a .b \B U B E 0 0 6 6 .B Term. River Valley Samples Pa* Z 2 PFHS <3991 3 M Environmental Laboratory Page 150 of 276 Report E 02-0443 D ata F ila r S \E t* ta rg t\ta r ta t\c h a i\d u d a jr - ,iSD020812fi.bSDUI)E0066.D 3 PFOA < 4 1 3 ) Tenn, River Valley Samples 4 FOSA < 4 9 8 ) 8 PFOS < 4 9 9 ) 3M Environmental Laboratory actCopi.-iv o -.;..1 Mi/ai Page 151 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0076.D Page l Report Date: 27-Aug-2002 14:11 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E tstarg et\targ et\ch em \d u d ej r . i\D020812A.b\DUDE0076.D Lab Smp Id 38032 In j Date 1 3 -AUG-2002 0 1 :1 2 Operator mla In st ID: d u d e jr.i Smp In fo E 0 2 -0443-38032; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Misc Info Comment Method \\Etstarget\target\chem \dudejr.i\D 020812A.b\D 020812A.m Meth Date 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD C al Date 1 2 -AUG-2002 1 6 :1 3 C a l F i l e : DUDE0027.D A ls b o t t le 26 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 Compounds 1 m s (399) 3 PPHS O) 3 PPOA (4 1 3 ) 4 POSA (4 9 1 ) S PROS (4 9 9 ) QUANT 3 IO NASS 399 399 399 399 399 399 399 4X3 499 499 CONCENTRATIONS RT EXP RT DLT RT RESPONSE ON-COLUMN (ng/m W PINAL (ng/m L) 3 .4 0 1 2 .5 4 0 3 .203 3 . BIB 4 .0 4 4 4 .2 1 5 3 . BOS 4.003 4.7B 9 4 .1 9 1 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .7 9 1 3 >962 4 .7 6 8 4 .1 6 0 0 .0 0 7 -0 .9 5 4 " 0.191 0 .4 2 4 0 .6 5 0 0.921 0.014 0 .0 2 1 0 .0 2 1 0 .0 3 1 ' 19361 147211 1966 2962 756 777 157296 94190 139473 190157 0.19664 4.72622 5 0 3 .7 9 6 5 0 3 .7 5 1 S 0 3 .9 2 9 5 0 3 .9 2 7 4.95909 4.94452 4.56920 5.19991 0 .1 9 7 4 .7 3 504 504 504 504 4 .9 6 4 .9 4 4 .5 7 5 .1 9 3M Environmental Laboratory Exact Cop; d n ( LiiJ(pi.'1--' initia! DaF- Page 152 of 276 Report E02-0443 S a ta F i l e t S S E ts ta r(a t\ta rs e tS c h a n S d u d a J i,` .iS B 020812A ,bM U S E 0076.D Tenn. River Valley Samples Paja 2 i j 3M Environmental Laboratory Exact Copy of Original .U n L , initial Date Page 153 of 276 Report E02-0443 Bata F il ! S \E ts ta rf tS ta rg *tS o h **\d u d *jr,iS D 0 2 0 8 i2 A .b \D U D E 0 0 7 6 ,D 3 PFOA <413) Tenn. River Valley Samples Pag* 3 4 FOSA < 4 9 9 ) 0 PFOS <499) 3M Environmental Laboratory &aciCopyo..: o,7>;,:,i! C` L C .J cV o^ "fa '- w Page 154 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0073.D Page 1 Report Date: 27-Aug~2002 14:11 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e : \\E tsta rg e t\ta rg e t\ch e m \d u d e j r . i\D 02 0812A.b\DUDE0073. D Lab Smp Id : 38029 In j Date : 1 3 -AUG-2002 00:39 Operator : mla In st ID: d u d e jr.i Smp In fo : E 0 2-0 4 4 3-38 0 2 9 ; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Mise In fo : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr .i\D 020812A .b\D 020812A .m Meth Date : 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date : 12-AUG-2002 16 :13 C a l F i l e : DUDE0027.D A ls b o ttle : 25 D ii Factor: 1.00000 Integrator : Falcon Compound S u b lis t : a l l . sub Target Version: 4 .12 Conpounda 1 PFB3 <a9> 3 PPH3 (3 9 9 ) 3 PFOA (4 1 3 ) 4 POSA (4 9 # ) S PROS (4 9 9 ) QUANT 8 IO HASS 299 399 413 498 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT 8XP RT DX*T RT RBSPOHSB ing/w lh) (n g / L ) 3 .4 0 8 3 .8 1 1 4 .0 0 9 4 .7 9 6 4 .1 6 7 4 .4 6 7 3 .3 9 4 3 .7 9 1 3 .9 8 2 4 .7 6 8 4 .1 6 0 4 .1 6 0 0 .0 1 4 0 .0 2 0 0 .0 2 7 0.028 0 .0 2 7 0 .3 0 7 69092 252177 3288B1 34000 631586 131570 2 . 5691 7.85210 21.8421 1.11439 20.1841 3 .2 9 0 4 9 2.66(H ) 7.85 2 1 .8 1 .1 1 IN) 2 0 .2 3 .2 9 QC F la g Legend M - Compound response m anually in te g r a te d . Exact Copy of 0n~:rr C illL fo o /a -- 3M Environmental Laboratory Page 155 of 276 Report E02-0443 D ata F i l : SN Etstar|;etN tiretS ch*B S dud*jr.iS D 020812fl.bS D U D E 0073.D Tenn. River Valley Samples Page 2 i PFBS <2995 1 3 M Environmental Laboratory Exact Copy ' C tllC .. ' j f / z f e L ' *ntfa* Page 156 of 276 Report E02-0443 D ata F ila s S \E tst*rtet\tarsetS chm S dudeor,i\D 020812fl.bS D U I)E Q C i73.D Tenn. River Valley Samples pae 3 4 FOSA <4981 S PFOS <499) 3M Environmental Laboratory Exact Copy of Origin-.! tY lL . i'il/o l L- Inia! Dato Page 157 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082B.b\DUDE0130.D Page 1 Report Date: 29-Aug-2002 07:12 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f ile \\Etstarget\target\chem \dudejr.i\D 020812B.b\D U D E0130.D Lab Smp Id 38030 In j Date 13-AUG-2002 11:0 8 Operator mla In st ID: d u d e jr.i Smp In fo E 0 2-0 443-38030; Water Sam ples; non-GLP; 7 / 1 7 / 0 2 ; OK Mise Info Comment Method \\Etstarget\target\chem \dudejr.i\D 020812B.b\D020812B.m Meth Date 29-Aug-2002 07:08 d u d e jr .i Quant Type: ESTD Cal Date 13-AUG-2002 06:44 C a l F i l e : DUDE0106.D A ls b o t t le 42 D il Factor 1.00000 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 Compounds 1 p ro s (295 a PFHS (3 9 9 ) 3 PPOA (9 1 3 ) 4 POSA ( 9 ) s PPOS (4 9 9 ) QUANT SIQ MASS 299 299 299 299 399 413 499 499 CONCENTRATIONS ON-COLUMN P IN A L RT SXP RT DLT RT RESPONSE ( n g /fflL ) (ng/m L) 3 .3 8 7 2 .4 9 8 3 .2 0 3 3 .7 7 7 3 .7 7 7 3 .9 4 8 4 .7 4 1 4 .1 3 9 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .791 3 .9 8 2 4 .7 8 8 4 .1 4 0 -0 .0 0 7 -0 .8 9 4 -0 .1 9 1 0 .3 83 -0 .0 1 4 -0 .0 1 4 -0 .0 2 7 -0 .0 2 1 197441 1231 2244 11248 8387299 4152125 7980357 8914428 2 9 2 4 .5 0 2 9 3 5 .4 4 2 9 3 5 .4 2 2 9 3 5 .2 0 4 2 4 .8 6 5 4 2 7 .8 6 0 3 0 0 .2 2 6 4 2 3 .6 7 3 2930 2940 2940 2940 425 428 300 424 3M Environmental Laboratory Page 158 of 276 Report E02-0443 Data F ila : S S ttargat\targat\cha\dud#Jr,iS D 020812B *b\D U D E 0130*D Tenn. River Valley Samples Paga 2 2 PFHS <399> 3M Environmental Laboratory Exact Copy <.\: <y Page 159 of 276 Report E02-0443 D ata F i l e t SSEtstarcetStarcetSehenN<fudejr*iSD020812BbSDUDE0130D 3 PFQA <413> Tenn. River Valley Samples Pace 3 4 FOSA <498> 5 PFOS <4W> 3M Environmental Laboratory Exact Copy r;;' ;: lL. \xij*/a Page 160 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudej r .i\D02082A.b\DUDE0092.D Page 1 Report Date: 27-Aug-2002 14:12 3M Environm ental Laboratory ,E02-0443 Tenn. R iv e r V a lle y Samples Data f i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 8 12 A .b \D U D E 0 0 9 2 .D Lab Smp Id : 38043 In j Date : 1 3 -AUG-2002 04:09 Operator mla In st ID: d u d e jr.i Smp In fo : E0 2-0443-38043; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Misc In fo : Comment : Method : \ \ E t s t a rg e t\ta rg e t\ch e m \d u d e j r . i\D 0 20812A.b\D020812A.m Meth Date : 2 7 -Aug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date 1 2 -AUG-2002 16 :1 3 C a"l F i l e : DUDE0027.D A ls b o t t le : 34 D il Factor: 1 .0 0 0 0 0 Integrator: Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Coapounda 1 PFBS (2 9 9 ) 2 PFHfl (3 9 9 ) 3 PPOA ( 3 ! 4 POSA ( 4 5 * ) 5 PPOS (4 9 9 ) QUANT S IG MASS 299 29 299 29 29 399 413 499 499 CONCBNTRATIONS ON-COLUMN PINAL RT BXP RT DLT RT RBSPONSB (ng/m L) (ng/m L) 3 .3 5 4 2 .4 5 1 3 .2 1 0 3 .9 1 0 4 .0 3 7 3 .9 5 2 4 .0 1 0 4 .7 9 4 4 .1 9 5 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .7 9 1 3 .9 8 2 4 .7 8 9 4 .1 8 0 >0.040 -0 .9 4 3 -0 .1 9 4 0 .4 2 4 0 .8 4 3 0 .1 7 1 0 .0 2 8 0 .0 2 9 0 .0 3 5 32948 739 8206 1244 1953 16543 9481 6471 30951 0 .6 7 0 6 1 5 0 3 .9 2 9 5 0 3 .6 3 4 5 0 3 .0 1 1 5 0 3 .7 8 6 0 .5 0 1 7 3 0.06868 0 .2 0 6 9 9 0.07297 0.671 504 504 504 504 0 .5 0 2 0.0687 0 .2 0 7 0 .0 7 3 0 ^CtCoynUJry.n-, 3M Environmental Laboratory Page 161 of 276 Report E02-0443 Data F t 1er S\Ettar*tStarttSchm SduJ*jr.iSD 020812ft.bSDU D E0092.D Tenn. River Valley Samples Page 2 1 PFBS <299) 2 PFHS <399) 3M Environmental Laboratory T ;; Original M L I2rj/iO1-- "'ira Data Page 162 of 276 Report E02-0443 D a ta F i la : S S E t ta rj t\ta rt tS c h *n S d u d *J r,i\D 0 2 0 8 1 2 A .b U > U D E 0 9 2 .D 3 PFOA <413> Tenn. River Valley Samples 9 PFOS <4OT> 3M Environmental Laboratory BCt&yy..; Page 163 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0067.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environm ental Laboratory E02-0443, Tenn. R ive r V a lle y Sangles Data f ile : \\Etstarget\target\chem \dudejr.i\D020812A.b\DUDE0067.D Lab Smp Id : 38025 In j Date : 12-AUG-2002 23:33 Operator : mla In s t ID-. d u d e jr .i Smp In fo : E 0 2 -0443-38025; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Mise In fo : Comment : Method : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 8 12 A .b \D 0 2 0 8 12 A .m Meth Date : 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date : 12-AUG-2002 16 :13 C a l F i l e : DUDE0027.D A ls b o t t le : 22 D il Facto r: 1.00000 In teg rator: Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 Ccpound. 1 ma 3 PFHS 3 PPOA 4 POSA 3 FFOS (391) (399) (413) (494) (499) QUANT S IS HASS 399 399 413 493 499 499 CONCSNTKATIOMS ON-COLUMN PINAL RT BXP RT DLT RT RBSFOKSB (ng/L) (ng/m L) 3 .4 0 1 3 .9 1 2 4 .0 0 3 4 .7 9 6 4 .1 9 1 4 .4 6 9 3 .3 9 4 3 .7 9 1 3 .9 9 2 4 .7 6 8 4 .1 6 0 4 .1 6 0 0 .0 0 7 0 .0 2 1 0 .0 2 1 0 .0 2 8 0 .0 2 1 0 .3 0 8 98538 247750 321649 29398 593659 135043 2 .9 9 2 0 6 7.71134 21.3198 0.96228 18.4924 3.40254 2.99(H ) 7 .7 1 2 1 .3 0.943(H ) 1 8 .5 3 .4 0 QC F la g Legend M - Compound response m anually in te g ra te d . &RC Copy L l!} C _ I fciii 3M Environmental Laboratory Page 164 of 276 Report E02-0443 Data F ile $ S N E tatargatS targat\cheS ciud*j r * i\D020812.b\DUDE0067* D Tenn. River Valley Samples Pae 2 3M Environmental Laboratory Page 165 of 276 Report E02-0443 Ft ! ; S S E ti1 4 rt tS t* rE e tS o h * n \d u d e jr. iSD020812A.bSDUDE0067. D 3 PFOA <413) Tenn. River Valley Samples Page 3 4 FOSA <498) 3M Environmental Laboratory a C U ji i J 1 V - SLOT' Page 166 of 276 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0069.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e : \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 8 12 A .b \D U D E 0 0 6 9 .D Lab Smp Id : 38026 In j Date : 12-AUG-2002 23:55 Operator : mla In st ID: d u d e jr.i Smp In fo : E 0 2 -0443-38026; Water Sam ples; non-GLP; 7 / 1 7 / 0 2 ; OK Mise In fo : Comment : Method \\Etstarget\target\chem \dudejr.i\D 0208l2A.b\D 0208l2A.m Meth Date : 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date : 12-AUG-2002 16 :13 C a l F i l e : DUDE0027.D A ls b o t t le : 23 D il Factor: 1 .0 0 0 0 0 In tegrator: Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 Compounds 1 PFBS (2 9 9 ) 2 PFH3 (3 9 9 ) 3 PPOA (4 1 3 ) 4 FOSA (4 9 9 ) S PPOS (4 9 9 ) QUANT SIQ MASS 299 399 413 499 499 499 CONCKNTKATIOMS ON-COLUMN FINAL RT B IP KT DLT RT RRSPONSB (ng/m L) (n g /a L ) 3 .4 0 1 3 .8 1 1 4 .0 0 3 4 .7 8 9 4 .1 8 0 4 .4 6 7 3 .3 9 4 3 .7 9 1 3 .9 8 2 4 .7 6 8 4 .1 6 0 4 .1 6 0 0 .0 0 7 0 .0 2 0 0 .0 2 1 0 .0 2 1 0 .0 2 0 0 .3 0 7 118567 255866 340061 31162 648655 140168 3.70420 7.9694B 22.6524 1 .0 2 0 7 9 20.7906 3 .5 6 8 0 1 3.70M 7 .9 7 2 2 .6 1 . 01(H) 2 0 .8 3 .5 7 QC F la g Legend M - Compound response m anually in te g ra te d . 3M Environmental Laboratory / // fo i-' Page 167 of 276 Report E02-0443 Sata F ila s S S E ttartat\tartatS chai*S dudajr.i\D 020812n.bS D U D E 0069.D Tenn. River Valley Samples Paga 2 1 PFBS <299> 2 PFHS <399> 3M Environmental Laboratory ^CopyofOriaina Page 168 of 276 Report E02-0443 D ata F ile s \\EttargetStaretSchiSclud#Jr,iSD 020812A.bSDU D E0069.D 3 PFOA <413> Tenn. River Valley Samples p4g 3 4 FOSA <498) 3M Environmental Laboratory Copy a- . Page 169 of 276 Report E02-0443 Tenn. River Valley Samples Data F i l e : \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D 0 20 8 2 A .b \D U D E 0 0 71.D Page l Report Date: 27-Aug-2002 1 4 :1 1 3M Environm ental Lab o rato ry E02-0443, Term. R iv e r V a lle y Samples Data f i l e : \\E tsta rg e t\ta rg e t\c h e m \d u d e jr.i\D020812A.b\DUDE0071.D Lab Smp Id : 38027 In j Date 13-AUG-2002 0 0:17 Operator : mla In st ID: d u d e jr.i Smp In fo : E 0 2-0 4 4 3-38 0 27; Water Sam ples; non-GLP; 7 / 1 7 / 0 2 ; OK Mise In fo : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr .i\D 020812A .b\D 020812A .m Meth Date : 2 7 -Aug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD C a l Date : 1 2 -AUG-2002 1 6 :1 3 C a l F i l e : DUDE0027.D A ls b o t t le : 24 D ii Factor: 1 .0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 Compounds 1 PPBS (2 9 ) 2 PFHS (3 9 9 ) 3 PPOA (4 1 3 ) 4 TOSA (4 9 0 ) 5 PPOS (4 9 9 ) QUANT SXO MASS 299 399 413 49B 499 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT EXP RT DLT RT RESPONSE <ng /m L) (ng/tL> 3 .4 0 1 3 .8 1 1 4 .0 0 2 4 .7 9 6 4 .1 8 0 3.86C 4 .4 6 7 3 .3 9 4 3 .7 9 1 3 .9 8 2 4 .7 6 8 4 .1 6 0 4 .1 6 0 4 .1 6 0 0 .0 0 7 0 .0 2 0 0 .0 2 0 0 .0 2 8 0 .0 2 0 -0 .2 9 4 0 .3 0 7 102829 405S93 412129 121332 808339 4108 86093 3.14446 12.7977 27.9672 4.00115 26.5743 3 7 9 .7 8 7 1 .7 9 7 4 3 3 . 1 4 (N) 1 2 .8 2 8 .0 4 .0 0 2 6 .6 380 1 .8 0 QC F la g Legend M - Compound response m anually in te g r a te d . ( >C<:. 