Document qa3V008MQZKLyavj99b1avBaK

ARA9.G - 136S Study Title T e n n e s s e e R iv e r V a l l e y S a m p l e s Author M ark E. Ellefson Study Completion Date 17 Decem ber 2002 Revised Report 06 January 2003 Performing Laboratory 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue S t Paul. MN 55106 Project Identification 3M Environm ental Laboratory Study # E 02-0443 Total Number o f Pages 276 001750 Report E02-0443 Tenn. River V alley Sam ples Table of Contents List of Tables.......................................................................................................................................... 3 Study Inform ation................................................................................................................................... 4 S um m ary................................................................................................................................................. 5 P u rp o se ................................................................................................................................................... 6 Test and Analytical Reference Substances......................................................................................... 6 Test System s......................................................................................................................................... 7 Method Summaries................................................................................................................................ 8 Preparatory Methods..............................................................................................................................8 Sample Analysis..................................................................................................................................... 11 Analytical Method................................................................................................................................... 12 Analytical Results................................................................................................................................... 13 Data Sum m ary....................................................................................................................................... 20 Statistical Methods.................................................................................................................................25 Statement of Conclusion....................................................................................................................... 26 References............................................................................................................................................. 26 List of Attachments.................................................................................................................................26 Signature Page....................................................................................................................................... 27 Attachment A: Analytical Method and SOP Deviations........................................................................28 Attachment B: Data Summary Tables.................................................................................................. 40 Attachment C: Sample Chromatograms.............................................................................................. 67 Attachment D: Sample Prep Sheets, Test Substance, and Test System Inform ation.......................230 Attachment E: Notes to F ile .................................................................................................................. 270 00X7Sx Report E02-0443 Tenn. River Valley Sam ples 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 S tudy.............................................................7 Table 3b. Description of River Water Analyzed in this S tud y............................................................ 7 Table 3c. Description of River Sediments Analyzed in this S tu d y.................................................... 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 M ethod.......................................................................... 9 Table 4e. River W ater Sample Data Quality O bjectives.................................................................... 10 Table 4f. River Sediment Sample Preparation Method.......................................................................10 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........................................................ 15 Table 6c. PFOA Calibration Standard Reprocessing Summary........................................................ 16 Table 6d. PFHS Calibration Standard Reprocessing Summary........................................................ 17 Table 6e. PFBS Calibration Standard Reprocessing Sum m ary........................................................ 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......................................... 25 00*; 52 Report E 02-0443 Tenn. River Valley Sam ples Study Information R e q u e s to r Dale L. Bacon 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 651-778-4736 Study D irector 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, Analytical Chemist Ognjenka Krupljanin, Analytical Chemist Experimental Dates Sample Analysis Initiation: 26 June 2002 Sample Analysis Completion: 12 November 2002 Location o f 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. 001753 Report E02-0443 Tenn. River Valley Samples Summary 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), perfiuorohexane sulfonate (PFHS), perfluorooctanoate (PFOA), perfiuorooctane 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 near the 3M facility outfall. Sampling Location 2 (SL-2) was across the reservoir from the 3M facility outfall. Sampling location 3 (SL-3) was downstream from the facility near the Fox Creek confluence. 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 (ng/g) PFOA (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 64.3 <LLOQ <LLOQ <LLOQ 60.9 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 113 <LLOQ 22.3 553 281 <LLOQ <LLOQ SL-1, RW SL-2, RW SL-3, RW PFBS (pg/mL) 84 <LLOQ <LLOQ PFHS (pg/mL) PFOA (pg/mL) 196 550 8 <LLOQ 7 <LLOQ River Sediments FOSA (pg/mL) 25 <LLOQ <LLOQ PFOS (pg/mL) 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 131 68 416 C CatFish, LM Large mouth bass, SM >Small mouth bass, RW = River water, RS = River Sediments, and n number offish per sampling group. 001754 Report E 02-0443 Tenn. River Valley Sam ples 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 o f the Test and Analytical Reference Substances. Test and A nalytical 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, Perfluorooctanesulfbnamide 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 White Powder Undetermined 95.0% T est and A nalytical 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. 236-1B-10 Frozen TCR-129 White Powder Undetermined 001755 Report E02-0443 Tenn. River Valley Sam ples Test Systems Table 3a. Description o f Fish Tissue Analyzed in this Study Fish Tissue Source Types Storage Conditions Location 1 Location 2 Location 3 Tennessee River Catfish Large Mouth Bass Small Mouth Bass Frozen Near the 3M facility outfall Across the reservoir from the 3M facility outfall Downstream of the Fox Creek confluence * The fish were filleted and representative aliquots of the fillets were analyzed. Table 3b. Description o f River W ater Analyzed in this Study Source Storage Conditions Location 1 Location 2 Location 3 River Water Tennessee River Chilled (approximately 4 C.) Near the 3M facility outfall Across the reservoir from the 3M facility outfall Downstream of the Fox Creek confluence Table 3c. Description o f River Sediments Analyzed in tills Study River Sediments Source Storage Conditions Location 1 Location 2 Location3 Tennessee River Chilled (approximately 4 C.) Near the 3M facility outfall Across the reservoir from the 3M facility outfall Downstream of the Fox Creek confluence 001756 Report E02-0443 Tenn. River V alley Sam ples Method Summaries The concentrations o f 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 Sam ple Preparation Method Table 4a. Fish Tissue Sample Preparation Method Step Fish Tissue Sample Preparation Method 1 Approximately 2 g of Fish Tissue and 8 mL of ASTM Type 1Water were homogenized. 2 The homogenate was centrifuged to eliminate the foam and then shakerWortexed to re suspend the homogenate. 3 Each homogenate was aliquoted into triplicate samples. This was accomplished by transferring 1.0 mL of homogenate to 3 separate 15 mL centrifuge tubes. Matrix spikes (MS) were prepared for every other homogenate. In this case, an addibona! 4 (4th) 1.0 mL of homogenate was transferred to another 15 mL centrifuge tube. TheMS's were spiked with 100 uL of a 1.0 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 i shaken for 20 min at 300 rpm. 6 After mixing, the samples were centrifuged at 3000 reffor 10 minutes to clarify the supernatant 7 The supernatant was decanted into new 50 mL centrifuge tubes and diluted with 4 0 mL of w ater. Waters C-18 Tri-functional, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned in the following manner. Approximately 10 mL of methanol was added to the columns and the vacuum was applied. 8 Once most ofthe methanol had been pulled through, ASTM Type 1Waterwas added (5-10 mL). When most of this was pulled through, more water was added (5-1OmL). When there was only a small amount of water left in the reservoir, the stopcock was turned to stop the vacuum to the column. The columns were not allowed to go dry. 9 The supemates from step 7 were passed through the pre-conditioned SPE columns. The aqueous eluentwas not collected. The columns were allowed to dry for at least 3 minutes. 10 The analytes were eluted from the SPE columns with 2.0 mL of methanol into autovials. See the preparation worksheets for other exact amounts, times, speeds, etc. 001757 Report E 02-0443 Tenn. River Valley Sam ples Table 4b. Preparation o f Extracted Calibration Curves fo r the Fish Tissue. Step Preparation of Extracted Calibration Curves for the Fish Tissue There were two extracted Fish Tissue calibration curves: Large Mouth Bass and CatFish. Rangefinding experiments were done to determine which Fish Tissues had the lowest endogenous levels ofthe analytes. Then, one Large Mouth Bass and one CatFish sample containing the least amount of endogenoustest substances were selected as the matrix to construct the calibration curves. The Smalt Mouth Bass was analyzed using the Large Mouth Bass calibration curve. The procedure for preparing the extracted calibration curves is the same as the Fish Tissue sample preparation, except the volumes were scaled-up to provide a homogeneous batch of fish tissue matrix. The differences are as follows: 1 Approximately 10 g of Fish Tissue and 40 mL of ASTM Type 1Water were combined and homogenized. 2 1.0 mL of homogenate was transferred to the appropriate number of tubes. 3 Each tube was spiked with the predetermined amount of spike solution. Table 4c. Fish Tissue Analytical Data Quality Objectives. Step Fish Tissue A nalytical Data Quality Objectives 1 All samples were prepared in triplicate. The %RSD should be s 25% Matrix spikes were performed on half ofthe fish of each type from each sampling location. 2 Recovery should be within 30% from expected values. A total of 18 matrix spikes were prepared for the Fish Tissue samples. Water blanks, consisting of an aliquot ofwater run through the entire sample preparation and 3 extraction process were prepared with samples from each sampling location. Water blanks containing < % LLOQ of each analyte for the data set in which they were run were considered acceptable. Extraction blanks, consisting of an aliquot of methanol run though a pre-conditioned SPE 4 cartridge, were prepared for each sampling location. Extraction blanks containing < !4 LLOQ of each analyte for the data set in which they were run were considered acceptable. 5 I Mid-level calibration curve points were used as CCVs. River W ater Sam ple Preparation Method Table 4d. River W ater Sample Preparation Method Step River Water Sample Preparation Method 1 Waters G-18 Tri-functional, Sep-Pak 1g, 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned in the following manner. Approximately 10 mL of methanol was added to the columns and the vacuum was applied. Once mostof the methanol had been pulled through, ASTM Type 1 Water was added (5-10 mL). When most of this was pulled through, more water was added (5-1OmL). When there was only a small amount ofwater left in the reservoir, the stopcock was turned to stop the vacuum to the column. The columnswere not allowed to go dry. 2 40 mL ofthe RiverWater was passed through a pre-conditioned SPE column. The columns were allowed to dry for at least 3 minutes. 3 The analytes were eluted from the columns with 2.0 mL of methanol into autovials. 001758 Report E02-0443 Tenn. River Valley Samples Table 4e. River W ater Sample Data Quality Objectives Step River W ater Sample Data Quality Objectives 1 Water blanks, consisting of an aliquot ofwater run through the entire preparation and extraction process, were prepared with samples each day samples were extracted. Water blanks containing < 14LLOQ of each analyte for the data set in which they were run were considered acceptable. 2 A non-extracted solvent calibration curve was used to quantitate the River Water samples. No extracted CCVs were prepared, a mid-level calibration curve point was used for this purpose. 