3M Environmental Laboratory Page 170 Of 276 Report E02-0443 S ata F ila s S\E tstar(ttS targat\chen\dudajr.i''D 020612A .bS D U D E 071.D Tenn. River Valley Samples P a ta 2 1 PFSS <299) 2 PFHS <399) 3M Environmental Laboratory CJ; ! i Page 171 of 276 Report E02-0443 D ata F ila s SSEt*targetSt*rgetSchenSc*Jdejr,i\D 020812A .bSD U D E007i.D 3 PFOA <413) Tenn. River Valley Samples Page 3 4 FOSA <498) 5 PFOS <499) 3M Environmental Laboratory Page 172 of 276 Report E02-0443 Tenn. River Valley Samples Data F i l e : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr . i\D02082A.b\DUDE007B.D Page 1 Report Date: 27-Aug-2002 1 4 :1 1 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 8 12 A .b \D U D E 0 0 7 8 .D Lab Smp Id 38033 In j Date 13-AUG-2002 01:34 Operator mla In st ID: d u d e jr.i Smp In fo E0 2-0 4 4 3-38 0 33; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Mise In fo Comment Method \\Etstarget\target\chem \dudejr.i\D0208l2A.b\D0208l2A.m Meth Date 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD C a l Date 1 2 -AUG-2002 1 6 :1 3 C a l F i l e : DUDE0027.D A ls b o ttle 27 D il Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compound* 1 PPBS (a) 2 PFHS O ) 3 PFOA 1 3 > 4 POSA (4 9 4 ) S PROS (4 9 9 ) QUANT S IO MASS 299 299 299 299 299 299 412 499 499 CONCENTRATIONS ON-COXiUNN PINAI RT RXP RT W X RT RESPONSE (n g /ttL ) (ng/mXa) 3 .3 6 0 3 .3 1 0 3 .8 1 9 4 .0 5 8 3 .8 1 3 3 .9 6 9 4 .0 1 0 4 .7 9 4 .1 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .7 9 1 3 .7 9 1 3 .9 8 2 4 .7 6 8 4 .1 6 0 -0 .0 3 4 -0 .1 8 4 0 .4 2 4 0 .6 6 4 0.021 0 .1 7 8 0 .0 2 8 0 .0 2 8 0 .0 3 4 26600 4235 1671 634 5685 5436 11537 5487 35066 0.45093 5 0 3 .7 0 6 5 0 3 .7 9 6 5 0 3 .9 3 3 0 .1 6 9 7 4 0.16213 0 .2 0 1 2 8 0 .1 7 4 5 6 0.20349 0 .4 5 1 504 504 504 0 .1 7 0 0 .1 6 2 0 .2 0 1 0 .1 7 4 0 .2 0 3 if f 3M Environmental Laboratory Page 173 of 276 Report E02-0443 D ata Filas SSEt*tareatStartatSchaSdudajr.lSD020B12ft.l>SDUDE0078,D Tenn. River Valley Samples F ata 2 1 PFBS < 29 9) 2 PFHS <399) 3M Environmental Laboratory - -'a Cc;j, cj-llC. y . o ^ 3#; Page 174 of 276 Report E02-0443 D ata F i l a i S S E t ta rja tS ta r{ e tS c h a i* \* jd e jr. i \D020812A. bSDUDE0C78. D 3 PFOA <413> Tenn. River Valley Samples Paja 3 4 FOSA <49S> S PFOS <499> 3M Environmental Laboratory C...'itehJ. Page 175 of 276 Report E02-0443 Tenn. River Valley Samples Data F i l e : \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D 0 20 8 2 A .b \D U D E 0 0 8 0 .D Page 1 Report Date: 27-Aug-2002 1 4 :1 1 3M Environm ental Laboratory E02-0443, Term. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr.i\D 0 2 0 8 12 A .b \D U D E 0 0 8 0 .D Lab Smp Id 38034 In j Date 1 3 -AUG-2002 0 1:5 7 Operator mla In st ID: d u d e jr.i Smp In fo E 0 2-0 443-38034; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Misc Info Comment Method \\Etstarget\target\chem \dudejr.i\D 020812A.b\D 020812A.m Meth Date 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date 12-AUG-2002 16 :13 C a l F i l e : DUDE0027.D A ls b o t t le 28 D il Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compounds 1 PPBS l a s 2 PPHS (3 9 ) 3 PPOA (4 1 3 ) 4 POSA (4 9 9 ) 5 PPOS (4 9 9 ) QUANT S IS HASS 29 399 413 49B 498 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DLT RT RESPONSE (ng/m L) (ng/m L) 3 .4 0 1 3 .9 1 2 4 .0 1 0 4 .7 9 S .0 9 0 4 .1 9 4 3 .3 9 4 3 .7 9 1 3 .9 0 2 4 .7 0 8 4 .7 B 4 .1 0 0 0 .0 0 7 0.021 0 .0 2 8 0 .0 2 8 0 .3 2 2 0 .0 3 4 2801 073 17031 0747 27S 51049 0.50070 0.20104 0.55003 0.21007 0.00294 0 .7 1 1 2 7 0.501(H ) 0 .2 0 1 0 .5 5 0 .2 1 0 0 .0 0 2 9 4 0 .7 1 1 QC F la g Legend M - Compound response m anually in te g r a te d . 3M Environmental Laboratory Page 176 of 276 Report E02-0443 D t* F i l : S S E ts ta rc tS fc * r(e t\c h S d u d * jr . i \DO2O012fl. hSDUDEOOSO. D Tenn. River Valley Samples Pae Z 2 PFHS < 3 9 9 ) 3M Environmental Laboratory Ci j 'Si ~UML U ll J , \fc S fe j O v ij Page 177 of 276 Report E02-0443 B a t F i l a i S 'sE tita r|;tS ta r{ tS ch B i S d u d*jr.i\D 02 0 8 12 ft.b \D U Iie o 0 80 .D 3 PFC (4 1 3 ) Tenn. River Valley Samples 4 FOSA <498) 5 PFOS <499) 3M Environmental Laboratory -fier o: Originai initial Date P ane 17H n f 97fi Report E02-0443 Tenn. River Valley Samples Data F i l e : \\E tstarg et\targ et\ch em \d u d ejr.i\D 208 2A .b \D U D E 0 08 4 .D Page 1 Report Date: 27-Aug-2002 1 4 :1 1 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f il e \\Etstarget\target\chem \dudejr.i\D020812A.b\DU DE0084.D Lab Smp Id 38037 In j Date 1 3 -AUG-2002 0 2:4 1 Operator mla In st ID: d u d e jr.i Smp In f o E02-0 4 4 3 -3 8 0 3 7; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Mise In fo Comment Method \\Etstarget\target\chem \dudejr.i\D 020812A.b\D 020812A.m Meth Date 2 7 -Aug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD C al Date 1 2 -AUG-2002 1 6 :1 3 C a l F i l e : DUDE0027.D A ls b o t t le 30 D il Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compound 1 PFBS t ) 2 PPHS (3 S ) 3 PFO 4 POSA ( 4 M ) 5 PROS ( 4 M ) QUANT S IS MASS 299 399 413 498 499 CONCENTRATIONS ON-COLOMU F IN A L RT BXP RT DLT RT RBSPONSB (ng/m L) <ng/mL> 3 .3 5 3 3 .8 0 5 4 .0 1 0 4 .7 9 6 4 .1 8 8 3 .3 9 4 3 .7 9 1 3 .9 8 3 4 .7 6 8 4 .1 6 0 -0 .0 4 1 0 .0 1 4 0 .0 2 8 0 .0 2 8 0 .0 2 8 32546 12978 14081 6547 43651 0 .6 5 9 9 9 0 .3 9 2 6 7 0.36547 0.20948 0 .4 7 6 0 6 O .C S O (M ) 0 .3 93 0 .3 6 5 0 .2 0 9 0 .4 7 6 QC F la g Legend M - Compound response m anually in te g ra te d . 3M Environmental Laboratory -'T /a i Page 179 of 276 Report E02-0443 Data F ila : S S E tU r*et\targt\ch*\dud*Jr.iS D 020812A .bS D U D E 0084.D Tenn. River Valley Samples Pas# 2 2 PFHS <399> 3M Environmental Laboratory '^'aci Co^y o; Ci'igina Irdtiaj i n- S s t3 Paae 180 of 276 Report E02-0443 D ata F i l a i S \E t* ta r s * tS ta rt tS c h a i S d u d e jr. iSD020812A, k>\DUD0084, D 3 P Ft C413> Tenn. River Valley Samples Paga 3 B PFOS <499 > 3M Environmental Laboratory i'w l ! l ~{ / / / l Page 181 o f 276 Report E02-0443 Tenn. River Valley Samples Data F i l e : \ \ E t s ta rg e t\ ta rg e t\ch em \d u d ejr. i\D020812A.b\DUDE0086.D page l Report Date: 27-Aug-2002 14 :12 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E ts ta rg e t\ta rg e t\c h e m \d u d e j r . i\D 0 2 0 8 l2 A .b\DUDE00 8 6 .D Lab Smp Id 38038 In j Date 13-AUG-2002 03:03 Operator mla In st ID: d u d e jr.i Smp In fo E0 2-0 443-38038 ; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Mise In fo Comment Method \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date 27-A ug-2002 14 :0 6 d u d e jr .i Quant Type: ESTD Cal Date 1 2 -AUG-2002 1 6 :1 3 C al F i l e : DUDE0027.D A ls bottle 31 D il Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 CoBpoundfl 1 FFBS (3 9 9 ) 2 PPH3 (3 9 ) 3 PPOA (4 1 3 ) 4 ROSA ( 4 S I ) S EPOS (4 9 9 ) QUANT S IO HASS 399 399 413 498 499 CONCENTRATIONS ON-COLUMN PINAL RT EXP RT DIjT RT RBSPONSB (n g / L ) (ng/m L) 3 .3 5 3 3 .8 1 2 4 .0 0 3 4 .7 9 6 4 .1 8 8 3 .3 9 4 3 .7 9 1 3 .9 8 3 4 .7 6 8 4 .1 6 0 -0 .0 4 1 0 .0 2 1 0 .0 2 1 0 .0 2 8 0 .0 2 8 34896 8214 15139 3452 44196 0 .7 4 2 6 6 0 .2 4 7 0 1 0.43379 0.10754 0.49338 0 .7 4 3 (N) 0 .2 4 7 0 .4 3 4 0 .1 0 8 0 .4 9 3 QC F la g Legend M - Compound response m anually in te g ra te d . Exact Copyof Original Dato 3M Environmental Laboratory Page 182 of 276 Report E02-0443 D a ta F i l a : S S E ta ta r te tS ta r te tS c h w iS d u d e jr . iSD 020812A . bSDUDEOOB. B Tenn. River Valley Samples Paga 2 2 PFHS <399> 3M Environmental Laboratory 'fMCopy of Origin Sate Page 183 of 276 Report E02-0443 D a ta F i l e r Y s E ts ta rg e tS ta rg e tS c h e m S d u d e jr. iSD020B12A. bMHIDEOOS, S 3 PFQA (4 1 3 ) Tenn. River Valley Samples Page 3 4 FOSA (4 9 8 ) 6 PFOS <499) 3M Environmental Laboratory ^xn.ct Copy of Origins! CttlL-Uikdp^ rnit!a1 Oe.to Page 184 of 276 Report E02-0443 Term. River Valley Samples Data F ile : \\E tstarg e t\targ et\ch em \d u d e jr.i\D 0 20 8 12B .b \D U D E 0 127.D Page 1 Report Date.- 29-Aug-2002 0 7 :12 3M Environm ental Laboratory E02-0443, Tenn. R iv e r V a lle y Samples Data f i l e \\E t s t a r g e t \t a r g e t \c h e m \d u d e jr .i\D 020812B .b\D U D E0l27 .D Lab Smp Id 38028 In j Date 1 3 -AUG-2002 10 :3 5 O perator cmc In st ID: d u d e jr.i Smp In fo E 0 2-0 4 4 3-38 0 28 ; Water Sam ples; non-GLP; 7 / 1 7 / 0 2 ; OK Mise In fo Comment Method \\E tsta rg e t\ta rg e t\ch e m \d u d e jr.i\D020812B.b\D0208l2B.m Meth Date Cal Date 29-Aug-20Q2 07:08 d u d e jr .i Quant Type: ESTD 13-AUG-2002 06:44 -C-a-l - F- i l e : DUDE0106.D A ls b o ttle 41 D ii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 Coapounda 1 PFB5 (299) 2 PFHS (399) 3 FPOA (413) 4 POSA (499) 5 ppoa (499) QUANT SIG MASS 39 299 299 299 299 299 399 413 499 499 COMCBKTRATIONS ON-COLUMN FINAL RT BXP RT DLT RT RESPONSE? (ng/mt) (ng/mL) 3.399 2.497 3.073 3.777 4.095 4.249 3.777 3.942 4.741 4.140 3.394 3.394 3.394 3.394 3.394 3.394 3.791 3.942 4.749 4.140 *0.004 -0.497 -0.321 0.393 0.491 0 .855 -0.014 -0.020 -0.027 -0.020 195309 943 9274 9440 402 439 7874701 3449302 4025349 7927444 2924.40 2935.48 293S.29 2935.33 2935.49 2935.70 392.549 348.429 302.105 341.793 2930 2940 2940 2940 2940 2940 392 384 302 342 3M Environmental Laboratory Page 185 of 276 Report E02-0443 D ata F il t \\Et*tar*atStarfat\oham SdudaJriSD 20812B*bSBU D E0i27*D Tenn. River Valley Samples Pas 2 iI .1 i 2 PFHS <399> 3M Environmental Laboratory -,;au Co/y ofOriginal initia) DaisQ V j ( L //d l/H - Page 186 of 276 Report E02-0443 Dt* F il* : S \E tst4 r * t\t rt tS c h e \o lu c l jr. i\D020812B.b\DUBE0127.D 3 PFOA <4i3> _ Tenn. River Valley Samples 3M Environmental Laboratory aci Copy or Original r Page 187 of 276 Report E02-0443 Tenn. River Valley Samples Data F ile : \\E ts ta rg e t\ta rg e t\c h e m \d u d e jr. i\D02Q812B.b\DUDE0133.D Page 1 Report Date: 29-Aug-2002 0 7 :12 3M Environm ental Lab o rato ry E02-0443, Tenn. R iv e r V a lle y Samples Data f il e \\E t s t a r g e t \t arget\chem \dudejr. i\D0208l2B,b\DUDE0133.D Lab Smp Id 38036 In j Date 1 3 -AUG-2002 1 1 : 4 1 Operator mla In st ID: d u d e jr.i Smp In fo E0 2-0 4 4 3-38 0 36 ; Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Mise In fo Comment Method \\E tstarg e t\targ et\ch em \d u d e j r . i\D020812B.b\D020812B.m Meth Date 29-A ug-2002 07:08 d u d e jr .i Quant Type: ESTD C a l Date 13-AUG-2002 06:44 C a l F i l e : DUDE0106.D A ls b o t t le 43 D il Factor 1 .0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 Coapounda I 1 PPBS (2 9 1 ) 3 PPHS (3 9 9 ) 3 PFOA ( 1 3 ) ; 4 POSA (4 9 8 ) S PPOS (4 9 9 ) QUANT SXG HASS 399 39 399 399 399 399 413 498 499 499 CONCBNTRTIONS ON-COLUMN PINAL RT RXP RT DLT RT RRSP0NS8 (n g / L ) < n g /i*L ) 3 >388 3 .0 7 3 3 .7 7 7 4 .0 8 5 4 .3 4 3 3 .7 7 1 3 .9 6 2 4 .7 3 5 4 .1 3 3 3 .8 3 3 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .3 9 4 3 .7 9 1 3 .9 8 3 4 .7 5 8 4 .1 8 0 4 .1 6 0 > 0 .0 0 6 >0.331 0 .3 8 3 0 .6 9 1 0 .8 4 8 -0 .0 3 0 -0 .0 2 0 -0 .0 3 3 -0 .0 2 7 -0 .3 2 8 303053 18005 9S08 820 817 8071912 3927038 8558553 7890357 906 2 9 2 6 .2 9 2 9 3 4 .8 8 2 9 3 5 .2 8 2 9 3 5 .6 8 2 9 3 5 .6 8 4 0 4 .8 7 0 3 9 8 .4 8 7 3 2 4 .5 3 5 3 6 5 .2 6 5 3 0 7 1 .2 5 2930 2930 2940 2940 2940 405 398 324 365 3070 3M Environmental Laboratory Exact Copy o r O .-'gif..; U/jj-l* Page 188 of 276 Report E02-0443 O a t* F i l : S S E ts ti r t t s t # r {tScheiKkSdudj r . iSDO2O012B. bSDUDE0133, D Tenn. River Valley Samples Pat 2 1 PFBS <299> 2 PFHS <39S> 3M Environmental Laboratory Exact Copy of Orh<n? UL Ck(jol6^ .nEffa Page 189 of 276 Report E02-0443 D a ta F i l a : S S E ts ta rs e tN ta rje tN c h a n S d u d a jr . S D 020812B .bSDUDE0133,D 3 PFOA <413> Tenn. River Valley Samples pa 3 4 FOSA (498) S PFOS <499) 3M Environmental Laboratory `'fCi Cirj - J2C /J l/f / l- Page 190 of 276 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\dudejr.i\D02082B.b\DUDE0136.D Page 1 Report Date: 29-Aug-2002 07:12 3M Environm ental Laboratory E02-0 443, Tenn. R iv e r V a lle y Saraples Data f ile \\Etstarget\target\chem \dudejr.i\D 020812B.b\DU D E0136.D Lab Smp Id 38040 In j Date 13-AUG-2002 12 :14 Operator mla In st ID: d u d e jr.i Smp In fo E02-0443-38040/ Water Sam ples; non-GLP; 6 /2 0 /0 2 ; OK Misc Info Comment Method \\Etstarget\target\chem \dudejr.i\D020812B.b\D020812B.m Meth Date 29-Aug-2002 07:08 d u d e jr .i Quant Type: ESTD C a l Date 13-AUG-2002 06:44 C a l F i l e : DUDE0106.D A ls b o t t le 44 D il Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l . sub Target Version: 4.12 Coopounda aanaaEBaaaaBPBeaB 1 PPBS (J9) 2 PPHS (399) 3 PPOA (413) 4 POSA (499) S PPOS (499) QUANT SIG MASS aaa 299 299 299 299 299 299 413 458 459 RT BXP RT DLT RT RESPONSE * SBiaiM* asgasiBwa a 3.38? 3.394 -0.007 200230 3.936 3.394 -0.4S8 9425 3,073 3.394 "0.321 13185 3.832 3.394 0.438 10649 4.023 3.394 0.429 485 3.777 3.791 -0.014 8246279 3.901 3.982 -0.021 3997548 4.741 4.748 -0.027 7955892 4.132 4.140 -0.028 776002S CONCENTRATIONS ON-COLUMN (ng/mL) PINAL (ng/mL) i H1 IHI 2926.37 2935.47 293S.11 293S.23 2935.70 41S.875 407.589 299.205 358.040 2930 2940 2940 2940 2940 416 40B 299 358 3M Environmental Laboratory Page 191 of 276 Report E02-0443 D ata F ila s S \E ts ta rg a tS ta rg e tS c h a n S d u d e jr, t\D020812B. b\DUDE0136. D Tenn. River Valley Samples Pag* 2 1 PFBS <299) 3M Environmental Laboratory i'.XdCi Ci/'.jj, , ; i: 1Ji im - CUtiCa.l U/':>,*vc/, Page 192 of 276 Report E02-0443 Data F ila : SSEttrsetStar5t\ohm Sdudjr.iSD 020812B.bSD U D E0136.D 3 PFOft <413) Tenn. River Valley Samples Pa{ 3 4 F08A <498) 5 PFOS <499) 3M Environmental Laboratory ISfflCt Copv r.: .'i- !. fpJta] );- Page 193 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY034.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environm ental Laboratory Data f ile \\E tsta rg e t\ta rg e t\ch e m \itch y .i\l0 21112.b \IT C H Y 0 34 .D Lab Smp Id 0443-W B-l In j Date 1 2 - NOV-2002 13:4 0 Operator mla In st ID: it c h y .i Smp In f o E 0 2-0 4 4 3-W B -l; Water B la n k ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Misc Info Comment Method \ \ E t s t a r g e t \ t a r g e t \ c h e m \ it c h y .i\I 0 2 1 1 1 2 ,b \ I 0 2 1 H 2 .m Meth Date 1 3 - N o v -2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date 12-NOV-2002 12 :14 C a l F ile : ITCHY026.D A la b o t t le 21 D il Factor 1 .0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4.12 Compound* 1 PPBS ( 9 9 ) 2 PFHS 0 9 9 ) 3 PFQA U l3 > 4 POSA < 4 9 5 ppos (4 9 9 ) QUANT S IO MASS 299 299 299 399 413 413 49 499 CONCENTRATIONS ON-COLUMN PINAL KT BXP RT DLT RT RBSFONSB (ng/m L) (ng/m L) 3 .4 2 1 3 .2 5 2 4 .1 2 9 3 .40 4 .0 3 9 4 .3 4 4 . 47 4 .2 0 9 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 . 67 4 .1 9 9 '0 .0 0 1 -0 .1 7 0 0 ,7 0 7 0 .0 1 0 0 .0 1 9 0 .3 2 8 0 .0 0 0 0 .0 1 0 37874 7026 7366 2541 13412 10274 1927 78922 0.55035 9 3 3 .5 0 0 9 3 3 .4 9 0 0.13306 7 4 4 .8 7 4 7 4 5 .0 5 0 0 .1 7 2 1 6 1 .0 9 1 1 9 0 .5 5 0 933 933 0 .1 3 3 745 745 0 .1 7 2 1 .0 9 3M Environmental Laboratory Beast Cop 'CMC Page 194 of 276 Report E02-0443 D ata F ila s S S E tsta rt tS ta r(e tS c h e S ito h y , iS I021112.b\ITCHY034. D Tenn. River Valley Samples PaCa 2 2 PFHS <399) 3M Environmental Laboratory Page 195 of 276 Report E02-0443 Bat F U ; S\E ttart^tStar*t\ch*\ltoha.iSI021112.bSIT C H Y 034.B 3 PFOA < 4 1 3 ) Tenn. River Valley Samples Pace 3 4 FOSA <498> 8 PFOS <49S> 3M Environmental Laboratory y ... iz/jffL- Page 196 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY035.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environm ental Laboratory- Data f il e : \\E tsta rg e t\ta rg e t\ch e m \itch y .i\l0 2 1112 .b \IT C H Y 0 3 5 .D Lab Smp Id : 0443-WB-2 In j Date : 1 2 -NOV-2002 1 3 : 5 1 Operator : mla In st ID: itc h y .i Smp In f o : E02-0443-W B-2; Water B la n k ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Misc In fo : Comment Method : \\E t s t a r g e t \ t a r g e t \ c h e m \ it c h y .i\l0 2 1 1 1 2 .b \ I 0 2 1 1 1 2 .m Meth Date : 1 3 -N ov-2002 0 9 :16 i t c h y . i Quant Type: ESTD C a l Date : 1 2 -NOV-2002 1 2 :1 4 Cal F i le : ITCHY026.D A lS b o t t le : 22 D il Facto r: 1.00000 Integrator: Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compounds 1 PFBS (a 9) 2 PPHS (3 9 9 ) 3 PFOA (4 1 3 ) 4 POSA (4 9 1 ) 5 PPOS (4 9 9 ) QUANT B IG NASS 299 299 299 399 399 413 413 499 499 CONCENTRATIONS ON-COLUMN RT EXP RT DOT RT RESPONSE (ng/m L) F IN A L (ng/m L) 3 .4 1 1 3.2S 2 4 .1 1 9 3 .9 3 0 3 .4 9 1 4 .0 2 9 4 .3 4 ft 4 .8*7 4 .2 1 9 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .9 3 0 3 .9 3 0 4 .0 2 0 4 .0 2 0 4 .9 4 7 4 .1 9 9 -0.0 1 1 0 .1 7 0 0 .6 9 7 0 .0 0 0 -0 .3 3 9 0 .0 0 9 0 .3 2 9 0 .0 0 0 0 .0 2 0 32544 S959 3295 3629 1344 14592 12065 2453 42341 0 .3 9 7 2 6 9 3 3 .5 3 0 9 3 3 .6 0 7 0.15642 0.10734 0.04324 7 4 4 .9 4 9 0 .1 9 4 3 4 0 .2 3 6 3 0 0 .3 9 7 934 934 0 .1 5 6 0 .1 0 7 0 .0 4 3 2 745 0 .1 9 4 0 .2 3 6 3M Environmental Laboratory Exact O ty y o fC rtijir r . Page 197 of 276 Report E02-0443 D ata F iU W E t it a r g a tS ta r g e t\c h e m \it c h y . 1SI0 21 1 1 2.bSITCHV035.D Tenn. River Valley Samples Pag 2 ti 2 PFHS <399) 3M Environmental Laboratory -'fact Copy or 0 riTM: Page 198 of 276 Report E02-0443 D ata F i l a : S S E ta ta r la tS ta r ja tS c h a n S itc h y . i S 10 3 1 1 1 2 .bSITCHY03S,B 3 PFOA (4 1 3 ) Tenn. River Valley Samples Pag# 3 4 POSA (4 9 8 ) %! 1* ;4 I 1 3M Environmental Laboratory & act Copy of Origina! o niq Page 199 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY038.D Page 1 Report Date: 19-NOV-2002 14:49 3M Environm ental Lab o rato ry Data f i l e \\E t s t a r g e t \t a r g e t \c h e m \it c h y . i \ l 0 2 1 H 2 .b\lTCH Y038 .D Lab Smp Id 0 4 4 3-38 0 4 4 -1 In j Date 1 2 - NOV-2002 14 :2 3 Operator mla In st ID: it c h y .i Smp In fo E 0 2 -0 4 4 3 -3 8 0 4 4 -1; S L - 1 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo Comment Method \\Etstarget\targ et\chem \itchy.i\I0 2 1ll2 .b \I0 2 lll2 .m Meth Date 1 3 - Nov-2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date 12-NOV-2002 12 :14 - C-a-l - F- i l e : ITCHY026.D A ls b o ttle 25 D ii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 Compound 1 FFBS (2 9 9 ) 2 PPHS (2 9 9 ) 3 PROA U M ) 4 POSA (4 9 ) S PPOS (4 9 9 ) quant s is HASS 399 299 399 399 399 413 413 49B 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DI/T RT RBSPONSR (ng/m L) (ng/m L) 3 .5 1 1 3 .9 7 0 4 .3 0 9 3 .8 4 0 3 .4 3 2 4 .0 4 0 3 .7 0 1 4 .8 8 7 4 .2 1 9 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .8 4 7 4 .1 9 9 0 .0 8 9 0 .S 4 8 0 .8 8 7 0 .0 1 0 > 0 .3 9 8 0 .0 2 0 -0 .3 1 9 0.020 0 .0 2 0 383859 2593 4148 122635 18909 29S590 211 1250415 2785277 10.5978 9 3 3 .6 2 7 9 3 3 .5 8 2 2 .7 1 9 9 9 0.48492 1 6 .1 9 4 9 7 4 5 .1 6 6 29.6711 67.6562 1 0 .6 934 934 2 .7 2 0 .4 8 5 1 6 .2 745 2 9 . 7 (H) S 7 .fi(n) QC F la g Legend M - Compound response m anually in te g r a te d . EcaciCopyoiOrisiiidl 3M Environmental Laboratory Page 200 of 276 Report E02-0443 Data F ila : S S E t*tar**tS ta rg etS ch * S itch 3 .iS I0 21 U 2 .b S IT C H Y 03 8 ,E Tenn. River Valley Samples Paga 2 2 PFHS < 39 9) 3M Environmental Laboratory :--xaci Copy i.r af-' Qac,..lfisL~ Page 201 of 276 Report E02-0443 H at F i l v t \ \ E t * t a r * tS ta rc e tS c h e n S i t chy . i S 1031112.bX1TCHY038.D 3 PFOO <413) Tenn. River Valley Samples 4 FOSA <498) 3M Environmental Laboratory l'ct C007 c>- Origina! cut,iUi4^ Page 202 of 276 Report EQ2-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY040.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environm ental Laboratory Data f i l e : \\E t s t a r g e t \t a r g e t \c h e m \it c h y .i\I0 2 1 1 1 2 .b \lT C H Y 0 4 0 .D Lab Smp Id : 0443-38044-2 In j Date : 1 2 - NOV-2002 14 :4 5 Operator : mla In s t ID: it c h y .i Smp In f o : E 0 2-0 4 4 3 -3 8 0 4 4 -2; S L - 1 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo : Comment Method Meth Date : : \1\3E-tNs target\ o v -2002 ta 0 r 9 ge :16 t \ch itc em hy \i .i t c h y.i\I0 Quant 21 T 112 .b ype: \l0 2 ESTD 1 1 1 2 . m C a l Date : 1 2 -NOV-2002 1 2 :1 4 C a l F i le : ITCHY026.D A ls b o t t le : 26 D il Factor: 1 .0 0 0 0 0 In te g rato r: Falcon Compound S u b lis t : a l l .s u b Target Version : 4 .12 Compound* 1 PFB3 <a*> 2 PPH3 (3 9 9 ) 2 PFOA (4 1 3 ) 4 POSA <491) 5 PPOS (4 9 9 ) QUANT B IO MASS 299 299 299 299 399 413 413 498 499 CONCENTRATIONS ON-COLUMN P IN A L RT BXP RT DLT RT RBSP0N5B (ng/m L) (ng/m L) 3 .4 3 2 3 .9 7 0 4 .3 0 9 3.B 40 3 .4 3 2 4 .0 4 0 3 .7 1 1 4 .8 8 7 4 .2 1 9 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .8 8 7 4 .1 9 9 0 .0 1 0 0 .8 4 8 0 .8 8 7 0 .0 1 0 > 0 .3 9 8 0 .0 2 0 -0 .3 0 9 0 .0 2 0 0 .0 2 0 383608 1970 62861 118901 13 878 260003 9S04 1361450 2885124 10.5904 9 3 3 .6 4 5 1.26871 2.63937 0.37675 14.1091 7 4 5 .0 9 3 3 2 .3 5 5 0 70.2517 1 0 .6 934 1 .2 7 2.5 4 0 .3 7 7 1 4 .1 745 3 2 .4 70.3(H ) QC F la g Legend M - Compound response m anually in te g r a te d . &< % : 3M Environmental Laboratory Page 203 of 276 Report E02-0443 D ata F ile : \\E tstareetStarjetSchi\itchy.iM 021112,.b\IT C H Y 040.D Tenn. River Valley Samples Pase 2 2 PFHS (399) R nuironm enta! ! aK rtrainm Braci Copy o: Origin a; l. taiial.iLfe t4a^ Paae 204 of 276 Report E02-0443 D t F i l e t \ \ E t s t r S t\t r * t\ c h e n \ltc h y .i\I 0 2 1 1 1 2 .b S IT C H Y 0 4 0 . I) 3 PFOA <413> Tenn. River Valley Samples PaE* 3 4 FOSA <498) C PFOS <499) 3M Environmental Laboratorv Cmc Origina o iiiU L. "i Page 205 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021H2.b\ITCHY042.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environm ental Lab o rato ry D ata f i l e : \\Etstarget\target\chem\itchy.i\l02lli2.b\iTCHY042.D Lab Snip Id : 0443-38044-3 I n j Date : 12- NOV-2002 15:07 Operator : mla In st ID: it c h y .i Smp In f o : E02-0443-38044-3; SL-1; MeOH Extract; 21 Oct 02; MLA Misc In fo : Comment : Method : \\Etstarget\target\chem\itchy.i\l021112.b\I021112.m Meth Date : 13- Nov-2002 09:16 itchy.i Quant Type: ESTD C a l D ate : 12-NOV-2002 12:14 "C a'l F i l e : ITCHY026.D A ls b o t t le : 27 D il Factor: 1 .0 0 0 0 0 In te g ra to r: Falcon Compound S u b lis t : a l l . sub Target Version: 4 .12 Compound 1 PPBS U S ) 2 PFHS U s s ) 3 PFQA ( 4 1 3 ) 4 POSA (4 S 8 5 PROS (4SS ) QUANT SIG NASS 299 299 299 299 412 413 496 499 CONCENTRATIONS ON-COLUMN RT BXP RT DLT RT RBSPONSB < n g /u L ) F IN A L (n g /n L ) 3 .5 3 1 4 .2 9 9 3 .6 4 0 3 .4 3 2 4 .0 4 0 3 .7 0 1 4 .6 8 7 4 .2 1 9 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .8 6 7 4 .1 9 9 0 .1 0 9 0 .8 7 7 0 .0 1 0 -0 .3 9 6 0 .0 2 0 -0 .3 1 9 0 .0 2 0 0 .0 2 0 482034 50026 111724 19590 2S3343 8515 1033771 2109105 13 .4694 0 .8 9 9 5 7 2 .4 8 4 4 5 0 .4 9 9 5 7 1 3 .7 2 0 1 7 4 5 .1 4 9 2 4 .4 6 3 8 50.3621 1 3 .5 0 .9 0 0 2.4 8 0 .5 0 0 1 3 .7 745 2 4 . 5 (M) 5 0 .4 QC F la g Legend M - Compound response m anually in te g r a te d . fr.3 u f Cm[ ; I 3M Environmental Laboratory Paae 206 of 276 Report E02-0443 D ata F ila i \^Etstarc#t\targatSehai<i\itchy*iSI02ill2.b\X TC H Y 042D 3 PFOA <413> Tenn. River Valley Samples 4 FOSA <498> 8 PFOS <499> 3M Environmental Laboratory 11 ' Paae 208 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY046.D Page l Report Date: 19-NOV-2002 14:49 3M Environm ental Laboratory Data f il e : \\E t s t a r g e t \t a r g e t \c h e m \it c h y .i\I0 2 lll2 .b\ITCHY046.D Lab Strip Id : 0 4 5 3 -3 8 0 4 5 -1 In j Date : 1 2 - NOV-2002 15 :5 0 Operator : mla In st ID: it c h y .i Smp In f o : E02-0 4 4 3 -3 8 0 4 5 -1; S L -3 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Misc Info : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \it c h y .i \ I 0 2 1 1 1 2 . b \ I 0 2 1 1 1 2 . m Meth Date : 1 3 - Nov-2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date : 12-NOV-2002 12 :14 C a'l F i l e : ITCHY026.D A ls b o ttle: 31 D il Factor: 1 .0 0 0 0 0 Integrator: Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 Compound 1 m a *) 2 PFHS (3 9 9 ) 3 PPOA (4 1 3 ) 4 POSA (4 9 9 ) S PPOS (4 9 9 ) QUANT S IG NASS 299 299 299 399 39 413 413 413 498 498 498 499 CONCENTRATIONS ON-COLUMN F IN A L RT BXP RT DLT RT RESPONSO (ng/m L) (ng/m L) 3 .4 1 3 3.9S 0 4 .3 0 9 3 .8 4 0 3 .4 4 2 4 .0 4 0 3.711 4 .3 7 9 4 .8 8 7 4 .5 9 8 4 .2 1 9 4 .5 8 8 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .0 2 0 4 .8 5 7 4 .8 6 7 4 .1 9 9 4 .1 9 9 0 .0 1 0 0 .5 2 8 0 .8 8 7 0 .0 1 0 -0 .3 8 8 0 .0 2 0 -0 .3 0 9 0 .3 5 9 0 .0 2 0 -0 .2 6 9 0 .0 2 0 0 .3 6 9 3252S4 2272 17131 13341 8750 48048 9113 7941 48310 5183 418454 11802 8.88037 9 3 3 .6 3 6 9 3 3 .2 1 0 0 .3 6 5 2 0 0 .2 6 6 5 1 1 .9 2 9 3 5 7 4 5 .1 1 5 7 4 5 .1 8 1 1.24672 0 .2 4 7 5 4 9 .0 7 8 1 7 1 3 5 4 .2 5 8.88 934 933 0 .3 6 5 0 .2 6 6 1 .9 3 745 745 1 .2 5 0 .2 4 8 9 .0 8 1350 Origina! C w . rxUl/x-' : y : D a to 3M Environmental Laboratory Page 209 of 276 Report E02-0443 D ata F ila s SSE ttar*atStarcatSohaiSitchM .iSI*2ill2.bM TC H V 046.r Tenn. River Valley Samples P a ja 2 1 PFBS < 29 9) 3M Environmental Laboratory an Or;sn 13- I i M Page 210 of 276 Report E02-0443 D ata F ila : SSE tstareatStarsetSchaM tehy,iM 021112.bM T C H Y 046.D 3 PFOA <413) Tenn. River Valley Samples Fa(a 4 FOSA <498) 3M Environmental Laboratory Piaci Cop CuiC : v ,.. . ! > Page 211 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\l021112.b\lTCHY048.D Page 1 Report Date: 19-Nov-20Q2 14:49 3M Environm ental Laboratory- Data f ile \\E tsta rg e t\ta rg e t\ch e m \itch y .i\I0 2 1ll2 .b \lT C H Y 0 4 8 .D Lab Smp Id 0453-38045-2 I n j Date 1 2 - NOV-2002 1 6 :1 2 Operator mla In st ID: it c h y .i Smp In fo E 0 2 -0 4 4 3-38 0 4 5-2; S L -3 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Misc In fo Comment Method \\Etstarg et\targ et\ch em \itch y.i\l0 2 1112 .b \l0 2 1112 .m Meth Date 1 3 - N ov-2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date 12-NOV-2002 12 :14 -C-a -l -F-i l e : I-TCHY026.D A ls b o t t le 32 D il Factor 1 .0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 Compounds 1 PPB8 U * ) a PPHLS ( S ) 3 PFOA ( 4 1 3 ) 4 POSA < ) 5 PFOS l4 > ) QUANT 8 IO NASa 299 299 299 299 399 399 413 413 498 498 499 499 CONCENTRATIONS ON-COLUMN PINAL RT SXP RT DLT RT R8SPONSB (ng/m L) (ng/m L) 3 .4 2 1 3 .9 4 0 4 .3 1 8 3 .8 4 0 3 .4 4 1 4 .0 2 9 4 .0 4 9 3 .7 1 0 4 .8 8 4 4 .4 1 7 4 .2 2 9 4 .5 4 8 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .8 4 7 4 .8 4 7 4 .1 9 9 4 .1 9 9 -0 .0 0 1 0 .5 3 8 0 .8 9 4 0 .0 1 0 -0 .3 8 9 0 .1 9 9 0 .0 2 -0 .3 1 0 0 .0 1 9 -0 .2 5 0 0 .0 3 0 0 .3 4 9 30S101 7189 12829 11449 18109 10665 <0231 8754 46172 4067 323943 4825 8 .2 9 1 2 8 9 3 3 .4 9 5 9 3 3 .3 3 3 0.33496 0.46772 0 .3 0 7 6 7 2 .6 1 8 5 6 7 4 5 .1 3 5 1.19716 0.22171 6.84538 1 3 5 4 .3 7 8 .2 9 933 933 0*325 0 .4 6 8 0 .3 0 8 2 .6 2 745 1 .2 0 0.222 6 .8 4 1350 I M e i.;; U -V 3 M Environmental Laboratory Page 212 of 276 Report E02-0443 D ata F ila* N \E tstar*atStarsatSch*m S ttcha.iSI021il2.b\IT C H Y 048,D Tenn. River Valley Samples Paja 2 1 PFBS < 2 M > 2 PFHS <399> 3M Environmental Laboratory 1.1 W - t C u p . usai y D b Page 213 of 276 Report E02-0443 D ata F ila ; SSE tstar|;etSt*'t*tSchem SitchaaSI021112.bS IT C H Y 048,D Tenn. River Valley Samples P*6 3 4 FOSA <498) 8 PFOS <499) 3M Environmental Laboratory Page 214 of 276 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\itchy.i\1021112.b\lTCHY05l.