3 No matrix spikes were preformed during the sample preparation ofthe River Water samples. R iver Sedim ent Sam ple Preparation Method Table 4f. River Sediment Sample Preparation Method Step River Sediment Sample Preparation M ethod There were 3 River Sediment samples, one from each sampling location. Triplicate samples plus a matrix spike were prepared for each location. Initially, sedimentwas transferred to 50 mL centrifuge tubes and centrifuged at 6000 RCF for 1 20 min. The liquid was decanted off and the remaining sedimentwas used for the sample preparation 2 Approximately 20g of sediment and 35mL of 1% Acetic Add (aqueous) were combined into 50mL centrifuge tubes. 3 Matrix spikes were prepared by adding 100 uL of 1.0 ug/mL spike solution to the predetermined MS tubes. 4 The tubes were capped, vortexed, and then shaken for 60 min at 300 RPM. 5 They were then centrifuged at 6000 RCF for 20 minutes. Waters C-18 Tri-functional, Sep-Pak ig , 6cc SPE columns with attached 70 mL reservoirs were placed onto vacuum manifolds and pre-conditioned in the following manner. Approximately 10 mL of methanol was added to the columns and the vacuum was applied. 6 Once most of the methanol had been pulled through, ASTM Type 1Waterwas added (5-10 mL). When most ofthis was pulled through, more water was added (5-10mL). When there was only a small amount of water left in the reservoir, the stopcock was turned to stop the vacuum to the column. The columns were not allowed to go dry. 7 The aqueous solutions from step #5 were decanted from the samples and passed through pre-conditioned SPE cartridges. The aqueous eluates were discarded. 8 i 20 mL of methanol was then added to the sediment samples. The samples were vortexed, shaken for 30 min at 300 RPM, and then centrifuged at 6000 RCF for 20 minutes. 9 The methanol was decanted, passed through the SPE cartridge and collected. An additional 4 mL of methanol was used to wash the reservoir and the column. 10 The collected methanol was then added to approximately 200mL of ASTM Type 1 Water. 11 This solution was then passed through a new pre-conditioned SPE cartridge. The aqueous eluate was discarded. 12 The analytes were eluted from the SPE cartridges with 2.0 mL of methanol into autovials. Report E 02-0443 Tenn. River Valley Sam ples Table 4g. River Sediment Sample Data Quality Objectives Step River Sediment Sample Data Quality O bjectives 1 All samples were prepared in triplicate. The %RSD should be 25% 2 Matrix spikes were performed on each sample. Recovery should be within 30% 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 information was not used because the data suggested it was impossible to recover spiked analytes 'from acidified waterwhen river sediment was not present Water blanks, consisting of an aliquot ofwater run through the entire preparation and 4 extraction process, were prepared. Acceptable values were <%LLOQ for the 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 points were used as CCVs. 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, W ater 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. Sampi e L ocation 1 i i 2 Catfish Lange Mouth Bass 3 Small Mouth Bass 4 River water 5 River Sediments 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 Sequence D020629 D020629 D020702 D020626 D020628 D020628 D020628 D020812 D020812 D020812 1021112 1021112 1021112 Date Sequence W as S TARTE U 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 0 0 1 ,6 0 Report E 02-0443 Tenn. River Valley Sam ples Analytical Method Sample analysis was based on ETS-8-155.1 "Analysis of Waste Stream, W ater 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. A n a lytica l E quipm ent Liquid C hrom atograph: Agilent/Hewlett-Packard* Series 1100 Liquid Chromatograph system Analytical column: Keystone* BetasilTM C182x50mm, 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 G radient T0.im00e 0.50 0.80 3.50 5.50 6.50 9.50 %10 B % 10 % 60 % 100 % 100% 10 % 10 % Mass Spectrom eter: Agilent/Hewlett-Packard* Series 1100 API/Mass Spectrometer Detector Software: Agilent ChemStation,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) u o ire i Report E 02-0443 Tenn. River Valley Sam ples Analytical Results Data quality objectives outlined in the Preparation Methods section were m et R egressions. 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. C alibration Standards. Standards ranging in concentration from approximately 1.0 to 1000 ng/mL 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 o f each calibration standard were calculated. High-end curve points that were outside the 20% criteria o f 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 o f Quantitation (LLOQ). C ontinuing C alibration V erifica tion (CCV). For quantitative determinations, a mid-level matrix calibration check was analyzed at least every ten samples to monitor instrumental drift, with a lim it of 20% deviation of the target concentrations. Low er L im it o f Q uantitation (LLOQ). The LLOQ was equal to the lowest standard in the calibration curve, with a level o f accuracy within 20%, that demonstrated a response greater than two times the response o f analyte in the blank samples. System S u ita b ility. 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 o f 5% for the mean area recovery was achieved. Lab C ontrol 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. 001762 Report E 02-0443 Tenn. River Valley Sam ples Table 6a. PFOS Calibration Standard Reprocessing Summary PFOS CONCENTRATION Sam pleT ype and Location Batch and A nalysis Date Lower Limit of Quantitation (LLOQ) Catfish, SL-1 0020629,29 Jun02 2.5ngfe Catfish, SL-2 Catfish, SL-3 D020629,29 Jun02 D020702,02 Jul02 2.5ng/g 1.0ng/g Large Mouth Bass, SL-1 D020626,26 Jun02 1.0ng/g Large Mouth Bass, SL-2 D020628,28 Jun02 2.5ng/g Large Mouth Bass, SL-3 D020628,28 Jun02 2.5 nglg Small Mouth Bass, SL-3 D020628,28 Jun02 2.5ng/g RiverWater, SL-1 0020812A, 12Aug 02 125pg/rtiL* RiverWater, SL-2 D020812A, 12Aug 02 125 pg/mL* RiverWater, SL-3 0020812A, 12Aug 02 125pg/mL* RiverWater, SL-1 D020812B, 12Aug 02 1.25 ngfaiL* RiverWater, SL-2 0020812B, 12Aug 02 1.25 nmL* RiverWater, SL-3 0020812B, 12Aug 02 1.25ng/mL* RiverSediment SL-1 raver Sediment SL-2 1021112,12 Nov02 1021112,12 Nov02 250 pg/gT 250pg/g* RiverSediment SL-3 1021112,12 Nov02 250pg/g* * Denotes sam ple preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 001763 Report E02-0443 Tenn. River Valley Sam ples Table 6b. FOSA Calibration Standard Reprocessing Summary FOSA CONCENTRATION Sample Type and Location Batch and A nalysis Date Lower Limit of Quantitation (L L O Q ) Catfish, SL-1 D020629,29 Jun02 2.5ng/g Catfish, SL-2 D020629,29 Jun02 2.5ng/g Catfish, SL-3 D020702,02Jul 02 2.5ngig Large Mouth Bass, SL-1 D020626,26 Jun02 5.0ng/g Large MouthBass, SL-2 0020628,28 Jun 02 5.0ng/g Large MouthBass, SL-3 D020628,28 Jun02 S.Ong/g Small Mouth Bass, SL-3 D020628,28 Jun 02 5.0ng/g RiverWater, SL-1 RiverWater, SL-2 0020812A, 12Aug02 D020812A, 12Aug02 25 pg/mL* 25 pg/mL* RiverWater, SL-3 D020812A, 12Aug02 25 pg/mL' RiverWater, SL-1 D020812B, 12Aug 02 1.25ng/mL* RiverWater, SL-2 RiverWater, SL-3 020812B, 12Aug 02 D020812B, 12Aug02 1.26ng/hnL* 1.25 ngimL* RiverSediment SL-1 1021112,12 Nov02 50pg/g* RiverSediment SL-2 1021112,12 Nov02 50pg/g* RiverSediment SL-3 1021112,12NOV02 ! 50 pg/g* *FaDcetonro.tes sample preparation method LLOQ. Method LLOQ * Instrument LLOQ/Method Concentration 001764 Report E02-0443 Tenn. River Valley Sam ples Table 6c. PFOA Calibration Standard Reprocessing Summary PFOA CONCENTRATION Sample Type and Location Batch and A nalysis Date Lower Liiy.ii orQ uantitation (LLOQ) Catfish. Sl-1 D020629,29 Jun02 5.0 ng/g Catfish, SL-2 D020629,29 Jun02 5.0 ng$ Catfish, SL-3 D020702,02 Jul 02 5.0 ng/g Large Mouth Bass, SL-1 D020626,26 Jun02 2.5ngfg Large Mouth Bass, SL-2 D020628,28 Jun02 5.0 ng/g Large MouthBass, SL-3 D020628,28 Jun02 5.0 ng/g Small Mouth Bass, SL-3 D020628,28 Jun02 5.0 ng/g RiverWater, SL-1 D020812A, 12Aug 02 50pg/mL* RiverWater, SL-2 D020812A, 12Aug 02 50pg/mL* RiverWater, SL-3 D020812A, 12Aug02 50pg/mL* RiverWater, SL-1 D020812B, 12Aug 02 1.25 ng/mL* RiverWater, SL-2 D020812B, 12Aug 02 1.25 ng/mL* RiverWater, SL-3 D020812B, 12Aug 02 1.25 ng/mL* RiverSediment SL-1 RiverSediment SL-2 1021112,12 Nov 02 1021112,12 Nov02 250pg/g* 250pg/g* RiverSediment SL-3 1021112,12 Nov02 250pg/g* * Denotes sample preparation method LLOQ. Method LLOQ - Instrument LLOQ/Method Concentration Factor. U 01765 Report E02-0443 Tenn. River Valley Sam ples Table 6d. PFHS Calibration Standard Reprocessing Summary PFHS CONCENTRATION Sample Type and Location Catfish, SL-1 Catfish, SL-2 Batch and A nalysis Date 0020629,29 Jun02 0020629,29 Jun 02 Lower Limit of Quantitation (L L O Q ) 2.5ng/g 2.5ng/g Catfish, SL-3 D020702,02 Jul02 2.5 ng/g Large Mouth Bass, SL-1 D020626,26 Jun 02 1.0ng/g Large Mouth Bass, SL-2 Large Mouth Bass, SL-3 D020628,26 Jun 02 D020628,28 Jun 02 1.0ng/g 1.0ng/g SmallMouthBass, SL-3 D020628,28 Jun02 LOng/g RiverWater, SL-1 D020812A, 12Aug 02 25pg/mL* RiverWater, SL-2 D020812A, 12Aug02 25pg/mL* RiverWater, SL-3 020812A, 12Aug 02 25pgAnL* RiverWater, SL-1 D020812B, 12Aug02 1.25ng/mL' RiverWater, SL-2 D020812B, 12Aug 02 1.25 ng/mL* RiverWater, SL-3 D020812B, 12Aug 02 1.25 ng/mL* RiverSediment SL-1 1021112,12 Nov02 100 pg/g* River Sediment SL-2 1021112,12 Nov 02 100 pg/g* RiverSediment SL-3 1021112,12 Nov02 100 pg/g* * Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 001766 Report E02-0443 Tenn. River Valley Sam ples Table 6e. PFBS Calibration Standard Reprocessing Summary PFBS CONCENTRATION Sample Type and L ocation Catfish, SL-1 Catfish, SL-2 Catfish, SL-3 Batch and A nalysis Date D020629,29 Jun02 0020629,29 Jun02 D020702,02 Jul02 Lower Limit of Quantitation (L L O Q ) S.Ong/g 5.0 ng/g 5.0 ng/g LargeMouth Bass, SL-1 Large Mouth Bass, SL-2 Laige Mouth Bass, SL-3 D020626,26 Jun02 D020628,28 vlun02 D020628,28 Jun02 1.0 ng/g 2.5 ng/g 2.5 ng/g Small MouthBass, SL-3 D020628,28 Jun02 2.5 ng/g RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 RiverWater, SL-1 RiverWater, SL-2 RiverWater, SL-3 D020812A, 12Aug 02 D020812A, 12Aug02 D020812A, 12Aug02 D020812B, 12Aug 02 D020812B, 12Aug 02 020812B, 12Aug02 50pg/mL* 50pg/mL* 50pg/mL* 1.25 ng/mL* 1.25 ng/mL* 155 ng/mL* RiverSediment SL-1 1021112,12 Nov 02 100pg/g* RiverSediment SL-2 1021112,12 Nov02 100pg/g* RiverSediment SL-3 1021112,12 Nov02 1 100pg/g* * Denotes sample preparation method LLOQ. Method LLOQ = Instrument LLOQ/Method Concentration Factor. 001767 Report E02-Q443 Tenn. River Valley Sam ples B la n k s . Method blanks, Milli-Q water taken through the solid phase extraction process, provided a measure o f method background. In this experiment, they were labeled as "WB". One set was prepared for each location. In the Fish Tissue portion o f the experiment, they were run with the Catfish samples. Acceptable values for the blanks were less than 50% o f the Lower Limit O f 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 o f 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% o f the Lower Limit O f Quantitation (LLOQ). A ll 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 are 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. 001768 Report E 02-0443 Tenn. R iver Valley Sam ples 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 o f 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. 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 001769 Report E02-0443 Tenn. River Valley Sam ples Table 7a. Catfish Analytical Data. LIMS U Sam pio Name A im 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. 07-2 SL-2. C-7-3 SL-3; C-1-1 SL-3; C-A-2 SL-3. 01-3 SL-3. 02-1 SL-3. C-2-2 SL-3. C-2-3 SL-3. 03-1 SL-3. 03-2 SL-3. 03-3 SL-3. 04-1 SL-3. C-4-2 SL-3. C-4-3 SL-3. 05-1 SL-3. 05-2 SL-3. C-5-3 SL-3. 06-1 SL-3. 06-2 SL-3. C-6-3 PFBS (ng'g) <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/g) <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 PFOA (^g/g) <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- column (ng/g) 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 Corr. for Smpl Prep (ng/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 69.8 69.1 69.8 Ave. Strici. D and 7oC.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 Oncolumn (ng'g) 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 <l l o q <LLOQ <LLOQ <LLOQ <llo q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 1.9 1.9 1.4 1.2 1.1 1.2 <LLOQ <LLOQ <l l o q 3.7 3.5 4.0 <LLOQ <l l o q <LLOQ <LLOQ 2.3 2.3 PFOS Corr. f or Smpl Prep (ng/g) 112 105 100 97.6 91.8 86.1 161 179 192 172 165 166 80.8 80.2 77.5 58.8 59.7 58.7 Ave. Stnd. D 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 001770 Report E 02-0443 Tenn. River Valley Sam ples Table 7b. Large mouth and Small mouth Bass Analytical Data. LIMS it Sample Name PFBS PFHS (ng/g) (ng/g) 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 <l l o q <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 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <llo q <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 <LL0Q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ PFOA Corrected for Smpl Prep (ng/g) 64.3 FOSA Corrected (ng/g) <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <aoa <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 <llo q 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 5669..90 <LL0Q <LLOQ <LLOQ 2.6 <LLOQ <LLOQ 9.7 11.8 8.5 53.1 54.1 56.9 <LLOQ <LLOQ <LLOQ <LLOQ <LL0Q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOO <LLOQ <LLOQ <LLOQ <LLOQ PFOS Coi rccteci for Smpl Prep (ng/g) 186 130 140 636 614 572 732 808 824 688 757 653 466 415 389 693 599 660 152 29.6 19.5% 607 32.5 5.4% 788 49.2 6.2% 700 52.7 7.5% 423 39.0 9.2% 651 47.8 7.3% 25.6 96.7 100 118 16.7 84.7 16.7% 531 547 541 20.0 569 3.7% 1771 Report E 02-0443 Tenn. River Valley Sam ples Table 7c. raver W ater Analytical Data. LIMS # 38025 38026 38033 38034 38037 38038 LIMS n 38025 38026 38033 38034 38037 38038 LIMS It 38025 38026 38033 38034 38037 38038 LIMS # 38025 38026 38033 38034 38037 38038 LIMS n 38025 38026 38033 38034 38037 38038 Sample Name SW01 SW01-Dup SW03 SW03-Dup SW02 SW02-Dup (,nPgJF/,BmSL, ,) 3.0 3.7 <LLOQ <LLOQ <LLOQ <LLOQ Sample Name SW01 SW01-Dup SW03 SW03-Dup SWQ2 SW02-Dup Sample Name SW01 SWOl-Dup SW03 SW03-DUP SW02 SW02-Dup Sample Name SW01 SWOl-Dup SW03 SW03-Dup SW02 SW02-Dup Sample Name .nPg3F/.Hm.SL.) 7.7 8.0 <LLOQ 0.3 0.4 0.2 (.n,,PgJFr/.Om_..AL. ) 21.3 22.7 <LLOQ <LLOQ <LLOQ <LLOQ ,nFgJO/,mSALa, ,)' 1.0 1.0 <LLOQ <LLOQ <LLOQ <LLOQ ,nPngF/,OmSL r SW01 SWOl-Dup SW03 SW03-Dup SW02 SW02-Dup I 18.5 20.8 I <LLOQ 1 <LLOQ <LLOQ <LLOQ f,oA(.rndl.ngju/j,ms.VteL.o)d.l,. 