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environm ental Laboratory Data f il e \\E ts ta rg e t\ta rg e t\c h e m \itc h y .i\10 2 1112 .b\ITCHY051.D Lab Smp Id 0 453-380 45-3 In j Date 1 2 -NOV-2002 16:4 4 Operator mla In st ID: itc h y .i Smp In fo E02-0 4 4 3 -3 8 0 4 5 -3 ; S L -3 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo Comment Method \\Etstarget\targ et\chem \itchy.i\I0 2 1112 .b \I0 2 1112 .m Meth Date 1 3 -N ov-2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date 12-NOV-2002 12 :14 C a l F ile : ITCHY026.D A l s b o ttle 33 D il Factor 1 .0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 I ut Cowpounds 1 PFBJS (2SS) 3 PFHS (3 J 9 ) 3 PPOA (4 1 3 ) 4 POSA (4 3 8 ) (439) QUANT SIG MASS 299 29 299 399 399 399 413 413 413 49ft 49ft 499 499 CONCENTRATIONS ON-COLUMN F IN A L RT 8XP RT DLT RT RESPONSE (ng/taL) (n g /n L ) 3 .4 0 2 3 .9 5 0 4 .3 0 9 3 .7 2 0 3 .4 3 1 4 .0 3 9 4 .0 4 9 3 .7 1 1 4 .38ft 4 .8 9 7 4 . Sftfl 4 .2 2 9 3.93 0 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .0 2 0 4 .8 4 7 4 . 847 4 .1 9 9 4 .1 9 9 -0 .0 2 0 0 .5 2 8 0.BB7 -0 .1 1 0 -0 .3 9 9 0 .2 0 9 0 .0 2 9 -0 .3 0 9 0 .3 6 8 0 .0 3 0 -0 .2 7 9 0 .0 3 0 -0 .2 6 364688 2069 18856 12125 2424 11470 54999 12405 12668 6S768 4044 42046S 4504 10.0353 9 3 3 .6 4 2 0.00434 0.33906 0.13055 0.32498 2 .3 2 2 4 2 7 4 4 .9 3 0 7 4 4 .9 1 5 1 .6 5 1 5 ft 0.22117 9.12623 1 3 5 4 .4 3 1 0 .0 934 0 .0 0 4 3 4 0 .3 3 9 0 .1 3 0 0 .3 2 5 2 .3 2 745 745 1 .6 5 0 ,2 2 1 9 .1 3 1350 C (/j 'm feiBaj V. 3M Environmental Laboratory Page 215 of 276 Report E02-0443 H at F ila s N S E ts ta rg a tS ta re a tS c h a n S ltc h a. iM 021112.bM TCHY051.D Tenn. River Valley Samples Pag* 2 2 PFHS < 3 9 9 ) 3M Environmental Laboratory Page 216 of 276 Report E02-0443 D ata F ila i \\E t*tareat\tarsat\chanM tchy.l\I< > 21il2.bS IT C H Y 051.D 3 PFOA <413) Tenn. River Valley Samples 4 POSA <498) 5 PFOS <499> 3M Environmental Laboratory Page 217 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\X02lll2.b\ITCHY053.D Page l Report Date: 19-NOV-2002 14:49 3M Environm ental Laboratory Data f ile \\E tsta rg e t\ta rg e t\ch e m \itch y .i\I0 2 lll2 .b \IT C H Y 0 5 3 .D Lab Smp Id 0453-38045-MS(3) In j Date 1 2 - NOV-2002 17 :0 6 Operator mla In st ID : itch v. i Smp In fo E02-0443-38045-M S( 3 ) ; S L -3 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo Comment Method \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y . i \ I 0 2 1 l l 2 . b \ I 0 2 1 1 1 2 .m Meth Date 1 3 - Nov-2002 0 9 :16 i t c h y . i Quant Type: ESTD C a l Date 1 2 -NOV-2002 1 2 :1 4 C a l F ile : ITCHY026.D A ls b o ttle 34 D ii Factor 1 .0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l . sub Target Version: 4 .12 Compounds J P7BS ( 3 9 * ) 2 PPHS (3 9 9 ) 3 PPOA (9 1 3 ) 4 POSA (9 9 9 ) S PFOS (9 9 9 ) QUANT S IO MASS 299 299 299 299 413 413 498 499 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DLT RT RESPONSE (ng/m L) (n g /a L ) 3 .4 3 3 3 .9 4 0 4 .3 8 9 3 .8 3 0 4 .0 3 0 3 .6 9 1 4 .8 6 7 4 .1 9 9 3 .9 2 0 3 .4 2 3 3 .4 2 2 3 .4 2 2 3.B 30 4 .0 2 0 4 .0 2 0 4 .8 6 7 4 .1 9 9 4 .1 9 9 0 .0 0 0 0 .5 1 8 0 .8 6 7 -0 .0 1 0 0 .0 0 0 -0 .3 2 9 0 .0 0 0 0 .0 0 0 -0 .2 7 9 1540798 713 118796 169555B 91396 6716 1092819 1285365 2917 45.9348 9 3 3 .5 0 9 2.88083 37.8097 40.2752 7 4 5 .2 5 0 25.8793 29.9181 1 3 5 4 .4 6 4 5 .9 934 2.8 8 37 .8 4 0 .3 745 2 5 .9 2 9 .9 1350 l'O ry c/i,<. '-'- S i 3M Environmental Laboratory Page 218 of 276 Report E02-0443 D ata F i l a } SSEta t a r g e t S t a r gatSchaaiSl tc h a . t M 0 2 1 1 1 2 . bS I TCHY0S3. D Tenn. River Valley Samples Page 2 Ion 293 2.4- r ! 2. 1 i . 8- l.B - 1 . 2- 0 .9 0 .6 0 .3 . 1 s Ss* \w -- 1.U t A j _______2_*__8____3(*X2 L_ 3 .6 4*0 I4 4 2 PFHS <399) 3 M Environmental Laboratory 1; ^ ... v n o tfis ; J&JtgfLs jmf r * M ! " Page 219 of 276 Report E02-0443 D ata F i l a i S S E ttarK atS tareetS chanS itcM y.iM 021112.bS ltC H Y 0S 3.O 3 PFOA (4 1 3 ) Tenn. River Valley Samples PaC 3 4 FOSA (4 9 8 ) 5 PFOS <499) Cupi o i O rig in a i Cp x &aa.! Dsi) 3 M Environmental Laboratory Page 220 of 276 Report E02-0443 Tenn. River Valley Samples Data F ile : \\E ts ta rg e t\ta rg e t\c h e m \itc h y .i\I0 2 1112 .b \IT C H Y 0 5 5 .D Page 1 Report D ate: 1 9 -N o v-2002 14 :50 3M Environm ental Lab o rato ry Data f ile : \\E tsta rg e t\targ e t\ch e m \itc h y . i\I0 2 1112 .b \IT C H Y 0 5 5 .D Lab Smp Id : 0 4 6 3-38 0 4 6 -1 In j Date : 1 2 - NOV-2002 17 :2 8 Operator : mla In s t ID: it c h y .i Smp In fo : E02-0 4 4 3 -3 8 0 4 6 -1; S L -2 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo : Comment : Method : \\E t s t a r g e t \t a r g e t \c h e m \i t c h y . i \ l 0 2 l l l 2 . b \ I 0 2 l l l 2 . m Meth Date : 1 3 - N ov-2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date : 12-NOV-2002 12 :14 C a'l F i l e : ITCHY026. D A ls b o ttle: 41 D ii Factor: 1 .0 0 0 0 0 Integrator : Falcon Compound S u b lis t : a l l . s u b Target Version: 4 .12 Compound 1 PBS (2 9 9 ) 2 FPHS <3S> 3 PPOA (4 1 3 ) 4 POSA (4 9 ) 5 FPOS (4 9 9 ) QUANT SZG MASS 299 399 399 399 399 413 413 498 499 499 C0NCBNTRATI0N3 ON-COLUMN PINAL RT BXP RT D liT RT RBSFONS8 <ng/L> (ng/m L) 3 .5 3 1 4 .0 8 9 4 .3 1 9 3 .8 4 0 3 .4 2 2 4 .0 4 0 3 .7 1 1 4 .8 8 7 4 .2 1 9 3 .9 3 0 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .8 6 7 4 .1 9 9 4 .1 9 9 0 .1 0 9 0 .6 6 7 0 .8 9 7 0 .0 1 0 0 .4 0 8 0 .0 2 0 0 .3 0 9 0 .0 2 0 0 .0 2 0 -0 .2 6 9 327380 5006 8043 173 S3 14192 53375 7259 120467 417236 11862 8.94256 9 3 3 .5 5 8 9 3 3 .4 7 1 0.45146 0.38350 2.23055 7 4 5 .2 1 9 2.92155 9 .0 4 9 3 5 1 3 5 4 .2 5 8 .9 4 934 933 0 .4 5 1 0 .3 8 3 2 .2 3 745 2 .9 2 9 . OS 1350 \i. i Uujj-., 3M Environmental Laboratory D ana 004 Report E02-0443 D ata F ila i SSEtstartatStargetSchai*SitchM ,iSIC>2ill2.bSlTCH Y 055,D Tenn. River Valley Samples Pas 2 1 PFBS <299) 3M Environmental Laboratory Report E02-0443 D ata F i l e t S \E ts ta r* a tA ta reatSoh*>Sito h y . iSI021112,bSITCHYMSB.D 3 PFOA <413) Tenn. River Valley Samples Page 3 4 FOSft < 498) B PFOS <499) '- C i C4h( `V# 3M Environmental Laboratory Pace 223 of 276 Report E02-0443 Tenn. River Valley Samples Data F ile : \\E ts ta rg e t\ta rg e t\c h e m \itc h y . i\l0 2 1112 .b \IT C H Y Q 5 7 .D Page 1 Report Date: 19-Nov-2002 14:50 3M Environm ental Laboratory- Data f ile \\E tsta rg e t\ta rg e t\ch e m \itch y .i\I0 2 1112.b \lT C H Y 0 57.D Lab Smp Id 0463-38046-2 In j Date 12-NOV-2002 17 :5 0 Operator mia In st ID: it c h y .i Sirp In fo E02-0 4 4 3 -3 8 0 4 6 -2 ; S L -2 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo Comment Method \\Etstarget\target\chem\itchy.i\I021ll2,b\I02lll2.m Meth Date 1 3 -N o v -2002 0 9 :16 i t c h y . i Quant Type: ESTD C a l Date 1 2 -NOV-2002 1 2 :1 4 C a l F i le : ITCHY026.D A ls b o t t le 42 D ii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound S u b lis t : a l l . s u b Target Version: 4.12 a 1 Compound 1 FPBS (2 9 9 ) (399) 3 PFOA (4 1 3 ) 4 POSA (4 9 1 ) S PPOS (4 9 9 ) QUANT S IS MASS 299 299 299 299 399 399 413 413 413 49B 499 499 CONCENTRATIONS ON-COLUMN PINAL RT HXP RT DLT RT RESPONSE (n g /n U (n g / t) 3 .5 1 1 3 .9 4 0 4 .0 9 9 4 .3 1 9 3 .8 4 0 3 .4 3 2 4 .0 4 0 3 .7 1 1 4 .3 5 9 4 .8 8 7 4 .2 2 9 3 .9 3 0 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .8 3 0 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .0 2 0 4 .8 8 7 4 .1 9 9 4 .1 9 9 0 .0 8 9 0.S 38 0 .6 4 7 0 .8 9 7 0 .0 1 0 -0 .3 9 8 0 .0 2 0 -0 .3 0 9 0 .3 4 9 0 .0 2 0 0 .0 3 0 -0 .2 6 9 232749 2668 5270 7437 18434 10544 35197 7629 12091 103503 393650 12978 6 .1 8 2 5 6 9 3 3 .6 2 5 9 3 3 .5 5 0 9 3 3 .4 8 8 0.47471 0.30507 1 .2 0 3 7 3 7 4 5 .1 9 9 7 4 4 .9 4 8 2.52745 8.49146 1 3 5 4 .2 3 6 .1 8 934 934 933 0 .4 7 5 0 .3 0 5 1 .2 0 745 745 2 . 5 3 (34) 8 .4 9 1350 QC F la g Legend M - Compound response m anually in te g r a te d . 3M Environmental Laboratory Page 224 of 276 Report E02-0443 D ata F i l a i S S E ts t a r c a t \ta r c a tS c h a * iS itc h y .iv.I0 2 ill2 ,b M T C H Y 0 B 7 .D Tenn. River Valley Samples Paca 2 1 PFB8 <299) 3M Environmental Laboratory Cnx Page 225 of 276 Report E02-0443 B at F ila i S S E t* tar{ tS tarj;* tS ch en S ito h y . iS 1021112.bSITCHV0S7,B 3 PFOfi (413> Tenn. River Valley Samples Pag 3 4 FOSft <498> 3M Environmental Laboratory c,vyorMum [ms Pane 22(5 n f 27(5 Report E02-0443 Tenn. River Valley Samples Data F i le : \\E ts ta r g e t\ta r g e t\c h e m \itc h y .i\I0 2 1112 .b \IT C H Y 0 5 9 .D Page 1 Report Date: 19-Nov-2002 14:50 3M Environm ental Lab o rato ry Data f il e : \\E tsta rg e t\targ e t\ch e m \itch y .i\I0 2 1112 .b \IT C H Y 0 5 9 .D Lab Smp Id : 0463-38046-3 In j Date : 1 2 - NOV-2002 1 8 :1 2 Operator : mla In st ID: it c h y .i Smp In f o : E 0 2 -0 4 4 3 -3 8 0 4 6 -3 ; S L -2 ; MeOH E x t r a c t ; 2 1 Oct 02; MLA Mise In fo : Comment : Method : \ \ E t s t a r g e t \ t a r g e t \ c h e m \ i t c h y . i \ I 0 2 1 1 1 2 .b \I0 2 1 1 1 2 .m Meth Date : 1 3 - Nov-2002 0 9 :16 i t c h y . i Quant Type: ESTD Cal Date : 12-NOV-2002 12 :14 - C- a-l - F- i l e : ITCHY026.D A ls b o t t le ; 43 D ii Factor: 1 .0 0 0 0 0 In teg rato r: Falcon Compound S u b lis t : a l l .s u b Target Version: 4 .12 11 !*" 1H 1H 11 Compound 1 PFBS (2 9 S ) 2 PFHS < 3 M ) 2 PPOA (4 1 3 ) 4 POSA (4 9 1 ) 5 pros (499) QUANT S IS NASS 299 299 299 399 399 413 413 413 499 499 499 CONCENTRATIOKS ON-COLUMN P IN A L RT EXP RT VIST RT RESPONSE (ng/m L) (ng/m L) 3 .5 4 1 4 .0 9 0 4 .3 1 9 3 .9 5 0 3 .4 3 2 4 .0 4 0 3 .7 1 1 4 .3 5 9 4 .9 9 7 4 .2 2 9 3 .9 3 0 3 .4 2 2 3 .4 2 2 3 .4 2 2 3 .030 3 .8 3 0 4 .0 2 0 4 .0 2 0 4 .020 4 .857 4 .1 9 9 4 .1 9 9 0 .1 1 9 0 .5 5 9 0 .8 9 7 0.020 *0.398 0 .0 2 0 -0 .3 0 9 0 .3 4 9 0 .0 2 0 0 .0 3 0 -0 .2 6 9 420079 6904 11582 25494 17014 40917 9580 11804 133252 478587 14760 11.6624 9 3 3 .5 0 3 9 3 3 .3 6 9 0.62654 0 .4 4 4 1 7 1 .5 2 6 5 3 7 4 5 .1 4 5 7 4 4 .9 6 4 3 .2 1 8 7 0 10.5027 1 3 5 4 .1 9 934 933 0 .6 2 6 0 .4 4 4 1 .5 3 745 745 3 .2 2 10 .5 1350 B aci Copy ,CmL fr ffftt S tfib 3M Environmental Laboratory Page 227 of 276 Report E02-0443 D ata F ile : \SE t*targtStare*tSch*i>i'vitcK a.iSI02iil2.bSITC H Y 0S9.D Tenn. River Valley Samples Page 2 1 PFBS <299 2 PFHS <399 3M Environmental Laboratory f-vsci Co'iv of on: a/fyfa Paoe 228 of 276 Report E02-0443 D ata F U * t SSEttartt\tare*t\oh>SitohM ,lM 021112.b\ITC H Y 0B 9.D 3 PFC <413) Tenn. River Valley Samples Pe# 3 4 FOSft <499) S PFOS <499) 6mc 3M Environmental Laboratory Page 229 of 276 Report E02-0443 Tenn. River Valley Samples Attachment D: Sample Prep Sheets, Test Substance, and Test System Information 3M Environmental Laboratory Page 230 of 276 Report E02-0443 Tenn. River Vallev Samples L a b R e q u e st: (Z)H H Tennessee River Valley Samples Sam ple Location 1, Large M outh a e 9 f U E iS 2 ! 1 SL-1.LM -1-1 SL-1.LM -1-2 S L -t, LM-1-3 2 1 0 ^7 -- 1 s I t* 3 cs a. j I ijj 1] 48 r l_ L il5 1 li fs 7 SL-1, LM-2-1 SL-1, LM-2-2 \,n m -- SL-1.LM -2-3 -- SL-1, LM-2-MS -- J SL-1, LM-3-1 S L -I.L M -S jrJ 3SL-1. LM-3-Jf SL-1, L M - 4 - / -- h, \ -N, 3 / w \ is SL-1, LM-4 - 3 SL-1, L M -4 - SL-1, LM-4-MS -- ---------- a SL-1. LM-5-1 SL-1, LM-5-2 SL-1, LM-5-3 SL-1, LM-6-1 --3, W o oc -5 4 $v $ SL-1, LM-6-2 SL-1, LM-fl-3 --- -- SL-1. LM-6-MS -- .N I. -3 N L Col2T/D/l 0 ? 5 5 t 7 ~ l J e i l 19 / * i l / h J ri 0 V,, S >L r > it Wf 1 n 8 /V 1-- ly , VJ s5 * 2 t li 8 f- i i 10 }' n 11 II li! 11 h H W II I) H i e ni 12 13 /f h II 14 s n r O V O c t. ___ 1 q pi cp 130 >v O3 0 \ ~ ** . J . N i-- 3 i. Col 9 Shaker ID.- O d t g l g. ..... 1Balance ID } l ' i _________ Tube tma/alza S & 'iL fih s h u f- ( r t f 7' Equll Start T/D /lld U H e ./a / lj7 < / 3 - 15 c o i 3 T/D/i iM f i / L . is i l l I Q j t j n L W aterlD Col 4 T/D T04^ i l I n / 6 ) - t ^ SDed/aettina L ? EquilStop T/D/li r . f l W x / t K / ( D - W Col 10 T/D iy.lT|m ( 3 / I lf /r t ^ O VTC C entrifuge ID: *T 7 > 3 L _______________ c o is t/d 7:2 c * * * (j / /s r i d - c m . (3tC E ^>R M R eadout % T T M inute I T \ Tem p *C 3 0 Cantrifuga ID:. ....... RCF/PRM Readout: 3 c O Q _M lnutes_ ,,Tam p #( c o m t /d n v i ) ^ t r zi y / d t - /v t ^ Col 12 T/D If-SCftt, (a / I Jf / b lC / YvC Col 8 T / D / l li? / 1Y /fa jX fr C C o l7 Solklno Standard ID * b D & 3 Water ID M i l l , - S / W V l . t S ____ Col 13 T/D i l l \C t C "S ~ Q ^ ~ Approximate Cone. I p p > Amount added I Q Q ^ L . t / d i i - g i L d ^ ____ i i . / _ i i _ / < i k _ o w : (T o / ' 3 M E n?v iro n m en tal L ab o(ra tpo ry / f & i C /T -lC Col 14 T/Df l/o ^ T /V . (a / fO / i ) ~ X C * ^ MeOH ID: TN-A * ~ S 3 t ) ^ iP .-rk * " ` ^ W ^J ( J i f f / f i V e r ? i t i l o ' t ) f e f i t t p Il O ri W Z - r t l A . W re /{ ) Traim i/3 >"(!" 1 ( fc*>) `ff :-T c~.A J ur/'V f i v '-'V Page 1 o /6 / f t W vW P eg et o tS /fv W .7 a p , A l i / # )- .tir - r * * ^ 3M Environmental Laboratory Page 231 of 276 Report E02-0443 Tenn. River Valley Samples lab Request: -0 V V^ i 1 SL-1. C-1-1 S L -1.C -1-2 SL-1, C-1-3 S L -1.C -2-1 1 !i Tl * I il 2 >05W L -- -- Tennessee River Valley Samples Sample Location 1, Catfish 1 3 4 $ r 5^1 si V Ijj 11i11 t _4__ 1s a* y /7 V s II S S| sJ i1 n 1s h3 h i(i If li l u II ill a rA 10 ys i12 12 ^ ! il "V _L -i v Ha' N7 \ SL-1. C-2-2 SL-1. C -2-3 -- A SL-1, C-2-M S N ^.oo'iSSL-1. C-3-1 N S L-1. C -3i2 3 's SL-1, C ' 3 ~ y \ -- V V S L -1 .C -4 -/ S U 1 .C -4 -J SL-1, C-4 - S L-1. C-4-M S y .o n ) -------- ------- . *v s SL-1.C -S -1 SL-1. C-S-2 S L-1. C-5-3 SL-1. C-8-1 ,,1 --. r -- tut Hla 's > 'SN V V. < V. 3U V j N i VV. vf / S L -1 .C -6 -2 SL-1, O S -3 SL-1. C-8-M S S L-1.W B -1 S L-1. W B-2 SL-1. SB-1 -- --. -- . -- -- * na A X L> N f --- >* - SL-1. SB-2 -- Z_ - - -- rs , IV J NZ. S. V S \vSi ^i: p) c. *' * "'s - Ai / ^3 V Tt N* k> \ NJ y . x j 0 sJ i _ a/ 5 - Jv i T VJ ,I N sP 3 .2 y. > J0 i s <e V- yO \ L LI 3 t 1 \ ,i \ si -- --- -- -- N --- - --- - C o l 2 T /D fl SflOQO A 1 /7 - 1 /?IJ j i t " 0 ji m , # k y ^ C / *' i * ( T ) (ft> . Batanee ID . 9 / V T u b e tepe/Bize P o /y f r y / 5 0 . C o l 8 S h a ke r ID f t ? - S E quil S tart T /D /llf- C H e n /' / fJ fr r fL ^ L ^ - C i 12 . O [5 i C o l 3 T /D /lp '/ f r y m fy f i t /0 ? v . V L C E qull Stop T /D /l It'.^ H W M t y /f t'X f W ater ID H t H t T C C ^ tA C o l 4 T /D /l f '. V f d t f j / ( I f l l O ^ Leed/eenlno ( 0 c o is t /d /i 'T ' & ^ k l o < K 4 )3 - C * * C Cantrtftjga ID:,: 1 L * - ________ SocoRCF/PRM Readout:. nJ f amp C. C o l 8 T IM ? .' 3 ^ 4 0 ^ fa l l i I 0 7 - v * C o l 7 S p ik in g S ta n d a rd 10 # ~ 7 *> A pproxim ate Cone. ( Am ount added / r Y li. L T /D /l ____ U - I J & - I Q ? r P H Col ?: T M / T - W S " ^ .S O rV ^ t . / / - o c 3M Environm ental Laboratory C o l 10 T /D /l O '.K fr I t / i r l O Z c v r IL CenMuge IP.^ T ~ Q ~2--___________ ^RC^/PRM Readout3 t f X 3 Minute I A )________ Temp x 2 3 c o in T / D / i U / I X / a a t jrr C Col 12T/Dflt.V ./D ^ iv s L i 1I t T / j L Water ID M i l l ' l ' Q l T f c f C O I11 T ID /lW f iv t ( i l l C( |0 3 --O **- Col14 T/D/l I'. IOi-s I C l \ c [ 1tT L , 0 * 1 MeOH ID: TN-A. V j l Qw J - A H ePrtlU LtfYc uCtr- /,Vlit -'.' Page2 o r0 ii - O /*/*> - f t * - 9 * Pc * -- rh ^ T tfe . -- / , k _ - /e X ^ -3 /*-/ - u r e r y /.,,,* / V A f V f 4 ) , (*//?cV - 0 ! >i- fa 0 / C j/1OeA/ " - / 0 ' i j C p i t l We/" Jf h ' i ' j -fvr i l c p ? C l t 4 - l l p t 't 3M Environmental Laboratory Page 232 of 276 Report E02-0443 Tenn, River Valley Samples Lab Request: fir Tennessee River Valley Samples Sample Location 2- Large M outh 4 Location 3-Sm all M outh B 1 e w tia 1 i SI 0 1 jj 1aS fli 1 f il 1 2 3 4S s SL-2. LM-1-1 SL-2, LM-1-2 SL-2. LM-1-3 .PST ' j l A -- - K 1 A\ SL-2. LM-2-1 SL-2. LM-2-2 SL-2. LM-2-3 SL-2. LM-2-MS -- -- SL-2, LM-3-1 SL-2. LM -3-7J SL-2. L M -3 -/J d a tila J -- - r* (N, V J \5 IX SL-2, LM -4-f SL-2, LM-4 A SL-2, LM-4 -1 SL-2. LM-4-MS i.a n e - 0 J -- -- >l V-r X 'w i N s, V. s i I S L -3 ^ 1 -1 o rt " Va. \ 1( ..T 0 !i Ir * 7 -7 S II ti j5 i l * I il n 1$ aa 1 3 il !! s 11 ItX f n i 10 -- hy jy -> r~ k A #N J V J AVJ ____ 1 ri A < _c ~~ iS X i A Ac C! > y Q s il F \? || lit i l 11.* 12 13 /V 4 % i, i if 14 h i i , Ji l 1 J a. X aN. ,T 1 J X > r -4 < ^4 0 Sk j V ____ ^ L s I s ys S L -3? ih ^ -2 S L -3 /& $ -3 S L -3 ,^ t -M S --- -------- * _A L* >>14 - N L - Ny ' 4.l NL v S )'4 y L A j 5!'1f Ws.i1 'i Col 2 T/D 1-1t o 1 I C J ilK C Col9 ShakerID D S - j _____ 1 limili 18 Oh xj C 3 Balance ID,. 9 .0 ________Tube type/sizeW h.foiff .j L Equl Start T/D/l II'. /Ojua i h /f/T L -C ^ C Col a T/D J jlj. I I ) Water ID M i n i T G C tV s EquilStop T/D/Hr.-Vmrri 1 ) /IV /tM L P W c o n o t /d /i ) a ; s s j ^ h i i %7 ( 9 r i v e Col 4 T/D/l ft. jjyv III / 0 / - ( JiSwed/iettina i f l CentrifugeID: ) (1 2 .__________ Col S T/D/l L ? l ( K I 3 CfV M (6cf/^RM RMdoutShU Minuto. |Q ______Temp*C oK3y Centrifuge ID: | C i ________ c o n i / /t d i J ' 5 ( < r \ L>/ 1 % / ^ X C h r C RCF/PRM Readout: Minute < y L _____ Temp o i l c o iu t/d/i ______ <? i f r i /V iA co i s t/d 9.' 3 iW i L n I M v y & * < Water ID H i_U > - & T C lC ^ lv jSx Col 7 Sulking Standard ID 4 0 ,3 3- 3 - ~7T Col fP TID/1 \ > < P ta 1 1 *> I f . ) IAC / H C / / 1 Approximate Cone.Vfy>vn Amount added) C i l i ' - L . Coi 4 1 0 A !< iiff M C W tA T/D/l I c l l b r I ftV -Q K f C M C W n /o i Ci 8J TWA- ^ 6 S' L /tS j0 7 ~ 3 M E nvironm ental L aboratory t*n < - MeOHIO; TN-A V./ O i i ' X - - ' .,01 (P L if t 7ry( po/f i t n t i y /'OtA /IH - ( j ) L j f r f T y , f 'F p ^ h y h J A St,, ? * - 3M Environmental Laboratory Page 233 of 276 Report E02-0443 Tenn. River Valley Samples T e n n e s s e e R iv e r V a lle y S a m p le s LabRequest:03-$</</1 SampleLocation2,Catfish s I I , 0(S/fld,l/D.-.idl at ai i j *1 e Wi 1 jjj 1 *B i^ jjl il H If ! IU f? i] f II I:lIl i| ! v -i y \f ll il ill ll jit i1 il il i 2 4 S 7 i e 10 11 12 13 14 SL-2,C-1-1 Jo?3^ A /] J - >^ "7? 4 A tr SL-2.C-1-2 i< N>-dV >? SL-2.C-1-3 -- *5 SL-2,C-2-1 ^osWTj SL-2.C-2-2 SL-2,C-2-3 -- SL-2.C-2-MS iF 42 SL-2.C-3-1 I5ilic| SL-2,C-3-JTJ SL-2,C -3 -f) -- .\ /g7 J1 3 A JI SL-2.C-4-1 ic & T t SL-2.C-4-0 SL-2C-4- i SL-2,C-4-MS --. -- ^3 SL-2,C-5-1 SL-2.C-5-2 ?00(fc o SL-2,C-S-3 -- SL-2.C-S-1 5s SL-2,C-6-2 SL-2.C-6-3 SL-2,C-e-MS V y .Cv,.J . VN -S V C" 'V. N V < 1 ,*5 Vd ( .J. u __X_ r* <3 <n e bLy c TOil V. -1 0 VJ .j _SJ K H C11 '00 i. o V N ^s C3 v. sr. k XNV3 0 V C** is N, O "'s. -J c, fLt,l vi r-aS\e yX% ?I t stS 1 * rS iN^ V* Ti> o 4 ui > 45^t-Vrirr-b--i- SL-2.C-7-1 J.m SL SL-2,C-7-2 \'__ i \; SL-2,C-7-3 SL-2.WB-1 -- . \ ' 7<'s ib) At\rf:k./ N \ ?i SL-2,WB-2 -- -- 4.Js. __'SfL y V SL-2.sa-i 6 > r</ T " 1\ t kJ /SL-2.SB-2 15----- \ - t oqX u X \ 'IO S - *<sx % 6 ti 3 0 0 2) C o l 2T /D /l_______ / j t d V S f ' I l t C C o l* Shaker ID O 5 ~ "J 1 J t e ______ __ Tub type/s a tC equ Stan T/D /l U .< C h *i(a < I f f l V O X C o l 3 T /D /l J ^ ' 4 f ) p v > ill caX P ^ W a te r ID W v ~ Q - T C L ^ V lA -S EquJStop T /D /l I l'A l^ I f l/ fiT /A T -C IW l coi io T /o /i ll iSjvr J h M jin l riv v (_ C o l4 T I O I I t o ( G k O f t s S w a m lin a ( j? c o i s T /D /i 1 ' 3 T / w L t i f f i t O - Centrifuge ID:. 2( bC ^ RMReadout3 c c .Minutes.l _ ,,T e m p ' c ^ C entrifuge :_ R C F/P R M Readout: M i r x j l . l ^ _________T a n x i ' C C o l 6 T /D /l? 5 L W 0 l l H i I t > - ( j f i - C . C o l 7 S p ik in g S ta n d a rd ID * 0 < p O 3 " 3 ~ 7 7 C o in T/D/l f l ^ V W M I K / l ^ C m C coi12T/D/i 13/Q 6 ifT i O water ID K A \ V\ \ " O l T C C f r \lA S Col T/Dfl 2>-it -] l iZ-yl f l V?J. A p p ro xim a te C o n e, p v * t A m ount added. I W j a L t / d/ i .tL - L & i a ___ ( a / ( t O b ' c * ~ c C fli5 :. T N ft- M b s ' n . 3 0 , ^ ( & / i X l 6 l -- c*+ *-c. 3M Environmental laboratory C O M 4 T /D /l A j V * / ' / /7 i/, / /'V > t/i MeOH ID: TW-A 4 5 * 2 ^ VjIQ ) L tf +d<y. j h o , <JM > - J* ^ .1 ^ u .7 ," W - /V of . J V /A 3M Environmental Laboratory Page 234 of 276 Report E02-0443 Tenn. River Valley Samples Lab Request: Tennessee River Valley Samples Sample Location 3, Large Mouth J TCi 9 1 I*% i 1 S ii a i il5 11 12 48 K 1SL-3. LM-1-t ; . o j c ,( L t SL-3, LM-1-2 SL-3, LM-1-3 SL-3. LM-2-1 -- J .o tllf \r i _T < j(l 1* 1, St ]| if 7 iL | a / S 1m s ! s \i J 5 2 f? U li II n 10 11 12 fS J ? lN _L w ! I Il il 13 14 y / Va i t j SL-3, LM-2-2 SL-3, LM-2-3 SL-3. LM-2-MS SL-3, LM-3-1 -- --- i SL-3, LM-3-1 SL-3, LM-3-1 SL-3, LM-4 SL-3, LM-4 SL-3, LM-4 SL-3. LM-4-MS SL-3, LM-5-1 SL-3, LM-S-2 SL-3, LM-5-3 SL-3, LM-S-1 OWrj -- -- n/ V itn O T j -- s '.' M u ta te V, 'S . 1 V Sa. 4. O sv ~*x: r- W SL-3, LM-6-2 SL-3, LM-8-3 SL-3, LM-B-MS -- -- * -IJ- - .I si \ , S- Ol 1 H VJ O O c'w SVJ SL-3. LM-7-1 Joiefit!T-t SL-3, LM-7-2 SL-3, LM-7-3 -- L. 4 tL > ( Coi 2 T / D / l ip il~l 103 CUC r> v! _s J N- \t V a. v c i 5r rjt JL. I h (lr S. Ad N5 M ?p* N. Ss Ci V A A s >* V \ - 1U % d \ I i I / / U i- A / sU * M II 0&5.UCol9 Shaker10 BalanceID *~lD Tube type/size]^ E quil S ta rt T /D /l IL ./tw , ( , I l f l , 1* Col j von O.HOpm 1 i l l I Waler10 M i Ui - 6 TO C i t o E qui! S top T /D /l( L ^ b iV v C l / W / ( j U ^ Coi io t/d/i C4c*n l r I K I X ctviC. Cola T/M TpOau, ie Ili/ I O l- Qoeed/eeltlna lo Centri/uga 10: | ( ^ 3 - ____________ co li T/D/i7:JSi*~ h i tir i (2 ai*, c ^ R C ^ /P R M Readout Minute ______Temp*C CenWugeID:_ .ZiJZ*________ 3OO0RC7/PRMReadout: Minute. XL Col T/o/i9.'lt'rw , (o i ( j f / f l . Ct/v-w Tenui*C /*? c o in T/D/il!43f.n 6r < H r/0 3 -C in C Col 12T/D/l VS - 6 - t l l j lA. water ID /jll : I t -P fv Col 7 Spiking Standard 10# Col 13 T/D/l l 5 O I y/Jl/d/ Ll Aooraximate Cane, t ^>0,- i Amount addedJ O O jaL T/D/l |V. --i--^JlK--r 5 sJjv i L_ Cal fr TNfl^HtsS Q 3DYVV b / t * f c n _ 3M E n w o n in e n W (.eboretory Col 14 T/D/l W / f / - i # * / * * 1 -T - ( t> K . O IO: t/S JO l/tW - ^ Q)Onl`j S i w r<-<> n > f ~^ ^ P eg eS ots , / / '>7rf > 6 ~ " 1 lr>~ i ` ^ ` $ 1 (J ) >i"J C-tit ff-Fk) f, c taeTnjf** ^ H 't*c& ,, r>` 3M Environmental Laboratory Page 235 of 276 Report E02-0443 Tenn. River Valley Samples IS - U O s c W C hi*>\ 5 - ($ , C ~ lb t Lab R equest: g ) - tft/< / > a 9 1 1 SL-3, C-1-1 SL-3, C-1-2 SL-3, C-1-3 i 2 i.mioJ --- I h 3 A Tennessee River Valley Samples Sample Location 3, Catfish BT 1 it il2 I j j j1 III 1! I1^ h 1C i%I a* u i? it i4 !1 ji fi In 3 fl if ?i! 4 5 < r 8 9 10 11 12 13 1s / . t \ 7 ^ / SL-3, C-2-1 1.%5-Ve / SL-3, C-2-2 SL-3, C-2-3 -- SL-3, C-2-MS SL-3, C-3-1 SL-3, C-3-1 -- l4 I.W S tf , 1y \ SL-3, C-3-1 SL-3, C-4 lo v i'h j i SL-3, C-4 y V. SL-3, C-4 -- % SL-3, C-4-MS SL-3. C-5-1 SL-3, C-5-2 SL-3, C-5-3 SL-3, C-fi-1 -- S< V JdfllMij -ft ^5 --. " x-r sf . t t O t t j s> l SL-3. C-6-2 SL-3, C-6-3 -- SL-3, C-6-MS ------ \ i SL-3, WB-1 SL-3.WB-2 SL-3, SB-1 SL-3, SB-2 -- - V --ffi __ V -b ' V s Sa 0 fk( l_ L J 4c < jd . o -- I-fe - X . n kl . 2i\n t - - h -- -I VU K X 4V- 5 Ir' V. 1 r *_JS> VT 'V / ^viJ \ n j VL > -N / f if 14 / ' i n - fik T7 K ' \4. , 15 C ol 2 (j l l l l O i C lU C JVuitjlVv/ 5ft>Balance ID C!OC>_________ Tube tvpe/alza '* L. C o i3 T /O /l i J Q O p n ( { I [ I t (T>-- C t * - * - Mt \ l IWater ID TC^^S C o l 4 T /P /ll'. O V ' Id i l k i t ^ - O ^ ia M U n M n a O ' C o l 5 T ID rt itg I O J-Q *~ C Centrifuga ID:. ' T c , - z RCF/PRM Readout.Z c c I C?--- ... . .Tmp*C Q C o l 6 T/D /f ) ' 3 r W r t / f l/ S / f c r f - C *-C . C o l9 S h aker ID . EquKStart T/D/li> .0A(j/f&/CO-mC. Equl Stop T7PJIil-SW G /UrtffLO^ . coi io Q lT m & t V p * L>i m 0 2 - CwiMtupaIP: I Ci _______ ^RCF^RMReadoul:.3QdD Minutt j JTarnp "C. coi it T / D / i L? i it) o x c*.. e Col 12TID/I /flfal 0 ) W ater ID . ri;lh -O PU { roc r/*>) C o l 7 S p ik in g S ta n d a rd ID * 11 COM3 T/P/! ( 7 ) 9 m i y " ! m A pproxim ate Cone. ) Q p W \ A m ount added lQ * ^ L lL T/D /l I p I i?CffiT M 4 8 :7 ^ * ^ ^ ^ r 3 iiiV ^ ^ V , g / 6 X ' 3M Environmental Laboratory C C o l 14 T/D ( P ? D 3 0 / X '. / t f / f o t M eOH ID : T N -A _ j ^ S M J - w ) 5 ) 4i? PstT\?'i * -- ** - M M ' (^ * / V Page 6 o 6 y in > f . l i s t ' 0J *. f" V l 1 I i I liti I-----1--_ J 1 i 1 1 1 1-- 4 1 1----------1 1 1 - i 7 - , --- u t e r i Uff7 t r t i f r Y r s ~ * r t t h & i G / f r f / p y * V f T r f t ' r t W ' U W t & { 3M Environmental Laboratory Page 236 of 276 0 5*0 Date Started: 15-Oct-Q2 Study Number: E02-0443 Method Used:_______________ Soil Extraction Worksheet Study Title: Tenn. River Valley Sediments. __ $ qV Type of Column Used: W ater c-18 tri-funct, Sap-Pan, ig, tec * * vt `v _________________L o t*: ___________________ Report E02-0443 c i 5 D : .D z 1a i 12 e e *9 Jt % ? f 11 U 4l % o 11 ji E i ea 1 li t" ! 11 t a i m 3 JeC i l 1m a o 2 ! i li s (1 A O lis 9 mv 9i Hf ? i 3 4 i 878 9 10 E02-0443-38044-1 T. R. V. Sediment 02*0443*38044-2 T. R. V. Sediment V 5 7 5 7 T F - . .. -16 i t r S y l . 0 & < t5 i T s iS" <s- . y l7 *r 02-0443-38044-3 T. R. V. Sediment ilo r z ? u y !/ \ s is E02-0443-38044-3M : T. R. V. Sedim ent MS 02*0443*3804S-1 T. R. V. Sediment n c .o tji 1/ V ys . G iS L u E02-0443-38045-2 T. R. V. Sediment 602-0443-38045-3 T. R. V . Segm ent E02-0443-38045-3M: T. R. V. Sediment MS M .. t H -- -- 777 S i} y %s S ' 'S is y y y Lr 1* iS E02-0443-38048-1 02-0443-38048-2 02-0443-38046-3 T. R. V. Sedim ent T. R. V. Sedim ent T. R. V. Sedim ent l i 1l l ? IO , C 4 T 9 S t X G 'J i -- Jl -- Jl -- *> iS s sr / s ir S y y iS U S 602-0443-38048-3M: T. R .V . Segm ent MS sy Ir y ty 602-0443-W B-1 W ater Blank, no sed. -- ) } \S S s Ir /r 02-0443-W B-2 E02-0443-LCS-1 02-0443-LCS-2 E02-0443-38044-4 W ater Blank, no sed. Lab Control S p ite Lab Control Spike T. R. V . Sw fim ent -- -- --n ir ir J t r {' \S i. y j? \r S is j i %/ 1/ y ir ls M oTy 02-0443-38045-4*. T. R. V. Sedim ent E 02-0443^804fM O : T. R. V . Sedim ent MS 02-0443-W B-3 W bter Blank, no aed. E02-0443-LCS-3 Lab C ontra/Spike 02-0443-38044-5 T. R. V. Sediment E02-0443-38045-5 T. R. V. Sedim ent 02-0443-38046-5 T. R. V. Sedim ent E02-0443-38046-5M ! U. R. V. Sedim ent MS 02-0443-W B-4 W ater Blank, no sed. E02-0443-LCS-4 Lab Control S pite ecu 6 I f . f iis ---- \S 3 ^ fW o / AO C o l 3: Balance ID f / V t /m IC S D - )3 S r / ( % P i T fcV / . * ! iA- n S ys U S y r -- y Jl V y U 1/ J l u4 y > y ji V -- } s *> f l \ s 4/ /y y y r? y ,y -- *<Q iS <> s it a-- / . . y 77?C ol 7: Centrifuga ID: '? Sneed: S* C*J** Ut/ JCpm L IS ts l* Lr * j w y C o l 4: Standard ID ' 1 0 S 0 - i P l ' j D uration: /-)/ ________ _ _ TUM .ton u n . - r standard Concentration: ! ih ivv? r s Am ount Standard Addad: C o l : T/Oa /.T / . /; : ? fi- t/o/i iQ iG t C o l 5 Standard ID: f t i 'lf j ~ Volum e Addad: 1 L n e ir t. C o l9 :T /a i ; , w 5 / . J / o , ? V / C o l 10: MaOH IP: T A A A - O A V W T fD /1 H i Q C i i r i v T t o f ' l i * - Volum e added: . n L _______ , . . T/D /l O t t i / / 3 7 T 9 1 / / j f - Col 6: T/D/l ' > t> ' J l . J . T *:j v , * t W - 1 i *ea0 a O 11 is \S IS y rIS y Ir y y y LyS yJ i-m ts tA y if y (X /> S V y w 4 i 15 s i 1]9a tt 12 13 i e il | i 14 i u s I] O I?JJiL 1L 16 16 1 17 _V* L S U iS tr y p y yy 7 y LS *r tr ir O ' Lr iS r is U Lr ir * .. . . Ir Ls L iS ir y Cr (S yy y Lr L cS ts s LS ir . y y LS StrataX. 