1.50 1.85 f,oA,rndl,gnju/j,ms.Vt,eL,,od.l,. 3.86 3.98 0.13 0.20 0.12 f.oA(,rndl:gnju/fjm.s.Vt.eL.o)d,l. 10.7 11.3 t.oA(,rndI:gj1nu/jms. tVeL, o)d, l,. 0.48 0.51 f,oA(.rdnlj,gnu//jm-s.VtL,eo)d.l. 9.25 10.4 Adjusted for cS-am.ppgl,/e,mPnL1 r),ep. 75 93 S,,Aadm(,jpupgsl,/et,medP_L, )r.feop1r. 193 199 6.5 9.8 6.2 Adjusted for So ampl1e Pnrep. ,pg/,mL, ), 533 566 S_Aadm,'jpupgsl./et.medPL, r),feopr. 24 26 SAadm(,jpupgsl/e,tmed,,PL, r),feop1r. 462 520 A,pvcejrimagL,e,)' 84 <UOQ <LLOQ A,pvgJe/r.ma.gL.e 196 6.5 8.0 A,pvge/r.ma.gL.e)' 550 <UOQ <LLOQ A, pvge/r,magL, e,) ' 25 <LLOQ <LLOQ A,pvgJe/r.ma.gL.e 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. 001772 Report E02-0443 Tenn. River V alley Sam ples Table 7d. River Sediment Analytical Data. UMS # 38044 38044 38044 38045 38045 38045 38046 38046 38046 l IMS ft 38044 38044 38044 38045 38045 38045 38046 38046 38046 l# 38044 38044 38044 38045 38045 38045 38046 38046 36046 LIMS # 38044 38044 38044 38045 38045 38045 38046 38046 38046 LIMS 38044 38044 38044 38045 38045 38045 38046 38046 38046 Sample 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 Sample 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 Sample 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 Sample 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 Sample 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 Column PFBS (ng/g) 10.6 10.6 13.5 8.9 8.3 10.0 8.9 6.2 11.7 On Column PFHS (ng/g) 2.7 2.6 2.5 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ On Column PFOA (ng/g) 16.2 14.1 13.7 <LLOQ 2.6 <LLOQ <LLOQ <LLOQ <LLOQ On Column FOSA (ng/g) 29.7 32.4 24.5 1.2 1.2 1.7 2.9 2.5 3.2 On Column PFOS (ng/g) 67.7 70.3 50.4 9.1 6.8 9.1 9.0 8.5 10.5 Adjusted for Inj Vol. (ng/g) 5.3 5.3 6.7 4.4 4.1 5.0 4.5 3.1 5.8 Adjusted for Inj. Vol. (ng/g) 1.4 1.3 1.2 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Inj. Vol. (ng/g) 8.1 7.1 6.9 <LLOQ 1.3 <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Inj. Vol. (ng/g) 14.8 16.2 12.2 0.6 0.6 0.8 1.5 1.3 1.6 Adjusted for Inj. Vol. (ng/g) 33.8 35.1 25.2 4.5 3.4 4.6 4.5 4.2 5.3 Adjusted for Sample Prep, (pg/g) 530 530 674 444 415 502 447 309 583 Adjusted for Sample Prep, (pg/g) 136 132 124 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Sample Prep, (pg/g) 810 705 686 <LLOQ 131 <LLOQ <LLOQ <LLOQ <LLOQ Adjusted for Sample Prep, (pg/g) 14B0 1620 1220 62 60 83 146 126 161 Adjusted for Sample Prep, (pg/g) 3380 3510 2520 454 342 456 452 425 525 Average, Std. Dev., and VuC.V. (pg/g) 577 84 14% 452 44 10% 437 137 31% Average, Std. Dev., and 7oC.V. (pg/g) 130 6 5% <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Average, Std. Dev., and %C.V. (pg/g) 732 67 9% 131 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ Average, Std. Dev., and %C.V. (pg/g) 1440 201 14% 68 12 18% 141 17 12% Average, Std. Dev.. and %C.V. (pg/g) 3130 541 17% 416 65 16% 457 52 11% 001773 Report E02-0443 Tenn. River Valley Sam ples Summaries for the average analyte concentration per sampling group and location are given below. Table 8. Sample Location, Sample Type, and Analytical Data Summary. Fish Tissue Sampling Location & Species Sampled PFBS (ng/g) PFHS (ng/g) PFOA (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=G) SL-2, LM (n=4) SL-3, LM (n=7) SL-3, SM (n=1) <LL0Q <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LL0Q <LL0Q <LLOQ <LL0Q <LLOQ <LLOQ <LLOQ <LL0Q River Water <LLOQ <LLOQ <LLOQ 64.3 <LLOQ <LLOQ <LLOQ 60.9 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ 113 <LLOQ 22.3 553 281 <LLOQ <LLOQ SL-1, RW SL-2, RW SL-3, RW PFBS (Pg/mL) 84 <LLOQ <LL0Q PFHS (pg/mL) PFOA (pg/mL) 196 550 8 <LLOQ 7 <LLOQ River Sediments FOSA (p g /m L ) 25 <LLOQ <LLOQ PFOS (pg/mL) 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 131 68 416 ICn nCuamtFbIsehr,ofLHMah Lpaerrgetmriopulitnhg bgarsosu,p.SM Small mouth bass, RW River water, RS River Sediments, and Attachment B contains additional data summary tables. S t a t is t ic a l M e t h o d s Statistical methods were limited to calculating averages, standard deviations and % coefficient of variation. 001774 Report E02-0443 Tenn. River Valley Samples Statement of Conclusion Fish Tissue: Fish tissue obtained from Sample Location 1 contained quantifiable levels of PFOA, FOSA, and PFOS. Fish tissue obtained from Sample Locations 2 and 3 contained quantifiable levels of PFOS only. River W ater: W ater from Sampling Location 1 contained quantifiable levels o f PFBS, PFHS, PFOA, FOSA, and PFOS. W ater obtained from sample Locations 2 and 3 contained quantifiable levels of PFHS only. River Sedim ents: 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 W aste Stream, W ater Extracts Or Other Systems Using HPLC-Electrospray/Mass Spectrometry". List of Attachments Attachm ent A: Analytical Method and SOP Deviations Attachment B: 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. U0 1 7 7 3 Report E02-0443 w Tenn. R iver V alley Sam ples Signature Page We certify that this report is a true and complete representation of the data for this study: *****>!* -- --------------- W illiam K. Reagen, Testing Facility Management Date '* 3 001776 Report E02-0443 Tenn. River Valley Sam ples Attachment A: A nalytical Method and SOP Deviations 001777 Report E02-0443 Tenn. River Valley Sam ples Document may be used, i f current, for 14 days from 11/21/2002 3M Environmental Laboratory M ethod Ana ly sis o f W aste Stream , W ater Extracts o r Oth er System s U sing h p l c -E lectrospray/M ass Spectrom etry M ethod N um ber: ETS-8-155.1 \ Author: Mark L. Anderson, Mark E. Ellcfson Approved By: A doption Date: | / 1 00 Revision D ate: o /* ^ 001778 Report E 02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 1.0 Scope andApplication_______________________________ 1.1 Ssycsotpeme:sTuhsiinsgmHetPhLoCd -deelescctrriobsepsrtahye/manaasslysspisecotfrowmasetterys.tream, water samples or other 1.1.1 Specific analytes, ions, matrices, solvents, solutions, quality controls, internal standard(s) and other parameters w ill be defined in the protocol or the sample preparation worksheets). 1.2 Applicable Compounds: Electrospray ionizable compounds. 1 3 M atrices: 1.3.1 Wsysatsetme Sstorreaams ds easnigdnoattheedrisnysthteempsromtoacyocloonrssiastmopfleaqpureepouarsaatniodn/owroorrkgashneicetsso)l.vent 1.3.2 WsolautetiroSnas.mTphleesminactlruidxewtailpl bweadteerf,ingerdoubnydtwheatperro, twoacsotleowrastaemr apnledporthepearraaqtiuoenous worksheet(s). 2.0 Summary of Method__________________________________________ 2.1 This method describes the analysis of electrospray ionizable compounds, using HPLCelectrospray mass spectrometry (HPLC-ES/MS). The analysis is performed by the mass selection o f a single ion characteristic o f a particular compound. 3.0 Definitions____________________________________________________________ 3.1 Atmospheric Pressure Ionization (API): Commercially available HPLC-ES/MS single quadrupole systems allow for various methods of ionization by utilizing a variety o f sources, probes, and interfaces. These include but are not limited to: Electrospray Ionization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ionization in these processes occurs at atmospheric pressure (i.e., not under a vacuum). 3.2 Electrospray Ionization (ES, ESI): A method o f ionization performed at atmospheric pressure, whereby ions in solution are transferred to the gas phase via tiny charged droplets. These droplets are produced by the application o f a strong electrical field. 3 3 M ass Spectrometer (MS): Commercially manufactured MS systems are equipped with single quadrupole mass selective detectors. Ions are selected on the basis o f mass to charge ratio (m/z) and subsequently detected. 3.4 M icromass MassLynx / HP ChemStation Software: System software designed for the specific operation o f an HPLC-ES/MS. Please refer to the manual for the specific instrument software. 3M Environmental Laboratory Analysis Using HPLCE-TESle-cMtro5s5p.1ray/Mass Spectrometry 001779 Page 2 of 10 Report E 02-0443 Tenn. River Valley Sam ples Document may be used, if current, for 14 days from 11/21/2002 4.0 Warnings and Ca u t io n s______________________ ______________________ 4.1 Health and Safety Warnings: 4.1.1 Use caution with the voltage cables for the electrospray probe. When engaged, the probe employs a voltage o f approximately 5000 Volts. 4.1.2 When handling samples or solvents wear appropriate protective clothing, gloves, and eyewear. 4 2 C autions: 42.1 Operate solvent pumps below a backpressure o f400 bar (5800 psi). If the backpressure exceeds 400 bar, the HP1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences______ , ______________________________________ 5.1 To minimize interferences when analyzing samples, Teflon should not be used for sample storage or any part o f instrumentation that comes in contact with the sample or extract 6.0 Equipment____________________________________________________________ 6.1 Equipment listed below may be modified in order to optimize the system. Document any modifications in die raw data as method deviations. 6.1.1 Micromass Platform LCZ Mass Spectrometer (or equivalent) equipped with an electrospray ionization source. 6.1.2 HP1100 low pulse solvent pump, solvent degasser, column compartment, and autosampler or equivalent HPLC system. 7.0 Supplies and Materials 7.1 Supplies 7.1.1 High purity grade nitrogen gas regulated to approximately 100 psi (or house air system .). 7.1.2 HPLC analytical column, such as a Betasil C18 column (50x2mm, 5 pm particle size) or equivalent 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 001780 3M Environmental Laboratory Analysis Using HPLCE-TESlc-8ct-r1o5s5p.1ray/Mass Spectrometry Page 3 of 10 Report EQ2-0443 Tenn. River Valley Sam ples Document may be used, if current, for 14 days from 11/21/2002 8.1.2 Milli-QTM water (ASTM type I), all water used in this method should be Milli-QTM water or equivalent, and may be provided by a Milli-Q TOC Plus system or another vendor. 8 .1 3 Ammonium acetate, reagent grade or equivalent 8.13.1 When preparing different amounts than those listed, adjust accordingly. 8.13.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g ammonium acetate. Pour into a 2000 L volumetric flask, add the aSptoprreopartiraoteomvotleummpeeoraftMureil.li-Q water, mix until all solids are dissolved. 8.1.4 Other solvents and solutions may be used as stated in the protocol or the sample preparation worksheet. 8 3 C a lib ra tio n Standards: 8.2.1 Typically two method blanks (Milli-Q water), two matrix blanks, and a minimum o f 5 solvent standards are analyzed with each group o f samples. 9.0 Sample Handling ________ ________________________________________ 9.1 Standards and prepared samples may be stored in capped autovials, capped 15 mL centrifuge tubes or other suitable containers until analysis. 9.2 If analysts will be delayed, standards and prepared samples may be refrigerated at approximately 4 C until analyses can be performed (refrigerator temperatures may have a detrimental affect on the solubility o f saturated solutions). 10.0 Quality Control__________________ 10.1 Blanks: 10.1.1 Solvent blanks, method blanks, and matrix blanks ore prepared and analyzed 'with each sample set to determine contamination or carryover. 10.1.1.1 When the study matrices consist of highly purified solvents such as Type 1 water or HPLC grade organic solvents, the method and matrix blanks may be represented by a single solvent blank. 10.1.2 Solvent blanks should be analyzed prior to each calibration curve. Method blanks and matrix blanks should be analyzed after the initial calibration curve but prior to the study samples. If carryover is a problem, consecutive solvent blanks may be necessary. 103 M atrix Spikes: 10.2.1 Matrix spikes may be prepared for each set of extracted samples (if applicable to the study) and analyzed to determine extraction efficiency. 3M Environmental Laboratory Analysis Using HPLCE-TESIe-8ct-r1o3s5p.r1ay/Mas* Spectrometry 001781 Page* of 10 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 10.2.2 Matrix spike duplicates may be prepared periodically to measure the precision associated with the analysis. 10.2.3 Analyze the matrix spike and matrix spike duplicate (if prepared) in the same run as the original sample. 10.2.4 Matrix spike and matrix spike duplicate concentrations should fidi in the mid range o fthe initial calibration curve or should be prepared at 1.5-5 times the endogenous concentration of the analyte. Spike concentrations should fidi in the low-range o f the initial calibration curve if extremely low levels are expected. 10.3 Continuing Calibration Verifications: 103.1 Continuing calibration verifications (CCV) are analyzed to verify the continued accuracy o f the calibration curve. 10.3.2 Analyze a mid-range calibration standard after every tenth sample, with a minimum o f one per sample set 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 o f analyte response to IS response and a known concentration of the analyte o f interest. The IS should be spiked at an amount that will fall within the mid-range o f the calibration curve. The IS should be added after the extraction process and before analysis. 10.4.2 A surrogate standard may be used for quality control. The surrogate is used to quantitatively evaluate the entire analytical procedure including sample preparation and analysis. The surrogate should be spiked at the beginning o f the sample preparation and should fall within the low to mid-range o f the calibration curve. 11.0 Calibration and Standardization______________________________________ 11.1 Analyze the standard curves prior to and following each set of samples. The average o f two standard curves may be plotted by linear regression (y = mx + b) weighted 1/x, or quadratic fit (y = axJ+ bx + c) using MassLynx or other suitable software. The calibration curves should not be forced through zero. 11.1.1 The closing calibration curve may be excluded if the CCV's meet acceptable criteria. If only the first curve is used, the calibration and standardization parameters are the same. 11.2 If the initial calibration curve does not meet acceptance criteria perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze. 11.3 For purposes o f accuracy when quantitating low levels o f analyte, it may be necessary to use the low end of the calibration curve rather than the full range. Example: when 3M Environmental Laboratory Analysis Using HPLCE-TESle-cgt-rtoSsSp.rlay/Mass Spectrometry Page 5 of 10 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 attempting to quantitate approximately 10 ppb o f analyte, generate a calibration curve consisting o f the standards from 5 ppb to 100 ppb rather than the full range o f the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting o f high concentration standards. 11.4 High and/or low points may be excluded from the calibration curves to provide a better fit over the linear range appropriate to the data or because they did not meet the pre determined acceptance criteria. Low-level curve points should also be excluded if their area counts are not at least twice that o f the method blanks. Justification for exclusion o f calibration curve points will be noted in the raw data. 11.4.1 A minimum o f 5 points will be used to construct the calibration curve. 12.0 Procedures____________________________________________________________ 12.1 Acquisition set-up - please reference the SOP that pertains to the specific instrum ent. Actual parameters will be recorded on the instrument printouts. 12.1.1 Set up the sample list 12.1.1.1 Assign a sample list filename using the first letter o f the name o fthe instrument (T for Tucker), the year (00 for 2000), the month (04 for April), and the day (T001012 for October 12,2000 on Tucker). If more than one list is made on the same day, use increasing letters of the alphabet starting with A at the end of the list 12.1.1.2 Assign a method (MS) file. 12.1.13 Assign an HPLC program (Inlet file). 12.1.1.4 Type in sample descriptions and vial position numbers. 12.13 Tspoecctrreoamteeatemr hetehaoddin, gclsicakndonsemleectthSoIdRi.n Stheet iAoncqizuaitsiiotnionmcoodnetraoslappapnreolptrhiaetnemanadss mass to 499 or other appropriate masses. A full scan is usually collected in addition to the SIRs. Save acquisition method. See the Micromass MassLynx GUIDE TO DATA ACQUISITION for additional information. 12.13 Typically the analytical batch run sequence begins and ends with a set o f solvent standards. 12.1.4 Samples are analyzed with a continuing calibration verification (CCV) injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor for possible analyte carryover. 123 Using the Autosampler/Column Heater 12.2.1 Place sample vials into the sample tray according to the sample list prepared in Section 12.1.1. 0 0 1 7 S3 3M Environmental Laboratory Analysis Using ETS-g-155.1 HPLC-Eleetrospray/Mass Spectrometry Page 6 of 10 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 12.2.2 Attach the proper analytical column in the column heater compartment. If using the switching valve, ensure that the tubing is run to the appropriate ports. 12.3 Using the Inlet Editor 12.3.1 Set-up the HP1100 using the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12-3.1.1 Sample size 10 pL injection 123.1.2 Flow rate = 300 pL/min. 12.3.1.3 Cycle time = 10.0 minutes 123.1.4 Mobile phase components: Solvent A: 2.0 mM Ammonium Acetate in Water Solvent B: Methanol (MeOH) Solvent Gradient: Time (xnixi) %B 0.00 5.00% 1.00 5.00% 4.50 95.0 % 8.00 95.0% 8.50 5.00% 10.0 Stop 12.4 Instrument Set-up 12.4.1 Refer to the Platform LCZ User's Guide, the MassLynx NT User's Guide, the ETS-9-36, "Operation and Maintenance o f the Micromass Platform LCZ Electrospray/Mass Spectrometer", or the SOP that pertains to the specific instrument 12.4.2 Checkthe solventlevelinreservoirs andrefill ifnecessary. 12.4.3 Check the rip o f the stainless steel capillary at the end o f the probe with an eyepiece. The tip should be flat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 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 SetHPLCpumpto"On". 12.4.63 Set the solvent flow to the desired flow rate. 12.4.6.3 Observe droplets coming out of the tip of the probe. A fine mist should be expelled with no nebulizing gas leaking around the tip o f the probe. Readjust the tip of the probe if no mist is observed. , ^_ U 01784 3M Environmental Laboratory Analysis Using HPLCE-TESle-8c-t1ro5sSp.r1ay/Mass Spectrometry Page 7 of 10 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 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response. Actual parameters will be recorded on the instrument printouts. 12.4.7.1 Drying gas 250-425 liters/hour 12.4.7.2 ESI nebulising gas 10-15 liters/hour 12.4.7.3 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 spectrometer information, and all other applicable information and store it in the study binder with copies taped into the instrument run logbook. 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 andCalculations______________________________________ 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. 13.1.3 Calculate actual concentration o f analyte in matrix (pg/mL): On-Column Concentration (pg/mL) x Dilution Factors = Calculated Concentration 14.0 Method Performance__________________________________________________ 14.1 The Limit o f 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. O' 3M Environmental Laboratory Analysis Using HPLECT-SE-le8c-1tr5o5s.p1ray/Mass Spectrometry Page * of 10 Report E02-0443 Tenn. River Valley Samples Document may be used, if current, for 14 days from 11/21/2002 14.2 Solvent and method blank area counts must be < V%that o f the lowest standard used in the calibration curve. 143 The coefficient o f determination (i2) value for the calibration curve must be greater than or equal to 0.980. 14.4 Continuing Calibration Verification (CCV) percent recoveries must be 30% o f the standard concentration. 14 3 Internal Standard recoveries should be within 50% o f the spiked concentration. 14.6 If criteria listed in this method performance section are not met, maintenance may be performed on the system and samples reanalyzed or other actions as determined by the analyst Document all actions in the raw data. 14.7 If data is to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed in the text o f the report 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 Recoups______________________ 16.1 Bach page generated for a study must have the following information included either in the header or hand written on the page: study or project number, acquisition method, integration method, sample name, extraction date, dilution factor (if applicable), and analyst 16.2 Print die tune page, sample list acquisition method and all other applicable information trouninlcolgubdoeoikn.the appropriate study folder. Copy these pages and tape into the instrument 163 Plot the calibration curve then print these graphs and store in the study folder. 16.4 Print data integration summary, integration method, and chromatograms and file in the study binder. 1 63 Summarize data using suitable software and store in the study binder. 16.6 Back-up electronic data to appropriate medium. Record the file names and location o f backed-up electronic data in the study binder. 16.7 Documentation o f analyte(s) and all reference substances will include trace numbers, lot #'s, purity, expiration, and storage conditions. 17.0 Attachments 17.1 None 3M Environmental Laboratory Analysis Using HPLCE-TESle-cHtro5sJp.1ray/Mass Spectrometry 001786 Page9of10 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 Platform LCZ User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA14 SRZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.2 MassLynx NT User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 183 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 o f Hewlett Packard HPLC 1100 System Equipped with a Mass Spectrometer Detector and/or a Photo Diode Array Detector". 18.5 ETS-9-36.0, "Operation and Maintenance o f the Micromass Platform LCZ Electrospray/Mass Spectrometer". 19.0 Affected Documents________________________________________________ 19.1 None 20.0 Revisions Revision Revision Number Reason For Revision Date 1 TitleChange 09 May 01 Section 1: Enlarged the scope of the method by including additional matrices. Also added comments about specific parameters will be defined in the protocol or prep sheets. SSSSeeeeccccttttiiiioooonnnns3381::: aCARnheddmad2neo:gdveRepddaetrmopaagoarrvlaalegopdrwharpaedlhfilefoofrweenrnieCncngeotsnfstvoyoersnsttehptimeeocnsuiasfailencvdocsfso.aoZmlft-tpeSworpnaurranaetdyi.vsp.ersoobleveinnttesralancdes.olutions. Section 9: Broadened the types of storage containers and conditions. Section 10: Added comments to allow for flexibility in quality controls for different types of studies and applicability. SSeeccttiioonn 1111:: AAddddeedd aa ppaarraaggrraapphh (a1ll1o.w4)inagllofowritnhgefeoxrctlhuedidnrgopopfidnigeosefccounrvdecpuorvinet.s and minimum number of curve points needed. Section 12: Added comments to reference the specific SOP's for set-up. Section 12: Corrected numbering. SSeeccttiioonn 1186:: AAddddeedd preafreargernacpehtoonthreecmoredthsoodffaonratlhyeteHs aenwdlestut-bPsatacnkcaerds.LC/MS. 3M Environmental Laboratory Analysis Using HPLCE-TESI-cSc-t1ro5Ssp.1nyrMass Spectrometry 001787 Page 10 of 10 Report E02-0443 Record of Deviation Tenn. River Valley Samples I. Identification Study / Project No. TN River Valley E02-0443 Deviation Type: D SO P ^M ethod Equipment Procedure (Check one) Protocol Other: Document Number: ETS-4-04.0 _________________________________ ________ - D ate(s) n Tu ^ o f occurrence: 3 r,sf ,9, 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 f^ " _ 1 .j. ,z ._ ' _ 7 1 7 ........ . Actual Procedure/process: The internal chain o f custody forms were not generated or used in the course o f this study. III. Actions Taken: (such as amendment issued, SOF[revision, etc.) N o additional actionw ill be taken, as the information cannot be recalled solqng afterthefact. Recorded By: /'t " ' /> ( { i t'l t- ^ ) 7 IV. Impact on Study / Project This deviation does not adversely affect the quality o f the data. Date: P h r <TL Authorized By: (StudypirCctor JEr.oiect Lead) /t 7T " (-'/s . - Dae: r XJUX788 3S i E nvironm ental Laboratoiy Deviation N o .__ / (assigned by Study Director or Project Lead at the end ot`study or project) Report E02-0443 Attachment B: Data Summary Tabues Tenn. River Valley Samples 017S9 Report E02-0443 Term. River Volley Samplee . ___ D020626Extrectad O1 90 3M Environm ental Laboratory Page 41 of 276 001791 Raport E02-0443 Tann. R iver V aley Sampias Ri ? 11-- : H *1* l g S lll i W * I8H M 0 s | |i rS 9 |{ 111iiasssiilSBSi3ssSli53sS mm =32* I 3 i2 3 2 ll9 ill m i s iiSse |S S H M iSOi!iiEl | | jl!H|]1399iSHS99SIfttaaa333S3133 ; t 9S tifili m ii m m m H i tt l il II |S []li i a s s s ii g I^ 2 is s s S3is i m m * l i8*83: ' m i m i 93 1 m m N n n M tv fi n|8g 3339 jM a M H ! 3 ! !l ,w . m in 88U88 48 8H0aS ^Bt I5t5i5l5s mu rm iis iI I II S 3M Environm ental Laboratory Page 42 o f 276 Report E02-0443 I I1 8 0 \ \ 3M Environm ental Laboratory Si.. D020628 Lars Mouth, Extnetod Curvo Sam * Location! 2 and 3 I I 1 H a S a np to N toto Im p h M A M P IE SAMPLE OUOEOO83.0 S H IM -3 -1 DUOEOOB4.D 3 L -1 U 4 -W T *m . to rV *8 *y M lft*p -t7 A n O E C M C A lA .2 0 A n a B T a n . W w VaMy M L M P>17 A OECMCMLA.2 0 Jun 02 T am . W w V a iM M l P iP -t7 AM 02.C M C M A .2 0 AM 02 H S eK T E S fU S iW 020B -5J , ia t * * m la/o k /m e e . 2 U MaOH Storte TN-A4B11S: OSJ w iflttP B K M LA A fIS ta r n Ptaarv a ia y M l P iapi7 Am q ig m c a h a . 2 0 A n 08 OUOC0066.O B U 1 L M 4 4 DUOCOOTOlO s u i LM-4*3 O U O m n E IL -L U M -M S T am . W w r vatoy M l fta ^ t r A n CB.C M C M A. 20 J in 02 T am . P M V ay PWL P im -t7 A n 0 2 CMCMLA. 20 A n 02 T am . M a r V altov Ptoh. toap-17 J im ICMCMLA. 20 A n 02 " SA M ?~Bk07X D . ti fa n . W w r Vatov A r ti ftio O T AM 02 U A A . Jun Q " U bflO H O S U 3 ;IM -M tm n . W var vatoy M l P np-17 A n 02 C IM W LA. 20 J in 02 T am . Riar vatoy FMl P nyM TJun 02 CUCABA. 