8&S100-FC H. 1000mgmL L u \S L (r StrataX, 8B-S100-FCH. l000m g/6m L / - 7 ) StrataX, 88^100-F C H , 1000mgmU L y u /y S y - S cc y im V * f rs 4 O* ir u V > StrataX , 8B -S 100-FCH. lOOOmg^mL StrataX. 8B-S100-FCH. 1000m gm L t r j * S trata C ia -E . 8B-S004-JCH-S, 1000mg/6mL S trata C18-E, 8B-S004-JCH-S. 1000mB/6mL Sbata C18-E, 8B-S004-JCH-S. iOOOmflmL S tnria C18-E, 8&-S004-JCH-S, 1000m gm L S trata C18-E, 8B-S004-JCH-S, 1000mg/6mL S trata C18-E. 8&-S004-JCH-S. 1ooomg/6mL c o i i n t /d/i & w ta tu * u - C iri 12: C entrifuge 1D:_ Soaed: C9 0 O tSknm D uration:. tom a ta n y Jnrf-Q?^/ S lA- C ol 1S :D luter ID:_______ Volum e o f sam pie added.. Volum tri Douent Added:. M uent IO_____________ I Final D ilution F a c to r.. von________ C ol 13: T /D /l I G a / Z l n c T C V l / M l S - /7 \ / _j C ol 14: T/D /l / g / l i Q f l O c T W l / M U C ol 16:lntem al Standard ID _ Interni standard Cone. Am ount Addad:. Volum e cri sample:, IS C oncentrt r m ___ -Exact CopyofOriginal __ Tenn. River Valley Samples Samle Extract Storaae i&zA ' l o - < L.r l / l I >` ii ' vh * 7j l 77M.ai I" .I n J i'^ i V c'i. I i.- V ' W J t 't_ r j J 0 n -7 T 7 /W y /. . s t & / A r e * j Initial Data U t# : $300-18, Production Lot: P300080902 StrataX, 8B-S001-JCH-S: C18-E Sorbent, Phenomenex Leri#: S201-13. Production Lot: P201081202 Pag 1 of 2 Report E02-0443 3M Environmental Laboratory Date Started: 15-Oct-02 Study Number E02-0443 Method Used:_______________ Soil Extraction Worksheet Study Title: Tenn. River Valley Sediments. "7N o te s : _________ Removed Bottles 2 o f 4 to r each location from Ihe refrigerator. Placed them o n e shaker at am bient tem perature a t 200 rpm . Caps were taped before placed on shaker. - l Z. /CA/Hjfre^tiTt.JOJXeeldat/aorfiLffd&mlP.tn of 6 7^0 ?D f a d eat i4 ~fubeKi tF7cio rT%er<ick mlamrcY<i/.aiyM_i#._y37t_\*_'7Zss'4eu{if~b*J^cTe).rerJt~)T\Iz&L>rDCeC-a\t.ca^__//$o01?c5Ja0Q^_^-'>5o, yaI}rISSi_d'_Of_>b/_'^V__r~U_aA_-i_4v__fjr_teS_tj_.r'_/,,_*_'f_a_--Lb_ri 0 0 0 R CF'i /o r elQ ut/** ~ TinJfn//ee) far vJ/ D r C a n t e d t k e, / t j u l t ) I . t o i ( ,p f > r a f > - _ l a & f i J p t ) 0/ r (' W ftlh i' d i f l mf l Ui C / S'n* liflr r / //! 0t i ) <*sP r* (U ) ,* u /- / K O x /iU 5 0 ff L. * !a . -C~PI?r ------- S I b j - l & C X s f'd P jL ----------------------- :A. ti . Tip / n j? * R-H. f iJS i f f /...7 C'c i~ t'A ,f P t * U j ) /?- r t r h T m <0 ~ i'/Z &* y r. J sZy Art!**-, T * l \ 7 ~ /* * i/*- < K O -.STJ __ _ __ V __________T h e \*/pit]hrr'j-^jT sgmn/ei &/<?*, h e Tt TtD/ so*fife'* v'csv T ' Lhe W i .? _h__'_p_a__ _( ) fL>-f.-- tI ^~ S D ,e______ T hgr- rVysit^tii-LJfier r rf>/ -O.!>.T ry riri.r.r. \ ts t Tro-i ^ -> " iAi* ?---*-->---*----- '#' - M_-_ - S*?Uf - / /y y c 7 /J UieJ `jr .L g / /1eC>/ to v/asti Me. h,iere/of t<>fu*>n - T A /~ A -0 (3 1 ! -/* fl4 - irkT 0X __________ -/3)ix>vtL uZ-yty? Of1/ - T A f-s1 /fl&ffiPsHUt-- >cj-eu -~T%e T4e__Qtf -fro-* ke step&j uscts %PE.,p<LC& h 0 rrf(eni /iy) __ ffjo/ Ji le c S ff 'py _J*. - - ~j T,%, y +a .__`J1t_1un sr Ma *t a e^D ___ --51__c *-L ' / h, / i, ,lfh -^Q _1T-uOr wC#r//yoj i --wWJ *f Tr yt f. ._~/~V* i*tt "T ~ *?< t ^-~ _ __ _ ~^g__ 5anjl/<n.1df-ehS ?~ ca/omrit usrs'r j~km oy/^c) Tt> LQnr/>jr~fs*7+ -H r <>L>/u V/a* C&X C P pT^3'' ^TraTs C~l % __ u ___________________Tke s-nre T k fn J u fr r ) w / u b S I*O H C T A /-J'0 6 X I\ __ _The.'ie mfuiHn '(fyyp'jf*r $- ke.Hi/i _ L i_ lO ftn Y o / ~t a $7?,i 6 i*-rlt j- -fas- a ^ OvfaftJ / / .^ , Q * /y '-h? s h h / i /.{ 1> '* * H * 'tM T h t 0 r)-? iv. n aSn i ' , U / r / y f S t> Y y l p C t f 7'V r' C r y j l t / r e / r H B a e t C c p T o f O r i g i n s ! InitialAl\Ar 9 - P /r (ft- Date Tenn- River Valley Samples Pa9 238 of 276 P ap 2o f3 Report E02-0443 Tenn. River Valley Samples Tennessee River Valley Samples Lab R e q u e st: ) Extracted Curve Information 1 t H 1mjQ m 9! a w!250 s 2!e j 1 ? 3*. p| * aS:a 14 If 1| M 1 11 ^ n 1H I 3d g iaf"fe !- lx 1 In 32 1a.-----E * 5 ^ lit III I i l! if ! UM1-&fUH2I-I403m(4/ 6 riCiTt-L-i-f-l-_--_- 5- M-<0/ W.6W i// i/ s \S7 I 9 10 t/ </ / (/ j ITii . 12 13 j' t/ i^ 14 i/ l/' Oirj\jrJjbii15onifi-Aiv (^an/sipir/-',PiHiJkij,,i-S/*if--,nfai/r*. cmik)i'<ih \ -V.f> 1 M AlJh'J2c o l T/D /l ___ iV Balance ID `Z Q O ________ Tube Ivoe/slza ^ S / * / - C o l 3 T /D /l ( g ft * cl l l l > n l 0 J M h W a te r ID f i U h 0 TOC P /,,> _________ C* C o l 4 T /D /l ( 7 / 3 5 ; ) / J .X ., / S p a a d /M ttin g X Z _____ . C o l 5 T /D /l /rX 'L -* ___ C entrifuge ID: Q & / / %~ iT - ^ RCFJ^RulReidourR7^ Minute 47TO c o io r i p n l l Q O )/ / X w ^ - t ^ Temp*C4& C o l 7 S p ik in g S ta n d a rd ID # O J 0 ) 3 - 0 / {? .) O iJ o /J A p p ro xim a te C one, t*/" / * * * A m ount added____________ CU 0 ' C > > J O S i O Y " C'SS> T /D /l / .J / / 7 .'d / 17 6 ) / 6 1 / 0 / I l K L _ i L / Z - V i J U 3 ~ 3MA E(rt,vVironmI Dantal. {.MToVrat.or4y V `/ i --------------- \ Cole Shaker ID \.. s: .* u. q dl S ta rt T /D /l i % 1 l * , U U r f h . q tfil S lo p T /D /l / V /t f J ( / 7 w 4 k r W S**1' CollO T /D /l ^ l I X - f / / 7- C entrfuga ID:.. ________________ 5 V 3 J.IC o i n T /D /l / ?/ / ! 01 s m Tamo"C/)} C o l 12 T /D /l f ^)l i J ^ 'l fi W a te r ID . M ' J h - Q T O C P h i C o l 13 T /D /l l b > 0 C o l 14 T /D /l / 3 3 p J j / J - i / V M eO H ID : T N -A f h ' O A o / l / W ) m L v h f U u Page1of1 3M Environmental Laboratory Page 239 of 276 Report E02-0443 Tenn. River Valley Samples Prep Date: Analysts Initials: Non GLP SPE Columns Extraction Worksheet 6/20/2002 OK Method Revision: Study Number: Q tio i ETS 8-154# - su*- H it , (fi E02-0443 J. Volume ot Sample Number sample or description filtered water blank E02-0443-38025 E02-0443-38026 E02-0443-38027 E02-0443-38028 E02-0443-38029 E02-0443-38030 E02-0443-38032 E02-0443-38033 E02-0443-38034 E02-0443-38035 E02-0443-38036 E02-0443-38037 E02-0443-38038 E02-0443-38039 E02-0443-38040 E02-0443-38041 E02-0443-38042 E02-0443-38043 E02-0443-38047 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml 40 ml Type of column used 1g. 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C1B lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 20S7B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, CI8 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 20S7B2 1g,6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, CIS lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 2057B2 1g,6ml, C18 lot 2057B2 1g. 6ml, C18 lot 2057B2 1g. 6ml, C18 lot 2057B2 Amount and spike mix used NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Elution solvent and volume MeOH TN-A-6116 2ml MeOH TN-A- 6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TNA-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TNA-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN-A-6116 2ml MeOH TN -A -6116 2ml MeOH TN-A-6116 2ml Comments - ^ 1 f // Extraction Steps (initial when/if done): C *ij condition column with MeOH; r-K . vacuum dry the column; c K Additional comments: wash with milllq: O f * ' filter sample; { C Pelute column with solvent; o/transfer extract Into an autovial , ,a J) /> ' ;Q {) bttft) c /( t-'i t<r'> \~t 1^,, on/'/ *V 4 y . l i f l l l f . S* <* ' ' / fft 3M Environmental Laboratory Vnttiai Page 240 of 276 Report E02-0443 Tenn. River Valley Samples Non GLP SPE Columns Extraction Worksheet Prep Date: 7/17/2002 Analysts initials: OK Volume of Sample Number sample or description filtered water blank E02-0443-38026 E02-0443-38027 E02-0443-38028 E02-0443-38030 40 ml 40 ml 40 ml 40 ml 40 ml Type of column used 1g, 6ml, C18 lot 20S7B2 1g, 6ml, C18 lot 20S7B2 1g, 6ml, C18 lot 2057B2 1g, 6ml, C18 lot 205782 lg, 6ml, C18 lot 2057B2 Method Revision: Study Number E02-0443 rJ * Amount and Elution solvent and spike mix used volume NA MeOH TN-A-H6 2ml NA MeOH TN-A- 6M6 2ml NA MeOH TN-A- 6 m 2ml NA MeOH TN -A -H i 2ml NA MeOH TN-A- 614. 2ml ^ Comments V "J -g_______ Extraction Steps (initial when/if done): P K condition column with MeOH; ( M wash with milliq; p ^ f ilter sample; D K -j/acuum dry the column; /? K ielute column with solvent; p / < transfer extract into an autovial \ Additional comments: oK 7 ^ 02. Exact Copy cf Oi : a&Initial r~ ^ e c ~ h ' c r m c ju ^ S . hi'Jo4fof**T Lf;1wsioJy<W ,, *fJtf, ^l*-H9" 3M Environmental Laboratory Page 241 of 276 Report E02-0443 3M Environmental L a b o ra to ry _________ __________ ___ Description: -i f c o r f r Lrt Fift ( u / j *. Date Prepared: A I Ju,, m _________ Storage Location: S M ULTI-LEVEL PREPARATION LOG Book No. 02 003 PageNo. 52 Solvent: / i e H __________ Standard ID # Description 02003-52-1 02003-52-2 02 003-52-3 02003-52-4 02003-52-5 02 003-52-8 02003-52-7 02 003-52-8 (ppb') s5 .S 10 a s se> 1 0 0 0 S 0 Component Standards Description hn 5o,i> /ft\r ID # Cone " ci72 i Oioyi-o+'v:?. 1 Ipt* Expiration Date )i/Vox Std 1 Std 2 Amount of Component Standard Added Std 3 I0 u t Std 4 0uL Std 5 Std 6 SOuL l& i/i Std 7 -- Std 8 -- --l-o--o-pfpfn--,* f-eft--',-!<---*-----/--f-i-x-- lOOfp* "h>/oi -- ---- -- -- -- Sj L -- -- ---- -- ---- -- -- _ Final Volume (?* ^ Final Concentration (ff^ 'S * a 3l sI O .S t o >5 So to o so Tenn. River Valley Samples ____________ Page 242 of 276 Standard ID# 02003-52-0 02003-52-10 02003-52-11 02003-52-12 02003-52-13 02 003-52-14 02003-52-15 02 003-52-16 Description Description Component Standards ID # Cone (ffb ) Expiration Date $00 Std 9 7 -S 0 !(P 0 0 0 -- -- Amount of Component Standard Added Std 10 Std 11 Std 12 Std 13 Std 14 -- Std 15 -- Std 16 * M t/ ft- ) Ala i- O l -- i 0 0 P/** uM / o \ -- |(M -- |5 v y C -- ^ 0uL -- U --. -- -- -- -- -- -- - ---- -- -- --' -- --- -- -- ---- -- r ~ ----- . Final Volume (*> 0 Final Concentration 500 * IO O O 0 " ' ''eZ -- -- -- <2>ufc -t^ 'U ii rc-c z it i,} - ^ Copyof Original R8viewed jU -J U O 51 D a te J I I II Report E02-0443 3M Environmental Laboratory Description: k - i t r . d s i ) C o t l ( o ' * Date Prepared: 3t Tu~ 0 Storage Location: M ULTI-LEVEL PREPARATION LOG Book No. 02 003 Page No. 54 Solvent -- " Standard ID # 02003-84-1 02003-64-2 02 003-54-3 02003-54-4 02 003-54-5 02003-544 02003-54-7 02 003-54-8 1s A S 5 )D 3 5 5 o too Component Standards Description ID # Expiration Cone Date Std 1 Std 2 Amount of Component Standard Added Std 3 Std 4 Std 5 Std 6 Std 7 Std 8 -ipiffi--n %f i1k-t1>--*A--iv---i-n----M----tO f----l--- h f1 OOfn $p)k* /InrinfllOft bhO&-0Y> ODn*** I'Ai/di */i 3 / oa -- 3 uL -- -- KL -- -- I0O -- -- c)i/ C -- -- S0U 10$UL ---- ~-- -- -- u L -- Final Volume O'1^ 3 <3 3 3 ak 3 Final Concentration I a .s S to 3 5 So f ... ....... TM " Standard ID # 02 0 03 4 4 -9 02003-54-10 02 003-54-11 02 003-54-12 02 0 03 54-13 02 003 5 4 -14 02 003-54-15 02 003-54-16 Description S0 0 ?So IO O Q -- ---- Component Standards Description ID # Expiration Cone Date StdS Std 10 Amount of Component Standard Added Std 11 Std 12 Std 13 Std 14 Std 15 Std 16 --I0 0 *fiip~ , r f i i f in f t t O H OOltn l & u t (9< sL 2 0 < ,L O u t- -- ft -- -- -- -- --- --- -- --- ---- -- -- -- -- -- -- -- -- -- -- -- ---- Final Volume i m L ) Final ConcentrationI ^ 0 IO o --- -- --- -- -- ----- -- ( 2 ) L c * t e .-vVrv^ "TK i r t - L w S " C.-V- j i y t s - t py of Original m tta g i initial Data Reviewed y-j n J f r Wi j 2 ' V t O R V k A & f i l -- Signatura, 52e Tenn. River Valley Samples Page 243 of 276 Page 244 0f 276 3M Environmental Laboratory 11 IIIt1 D escription: K s A C x x r \ , < __________ D ate Prepared: J n r ru ^ P n x _________ Prepared By: r 'JO.C. Storage Location: E xpiration Date: M U LTI-LEVE L PREPARATIO N LOG Book No. 02 003 Page No. ____50 _______________________ S o lv e n t:_ M e o H _________________ __________________ 3M T ra c e # : T N f t - ^ s a o Standard ID # 02 003-50-1 02003-50-2 02 003-50-3 02003-50-4 02003-50-5 02 003-50-6 02003-50-7 02003-50-8 r-- "-- Description " Com ponent Standards D escription ID # Cone E x p ira tio n D a te Std 1 MW ---IO------^^n-1#--v-x---- M----W-------______________ _ rs io P J -'T R V i' **' cu n o s -3 1 lo O p flr * -------------- u /3 3 fo i- I J U I l/ / - -- Std 2 5 > L ------ S -a=> .iQ C h t* 9SQ LU. Am ount o f Com ponent Standard Added Std 3 Std 4 5 om l. IO O >lL ---- Std 5 S S O ^u L- Std 6 5C O >L- ---- Std 7 lO y n L - Std 8 -- as> L Finai Volume Final Concentration, o n V . l.O 3-5T SO IO a s so ID O > a s 'o Standard ID # 02 003-50-9 02 003-50-10 02003-50-11 02003-50-12 02 003-50-13 02003-50-14 02 003-50-15 02 003-50-16 D escription H* In iV /^ M i Y Description Com ponent Standards ID # Cone SQ3flb. E x p ira tio n D a te Std 9 -J-2dtT !__ u / a V o i . o a o o a - 3 3 1Q C o V -- SCp**- n s o o *L S td 1 0 -- ~ |5 ^ L 1 0 9 O !. Am ount o f C< m popent S tandard Added Std 11 -- lO O ^tL St . I S K 1 3 Std 14 ^ ____ Std 15 Std 161 Final Volume Final Concentration, p n t > ( > O X - P o 7 l* ~ o i . ExactCopyof Original /HA Initial Data I v i^ - 5oo 150 -> IO G Reviewed bv Signature, A .