20 A n 02 SAMPLE DUOB0077.0 SL-S.LM-a-1 DUOE0071O S t-3 . U L M a K T SAMPLE AM PLI SAMPLE SAMPLE SAMPLE DUOEOOS1.0 M aO H Itortt DUOC6S6LO S L 4 .U S - OUOEOOM.O B L A IM -3-1 OUOEOOB4.0 3 L -X L IL M DUOCOOMO 3 L 4 .U L 9 9 T am . M ia r vatoy M l Piap-17 A n 0 2 CMCMLA.20 Jun 02 T a m (m t vaia y M l Prap>17A n 0 2 CMCABA. 20 A n 02 ftT a n . W v VWto* PWl Pne-17 A n 02CM CA2A. 20 Jto i 02 MaOH flto rte TMJLC611 OSJ m to rn i: MLA/UCC m. *>jwT a rn torVam yPtoK. P i*p -lf Ju n ttc ia c /M L A . 2 Jua T a rn to w r Vatoy M l M p -1 7 A n Q2CUCABA. 20 A n 02 T a rn tonar vto ay n a ^ v jm u u a a u to tA . ut T a rn touw V rttoy n m . toap>17 Jun 02 CMCA2A. 20 J in 02 SAMPLE OUOEOOMD SLA LM -L1 T arn, to rn r V to w M l Pt w 17 A n 0 2 CMCASA. 20 J in 02 s w n i T K oS T d MaOH S tar* ~ 3a m P C T " S jd E o D s h u m j 1 M U OUCSCOM.P SL-3.LM -4-3 PU O E W S O B L 4 . LM -4-M OH Storte TN-A461 1 1 06 Ju n O rto t: M LA A li fa n . to varVatoy M l P r^-1 7 A n 0 2 C M CAtlA. 20 Jun 02 T a rn tonar VaSty P lrtL toaplT A n 0 2 CMCASA. 20 Jm 02 T ana M varVM M y P to l P ra |H 7 Jun n CM CASA. 20 Jun SS OUOC0OS1P S L 4 .L M + 1 T a rn W w r vatoy P W t % *p -1 7 Jin 0 2 CMCASA. 20 Jm 02 OUOCOQSEO S L 4 .L M 4 4 T n n . RWarVasw PW L P ne-17 A n Q2CMCABA. 20 J in 02 ` l ii in iu O e O O S lO 0 2 0 0 M W * E x n a to LU A rti O r a . cS A -O T .1 0 0 *1 M LACM CAM E.2 1 Jin DUOE0064J3 MaOMStorte MaOH S torte THACS1 1& OSJun OStoPak ULAAlEE D U O C O O K B T L 4 .U JO T a rn tovar V W ayT to i P np~17A n 0 2 C M C A tlA 20 A n 09 D U K O eaS P $ L 4.U M 1 T a n ftn a r Vtoay PUB P np-17 A n 0 2 CMCAUA. 20 A n 02 OUOCQOB7.D S L4.LM O E SAMPLE DU0E809BD SL-S .U LS A P O C B toa iC S L A IM S MS T a rn tosar Vatoy M v Prap-17 A n (a .C lfC A IL A . 20 A n 02 T a rn tovarVatoy FVh. Prap>i7 A n 0 2 CMCMLA. 2 0 Jun 02 Tm m varV m w M S . P tort-17 J u n 0 2 CMeflSLA. 2 J m *2 m & F o r B utitto b MaOHMfik - fs s R r MaOH B tortc T N A 46 1W 01 J w O tD a ): U L S S f T a m tia r V rtS rfiS r^ n p -^ T A n QIO SCa K a A n T L RHarVWHy M l P iap>l7 A n 0 2 CMCAILA. 2 0 A n 02 OOEOIQSO SLA. U 4-7A T n n . to v Vasay M v P iap-17 A n 0 2 CMCAHA 2 0 Jun 02 OUOCOKMO S LA -S M -M T a rn U rtar vasay p m l Piap*17 A n 0 2 CMCASA. 2 0 J in 02 OUOE01OSD JL4.SM M 3 T arn. to w rV a to r M l Pfaa-17 Jun 0 2 CMCAHA. 2 0 Jun 02 MaOH S torte THA-081 t OSJun f lU : M lA A lE * "SAM PLE DUOED107P 020094207 DOOIOSO L -1 S M -1 - DUOS6101D IU W > 1 -M ouoeonab AU aoT F M d U l P to iC una. 0 2 0 0 4 2 4 7 . TOObc. IBJW CM CAKE.21Jun ta m . M w Vtoay M l Pip -17 Jun 0 2 CMCMLA.2 0 Jun 03 Tm M n r V a ia * P toh. P im -f7 Jan 0 2 CMCASA. 20 J m 02 * lr tra r tto LM R ahC w m . Q 200M 247. lOOpp.M L A O A C A ^ K n MaOH B W * TH A4S 11& OSJ m OMpOk M L A A ltf o u o e o m o m io h m SAMPLE D u o e o m p MaOH S torti MaOH S torte TMJL0S11 2 OSJun OBypaK M LAAlEE MaOH S torte TNA41S11 2 OSJ m O M a): MLAAMS ----------- F w n m r ------------m m m " ------------F w r p m r *TM * ' S T % A ia * Am am i o rn a i % A rsa AT aTmTn t 27*42 SLOQ 33683 SLOQ 68086 BLOQ 22037 27aaa 2135701 LO G SLOQ 99.0 21426 9B% 33608SB SLOQ SLOQ 90J 30636 100% lh S 3 *3 BLOQ 1&&.0 1S2S0 ta s s a 1S300 13S0S 121S91S M5Q SLOQ SLOQ SLOQ SS.7 12036 13360 6476 10SIS 1666*36 SLOQ BLO SLOQ SLOQ 46J 14047 27336 22S37 23749 4% 62*164 LOO BLOQ BLOQ BLOQ 442 T E oa" 13207 12072 1S0BS 17S0S isa o s 20045 133SS 1 0 2 7 BLOG 106S7 SLOQ_______ 6304 S L ff^ I267 SLOQ 16879 SLOQ 1413* SLOQ 12291 SLOQ 12607 101 104% s t f iis r SLOQ SLOQ k BLOQ LO Q SLOQ BLOQ 100.S 9*668 12761 01M 7 80935 9 4 8 0 69*14 101% 1716039 1k BLOQ BLOQ BLOQ LOQ BLOQ SLOQ 102.0 12222 10*1313 m as 1812 173*2 12*07 SLOQ 4U SLOQ SkQ SLOQ SLOQ no 1766866 5762 796 2170 3164 SLOQ 47.1 BLOQ SLOQ BLOQ BLOQ 12470 64% 969972 17754 26*77 10099 2S794 %OQ 410 SLOQ BUM BLOQ SLOQ 12351 14^4 1 2 *3 * bL SUM SLOQ 4082 5736 7383 SLOQ BLOQ BLO KMS2 2*406 2474 BLOQ LQ SLOQ 117M 1I A 12702 SLOQ 1764116 4 8 J T % 664400 4029 BLOQ 14194 47J LO Q 10423 21*13SS tO Q 1014 337 ice% 3341760 BLOQ 989 13751 100% 1714082 BLOQ 1D1E 13212 14411 1134 13347 1437 103*112 113*2 23963 247QS 2240S 10866 11225 ma 2204743 SLOQ k SLOQ SLOQ SLOQ 424 SLOQ SLOQ SLOQ SLOQ SLOQ SLOQ k 1GB2 11921 73 5179 5301 4999 19106*1 5 4 *0 64*7 9 40 1292 12780 198S 103% 3321739 BLQQ BLO L 0 BLOQ BLOQ 44J SLOQ BLOQ BLOQ BLOQ BLOO to .0 0 SLOd mi 19422 BLOQ 19783 BUM 13113 BLOQ 19611 SLOQ 12044 BLOQ 8% 6667*2 4LS 1111 lO G k 62604 BLOQ 93144 BLOQ 96973 BLOQ 52*02 - g f f l . T l2 b U M 98% 1717400 101. 1*0*1 SLOQ 13199 10SSS1S 4 4 J 17*6342 1 5 5 5 T T -- t o n " 103% 3309089 BLQ 419 100.4 H JU 97% 74431 47E 100% 1726637 " ita .'# ' 13*21 L 0 Q 2S9 BUM 12646 LOQ io s a * 161 SLOQ SLOQ 3100 1*49 LOQ BLOO 9C 0 63*6 LOQ BLOQ ... H % A ra * 1 M 8880* B8M 9 3 6 0 3 S0B4 114107 116125 120642 1943492 78113 1*44 74940 7*319 24287 2*422 2 *1 *9 %102% W ooA 74 1 1 8 8 8 ** 264*4 22172 21371 1924 3119 M ia 6472* 9% 18*818 38242 3 *3 102% 2967*01 404 3*610 27071 29221 Z7S80 % 138M1S 476* 22*37 24212 41012 40143 1997 1C0% 2823130 to rt 64% 109037 103% 26*8243 1 1 0 0 UM " BLOQ BLOQ BLOQ 104J BLOQ BLOQ BLOQ LOQ 94J L SLQ. BLOQ BLOQ BLOQ BLOQ BLOO mo BLOQ 37.7 SLOQ BLQ LOO U M 8L k SLOQ 517 BLOQ SL0 10U LOQ LOQ BLOQ BLOQ LOQ 4LB k tu b PQ U5Q 8U M BLOQ BLOQ 1Q1J Ut 33A 1003 LOQ SLOQ LOQ ------------ m r r a n ----------ih m * % 17 106% 43337*3 1108B7 2S380S2 BLOQ 28*7*32 2940014 1N% -E S T -5 5 B S -- K S 5 ------------ 113*02 71142 BLOQ 71*542 BLOO 57*044 5778S1 _ f is a _ 102% 42*0342 108.4 10M 02 tU 30 78% 3*8722* V A M1CS% 61614 997130 4662*3 8N 164 104611 BLOQ BLOQ BLOQ LOQ BLOQ 1013001 102*0*1 188% 2S13X62 9 1 3 361* 109% 4200940 112914 93*666 8 0 *1 *2 8*433* 906897 11% 233X1*1 109*2 ~ 110 Ut BLOQ 411 LOQ BLOQ 1012 BLOQ RLO BLOQ BLOQ BLOQ k6 96% 10% 80*706 8*323* 42*027 48*574 NM S* 102% 42404*3 BLOQ LOQ LOQ W M 104% 4S M *1 ~ w s 2*11814 ..,, m . 101% 3 s a r 10 40 LOQ 46% 103% 7M B 87703 BLOO Tenn. River V a le y Samples Page 43 o f 276 001792 R tp o it E02-0443 3M Environm ental Laboratory ............ .e. D020629 C HR ah, Ei Iik W C u re ne itw*U ! iM ffe H * MaOHBMCTNAOmivM JIM MUMB ItaOH TMMB1IS;MJim OBtea;UMU ItaOHtaW TNJMN11S; Jim 0MP4:aiUMCt UaOHa w TWA4A11 Jim n m f. MUMCC maaomcieuoMai im e iie n DUMAMID BMM647 02*834447 UaOHA M 020A34644; 1A.t4 FMiCanal CMC:2IJe B Bien>sMB; bool* n e canaa:CMCa Je a 820G3W4U; lOBUwneCuMCMC;Jwtt UaOH THJLBUt J e " " * * * UaOHBM: THA4AU8;OSJanBMP);MMWB UaOHBUM:TH-40811;MJ e 0ip6);***** Bern OMBMBW: tOMBPn e CanMCMC;a M a WJwn e Cww;CMC;a JWa BMOeJMT: fWSpBn e OMMTCMC;a Juaa e w M e a; ie*B necw w C M C ;ajee boos-amt; MDSpfunecwwcCMCiaJuia UaOHBUrtLTHJMMUIcMJw atrpa); IftMteE UaOH*W TNJUHUlWJeBgipa);U M IH UaOHBMl-THAWAU;MJim M a* MUABK MM pwhoabo a ao cim i M IM U M Mm.an.iM m m enM ouosoasro MCO-frOI 0034647 hSMCMMA m oouM i OUManio mnm.KA.ifi 00034411 uaOHBwe UaOHBUM MMMMn 0U0CDAA1D h M R M aoaiiiB T DUOC0H1O a n u t ff oOSSaott NMMMK IM H IM D M m u n MaOHOUe M M SM in 8H09-9M1: iJ a * necunMCMC; a jm a 03*B34642;ll4neCua;CUe; X M O O M M W ; 04*6 n e C M CMC;a J a CBS4Mk M.0M n e C w w CMC;a JWa eaaMMS; 2&MMn e chmk cue;a jm a mm i m n* n itra t n en m n ir - n ur H BMBMfta. ieoswBneeMvaKCMC:aJMa B2DBMBW;PB.BMn e Cum k CMC:a Je a M M : 0SpwnecuwacCMC;aJea awo-ac-w; m B e ^n e cim w C M ca je a oioaoweH; iaooo n e b ra e CMC;a j* a UaOHM e TM *1IS; Jwfleek*aAMet IMOKBlM:TH*4eUS;a Jw a e fc*H M * UaOHMW TMvMBtU;JeflM M t MAMB anfcMM oooowtof;im c cu ne m ; mummcw b; j i je Mam M07; WCpMcune m . MCMTMTJIg;21 Je M M 1OT;KM** CMPMMia; ULACMCUK;21 ie BBBBS4M 7:ifla#ruruiiM am yuurM CM i:HJe BBOOUMT: U M * cane nr. MLMCMOIK21 Je a ueOHm * . TH4eeii t a jw eepM; Mjwae UaOHMW TNJUB111 Jim BMpttUUMK UaOHMaw 1NA4B11tMJeOJApak MLMMU MM 1AMAU eaoBMS-tt cane w e e u e u c w e ti 1 t i A20034M1: M C iM B M iM W iK M ttllM iH DM M M ;IJw ca iew eM L*rM rl aB i;2ije<H IQAMI I BB BM8MM3: SMc e w ia r MLMCaewS21Je a ~jaw n II '6'. hum c g ie w e MUCMOtatit Je a eooMUC:a w cane mmm iM C M O M th Je a aaow a o M e ^ ^ n e w e A M C M a u a tiJ e a n e o n iff e m u u r : ie c e e e n m m m c m d i jw b IHM M g20C3440W?Uae raffiTaea; U W M C a t21 Je a BMWI I B1BB1I I 11 mow h i i tU N B M M P a a iw TMWeMMa: MIMTMCBM21 J ie a B2agSift7sacehe w e ia.M-MCMg.2i am a bm o m m i: iM D aecaneH K>M C M caa.aJe a iMOHM<c 7M *a ii t a JeMKwk ifcwee VtOHBMnk UaOHBMWTH JK B U taJe on.a t m UaOHBM UeOHM W T M A an ta JeBM ak UAMBB --'tm T'STvuuy n a e je n cmcma Je a QUOMOM-O BL-1;C>1-1 0U0UPM.0 L-1 C*1-3 puoeoMio n w - i TanwIMrVWvnULMa-n Je a CMCMA J e a t m. veay n e M e n Je a cucM A a Je a Tm .wwve e n e M e n Je a CMCMAa Je a TantWerve*v n e M e l? Je a CMCMXa Je a UaOHBW* UMOMMW T H * * a JetakMfc WUMGK DUO0 OAA.O 3L-1.&M T w . Mwve e n e n e irje a C M C w uaje a BULC4-M TarntMnrVM n e M e n Jwia CMCMULa Jwia L1.C4>1 H .C -34 DU0EM710 B.-VC-M fm M r vau n e M e Je a ch m a a Je a TantW e MUy n e M e ll Je a eUCMA a je a TeatMarye n n e Mw17 Je a CMCMAe Je a M. MUS BIB A7B1 MM MM. Bt^Q ILOQ BLOQ 2*27 I0AAAB 137BBBB MOM 20*4* 1*731 B7B 20BB00B 211M 1 2120IM 2MM37 2112MB 1MM 10341 110 3MB7 71MB 143*07 2M346 CBN 11*7740 214MM 44*3*20 7BM731 lOSTBMft 12*1MM 7*2*1 2T121 19BM IflMB 1BBM1B 1*17372 140MB M17M* KOMM 0.1 BJ BbOO BLOQ 127* 1313 1334 1224 1214 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ LI 124 32B *74 1334 2M4 04 04 04 BLOQ BLOQ L0Q BLOQ ai i *74 BB4 74 M.4 lO B *444 1374 77 4 ltt* MOT? M3 131MB 223*30 94T7B MOB .w nrn. att S33B7 BBBllBB TBBBat I14M IBM T24M 147 12MB tr io 12BB4 12H3 Wa 11717 1123BM MB3B 1S3M 1M1B BLOQ BLOQ BLOQ L0Q ko BLOQ 11 4.1 2*4 bi 1004 247.1 101.1 04 04 LOQ BLOQ BLOQ LOQ LOQ LOQ BLOQ LOQ BLOQ U4 % Ana U M m. UM 6 6 MM LOQ 41 % Ana A n noM. u t 06 207*7 LOQ 30M2 LOQ 23BBH 170 12CMI71 LO 12MB0 74MB 14BB BLOQ 40 BLOQ 2441M1 7BJ 347MB 2442744 24041*7 7tB 2S11BB 11710 LOQ 544S LOQ 2734 LOO xn t MCQ >4*73 LOQ 2B 0 U 77IS 4.7 >227 U 7*727 22.1 1407410 4U 2344414 .7 S223M3 i 21012 U 12390272 L0 uaowsi 10*171 10 4B734 12 17*01 LOQ Am MO loo 4 211*0 101J * 30M444 i j 1014 31230 101.7 -TL 3144477 W J 31MBS2 ia . 1B12 LOQ **7* BLOQ 11973 BIT 1140121 11S21 M4 11970B 4.7 117MM 712 173 BLOQ 1041 LOQ 4M LOQ M*1 BUDO 2207 LOQ 44112 11 LOQ 1B10N 74 3COBO 111 MOB 27.7 12130 734 2BB7 14*4 41*6437 04 S7BS741 04 71113 S32B LOQ 24014 BLOQ 14044 BLOQ ME 10M4 BLOQ 102.1 144MM 1044 M 1627441 1024 1072 163MM WB4 WK 1M1M0 1074 W.0 WS*744 WH ra t 4422 22 27 2B4 447 IM 100477 OB 1MB * 2M7B 11M UOMO 10M tk tW im 212KB7 IM M32DH 10M M isa i M UI4MM M MB7B3 1344 2MM IBM41 11234 BM 7IO tea t J** 30*7 S til 13M UM * 22 134 LOQ LOQ k 66 12 2J 114 1022 2402 02 ao oa u LOQ LB LOQ LOQ LOQ MOS__ BLOQ SL0Q 411 BLOQ LOQ LOQ UM 112% IBM 104% 100% M% 102% 100% M M M M% 114 10B4 74 77 i9 m OB 7777 10BOB JOBB 411MB W323M 31WB 473MT Bl124 734BB 7S4U 290H M71B " 771 23377 23*37 2B77S 14*20 100 14422 7101 1MM 202 34117 aoo LOQ LOQ LOQ LOQ 14 34 t!4 217 4*4 1B4 2413 0J 04 04 . LOQ LOQ LOQ LOQ LOQ BLOQ LOQ LOQ LOQ LOQ 414 LOQ LOO LOQ ra n a r im p r % Are WML % ATM Aawww aee % 64 270734 17 HAU 1 2SA0M 13 B3M ANM LOQ 1017 MO LOQ 3M1 BLOQ 2M LOQ 10*771 84AB UM* *2010 12*44* 124 LOQ LOQ LOQ BLOQ LOO 27*626 B4422 1331414 2M36M 1B41M to4 r.4 813 1104 24 3AS0M 12*M8> 34*3001 24 113 310 734 1734 149414 1 1 14 1173*0*1 04 04 MOQ Avar 14114 1044 % 27ia 1104 W% 24461S3 0.7 S S S - 10M4 u ii 1114 1114 ma As 1114 *% M IM 1112 4% 384844A 1870 381*1*7 LOQ LOO 1114 1117 1124 1114 1114 LOQ OB 104% 41DM 13M 100% M 2% WM 100% fl % 0% 0% 16442116 HB 32B 233M IBM 144W7 4123 104173 13% 126 14S4 143313 S 3-- 1.3 12M WM 24 164 4.1 4MM4 213 4BJ 1M7 107% 7114 12M.4 17 MOQ MOO 18 12 12 U 64 ILOQ 24 814 74 7.1 74 MM IBM 194B1N U1% 1IM77 1*3741 S2B7I 4*84 WM 742237 0.7 14 1M4 04 A4 LOQ LOQ LOQ 114 1A4 BLOQ 174 Aee 1134 M 1118 4% M UM M M 1M% DM Tenn. River Valley Samples Page 44 o f 276 01793 U01794 Report E02-0443 Tenn. River Valley Sample 5 j I 3M Environm ental Laboratory Page 45 o f 276 001795 Report E02-0443 Tenn. River Valley Samples lifM I H tflH sM e s: s< IM 11 illi i H S iU N it [ ] ^ S S ^ ii^ 3 ili2 3 3 ^ s 3 ii i3S 9 liig ^ 33St|i n m u m gggHHigi (liisiislii! mim HU S ili i m m[lfg S 39 9 ; S ii ^ S 3 ^ s i3 S39 9 i H iiI 55S i m m m iiii ifli m mmi [l32233i5It23sS2=2S5Sls33ami|g|g|f2f|3 iUS9 25Sigg22 is s a li nm s ig ili tem i n i i I lf9S 9S 25iS 3iK S 3S S 33^iS i3399S li3ii m m p a m m m m liiiilliiifi m nm iiim i m n m l! ijj jj 3M Environm ental Laboratory Page 46 o f 276 Report E02-0443 . D020702 CatFtoh, Extractad Curva Sirnpte Location 3 A ita i n M M M M rt ouoaom e o u c a o o rro o a o o itw hnpAMl AlM rAwl--aMnym. r T an Tm t.aWnnrVrMMrAfMHtPPrnap-.11TTJJmw00.CCMMCCMMUULL.30JJtmfiCS1 1601667 34330 MJ ILO Q 130 1" OTTWaaoOlno&O.lWN*AVWwMM*VrvMM;VM1A0eMw0*apnWtWAAPHC*nlMpPPt1MM.Wl7Spi1.Oj1:M77WMJJ0mmJ!8uM0O.nCUOMCCCMUMMCWCCCM)A;AMMMLIBUAAA.U;JaOMiJjJHMJmmuniQA0*l3 2140060470 2333063 1000 17106 JMLOQ 0 .4 ILO O LO O 0 T e m im i ATM A a a l 3 0 3 3 0 "S" e so ILO O 1271 ILO O 006 460714 * :9 Q _ 101.3 LO O S70 ILO Q % Aim M% 10600 3107 10% s & f r 110 L 4 .& + 2 T o n R N rV * |i A H Arap'17 J a i OS.C M C M U 30 A a i 83 21371 AI#U" niiMWWj IMfrH ---TTTfaaannn~IMNtR*MOpmMHwrVrOVVVMOtMMMMMcyv^rTAnAA1MHMHHir.0PP7A0>rmra1n^p1.a*.101ll7:7770JJJ6JumwmJnui0O0n033H3O...COCaCiMUCmGAC)Q;MMMMMAAAAUM333000.63JAJEImJamii0033a 10443 1T060601A6 1110 -M661 "ampi* AM PLI SAMPU OUOBOO0.O niOnUiMOnCiMnOeOus0.nOw ~E<Ith0a^.0O-i0wcH3*4M%4o4e27* suiD u o o o n .o o u ccoo oio aaoctt-Aor " tt-Ttaaaennnn HHMHwP*eva*vVVVMaMaMnny* AAAAHHHHPHPPmniro^p-.11f-Tl?7TJJJjMmmm C000Q033....iGCCC^MMMMrCCCCAA4MMiLIaAUAA.333l00JiJJJ^Mmmun000nn030 " ~* TTTTTaanaaanWnnnA.MWWWaMrMwVPwrrkMvVvVOaMMaMaasncyyyrTAAAAANHSHHHHAPM4PHAPBnSmnm1p^p^h1-1--311*1i7:777*70J*JJJJ6nmmmm*J0mn000033333.0A..C..8CCCCMa0MMMMMeCCCCC:AsMMHMMHiIUUUAUfAe....3333MJh0000OJJJJEmmmmJun00CnO303Bat 016737 UM13327 2300006 10140 110760 30337 30071 0140 17404 231703 LOO ILO O IU 00LL10OO00OQ0 *0LOQO 07J MJOLOO OLOO aILtOoQo 07LOO 133% 0% 133% 0% 231010 3071 3303 0 210 3077 414111000 261130 707 3347 304 4413440330 ILO Q W4iMOQ 0% ILO O LO O 0L0O0O 1010 ILO O ILO O 0f.4lft-.