-- ./ j Date i Tenn. River Valley Samples Report E02-0443 3M Environmental Laboratory 9 Prep date: Analyst: Target analytes: Exact concentration of every point of every analyte O ~Vi 1 CMC ___________ Solvent & TN-A #: |M M H T M f t - - ~ l , ^ C \___________ final Volume of each point: ____________________ FCSA P r X& , _______________________________________ Standard mix used for preparing the curve: rP M frs g Book No: 02003 Page No: so ZO (t> *o o 3. m o K) 2 J* CO _______ Term. River Valley Samples ___________ Page 245 of 276 W - o n o * l & initial Dais Reviewed by: Signature, Date i Report E02-0443 Tenn. River Valley Samples rr civ SINGLE COMPONENT PREPARATION LOG Date; * 1 O c i i/?2 Analyst: / VJ L .i-_____________ Book No. 02 050 Page No. 34 iDescription: m / e n f i k / i t v _ m V i t t n lz 0 > l PFi. r i A s Pf O 3 Stock Number_ Weight orVolume Used: I / 00i/ i- Concentration or Purity:_ im ft* Corrected Weight: Final Voloma: Storage Location: 3 V 'F lr Balance ID: A /A Other Correction Factors: Solvent and TN-A . Number i / j l f / u t J W u 7 / > r - (A 'U r roc /%>) Final Concentration: ) Expiration Date: g) 3 A/UA ExactCopyot Original "7' ' /j Reviewed by/ ^ U I s L / i i s d - l c , ' 1 1 / ( / 2 ^ S tonatura, f J O ale 3M Environmental Laboratory Page 246 of 276 Report E02-0443 Tenn. River Valley Samples MULTI-COMPONENT PREPARATION LOG Book No. 02 002 Page No. 33 Description: .. Date Prepared: ( p / I f f I DO-- Prepared By:_ CMC_______ Storage Location:_ a n d Expiration Date: / S o lve n t: 3M Trace #: TN-A- f n l l l n Description V fpb F o S ift P f OP. PrBS Standard ID # 02002-33 I Component Standard ID# voteci -i~ r Cone, or Purity 3ns- PP1^ OSlOOt^Ci 4 70^ f? ** o a .c D i'O jri 3 \ U 0 Expiration Weight or Date Volume V i o l o * , "TS n^L 551^ L. \J /o|b3 oM t W S^l Corrected Weight Final Concentration Balance ID - , 9 --1 NA to ft I0. Oppyw 100,^ ppvw "-C. 6 jOPnrx " / 3 j > O a o o l-^ q 33CM lO'V - ppiv^ a j j l ? ) b i \ \F _____ ^ . ------- - ii 1 P j C ...... ................ Final Volume |Dp^\Approximate Concentrationof the mix ) rt(A-ExactCopyof Origina! Initial Reviewed Signature, Date 3M Environmental Laboratory Page 247 of 276 Report E02-0443 Tenn. R'rverValley Samples SINGLE COMPONENT PREPARATION LOG Pa* tifitiQl*- Analyst_______C AA.C_____ Book No. 02 022 Page No. 77 Description: t p ^ / w S 'i l^jt_ M tV ? Stock Number (&*Q> - , , * r - p e t & l 2 ~ 3 ^ Weight orVolume Used: 2m - i . ,c w ' ce lD : Concentration or Purity:___ I D Q p p p r t CorrectedWeight_ <-1 ! 1* 17f (T -'- SolventamNnduTmNb-eAr.,^ ; U i:QLI f X- .yt UAV Final Volume: Storage Location: >S,nL AA cL i PpWLFinal Concentration:____ Expiration Date: I t j 3.^ j O ' L - ^ ExactCopyof Origini MA- tfNlkW Initial Data/ Reviewed by: Slanatura. 3M Environmental Laboratory Page 248 of 276 Report E02-0443 Tenn. River Valley Samples < SINGLE COMPONENT PREPARATION LOG m _______ Analyst, A l l A ____________ BookNo. 02040 Page No. 80 : /% Description: Arctic ActJ. /"h b - Q Stock Number_ ( f jp /ftA - u tf ft b j Weight orVolume Used:_ Concentrationor nPurity:_ CorrectedWeight:_ ma Final Volume:_ M L_ BalanceID:_ Other Correction _ Factors:, Sotvent and TN-A __ Nummbbeer:r, ,lk-f2 TOC P/u S __Final Concentration:, 13L Storage Locatlon:_ y ^ F k frm ___ ExpirationDate:, c g *# * L&x v$ Reviewedby: Signature, D ate 3M Environmental Laboratory Page 249 of 276 Report E02-0443 Tenn. River Valley Samples Date: SINGLE COMPONENT PREPARATION LOG | - t O - O Z __________ Analyst:________C K ) _____________ Book No. 02 001 Page No. 17 Description:______ '7T ~ R S Stock Number Weight or Volume Used: Concentration or Purity: % e% Corrected W eight *U Final Volume: `Slid Storage Location: & Balance ID:_________ Other Correction Factors: iJA MeOH fa-A3Solvent andTN-A Number Final Concentration: Expiration Date:______ f-J0 * 0 ynafP pV] a *. 3M Environmental Laboratory Page 250 of 276 Report E02-0443 Tenn. River Valley Samples Oate:_____ J - j O - O S Analyst OK- Description:__ SINGLE COMPONENT PREPARATION LOG Book No. 0 2 001 Page No. 19 Stock Number______ O S , ^ Weight or Volume Usedd:: i 1 - 3 "7 GA ( / T T c Concentratlon or I P u r it y : . ....... U E C U L Corrected Weight: ik i Balance ID: Other Correction Factors: M. Solvent ainndd TTNN--AA Number ,I / . A "H e Q H I f f i i * r <2 ^> 5 *2 Final Volume: 'S A v t ____ _ Final Concentration:______ Storage Location:. flu jfcoC Expiration Date: 1 )0 *0 3 ^ C O P V o f O ria n a ' Reviewed by: 3M Environmental Laboratory Page 251 of 276 Report E02-0443 Tenn. River Valley Samples Feb SINGLE COMPONENT PREPARATION LOG Analyst / j ( A ' _____________ K KDescription^ PFOS book No. 02 0 0 1 Page No. 84 Stock Numben_ Weight or Volume Used: V ( p .J D d b j Concentration or Purity: Corrected Weight: Balance ID: m. Other Correction Factors: Solvent and TN-A Number: A ffir m * ) ^ ^ z/rrh>J Final Volume: Storage Location: ^ L L 01/pp*Final Concentration: ^ 3 3 Expiration Date: Fei>0 3 Exact Copyof Original l . L M ftiMaf Oats Reviewed by:_ CLJiLll^,j* ~JjJT--- Signatur;- I Data 3M Environmental Laboratory Page 252 of 276 Report E02-0443 Tenn. River Valley Samples Date: Analyst:^ SINGLE COMPONENT PREPARATION LOG Book No. 02 001 Page No. BS Description: r c - N i / p r o a ______________________ Stock Number: 9 *10*>(2) ~C30 Weight or Volume Used: r ~ lU ^ i ( u ' Z ) f f a i t y ______________ / i it I Balance ID:_______ / I f Concentration or (S f o / Purity:_________ 7 b ` 0 ______________ Other Correction ___ Factors:_____________ Corrected W eight H tO U h A /.A -M / Final Volume: i Final Concentration: r?IJ Storage Location: 21J T \r - Expira'lon Date: F * > 0 3 > ExactCopyof Origina! ! /lM-00lDec tniHai Date Reviewed by. 3M Environmental Laboratory Page 253 of 276 Report E02-0443 Tenn. River Valley Samples Date: Analyst SINGLE COMPONENT PREPARATION LOG _____ /1 \A _______ Book No. 02022 Page No. 66 Description: PfBS ! L- 70SZ,ur3 CCjP, so,*) TCR-me>n-e>?t / 1 cr -ss ? Q }/m >) Weight orVolume Used: 0 50$5q o> Concentration or Purity: 973% Balance ID: Other Correction Factors: m- Corrected Weight -W lf .. .... Solventand TN-A NTumber M e O M f J A / Final Volume: ^ S- ) _ Storage Location: Final Concentration: Expiration Date: Reviewed by: S io n s tu r /'/ D al J 3M Environmental Laboratory Page 254 of 276 Report E02-0443 Tenn. River Valley Samples SINGLE COMPONENT PREPARATION LOG Dato: s O o 'J u - n e . i - '-- Analyst: C M C _____________ ook No. 02 022 Page No. 79 Description: X ~ tv-\< \ c . ( p p K W ______________ ( fij) - * * * * * * Stock Number ( ^ r g ^ S . r g 3 --------------------- Weight or Volume Used: iQ y U L - Balance IP: V -Jfii Concentration or Purity: }Q0p(3)V\ Corrected W eight Other Correction Factors: Solvent and TN-A Number W QH . TN fl ~ 4 S J O Final Volume:_____1 l ^ r y t L Storage Location: ad. Flnal Concentration: d^fExpiration Date: M Reviewedby: S lgnalui, 0X Dal 3M Environmental Laboratory Page 255 of 276 Report E02-0443 Tenn. River Valley Samples TCR# Substance trade name or reference #: Substance/chemical name: Lot/batch #: Location of synthesis. Fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M# Entered by (Initials) LAC Std Locatlon/Storage F19, Frozen Amount of Retain 0.3610 g TCR-83 nan TCR Receipt & General Information TCR Substance # SE036 Perfluorohexanesulfonata Primary std Received from: George Moore Date Received: 09/03/1999 Amount received (wt. or vol): 154 g, 277.38 g gross w t C6F13S03-K+ white powder 10/18/2006 98.8% LAC 01/17/01 NB120087-69 Date Entered 09/03/1999 Initials Number/size of containers: Shipper: MSDS (y/n) Records received: 1/150 mL glass container Courier Y (J N MSDS, NMR Characterization Request #59085 Interim final report from Centre and Certificate o f Analysis. LAC 04/26/01 Checked By Date Date Checked by (Initial/Date) Initials Date 10/19/1999 Checked by (Initial/Date) Comments Standard has been moved to Freezer 19 in room 347 KJD 06/06/00 Sent to Centre Analytical fo r Certificate o f Analysis Analysis on 07/06/00 LAC 07/31/00 Standard was stored at room temperature prior to 06/06/00. LAC 12/19/00 Shipping Codes: 41-2600-9459-8. LAC 06/14/01 Original label - 8/4/99 RWW-11/2/01 Initials Shipping com m ents: NOT REGULATED, 3M shipping IO *1 -2 7 0 0 -4 6 4 7 -3 . LAC 01/10/02 Attachments Date Checked By Date se036msds.pdf se036nmrreq59085.pd EOO-1878-COA-SE036-PFHS-R Archived/Substance Not Available] a 3M Environmental Laboratory Page 256 of 276 Report E02-0443 Tenn. River Valley Samples TCR# Substance trade name or reference #: Substance/chemlcal name: Lot/batch#: Location of synthesis, fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M# Entered by (Initials) LAC Std Location/Storage F19, Frozen Amount of Retain 0.2233g TCR-29 PFOSA TCR Receipt & General Information TCR Substance # IMSII Perfluorooctane sulfonyl amide or Perftuorooctanesulfonamlde AC KJD 7/24/00 L-15709 Building 236 Received from: R. Buckanin Date Received: 04/20/1999 Amount received (wL or voi): 124.98g gross w t C8F17S02NH2 Number/slze of containers: light yellow waxy solid MCH 07/22/99Shipper 10/31/2006 MSDS (y/n) TBD, KJO 06/06/00 Records received: NA Date Entered Checked By 1/100 mLglass container Road Runner Y </ N MSDS, summary page of FID analysis #67915 Date Initials Date Checked by (Initial/Date) Initials Date 10/16/1999 Checked by (Initial/Date) Comments Initials Gross weight difference due to removal of parafilm LAC 04/28/99 Standard has been moved to Freezer 19 In room 347 KJD 06/06/00 Standard was stored at room temperature prior to 06/06/00. LAC 12/19/00 The expiration date was assigned based on hydrolysis study EL-1132 and photolysis study W2783 which showed this compound to be stable. LAC 10/31/01 Original label dated 3/18/97 - RWW 10/26/01 Shipping Comments: NOT REGULATED, shipping code LB-1000-1570-9. L-15709. LAC 01/08/02 Attachments Date Checked By Date sd029msds.pd sd029fid57915.p I; C i rchived/S ubstance Not A vailable / 3M Environmental Laboratory Page 257 of 276 Report E02-0443 Tenn. River Valley Samples TCR# Substance trade name or reference#: Substance/chemical name: Lot/batch #: Location of synthesis, fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M# Entered by (Initials) KJD Std Locatton/Storags F19, Frozen Amount of Retain 0.2737 g TCR Receipt & General Information TCR-123 PFOA (POAA) TCR Substance # TC R -isea-flsa FC-143 Ammonium Perfluorooctanoata (Primary Std) 332 3M Received from: N/A Date Received: 02/02/2000 Amount received (wt. or vol): 278.20 g gross wL C7F15COO-NH4+ White powder KJD-2/2/00 10/31/2008 95.0% LAC 01/17/01 N/A Date Entered Initials Initials Number/size o f containers: Shipper MSDS (y/n) Records received: 1/ ~200 mL glass bottle Unknown Y < >N MSDS Interim final report from Centre and Certificate of Analysis. LAC 04/26/01 Checked By Date Date Checked by (Initial/Date) Date 02/17/2000 Checked by (Initial/Date) Comments Initials Was originally TN-A-2143, KJD 2/21/00 Standard has been moved to Freezer 19 In room 347 KJD 6/6/00 standard was weighed on 9/28/00. Standard was stored frozen at -20C+/-10C until shipment on 1O/O3/Q0.LAC 10/03/00 Shipping Codes: 98-0211-0891-9/FC-SO0O-0192-O(<30 g on dry Ice) LAC 06/14/01 Standard stored at room temperature prior to 6/6/00 LAC-12/26/00 Label-recorded-10/98 RVVW-11/6/01 Shipping comments: REGULATED-TOXIC Dangerous goods In excepted quantity of Class 6, UN2811. 3M Shipping ID: 98-0211-7394-7. (4 lb. carton) fully regulated. LAC 01/09/02_______________________ Attachments Date Checked By Date tcr99030-30msds.pdf E 00 -17 6 3 -C O A -9 9 0 3 0 -3 0 -P F O A -R O Archived/Substance Not Available i w ip ) 3M Environmental Laboratory Page 258 of 276 Report E02-0443 Tenn. River Valley Samples TCR# Substance trade name or reference #: Substance/chemlcal name: Lot/batch *, Location of synthesis, fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M # Entered by (Initials) 1 KJD I Sid Location/Storage | F19, Frozen Amount of Retain 0.1867 g TCR Receipt & General Information TCR-129 PFOS TCR Substance # li"!...... FC-9S Received from: Potassium perfhiorooctanesulfonate N/A AC KJD 7/24/00 215 Date Received: 02/02/2000 N/A Amount received (wt. or vol): 40.1441 g gross w t C8F17SOS-K+ white powder 12/01/2010 TBD.KJD 5/5/00 N/A Date Entered Initials Initials Number/size of containers: Shipper MSDS (y/n) Records received: 1/ 60ml nalgene bottle N/A Y <_> N MSDS Checked By Date Date Checked by (Initlal/Date) Date 02/17/2000 Checked by (Initial/Date) Comments Initials Waa originally TN-A-2144. KJD 2/21/00 Standard has been moved to Freezer 19 In room 347 KJD 6/6/00 Shipping Codes: FC-S000-0185-6(<30gondry Ice) LAC 06/14/01 Standard was stored at room temperature prior to 6/6/00 LAC 12/26/00 Received 5/96 RWW 11/6/01 Shipping Comments: Dangerous goods In excepted quantity of Class 6, UN2811. REGULATED-TOXIC 98-0211-0888-6 C>30 g (1 oz sample)) Not on dry ice. LAC 01/08/02 Attachments Date Checked By Date | 1 | I tcr9903Q-36msds.pdf p^rrehive/Substarice:Not Available | 3M Environmental Laboratory Page 259 of 276 Report E02-0443 Tenn. River Valley Samples TCR # Substance trade name or reference #: Substance/chemical name: Lot/batch #: Location of synthesis, Fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M# Entered by (Initials) KJD Std Location/Storaga Freezer F-19, frozen Amount of Retain 0.2826 g TCR Receipt & General Information TCR-SH PFBS TCR Substance # TCR-00017-071 Potassium perfluorobutana sulfonate 2 W ildlife Received from: W ildlife Date Received: 06/30/2000 Amount received (wt. or vol): -100 g, 121.5265 g gross w t C4F9S03-K+ good/ fluffy white crystals 01/17/2007 97.3% LAC 04/26/01 L-7038 LAC 01/03/01 Date Entered Initials Initials Number/siza of containers: Shipper MSDS (y/n) Records received: 1/ -100 mL plastic container unknown Y( )N MSDS Interim final report from Centre and Certificate o f Analysis. LAC 04/26/01 Checked By Date Date Checked by (Initial/Date) Date 06/30/2000 Checked by (Initial/Date) Comments W ildlife international Number 5292 KJD 6/30/00 Standard Is being stored in Freezer F-19 at -20C KJD 7/17/00 Formula added on 07/24/00 by KJD Sent to Centre Analytical fo r Certificate of Analysis Analysis on 07/05/00 LAC 07/31/00 By F-11926 process LAC 01/03/01 Shipping comments: NOT REGULATED, (based on shipping code o f LB-1000-0703-8). LAC 01/10512 Attachments Initials Date Checked By Date tcrOQ017-71 msds.pdf tcrOO017-71 lotinfo. B E00-1877-COA-QO017-71 -PFBS-R : O rchlved/Substance Not Available J 3M Environmental Laboratory Page 260 of 276 EN R SfMPAj Irvri-Z ^wZ*z. Report E02-0443 3M Environmental Laboratory Atlanta Goleta O Wilminton Boston Houston ___ Dallas Okemos Walnut Creek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page -of. o s -t- c: . Q1V ils/<rccnut. HALi C n tr iv r A n te e t. <L2T.VrV r-\\ ( n IhoSTi.^ a n a l y t i c a l ^r e q u e s t > Client: Project No. UQHOi / ////////// // ' I ( U i . >& t U 1i r y___b__. ___________________ i :__/ - II II 'k Sample ID Date Time Comp Grab No. of Sample / i 7 Cont. Media / N r !i Ir l l II II II ! II ! / II Comments ivX " $>VJO\ V. VjVv/Ol " Q w p * W O I - L o u 'i. < S W O l - M ar) V L. P i s C O -- i- w / r S C 0 l-/1 a a | r iV i\ S V 03^ M IJ fi h . /I n II h t n u * ISSO n l\ noa X1 1 X X XX VX/ H I4 1 1 1 X1 \ Total Number of Containers Relinquished By ' .... i. Date U/jhi --i FORM ENT-131 11S "L` i y4f{sr A \/ z' J & ir - V Time !>a0 _f *''*'?* * * 'Ig O Z S 1 602. > 3S02.S 1% O X r V 02O ==SS^ - -- 3s o t ] Received By biaul UJW jJ Uli^Lindi h KlDe i Initial Data y ^ X ^ r-/3 r~ 7 'Arr*? , : .. nDa,te T_ime /! i "(U h U-.o^ Tenn. River Valley Samples Page 261 of 276 E RX _, \z c n - ( _ S f M f - t i S i r - j t l - "\ #I / o Z Report E02-0443 3M Environmental Laboratory Atlanta Goleta Wilminton Boston Houston __ Dallas Okemos Walnut Creek O Dearborn Olympia . East Greenwich Edmond Sacramento Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page J 3-- ofA e----.--------- -- ------------ *----------- i--ul eCMn^M,AWwIIIOIa*.Us-f-i-i-f-*-/* --------- 1--------------------- Client: ' Prajent No. l '7 `3 l D ) ANALYTICAL REQUEST i E S n fa ty , K d . & v V I AJcMMo Sample ID Date Time Comp Grab U o ^ -D u p C ,W ls - L o w t f j l l OifOO HtjoS \t * X >V 0 3 - M ^ e / I y W CQ. SW C Q -$^Q Oo) - L o w lo d o A_ x XX U fO 'i'/W X fS C O ^ - Lou F S co '^ W T r't p b l<fnK ^ 1 j n! / >1/ X V Total Number of Containers No. of Cont. '/4 v Sample Media / N/ 1*/tVy / // / // / // // / . / / / / / // / / / / / / / / / // // / Comments 1 1\ 1 OSOl 3 *03 6 lio y ir 1 \ ) i- y io ^ \ y 'o r o \ V > f 4 1r 3 5 C K /-3 10 tu w FORM ft ENT-131 Relinquished By - ' Date Time i3oo Z' "* Received By 3 r~ * 1 J ` Date Time S tile n I.& 3 L Tenn. River Valley Samples Page 262 of 276  Atlanta Goleta Wilminton E RX Boston Houston ____________ Dallas Okemos Walnut Creek 02-O W jp / V I r t li \ **/ Dearborn Olympia Q East Greenwich * Sacramento Q Edmond Tacoma Gig Harbor Ventura Report E02-0443 3M Environmental Laboratory Tenn. River Valley Samples Page 263 of 276 FORM ENT-131 W 7 r0 y + *\ Report E02-0443 3M Environmental Laboratory Atlanta Goleta Wilminton Boston Houston ___ Dallas Okemos Walnut Creek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page .o f-S L 0 3Client: Entrix Cor Projec1Nn. ! /"Hfi 5 itESS&jWrti.U.hl1 Airbill No . 7 '5 -*W - ANALYTICAL REQUEST ,*v/ f i l l /// //// // *sy f I/ I / /I I / /I I / /I I / /I I / /! Sample ID IffSrl ! I !Date Time Comp Grab No. of Cont. S.a.mple Media // >*// // // // // // / /f /i l/ l / i / / / // / / / / / / // / I l / /I / /I ^ Comments lc& -LM o\ S U I - UM J t)L Dl - L P \ o \ J C l 0 \ - l M d l1 SLi- lf\O J SL01 - i * \ O b J fL0i " C A i Ol J Gl)-'C i\To^ U l -C TZ l)-O M 6H \" H i u X \ JL 1 J V/ Total Number of Containers 7HM - L -4 Relinquished By X lA l l i l ) \ \. \ V 4/ Io Date Time )3r/>0 ., yy 7 tf.S f *3%*f-i v 3 o ' *s' > 3 IC V/Ov^n, ). 1'K II'a* 1 C?rVi*t., . di 3h j I & C>o 3 3 ) !^>v. ; nt- 5 c^_ S r-ivi j il irr. 3 ! Gy 3tw . V Ib. Ij :i 'S i n-,^ ~J /j. j 4. &l i A- ? i) 1M:I, 6 //'. i A 2o i a'Mor:apj-oirioOnpgrmf/aii h-i'/i^ -.-'-X---/-/?--.------ j Received By tonfai Date Time 7 l -L -^ tj/zc/o?. / i' -- h n tfio h -i \V.CTO ; FO R M f ENT-131 Tenn. River Valley Samples Pa9 264 of 276 Report E02-0443 3M Environmental Laboratory 1 -/ f ... t Atlanta Goleta Wilminton E R X: 0 ^ - 0 3 ^ ' i Boston Houston __ Dallas Okemos Walnut Creek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page 3 ofJ3 Tenn R ,ver Va,,ey Samples Pa9e 265 of 276 FORM ENT-131 D Atlanta Goleta Wilminton EN TR X Boston Houston _________ _ Dallas DOkemos Walnut Creek Dearborn Q Olympia East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura Report E02-0443 >> Term. River Valley Samples ~l - ...... .  Atlanta Goleta Wilminton ENT R X bOZ-O'l^ Boston Houston n Dallas D Okemos n Walnut Creek Q Dearborn Olympia East Greenwich Sacramento Edmond Tacoma CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page - Gig Harbor Ventura Tenn. River Valley Samples FORM ENT-131 i EN TR [sOl-O^, Report E02-0443 Atlanta Goleta Wilminton Boston Houston _ _____ Dallas Okemos Walnut Creek Dearborn Olympia East Greenwich Sacramento Q Edmond Tacoma CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page Gig Harbor Ventura IJ ----- of P o:._. k n v w .U s e k .., u \ - _____ Kw .j ANALYTICAL REQUEST Client: Project No. / // // // // // 3S!, ' M & - U . { L U U . no Sample ID Date Time Comp Grab 'Urn * S L 0 3 -L M 0 6 l > Z -L M p$ Z i ^ -S lH o l S ld V iN 0 7 il V tt 1 l o ^ ' C A t O SLOP -C A T > S l ^ -C f^ o S W ua M It l f -C h T O H S L 'S -C A T O S ' H >1 \y Total Number of Containers No. of Cont. 1 \ \ ! \ 1 Id / >? / y / / / Sample / * / / . - / / / / . . . . /i.<sy / / / // Media / i y / / / / / // // // // // // // // // // // // Comments y V \ -A V * * , 3/1.. "a 3^0 j 1 *K P'- ?3-? 3 7 7 W O k f t * * . 3? > 2: >? i 6 / Ik *1 f>T . / /t. } 0 z _ . * / 'c? i ? t 3& h t. %a7. Nb X / 3* 3* acrcopyofOiH/.v ' P o i. t Relinquished By V Date Time W . Received By \J n S a Date Time ___________ -- ________ v/^o/q? / C 6 7 f k /o t /.' -.CT FORM # ENT-131 Tenn. River Valley Samples O Atlanta Goleta Wilminton toz-O 'iu 7 Boston Houston _ Dallas Okemos Walnut Creek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page - Z . o f J Z SO CD o E sm Tenti. River Valley Samples fFORM ENT-131 Report E02-0443 Attachment E: Notes to File Tenn. River Valley Samples 3M Environmental Laboratory Page 270 of 276 Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project o r Study N um ber: E02-0443_________________________________________ __________LIM S Num ber: NA___________________________ Affected Data: D020626Extracted, D020628, D020629, and D020702 __________________________(Fish Tissue) Ts1h.hoeuflodlhloawveinbgeseanmlapbleeslewdearse"m-1is-2la"b.elTehdeinlistthiesirarsefsoplelocwtivse: sequences. They were all labeled as "-1-1" when they D020626Extracted: DUDE0055, D020628: DUDE0056 and DUDE0075, D020629: DUDE0063 and DUDE0096, and D020702: DUDE0062. A2.ll of the fish tissue sample preparation was done at the same time; therefore, Water Blanks (WB) and Solvent wBlaasndkosn(eSBsi)nwceetrheedWonBe swainthdeSaBchs aSraemfoprleeLxaomcaitniionng, tnhoet swaimthpeleacphredpiafrfaetrieonnt tpyrpoeceosfsfaisnhdfarroeminedaecphelnodceantitoonf.thTehis species of fish being analyzed. The WBs and SBs were analyzed with the Catfish samples. For this reason, there are not any WB or SB data contained within the Large Mouth or Small Mouth analytical sequences. 3Tttclrha.oihbepneelttilrafceiiiapdsnthleewicrstiai.(sttChseuosT"el-auhMsrmeeaSmwng"epe2wnil)eg,eeshrhratweatadeesrdpreweifrkaraeoetncedmoarwlraytddhizetdeehdedhtdiohnin(metChtsoroepiglpi"uekl-nmie1caa"nstteore3lo(.u)Mw,tEiasoSnanoscdhfiatntrhfheiCeesanhoFllhstuioiossmhmsguneToen7igsep.esranuariteezenepddtraes(tpaCtmhsohiplsueleemtitmwsn.ea4)sI).tfbiiTsreshfntoeowrtseeauiimntgtwhpilelaedCssoostlehuupatmatinrwnatote6eradethiantto 4eT.nhdeofgisehnotiusssuaenathlyattewcaosncuesnetdraintiothne. eTxhtrisacwteads fdiesthercmurivneesdwduasrinfrgoma ptrheelifmisihnatirsysuraensgaem-fpinledwinigthetxhpeelroimweesntt.amount of wT5.haes "eExtnraabctleedd"fiisnhtthisesquueasnttaintadtaiordn csuorfvtwesarhea,dbuat0itpwpbascnuorvtecaplociunlta.teTdhaiss ppoairnt towf tahsepcaurrtvoef. the calibration curve and 6T.he 10 ng/mL standard curve point in the Extracted Large Mouth Standard Curve had 21% and 22% deviations, exceeding the criteria by 1% and 2%. These points were not excluded from the curves and their inclusion had no negative effect on the data quality due to the point being surrounded by at least two passing calibration points on both sides. 3M Environmental Laboratory Page 271 of 276 Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443______________ __________LIMS Number: NA____________________ Affected Data: 1021112/River Sediments L1.ab Control Samples (LCS) were performed for the River Sediments. However, the information was not used because the data suggested it was impossible to recover spiked analytes from acidified water when river sediment was not present. 2TT.hheesienjseacmtipolnesfiwleesrferommetthhoedsdeeqvueelnocpem1e0n2t1o1n1l2yt.hat are after file Itchy062 are not part of the reportable analyses. Recorded Date: 3M Environmental Laboratory Page c*L f l - Page 272 of 276 Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-Q443 LIM S Num ber: NA______________________ Affected Data: D020812A and D020812B. As1e.lqludeantacethisatmisadineDup02o0f811621AinajnedctDio0n2s/0f8il1e2s.BFairleesfrDomUDoEne00o0r1igitnoaDl sUeDquEe0n0c9e6: Dar0e2f0o8u1n2d. iTnhtheeDs0u2b0-s8e1q2upenarceent D020812A. Files DUDE0097 to DUDE 0161 are in sub-sequence D020812B. The parent sequence was broken up into two separate sub-sequences after LC/MS analysis to simplify data analysis. Linoswubc-osnecqeunetnracteioDn0s2a0m81p2leAs.that fall in the bottom end of the standard calibration curve (0.1 ng/mL to 50 ng/mL) are Very high concentration samples that required small injection volumes that fall in the top end of the curve (5 ng/mL to 1000 ng/mL) are in sub-sequence D020812B. There are not any files that are contained in both sub-sequences. 2There are two different extraction dates for the samples: 20 Jun 02 and 17 Jul 02. This is due to a re-extraction of 5 samples whose results were questionable. Tm33333333333333333a333.8888888888n88h8888888a0000000000d000e000300t22r22233334333343444if5678902351647x839027olslopSSFFSSFSSSSwiSSFSTTSFkWWBWSSWWWCWWWWWWCrrieiniCC0SspSp000000000g000:2000120311233312BB221a-12---------Lr-lDlM-LLDM-DLMaaeMLOMoonOunuueoteeWwewkpkhppedWwddded##12LIMS numbers and the sample names of the samples and their FFMSLSBWoeCw=d====FSFMLiaieomeelwlddpdiBlFueSlmiaaWemnldFkapitSleeelprd(iCSkSoeapnmitkrpoelle Location) associated duplicates and 3M Environmental Laboratory Page 273 of 276 Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: EQ2-0443 LIM S N um ber: NA______________ Affected Data: D020626Extracted Iln. the D020626Extracted sequence there were not any Extracted CCV curve points run. All subsequent Fish Tissue sequences had extracted CCVs included. The unextracted CCVs were quantitated against the unextracted fish curve, 02003-050, using an Excel spreadsheet. All of the unextracted CCVs passed and the results are found in Appendix B: Data Summary Tables. Recorded By: Date: 3M Environmental Laboratory Page j_ ofj6. Page 274 of 276 Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number; E02-0443 LIMS Number: NA Affected Data: All Data N o te : T h is is to e x p la in h o w th e q u a n tita tio n was p e rfo rm e d o n th e d a ta . Tc1a.hseese,nhtiirgehclaelviberlactuiornvecpuorvinetws waseerent"eDreidsaibnlteodt"heinqtuhaenstoitfattwioanresoafntdwwareereanrdemthoevceudrfvreomwatshethceunrvaenaclaylzceudla. tiIonnm. anIyn all instances in which this was done, the disabled curve points show a recovery of 0%. Low end curve points that had % Recoveries that exceeded the criteria or were <2X the solvent blanks levels were ndoetteurmseidn.atTiohnesoefpthoeinLtsOwQe.re still included in the calibration curve calculations, however, they were not used in the 2Ilon.wthoerraawnedgaattaivtheavtacluoemaersefarosmsigtnheedTaanrgeexttrseomftewpaores,itcivoencveanlutrea.tioTnhsetsheavtawluoeusldarneoeramsaillylynboeticqeudandtuiteatteodthaesiar very aobfnqouramntailtlaytiloanr,gaerveaclhuaesngaelodntgo w"BitLhOveQr"y stmo ealllimarienaatceoaunnytsp. oTsshiebslee vcoalnufeuss,ioanlo.ng with values that are below the limit Recorded By: Date: 3M Environmental Laboratory Page S_ of 6 Page 275 of 276 Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443 __________LIM S Num ber: NA_______ Affected Data: Fish Tissue Iln. the sample preparation process of the fish tissue, after the homogenization process (Step 4), the homogenate is centrifuged for a short time and then shaken (Step 5). The centrifugation was done to eliminate the foam that developed during the homogenization process. The homogenate was then shaken/vortexed to make the solution homogenous again. 3M Environmental Laboratory Page Q_ofb_. Page 276 of 276