~Jf% .4MMS.... 13% 100 111100 0L0O0O 14441 161 LOQ 1470 IL*O/.Q 0AW 43J XO ra u (u n m nr % Am Ama 4M 100%n L . 0% 17006 230110 -- i-- i 0337 ILO Q 4332 LOO LO Q 100% 0 3 0 0 aoQ 0O O 4 1000 4% 47 86 7 103.1 LO O 3047 LOQ _ ILO Q 11013 XT LO Q gblaUg..,.. mJA 3600 301010 640 10 MJLOQ .fm LO Q LO Q - 346010 61001 138306 OLOO ILO Q LO Q LO Q B4LO4O LO Q LOQ LOO WLOUO.1 6t% 043 1163633 460 6446 UTM ILO Q ILO Q jm .. i 11.0LOQ 104% IMLOQQ LOQ ILOO n* 17100 000 7060 1 0 .4 IL4O14Q LOQ LOQ LOQ fLrOvfOe % 0% 100% 0% 7u2% Laboratory Tenn. River V a le y Samples Page 47 of 276 001796 D020812A 001797 Report E02-0443 Tenn. River Valley Samples 1M i t i ssllsllll mmI l li laaai: im agii* as lussiti IIII Sii i l i l mmm M SSK m im iila l {ititi fii'S tII I sa??!5 ssss! qqq* ssas33SS!i*S m m m m m HS* SSi^I^SlggSi^I I S B 2 *-a - iiilsiS S mi SiiSMXMI m m s ii ni m Is s is i m n |ilS iiE iil I till 319U ?SS3333 m m S ! 9i 2i m m m m 3s93a|aiii3ISs|ag ! issa?* m m S iiti! l i l i i l l ! m m m mm l i l l l i l i i i l l gB* {ititi n u a ii $ I HlgssansiSl m n S352 Ssa 33SS i^ ^l m m SS&21 a m l - !| ti s ls is s il ilS S i uh l ilifi SlIilll sisSS m m 8838 lj 3 titts & ti& 6 |3 l i i i i i ifa*"~?B5 f lig i i i l l i i i i l i b i i l l l b l l i l i i l b i i i l i l l i i i i l ooooooogo e o o e ooeeeI `l 1* '! I 3M Environm ental Laboratory Pape 48 of 276 D020812A Report E02-0443 3M Environm ent*! Laboratory Tenn. River Valley Sample go u99 ! 1 Page 49 of 276 9ZP OSs6d A jo j*Jo q e ~ | |B)U 9u iu o (a u 3 yyg I ii s s id u o s i A |d u u a x cm -zoa vodsu 001799 9IZ JO JS OBd Ajojuoqri |(juouiuai|AU3 ne 1021112 OISOO 8|duiBs to||> A JMM 'u u a i C*KW03 IKXtea R poit E02-0443 3M Environmental Laboratwy T0 8 T0 0 Tenn. River Valley Semples Page 52 of 276 Report E02-0443 Tenn. River Valley Samples 1021112 River Sediments Sample Locations 1,2, and 3. PFBS(299) |VmuLoi-i) 222222222000000000 SampleMama 000000000444444444445904500333333333---------330333333880686868000000000444444444640454800---------111332223 Samplebite Area EEEEEEEEE000000000222222222---------OO0000000444444444444444444333333333---------333333333888888888000000000444444444443568845---------233312211;;;;;;;;;SSSSSSSSSLLLLLLLLL---------111332322;;:;;;;;; 4414111 343233433288862320532354720280106370585308647149408099 OnA(n-mCg/oomhuLinm)tnOAn(n-vCfalfortnahLgaa)nn fCo(ornrbgr/iemi.cLtVe)di 11111888803001....9..32..9.85607 11. 9.1 8.9 456454535.........117430538 CSaomr(rpP0444a95535lS741322c007e333tW199802Pedrafopr. %SAtuCvdVer0(apgagen/g,d) 113544148041753343%%%7274 PFHS (399) 20 0443-30044-1 E02-0443-38044-1 ; SL-1; 1 122635 20 0443-30044-2 E02-0443-36044-2; SL-1; 1 110901 20 0443-30044-3 E02-0443-38044-3; SL-1; 1 111724 20 0453-30045-1 E02-0443-38045-1; SL-3; K 13341 20 0453-35045-2 E02-0443-38045-2; SL-3; 1 11489 20 0453-38045-3 02-0443-38045-3; SL-3; 1 12125 20 0463-38040-1 E02-0443-38046-1: SL-2; 4 17353 20 0403-38040-2 E02-0443-36046-2; SL-2; 4 19434 20 0463-38046-3 E02-O443-38046-3; SL-2; 1 25494 27 2.0 25 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 2.6 BLOQ BLOQ PFOA (413) 20 0443-38044-1 E02-0443-38044-1; SL-1; 1 295590 16.2 14.7 20 0443-38044-2 E02-0443-38044-2; SL-1; 1 260003 14.1 20 0443-38044-3 E02-O443-38O44-3; SL-1; 4 253343 13.7 20 0453-38045-1 E02-O443-35O45-1; SL-3; 4 48045 BLOQ 2.8 20 0453-35045-2 E02-O443-38045-2; SL-3; 60231 26 20 0463-36045-3 E02-0443-3804S-3; SL-3: t 54999 BLOQ 20 0463-38040-1 E02-0443-38046-1; SL-2; 1 53375 BLOQ BLOQ 20 0463-38046-2 E02-0443-38046-2: SL-2; 1 35197 BLOQ 20 0463-38046-3 E02-O443-38O46-3; SL-2; 1 40917 BLOQ POSA (493) 20 0443-38044-1 E02-044S-3844-1; SL-1; 41250415 29.7 28.8 20 0443-38044-2 E02-0443-38044-2; SL-1; 1361450 32.4 20 0443-38044-3 E02-0443-38044-3; SL-1; 41033771 24.5 20 0453-38045-1 E02-0443-38045-1; SL-3; 4 48310 1.2 1.4 20 0453-38045-2 E02-0443-30045-2; SL-3; 4 48172 1.2 20 0453-38045-3 E02-0443-3804S-3; SL-3; 1 65768 1.7 20 0463-30046-1 E02-0443-38046-1; SL-2; i 120487 29 2.9 20 0463-30040-2 E02-0443-38048-2; SL-2; 4 103503 2.5 20 0463-30046-3 E02-0443-38046-3; SL-2; 133252 3.2 PFOS (499) 20 0443-36044-1 E02-O443-38044-1; SL-1; 42785277 67.7 62.8 20 0443-38044-2 E02-0443-38044-2: SL-1; 42885124 20 0443-38044-3 E02-0443-36044-3; SL-1; 42109105 70.3 50.4 20 0453-38045-1 02-0443-38045-1; SL-3: 418454 9.1 8.3 20 0453-35045-2 E02-0443-36045-2; SL-3; 4 323943 6.8 20 0453-38045-3 E02-0443-38045-3: SL-3; 420485 9.1 20 0463-38046-1 E02-0443-38046-1; SL-2; A 417236 9.0 9.3 20 0483-38046-2 E02-0443-38046-2; SL-2; 4 393650 6.5 20 0463-38046-3 E02-Q443-38046-3; SL-2; 4 478587 10.5 1.4 1.3 1.2 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 8.1 7.1 0.9 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 33.8 35.1 25.2 4.5 3.4 4.6 4.5 4.2 5.3 136 132 124 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 806 704 685 BLOQ 13t BLOQ BLOQ BLOQ BLOQ 1481 1615 1221 62 60 82 143 124 157 3377 3506 2514 452 341 455 443 415 S14 130 6 s% BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 732 80 9% 131 BLOQ BLOQ BLOQ BLOQ BLOQ 1439 200 14% 60 12 18% 141 17 12% 3132 540 17% 416 85 16% 457 51 11% R333a885g333000M588444S000f584ai444---wMMMm456npSSSplHeiWmt221w222(009g000m...03)..9.140y100m ci tmtw--watphn. Average o t triplicata C orra cte d fo r In i. Voi. On-Col Amount * 0.5 C orrected fo r Sam ple Pran O ii-C o lA m o u n t*Q .8 *2 * 1008 Sample W eight (Ava) T ! tie Final V d of the Extract (mL) S M C onM w ttal 1/3/2003 001802 Pag 13 o f 21 Report E02-0443 Tenn. River Valley Samples E02-0443 Combined Large Mouth Bass Data Table PFOA 413) ! PFOS (499) I J U MS Sample Name Amount ng/g Amount ng/g Amount ng/g Corrected forSm pt Prep (ng/g) Amount ng/g Amount ng/g Corrected Ave, Stnd forSm pI Dev, and Prep (ng/g) %CV 42798 SL-1 ; LM-1-1 BLOQ BLOQ BLOQ SL-1; LM-1-2 BLOQ BLOQ BLOQ SL-1. LM-1-3 BLOQ BLOQ BLOQ 42799 SL-1. LM-2-1 BLOQ BLOQ BLOQ SL-1. LM-2-2 BLOQ BLOQ BLOQ SL-1. LM-2-3 BLOQ BLOQ BLOQ 42800 SL-1. LM-3-1 BLOQ BLOQ BLOQ : SL-1. LM-3-2 BLOQ BLOQ BLOQ SL-1. LM-3-3 BLOQ BLOQ BLOQ 42801 SL-1. LM-4-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 18.5 13.0 14.0 63.6 61.4 57.2 73.2 80.8 62.4 68.8 185.5 130.0 139.7 635.5 614.0 571.7 732.1 807.7 824.4 688.4 152 29.61 19.5% 607 32.49 5.4% 788 49.18 6.2% 700 SL-1. LM-4-2 BLOQ BLOQ 6.4 64.3 BLOQ 75.7 757.0 52.70 42802 SL-1. LM-4-3 SL-1. LM-5-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 65.3 46.6 653.3 465.5 7.5% 423 SL-1. LM-5-2 BLOQ BLOQ BLOQ BLOQ 41.5 415.0 39.03 ; SL-1. LM-5-3 BLOQ BLOQ BLOQ BLOQ 38.9 388.7 9.2% 3 42803 SL-1. LM-6-1 BLOQ BLOQ BLOQ SL-1. LM-6-2 BLOQ BLOQ BLOQ BLOQ BLOQ 69.3 59.9 693.2 599.1 651 47.78 SL-1. LM-6-3 BLOQ BLOQ BLOQ BLOQ 66.0 660.2 7.3% J 42804 SL-2; LM-1-1 BLOQ BLOQ BLOQ I1 SL-2; LM-1-2 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ A SL-2. LM-1-3 BLOQ BLOQ BLOQ 42805 SL-2. LM-2-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 2.6 25.6 SL-2. LM-2-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-2. LM-2-3 BLOQ BLOQ BLOQ BLOQ BLOQ 42806 SL-2. LM-3-1 BLOQ BLOQ BLOQ BLOQ 9.7 96.7 100 SL-2. LM-3-2 BLOQ BLOQ BLOQ BLOQ 11.8 117.6 16.68 SL-2. LM-3-3 BLOQ BLOQ BLOQ BLOQ 8.5 84.7 16.7% 42807 SL-2. LM-4-1 BLOQ BLOQ BLOQ BLOQ 53.1 530.8 547 SL-2. LM-4-2 BLOQ BLOQ BLOQ 11 SL-2. LM-4-3 BLOQ BLOQ BLOQ 42808 SL-3; LM-1-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 54.1 56.9 BLOQ 540.9 569.4 20.02 3.7% SL-3; LM-1-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-1-3 BLOQ BLOQ BLOQ BLOQ BLOQ \ 42809 SL-3. LM-2-1 BLOQ BLOQ BLOQ 't SL-3. LM-2-2 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ ;;j SL-3. LM-2-3 BLOQ BLOQ BLOQ 42810 SL-3. LM-3-1 BLOQ BLOQ BLOQ ,,4 SL-3. LM-3-2 BLOQ BLOQ BLOQ ,t SL-3. LM-3-3 BLOQ BLOQ BLOQ 42811 SL-3. LM-4-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-4-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-4-3 BLOQ BLOQ BLOQ BLOQ BLOQ 42812 SL-3. LM-5-1 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-5-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-5-3 BLOQ BLOQ BLOQ BLOQ BLOQ 42813 SL-3. LM-6-1 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-6-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-6-3 BLOQ BLOQ BLOQ BLOQ BLOQ '' 42814 SL-3. LM-7-1 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. LM-7-2 BLOQ BLOQ BLOQ I 1 SL-3. LM-7-3 BLOQ BLOQ BLOQ 42815 SL-3. SM-1-1 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. SM-1-2 BLOQ BLOQ BLOQ BLOQ BLOQ SL-3. SM-1-3 BLOQ BLOQ BLOQ BLOQ BLOQ Corrected for santole Dien. = Amount (ng/g) * 10 3M Confidential ____________ SL-1, LM_________ PFOa PFS Average (ppb) : 64.3 553.4 Stnd. D.: NA 220 1/3/2003 SL-2, LM PFOS Average (ppb) : 280.8 Stnd. D.: 251 0 0 1 8 0 3 Page 14 o f 21 Report E02-0443 Tenn. River Valley Samples E02-0443 Combined CatFish Data Table UMS# 42777 42778 42779 42780 42781 42782 42783 42784 42785 42786 42789 42790 42791 42792 42793 42794 42795 42796 42797 E frH rflfl l M tE U I t a i l Sem ple Neme Am ount n g/g A m o u n t ng/g A m ount ng/g SL-1; 0-1-1 SL-1; C-1-2 S L-1.C -1-3 SL-1. C-2-1 SL-1. C-2-2 SL-1. 0 2 -3 SL-1. C-3-1 SL-1. 0 3 -2 SL-1. 0 3 -3 SL-1. 0 4 -1 SL-1. C-4-2 SL-1. C-4-3 S L -1 .0 5 -1 SL-1. 0 5 -2 S L -1 .0 5 -3 SL-1. c-e-1 S L -1 .0 6 -2 SL-1. 0 6 -3 S L -2 ;0 1 -1 SL-2; 0 1 -2 S L -2 .0 1 -3 S L -2 .0 2 -1 SL-2. C-2-2 SL-2. C-2-3 S L -2 .0 3 -1 S L -2 .0 3 -2 SL-2. 0 3 -3 S L -2 .0 4 -1 SL-2. 0 4 -2 SL-2. 0 4 -3 SL-2. 0 5 -1 SL-2. 0 5 -2 S L-2 0 5 -3 SL-2. C-6-1 SL-2. C-6-2 S L -2 C-6-3 S L -2 0 7 -1 S L -2 0 7 -2 S L-2 0 7 -3 SL-3; 0 1 -1 SSLL--33.; 0C1-1--23 S L-3. C-2-1 SL-3. C-2-2 SL-3. 0 2 -3 SL-3. 0 3 -1 SL-3. 0 3 -2 S L -3 .0 3 -3 S L -3 .0 4 -1 SL-3. C-4-2 SL-3. C-4-3 SL-3. 0 5 -1 S L -3 .0 5 -2 SL-3. 0 5 -3 SL-3. C-6-1 SL-3. 0 6 -2 SL-3. C-6-3 8L0Q 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 BBLLOOQQ 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 BLOa BLOQ BLOQ BLOQ BBLLOOQQ BLOQ BBLLOOQO BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOO BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ ' BLOQ Am ount n g /g S.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 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BBLLOOQQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ P A (4) ' C orrected fo rS m p l P rep (n g/g ) 58.7 53.5 520 44.5 41.7 39.1 70.5 70.8 73.8 39.3 36.7 36.2 91.0 90.7 87.5 69.8 69.1 69.8 A ve, S tnd Dev, end %CV 54.7 3.49 6.4% 41.6 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% Am ount n g /g 11.2 10.5 10.0 9.6 9.2 6.6 16.1 17.9 19.2 17.1 16.2 16.6 8.1 8.0 7.8 5.9 6.0 5.9 BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOO BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ BLOQ 1.9 1.9 1 .4 1.2 1.1 12 BLOQ BLOQ BLOQ 3.7 3.5 4.0 BLOQ BLOQ BLOQ BLOQ 23 2.3 PFOS (499) C orrected fo r Sm pl Pm p (ng/g) 112.1 104.7 100.3 97.6 91.6 86.1 161.2 179.4 192.4 171.5 181.9 165.8 80.8 80.2 77.5 58.8 59.7 58.7 I A ve, S tnd Dev, end %CV 106 6.00 5.7% 91.B 5.77 6.3% 176 15.67 8.8% 166 4.82 2.9% 79.5 1.74 2.2% 59.1 0.57 1.0% 18.6 17.21 ie.o%18.7 1 4 .0 2.75 11.5 11.73 11.5 0.44 1 22 3.7% 36.9 35.1 40.4 37.45 2.72 7.3% 23.5 23.2 23.32 0.19 0.8% C orrected fo r am ple orno. Am ount (ng/g) * 10 _______________ S L-1.C ____________ ________________ FOSA PFOS A verJ g * (p pb ) : 60.8 1 13.4 S tnd. 0 .: 18.6 45.6 ________ SL-3, C _______________ PFOS A ve n g e (ppb) : 223 Stnd. D.: 10.6 00X804 3M giMwnm--UH aban to y 3M Environmental Laboratory 1/3/2003 PQt 1 9 *2 1 Page 55 of 276 ReportE02-0443 Tend. River V atey Samples ! II* 9 9 99 JM M I999 999999 |3* 2 ai l! <M i Hi gso *%* 9 9 9 9 9 9 9 9 9 9 9 9 fiil?1 13 s w 1! ^ 99 99 9 9 9 9 9 9 9 9 9 9 9 9 lu i<f llib 9 9 ; 9 9 9 9 9 9 9 9 9 m i mm lili l l'iiiilliiif ili|2 Uhi! 11 II % . l .il l 1112 II!! in imlis si!lm'Iilii*s il f ni t illlilil I ! |! !!!h f i f i I ifjl i 11 m ft iii ii i i* 535353:31 i 335 3J3 m i B* i!I i! i i 3M Environm ental Laboratory Page S6 o f 276 SOSTOO 4 1021112 Condensed R iver S edim ents Dets Table 001606 Report E02-0443 $5 Tenn. River VaRey Samplee \i 3M Environmental Laboratory l Page 57 o f 276 E02-0443 R iver Sedim ent! M atrix S pite % Ri Report E02-0443 3M Environmental Laboratory 001S07 Tenn. River VaOey Sam plet s*9 l 1 Page 58 o t 276 E02-0443 Combinad Rivar Water Cata Tabla Report E02-0443 3M Environm ental Laboratory 80STO0 Tann. Rtvar V atey Sam ple* Page SB o f 276 Report E02-0443 Tenn. River Valley Samples E02-0443 Condensed River Water Data Table LIM S 3B025 38026 38033 38034 38037 38038 38028 38030 38036 38040 38042 38025 38028 38033 36034 36037 38038 38028 38030 38036 38040 38042 38025 3802 38033 38034 38037 38038 38028 38030 38038 38040 38042 38025 38026 38033 38034 38037 38038 38028 38030 38036 38040 38042 38025 38028 38033 38034 38037 38038 38028 38030 38036 38040 38042 Sam ple Name SW01 SW01-Dup SW03 SWOS-Oup SW02 SW02-Dup SWOl-Med FSC01-Med SWD3-Med SW02-Med FSC02-Med SW01 SW O l-D up SW03 SWOS-Dup SW02 SW02-DUP SWOl-Med FSC01-Mad SW03-Med SW02-Med FSC02-Mad SWQ1 SWOt-Dup SW03 SW03-DUP SW02 SW02-0UP SWD1-Med FSC01-Med SW03-Mad S V 2-M ed FSC02-Mad SW01 SWOl-Oup SVW03 SWOS-Dup SW02 SW02-DUP SVW1-Mad FSCOI-Med SWD3-Med SW02-Med FSC02-Med SW01 SW01-Dup SW03 SW03-DUP SW02 SW02-DUP SWOl-Med FSC01-Med SWD3*Med SW02-Med FSC02-Med In). V oi. (u L ) 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) E SAr r 0 n * Adjusted fo r > "iV b l.(n g h n L ) 3.0 3.7 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ PFHS (399) 1.50 1.85 Adjuetad fo r Semple Prep. ipg/lm L) 75 93 7.7 8.0 <LOQ 0.3 0.4 0.2 392.6 424.9 404.9 418.9 413.1 PFOA (413) 3.88 3.98 0.13 0.20 0.12 1963 2124 2024 2079 2066 193 199 6.5 9.8 6.2 21.3 22.7 <LOQ <LOQ <LOQ <LOQ 388.4 427.9 398.5 407.0 416.9 FOSA (498) 1Q.66 11.33 1942 2139 19S2 2038 2065 533 566 1.0 1.0 <LOQ <LOQ <LOQ <LOQ 302.1 300.2 324.5 209.2 308.3 PFOS (499) 0.48 0.51 1511 1501 1623 1498 1542 24 28 18.5 20.8 <LOQ <LOQ <LOQ <LOQ 361.8 423.7 365.3 358.0 426.8 9.25 10.40 1809 21' 8 1826 1790 2134 462 520 Average (pg/m L) 84 <LOQ <LOQ 196 6.5 6.0 550 <LOQ <LOQ 25 <LOQ <LOQ 491 <LOQ <LOQ A dueted to r In i. Vol (no/m U For 20 uL injection * A m o u n t/2 For 2 uL injections A m o u n t's Adlueted fo r Semple Prap (paM lL) (A dietad for Inj. Voi. / 20) * 1000 20 it the factor o f original concentration 1000 Is the conversion from ng to pg. o o is o s 3M C onfidante 1/3/2003 Psg 20 a l 21 3M Environmental Laboratory Page 60 of 276 Report E02-0443 Tenn. River Valley Samples E02-0443 Tenn. River Valley Samples Sum m ary 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 Water, Sample Location 1 River Water, Sample Location 2 RiverLWo caatetiro, nS3ample River Sediments, Sample Location 1 River Sediments, Sample Location 2 River Sediments, Sample Location 3 PFBS (ng/g) <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <L0Q PFBS (pg /m L ) 84 <LOQ <LOQ PFBS (pg/g) 576.9 436.9 452.0 Location Averages PFHS (ng/g) PFOA (ng/g) FOSA (ng/g) <L0Q <LOQ 60.9 <L0Q <LOQ <OQ <L0Q <LOQ <LOQ <L0Q 64.3 <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ PFHS (pg /m L ) 196 <LOQ PFOA (pg /m L ) 550 <LOQ FOSA (pg/m L) 25 8 <LOQ <LOQ 7 PFHS (pg/g) 130.5 <LOQ PFO A (pg /g) 732.4 <LOQ FOSA (pg/g) 1439.0 <LOQ <LOQ 141.4 <LOQ 130.5 68.0 The Fish Tissue results are calculated by taking the average of the averages. Please refer to Combined Large Mouth and Catfish Data Tables for averages of samples. PFOS (ng/g) 113 <LOQ 22.3 553 281 <LOQ <LOQ PFOS (pg /m L ) 491 <LOQ <LOQ PFOS (pg/g) 3132.3 457.3 416.2 3M Confidential 3M Environmental Laboratory 1/3/2003 001810 Page 21 of 21 Page 61 of 276 Report E02-0443 3MPm/irnnmpnlalIahAralnrv Solvent Curve: 02003-50 SWeBqMuHeVnIcVe*:. Dfc020626Extracted -Am* /' CurveCne? DUDE0013 1 OUDE0014 2.5 DUDE001S 5 OUDE0010 10 OUDE0017 25 E E H ilD 50 100 DUDE0020 250 DUDE0021 500 DUDE0022 DUDE0023 1 1 1 1 D020626Extracted CCV Calculation 41605 89393 162263 313633 739433 1369316 2407273 5416416 6696793 PFBS _ w m 1 fT?r?`V. 't1.'jr r -r/' 1.000 . _ 41605: >0.04 j- . 1 2.500 : .. . 89393 .. .1.61 m s 1 5.000 162283' 4.65 -6.9 ` -0.T.. 0.0 V 0.0'V: r.. 10.000 : 313833 1 25.000 739433 1 . 50.000 1369316 10.59: 5.9 . 0.0 27.51. '10.0- - .0.0- ;; 53.25 6.5 * 0.0 1 100.000 2487273 101.29' 1.3 0.0 . i 250.000. 5416416- . 246.66 -1.3 10:0 1 1 500:000 0.000 8896793 0 50132 -1.65 HmHSim| 0.0 ,, 0.0 * t 0.000 .. . 0 1! 0 1.65 H H 0.0 kggRSBai j 0.00 jTfromxhartiaa I.62E+01 b-i.i.ii 25774.0409 42668.7254 .: ''neV-!;-. DUOEO65 DUDE0078 DUDE0061 rMparne.r cone,Jtencuva ^CCVlnifci 2463356 .101.11 100 10196. * 2451622 99.70 100 . 100% - 2445634 99.44 1.65 100 . 99% ,o 1.65 0 1.65 0 -1.65 0 1.65 0 1.65 0 1.65 0 IMConMntl 12/12/2002 flirtCcW dOrti1 DO n P a g tlo fd , Tenn. River Valley Samples 001811 Report E02-0443 D020626Extracted CCV Calculation PFHS -2.216*01 31284.4258 487S4.7S31 od dd o d o d oo' Oo oo o d Oo dd od i|hg so i7 i r>. d s CM d y d 13 i*? sy foc8R N 5o 8 s<Ns 8 a Ij BN o> rt 1 2 i01 d b io 1 | oi uj o 8 1 8 1 80 SN 1 id d v- o I 11 ii 3 s Na %0 5 ! I i iS o - m d o8s88 f- s|J n m <0 i-:n i I' I 1 I 3Ol i iiQ S '3 3M Environm ental Laboratory Solvent Curve 02003-50 IDUDE0019I (OUOEOQ23I 001812 Tann. River Valley Samples I N |. 103% | 1 %0l i g b o b o o o' o ff l i g8 8 n vi "I 1 3 i 8 o 2 'S it'j II 331 * aas8 s lOI 38 louoEooaij Pan fi* n f 57fi Report E02-0443 Tenn. River Valley Sam ple* n* ! CTSTOrt IOUDE0055J| 1459295-11- 109.37 I ! 111.66 | | 1477410 | P1 O p b o p 6 O 1881 - H & wNN N N 4 7 fji <vi rji Cs fl m S 1 mf*8i i o 3 Report E02-0443 o n 5.. o d oo o o o d d oo' od t- a ---------- 3M Environm ental Laboratory 3a 3 8 40 0 Q IIU l !',5'n i SolventCurve: 02003-50 1OUOE00141 IDUDE0015I IDUDE0017I 10UDE0018I IDUDE0020I IDUDE00211 IDUDE00221 8 - ciMin o 8 8 I; *4 I UVSIZ I iI | i F i I 2665321 | I 6144956 | 1 11083740 | POOO'OOS 1 D020626Extracted CCV Calculation FOSA s cgfsa I o sI 3 1'2.500 :|| I 5.000 | I 10.000 :| i 25.000 I ,50.000.1 \ 100.000 I I250.000 I ii $i I 5> tv s -71306 I 0.000 | 0.000 I f OO m wf i ? 88 $ 1 S' d R0 4 5). 8* 8 j i'101.39^:1 2 <0 9d dd od odmi3g so 9701.53073 Tenn. River Valley Samples f 001814 Report E02-0443 "I'tiLfll". s 3 -1.10E+01 25197,6029 ;%? 316501.997 Tenn. River Valley Samples rt 001815 4 1 * 1 S 8 o o o O o <s o i fc8 8 8 S CD o3 n r<4 r V) & r4 H s (n Cr to oi <4 <4 cJ 1 300424 1 # !1 a g m o jj i S''l 1 Q Report E02-0443 Attachment C: Sample Chromatograms Tenn. River Valley Samples 3M Environmental Laboratory Q01816 Paae fi7 nf ?7fi Report E02-0443 Tenn. River Valley Samples Data File: DUDE0056.D Report Date: 27-Aug-2002 13:27 " Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0056.D Lab Smp Id SL-1. LM-1-3 Inj Date 26- JUN-2002 23:16 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method Meth Date \27\-EtsAtuagr-g2e0t0\2ta1r3g:e2t2\cdhuedme\jdru.diejr.Qiu\aDn0t20T6y2p6eE:xtErSaTcDted.b\D020626extra Cal Date 26-JUN-2002 22:00 Cal File: DUDE0049.D Als bottle 43 Dil Factor 1 .0 0 00 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds Il PPBS(299) 20PFH3 (399) 21PPO(413) 22POSA(499) 22POS(499) MAASQUANT SZ8 RT EXPRT OLTRTRESPONSEON(Cn-CgOO/NmLCULEM)NNTRATI(OnPNgINS/mALL) 442223344439191999999939939999999 333433344443............797913049154027570947700S33539919451 333333444334............733779911377999999977199211220044122*----000000000000............013320341000010921430190735711217340 190911135159214594439300532979378475299809254294757194 95599901115905.39345030519371.83973991..70......2775334547..530219399955313949495905 0111.19998855588418233505500.500803744999 Exact C o r/c f Orig - n ii-s\ Initiai Dais 001S17 Report E02-0443 Tenn. River Valley Samples Data Filat SSEtstar(ttStarttSchaSduda,Jr.iSD02062fiExtractad.bSDUDE0056.D PC 2 Exact Crpy nf Original ( i ll( /.-3//n//'>-- Initial Dato o l lv i Report E02-0443 Tenn. River Valley Samples Oata F ila i SSEt i t i r fatSlircatSchmSdudajr. 1\D02026Exfcrctd. bSDUDE0056,D 21 PFOft <413) Pt 3 23 PFOS <499) Eact Copy o Origino! f - i :-r initial Data 0 0 1 8 4 .9 Report E02-0443 Tenn. River Valley Samples Data Pile: DUDE0058.D Report Date: 27-Aug-2002 13:27 " Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chera\dudejr.i\D020626Extracted.b\DUDE0058.D Lab Snip Id Inj Date SL-1. LM-2-2 26- JUN-2002 23:38 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 II Misc Info Comment Method Meth Date Cal Date \2\7E-tstAaurgg-e2t0\0t2arg1e3t:2\2chedmu\ddeujdre.jir.i\QDu0a2n0t62T6yEpex:traEcStTeDd.b\D020626extra 26-JUN-2002 22:00 Cal File: DUDE0049.D Als bottle 45 Dil Factor 1 .0 0 00 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 4 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Coapoundo 1 PFBJ law) 30 PPHa (3) 21 PPOA (413) 32 22 PpOroSAs (454) (499) QUHANATSS810 22223434499991919999339*9 449P9* ST BXP RT DLT RT RESPONSI ON(Cn-COgO/NLCULEM)NNTRATI(OnPNgIN/SmALL) 333333443.........387173825024948024C37028895 333333343.........333379977888899499111120202 ----000000000.........11020302029714403033115770 44..157045 44..117744 00..040341 331011441S22132745424045419124397228558563C7372084348 555085815553.5.0940333739659......<3555855.2947889456454814879 1C(l1.400.03( 01.6558855.951355055660844934 1<618.40 Exact Copy of Orignal d rU I i initial Data I P nw irnnm pnfal I ahrtratnrv * U 01 20 D e n a *74 T 7C Report E02-0443 Tenn. River Valley Samples Data Fil: SSEtsUrc*tSUrtt\eb\dud*jr. i\D020626Extrcti.bSDUBEOOSB.D Pt 2 1 20 PFH8 <399) I - Cm /rnnm A ntal I horatorv Exact Copy r.' Origin,i! -C W Initiai oate 001821 Pan 79 of 276 Report E02-0443 Tenn. River Valley Samples Bat F it: SSEtstai*e*t\targatSchM>Sdudjr.iSB0226Extract*d.bM>UDE00S8.D 21 PFOA <413) 22 FOSA <498) 23 PFOS <499) Exact Copy of Origina! 1 3 / h i/ X. Initta) Date 001822 Report E02-0443 Tenn. River Valley Samples Data File: DUDE0063.D Report Date: 27-Aug-2002 13:27 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0063.D Lab Smp Id SL-1. LM-3-2 Inj Date 27-JUN-2002 00:33 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method Meth Date \27\-EAtusgt-a2r0g0e2t\1t3a:r2g2etd\ucdheejmr\.diudejrQ.uia\ntD02T0yp6e2:SExEtSrTDacted.b\D020626extra Cal Date 26-JUN-2002 22:00 Cal File: DUDE0049.D Als bottle 49 Dil Factor 1 .0 0 00 0 Integrator Falcon Compound Sublist: all.stob Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Congpound Variable Compound* IBPPM{39) 30PPHS(399) 31PPQA<413) 33POSA(491) 23proa <499) QIAMTSXG MASS RT EXPRT DITRTRESPONSEON(nC-CgOO/NmLCULEM)NNTRAT(IOnPNgINS/mALL) 229999 2233999999 444441991933999 3333334333444.............3B7717945159BC97137470951BB4355453732 3333333334444.............3373397711977BB9389997759(2222411043101-00000000000O0.............122303410004o304404383000o757902141767o 39262113465123145(337354509434717734673773553368095602870 48555588118300550359605.79.3397138937..87....0..2.5637476317..43730419467S1371C079875169 4811968805555888.928305355510.8800837944409 Exact Copy of Origina! J j y i . L-xJ/lQ T- Initial Date 01 23 Report E02-0443 Tenn. River Valley Samples Data F il#: S\EttarsttStarstt\chtaSfcJdtjr.:M020i26Extractl.b\Din)E0063.J Pagt 2 Exact Copy t;.f Original 001824 Report E02-0443 Tenn. River Valley Samples Data Fila; SSEt*trjtStaretSch*i.Sdudajr.i\T0202Extraetad.bSDUDE0063.D 21 PFOA (413) paCa 3 OECt Copy of Origin's! Initial 001825 Report E02-0443 Tenn. River Valley Samples Data File: DUDE0068.D Report Date: 27-Aug-2002 13:27 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020626Extracted.b\DUDE0068.D Lab Smp Id: SL-1. LM-4-2 Inj Date : 27-JUN-2002 01:28 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method Meth Date : : \27\-EAtusgt-a2r0g0e2t\1t3a:r2g2etd\ucdheejmr\.diudejQru.ain\tD0T2y0p6e2:6EExStTrDacted.b\D020626extra Cal Date : 26-JUN-2002 22:00 Cal File: DUDE0049.D Al s bottle: 52 Dil Factor: 1 .0 0 0 0 0 Integrator: Falcon Compound Sublist:all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1PFBSUt) 20P7HSUt) 222121PPtvOPoOSaAA(((4449193l))) QUNAANSTSSIO RT BXPRT DLTRTRBSPOKSBON<O-nCOgO/NmLCULSM>NNTRATX(OnFHIgNS/AaLli) 223334444241999999999939999999999 33333334434..........7.353177914(C5O5929997*7433299974S33443333344...........397137731179999997977(22101224144----00000000000...........241300003403390000430039975702107 34114951543971521115019535054(6352575071114745092959 50507105991...55500.455459939993.132340...0.776555379..3924952371(56459459195 0006711...569659965.51433511995.93737400040 Exact Copy c i Origina! biitial Oats 001826 Report E02-0443 Tenn. River Valley Samples Stata Fil*: VsEtstargetStar-f*tSch*nSdud*jr.i\D020624Extr*ct*d,bSDUBE4468,9 pe* 2 18 PFS8 <299) Pnuirnnmantal I aKrtPotnni Efct Ccpj n' Z a h l ., i v / t c l t r .L- JnitlaJ osta 001827 Report E02-0443 Tenn. River Valley Samples Data File: SSEtstartetStartetSchenSdudejr,i\D02062{Extraete<l.bSSUDE0068.D 21 PFOA <413) Pit 3 22 FOSA <498) 23 PFOS < 4 > iIaI ikrtenli Exact Copy of Origina! 1-2-J/n /ni Oats 001828 n ... 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 Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020S28.b\DUDE0058.D Lab Smp Id: SL-2. LM-2-1 Inj Date : 29-JUN-2002 02:15 Operator : mla Inst ID: dudej r .i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 13:01dudejr.i Quant Type: ESTD Cal Date : 29-JN-2002 00:48 Cal File: DDDE0050.D Als bottle: 28 Dii Factor: 1 .0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Conpounds It FFB5 (299) 20 PFHS (399) 21 PFOA (413) pros22 POSA (499) 23 (499) QUANT Sir, MASS 299 299 299 399 399 413 490 499 499 COHCENTRAT-CNS ON-COLUMN PINAL RT BXP RT DLT RT RBSPOKSS (ng/raL) tng/mL) 3.390 3.103 3.757 3.005 3.545 4.004 4.776 4.101 4.605 3.308 3.300 3.380 3.798 3.790 3.997 4.769 4.174 4.174 0.000 -0.205 0.369 0.007 -0.2S3 0.007 0.007 0.007 0.431 15144 2946 2208 10047 540 25432 65904 1348329 20726 569.524 569.996 570.025 786.229 786.477 815.277 1805.85 2.56372 1659.69 570 570 570 786 786 8 1 5 (M) 1880 2.56 1660 QC Flag Legend M - Compound response manually integrated. Exact C o p y of Original 001829 Report E02-0443 D ata F ila : \\E ts ta rs a t\ta rc a tS c h a n S d u d a jr,i\D -)Z 0 6 2 8 .b S D U D E 0 9 S 8 .D Tenn. River Valley Samples Paca Z Exact Copy of Origina! x a a l_ j.3. f / t r t. Initia] Date 0011,30 Report E02-0443 Data FU: SSEt*t*re*tStarttSch*Sdud*Jr. tSD020628. b\DUBE00S8. D 21 PFOft (413) Tenn. River Valley Samples Pat 3 22 FOSA (498) 23 PFOS (499) Exact Copy of O r#;; teiaJ Osts 001831 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0064.D Page 1 Report Date: 09-Dec-2002 13:07 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0064.D Lab Smp Id: SL-2. LM-3-2 Inj Date : 29-JUN-2002 03:21 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info : Comment Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date : 29-JUN-2002 00:4B Cal File: DUDE0050.D Als bottle: 33 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound IB PPBS (a s s ) 20 PFHS (399) 21 PPOA (413) 23 POSA (498) 23 PFOS (499) Quurr sic MASS 299 299 299 399 413 499 499 499 CONCENTRATIONS OH-COLKN FINAL. RT EXP RT DLT RT RESPONSE Ing/oiL) (ng/mL) 3.401 3.210 3.771 3.818 4.017 4.789 4.194 4.825 3.388 3.388 3.388 3.798 3.997 4.769 4.174 4.174 0.013 -0.178 0.383 0.020 0.020 0.020 0.020 0.451 22037 3476 3793 17063 38939 98985 1627015 1774 569.257 569.976 569.964 0.08850 814.559 0.72476 11.7650 1660.28 569 570 570 0.0885(H) 814 (M) 0.725 11.8 1660 QC Flag Legend M - Compound response manually integrated. initial >03Cat I0 1 L 3 Z Report E02-0443 D a t F ila s V t * t * r g t \ t a r { t \ e h * \ d u d Jr . i\L ')2 0 6 2 8 .bMHIDEOOW. D Tenn. River Valley Samples P * l* 2 P m /ir^ n m a n tflil I ahrtref f ci Copyof Original initial Dqq C 1633 Report E02-0443 Data Filai SSEttarial\tartt'*cha\dudajr,iM20628,bSDUDE0064.B 21 PFOfl <413) Tenn. River Valley Samples Paca 3 22 FOSA <498) Exact Copy of Orloina; initiai Date C u io 3 4 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0070.D Page 1 Report Date: 09-Dec-2002 13:07 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020628 .b\DTJDE0070 .D Lab Smp Id: SL-2. LM-4-3 Inj Date : 29-JUN-2002 04:26 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr .i\D020628.b\D020628.m Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date : 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle: 37 Dil Factor: 1 .0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds IS PFBS (299) 20 PFHS (399) 21 PPOA (413) 22 POSA (498) 22 P?OS (499) QUANT SIG MASS 299 299 299 399 413 491 499 499 499 CONCENTRATIONS OK>COLUMN PINAL RT EXP RT DLT RT RESPONSE (ng/mL) ng/mL) 3.388 3.183 3.757 3.805 4.003 4.774 4.174 3.805 4.605 3.388 3.388 3.388 3.798 3.997 4.769 4.174 4.174 4.174 0.000 -0.205 0.369 0.007 0.006 0.007 0.000 -0.369 0.431 13695 1232 1592 10665 23745 120542 2949014 2773 32944* 569.580 570.062 570.049 786.213 115.366 1.45583 56.9432 1660.25 1659.31 570 570 570 7 8 6 (M) *15 <M) 1.46 56.9 1660 1660 QC Flag Legend M - Compound response manually integrated. Staci Copy of Originai A* C iniiia) Date aoxss Report E 02-0443 Data F ile t \\E t t ta r je t \ tarjetSchenSdudj r . iSD020628. bM)UIIE007').D Tenn. River Valley Samples Pate 2 18 PFBS <299) Exact Copy of Origina X2L_ <3Ji.qI q initiai Oats 001836 Report E02-0443 Data F ila ; NSEtstarttStarfetSeh*iSdu<l*jr.lSIW20628,bSllUlJE0070.D 21 PFOA (413) Tenn. River Valley Samples P*S* 3 22 POSA (4 9 6 ) 23 PFOS (499) Exact Copy 'T !i> -C Y L . Initiai Onte 001837 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudej r .i\D02062B.b\DUDE0076.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\DO2O620 .b\DUDE0076 .D Lab Smp Id SL-3. LM-1-3 Inj Date 29-JN-2002 05:32 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020628.b\D020628 .m Meth Date 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle 42 Dil Factor 1 .0 0 00 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable pound 18 pros (299) 20 FFHS (399) 21 PFOA (413) 22 POSA (9) 23 PFOS (499) QUANT Sia NASS 299 299 299 399 399 413 498 499 499 CONCENTRATIONS OM-COLUMN RT EXP RT DLT RT RESPONSE (ng/L) FINAL (ng/mL) 3.388 3.189 3.764 3.805 3.559 3.996 4.899 4.174 4.611 3.388 3.388 3.388 3.798 3.798 3.997 4.769 4.174 4.174 0.000 -0.199 0.376 0.007 -0.239 -0.001 0.130 0.000 0.437 17998 3724 1636 16875 3229 60835 78316 716542 12921 569.414 569.966 570.039 0.08359 786.407 0.95299 0.02433 1637.71 1659.94 569 570 570 0.0836 786 0.953(H) 0.0243(H) 1640 1660 QC Flag Legend M - Compound response manually integrated. Exact Copy of Origina1 Data 001838 Report E02-0443 le t* F ile* SSEt*t*Pe*tSt*rtt\ch*i%\dud*jr.lS228.bSBUDE007i.D Tenn. River Valley Samples Pa* 2 ExactCopyo: Originai initial Ls/ib Jj j . Cou- 01U 39 Report E02-0443 D a ti F l i t : SSEtstarctStar(*tSehn\dud*Jr. 1SD020628.bSDUDE0076D 21 PFOA (413> Tenn. River Valley Samples Pag 3 22 FOSA (498> ExactCopvr ' Onrn nL_ t /to initial ote 001840 Report E02-0443 Tenn. River Valley Samples Data File: \\ Et st ar get\targe~\chem\dudej r .i \ D 0 20 62 8.b \ D D E 0 0 8 9 .D Page 1 Report Date: 09-Dec-2002 13:08 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0089.D Lab Smp Id SL-3. LM-4-3 Inj Date 29-JUN-2002 07:55 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date 09-Dec-200213:01 dudejr.i Quant Type: ESTD Cal Date 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle 52 Dil Factor 1 .0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 18 PFBS (as9) 20 PFHS (3991 21 PPOA (4X3) 22 FOSA (498) 23 PFOS (4991 QUANT Sin HASS 299 299 299 399 399 413 498 499 499 CONCENTRATIONS ON-COLUMN FINAL FT EXP FT DLT RT RESPONSE ing/mL) ing/mL) 3.395 3.190 3.757 3.805 3.552 4.003 4.769 4.174 4.605 3.368 3.388 3.388 3.798 3.798 3.997 4.769 4.174 4.174 0.007 '0.198 0.369 0.007 -0.246 0.006 0.000 0.000 0.431 12936 3732 1991 7393 2451 24746 64726 1029061 18761 569.610 569.966 570.033 786.298 786.427 115.313 . 1885.89 1627.64 1659.75 570 570 570 786 786 8L5 (M) 1880 1630 1660 QC F la g L e g e n d M - Compound response manually integrated. Exact Copy of Ordina? U U lo /o x - rnitiai Oat 001S41 Report E02-0443 Tenn. River Valley Samples 18 PFBS <299> 20 PFHS (399> Exact Copy of Origina! 001^42 Report E02-0443 Dt Filet S\Et*t*rttSUrt*tSehS*KlJr.iM20628.bM)UDE0089.D 21 PFOA (4 13) Tenn. River Valley Samples pn 3 2 3 PFOS <499> Copy of Original '-n,lia{ Date O I8 4 3 Report E02-0443 Tenn. River Valley Samples Data File: \ \ E t st ar ge t\ tar ge t\ ch em \d ude jr.i\D020628.b\DDE0102.D Page 1 Report Date: 09-Dec-202 13:08 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020628,b\DUDE0102.D Lab Smp Id: SL-3. LM-7-2 Inj Date : 29-JUN-2002 10:18 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date : 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle: 62 Dil Factor: 1 .0 0 0 0 0 Integrator : Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 18 P7BS 1299) 20 PPHS (399) 21 PFOA (413) 22 POSA (499) 23 PPOS (499) q o a k t sia NASS 299 299 299 399 413 498 498 499 499 CONCENTRATIONS QM-corow PINAL RT EXP RT DLT RT RESPONSE (ng/mM [ng/aL) 3.388 3.176 3.757 3.799 3.997 4.769 4.441 4.175 4.598 3.388 3.3BB 3.388 3.798 3.997 4.769 4.769 4.174 4.174 0.000 -0.212 0.369 0.001 0.000 0.000 -0.328 0.001 0.424 24706 1376 1023 9487 62864 23637 779 906705 29289 569.154 570.057 570.071 786.244 1.06124 1887.28 1888.05 1631.60 1659.43 569 570 570 786 <H) 1.06 18 90 1890 1630 1660 QC Flag Legend M - Compound response manually integrated. SraciCopyc.` Oricirur- Me 001S44 Report E02-0443 Data Fila: S\Etstai^atStargatScheiXdudaJr.i\I20i2a.b\Din)E0102.D Tenn. River Valley Samples Paga 2 Exact Copy of Original CJn ( / p / z o / Cr*. Initial Data 001845 Report E02-0443 Sat* F ilt VsEtit*rt*tSt*rs*tSehMiSdud*Jr.lMK20628.bM)USE0102,D 21 PFQft <413) Tenn. River Valley Samples 22 FOSA <498) 23 PFOS <499) 3M Environmental Laboratory Exact Copy of Origin'-.: C iv it a d l l< n - initial O aio 001846 Page 97 of 276 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\tar ge t\ ch em \d ude jr.i\D020628.b\DUDE0104.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0104.D Lab Inj Smp Id: Date : SL-3. SM-1-1 29-JUN-2002 10:40 Operator : mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date : 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle: 6 5 Dil Factor: 1 .0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 18 PPBS (299) 20 PFHS (399) 21 PFOA (4X3) 22 F0SA (498) 23 FPOS (499) QUANT SIG MASS 299 299 299 399 399 399 13 498 499 499 CONCENTRATIONS ON-COLUMN RT EXP RT DUT RT RESPONSE (ng/mL) FINAL tng/mL) 3.368 3.190 3.757 3.812 3.566 4.174 3.996 4.769 4.174 4 .60S 3.388 3.388 3.388 3.798 3.798 3.798 3.997 4.769 :i74 4.194 0.000 -*0.198 0.369 0.014 -0.232 0.376 -0.001 0.000 0.000 0.411 10955 2138 1256 11252 5688 975 55673 41082 429027 15*11 569.686 510.027 570.062 786.197 786.343 786.466 0.67774 1886.69 1646.86 1659.05 570 570 570 786 786 786 0.678(H) 1890(H) 1650 1660 QC Flag Legend M - Compound response manually integrated. Exact Copy c f Original Initlal Data P ew rcN nm A nlal I 01 47 n...An.fM*f/ Report E02-0443 Data Fila: S\Et*tarsatStargatScha\dudajp.iSD020628.b\DUDE0104.D Tenn. River Valley Samples Paje 2 18 PFBS (299> Exact Copy o f Origina L!rs*iiia(! r i /O^a/tea 0Qlt48 Report E02-0443 D ata F i 1*5 S S E tsta r^vtS tarca tS chm S du daJr, iSD,>20428.bSDUDE0104.D 21 PFOA <413) Tenn. River Valley Samples 23 PFOS <499) E 'c sc i C op y o f Original .Chn? .. *J1joJj p _. initiai Ogin 001849 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0105.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\targst\chem\dudejr.i\D020628.b\DUDE0105.D Lab Smp Id: SL-3. SM-1-2 Inj Date : 29-JUN-2002 10:51 Operator mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment Method : \\Etstarget\target\chem\dudejr.i\D020628.b\D020628.m Meth Date : 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle: 66 Dil Factor: 1 .0 0 00 0 Integrator : Falcon Compound Sublist:all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds U18 PFBS 99) 20 PFHS (399) 21 PFOA (413) 22 POSA (498) 23 pros (499) QUANT Sia HASS -- 299 299 299 399 399 399 413 498 499 49 RT - 3.388 3.182 3.764 3.82S 3.S52 4.194 3.996 4.769 4.174 4.408 BXP RT 3.388 3.388 3.388 3.798 3.798 3.798 3.997 4.769 4.174 4 .1 7 4 DLT RT 0.000 >0.206 0.376 0.027 -0.246 0.396 -0 .0 0 1 0.000 0 .0 0 0 O.4 3 1 RESPONSB 11225 1896 1US 12780 6122 930 52802 40143 469574 1424 CONCENTRATIONS ON-COLUMN PINAL (ng/mb) <ng/iaL) 569.676 570.037 570.067 786.158 786.331 786.467 0.52474 1886.72 164S.S8 1649.8 570 570 570 786 786 786 0.525(H) 1890(H) 1640 1660 QC Flag Legend M - Compound response manually integrated. Exact Copy origin al C U iL - U L i P - inSial Data i>18S0 Report E02-0443 Data Fi la: s\Et*tar|tStrs*t\eh*iVdud*jr.iMW20628.bSDUlJeoiO5.D Tenn. River Valley Samples Pit* 2 18 PFBS <299) xt Cupv of Original ritla l Data 001851 Report E02-0443 Hat F ila : SSEtstars*tStar(*tSe>wSdud*Jp.lSDSe28.bS0UDE010S.I) 21 PFOA <413) Tenn. River Valley Samples P ,. 3 2 3 PFOS <499> Exact Copy of Origins} U ia l-- initial Date 001852 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr .i\D020628.b\DUDE0108.D Page 1 Report Date: 09-Dec-2002 13:08 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020628.b\DUDE0108.D Lab Smp Id SL-3. SM-1-3 Inj Date 29-JUN-2002 11:25 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\Etstarget\target\chem\dudejr.i\D020S28,b\D020628.m Meth Date 09-Dec-2002 13:01 dudejr.i Quant Type: ESTD Cal Date 29-JUN-2002 00:48 Cal File: DUDE0050.D Als bottle 67 Dil Factor 1 .0 0 00 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1 FFBS <399) 30 PFHS (399) 21 PFOA (413) 22 FOSA (498) 23 PFOS (499) QUANT SIG MASS 299 299 299 399 413 499 499 499 CONCENTRATIONS ON-COLUMN FINAL AT EXP AT DLT RT RESPONSE (ng/raL) ng/mL) 3.368 3.183 3.764 3.798 3.996 4.762 4.174 4 .598 3.389 3.388 3.388 3.798 3.997 4.769 4.174 4.174 0.000 -0.205 0.376 0.000 -0.001 -0.007 0.000 0.424 16091 2727 1588 13195 S4265 44388 458983 15684 569.488 570.005 570.049 786.147 0.60270 1886.57 1645.91 1659.85 569 570 570 786 <M) 0.603 (M) 1890 (Ml 1640 1660 QC Flag Legend M - Compound response manually integrated. Exact Copy of Origina! L iti/ ._ 2 //o /o ^ Initial Date IL4 M Cl mi 01ZS3 Report E02-0443 Bt F ile: SSEtstrtetSUrt*tScheeSdudejp.lSl20t28.bSBUXC0108.D Tenn. River Valley Samples Pat* 2 E x sc l C opy of Odoifui L 2//o /c. initiai o ift" 001854 Report E02-0443 Dt* Filet SSEt*tr*tStrttSch*>S<ludejr.lM20628.bM)UllE0108.D 21 PFOft <413) Tenn. River Valley Samples P ift 3 23 PFOS <499) Exact Copy or Original f - i +j( n h o f x initia] Dato ^ O lS S S Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D0206~29 ,b\DUDE089 .D Page l Report Date: 27-Aug-2Q02 10:06 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0089.D Lab Smp Id SL-1. WB-1 Inj Date 01-JUL-2002 04:25 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr .i\D020629,b\D020629 .m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date 30-JUN-2002 22 :4o Cal File: DUDE0058.D Als bottle 47 Dil Factor 1 .0 0 0 0 0 Integrator Falcon Confound Sublist:all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable .-i 1 Compound is PPBS (2 9 1 ) 1 20 PPKS <299) 21 PPOA (4 1 2 ) i 22 POSA (9) 23 ppoa (499) ,,,,*i QUANT SIG MASS 209 299 299 399 413 490 499 499 CONCENTRATIONS ON-COLUMN PINAL RT KXP RT DLT RT RESPONSE (ng/nL) (ng/L) 3.313 2.944 3.1 3.790 4.004 4.770 4.100 4.005 3.3B1 3.301 3.301 3.792 3.990 4.750 4.1(0 4.100 -0.000 -0.437 -0.210 0.000 0.014 0.020 0.020 0.437 23S77 470 2901 0170 10932 7049 90922 22025 1223.22 1224.54 1224.39 0.10435 019.144 2744.00 1274.91 1277.09 1220 1220 1220 0.104 19 2740 1270 1200 Exact Co# oJ'ting fmOiia!L . o*t>:\fo?-- 001856 Report E02-0443 Data F ila: S\EtstarcatSUr(atSchan\dudajr.iSD020629.bSDUK0089.D Tenn. River Valley Samples P aja 2 3.9-; 3.6^ 3*3^ 3. 0: 2.?-: Ion 299.00 frvprS. v 1.*8--: " 1.8-, 1 n2 k ^0. 9: 7 1 ./LIJ\ *- V^. _ -- 3.00 3.20 3.40 3.60 3 .BO ________________ Hin_________________ 20 PFHS (399) tact Ccpy j ; 'j.lcii:.' tZ /Jc/a i- feiitial Oa& 001S57 Report E02-0443 BU F ile t SStitri*tStrc*tSchSdudJr. I\D020629.b\DUDE0089.D 21 PFQA <413> Tenn. River Valley Samples 22 FOSA <496> Beaci Copy or Origina! C'l'iijt2ia.lL . li JD/aoto/qi-- U01bS8 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0127.D Page l Report Date: 27-Aug-2002 10:07 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0l27 .D Leib Smp Id SL-2. WB-1 Inj Date 01-JUL-2002 11:23 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 03 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle 76 Dil Factor 1 .0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound* 1 PFBS(a> ao PPH(3*1) PPOAa i (413) POSAaa (4 **) PPOS(4*1)aa QUMANASTSSIO RT SXPRT DLTRTRUFONSBON(nC-COgOM/tLCtULRMN)TNRATX(OnPNIgNa/A*LL) 399 3.319 3.391 -0 .0 4 3 31973 1 3 3 3 .3 2 1220 399 3.17 3.391 -0 .3 0 5 3794 1 2 2 4 .3 5 1330 399 3.791 3.79a -0 .0 0 1 3414 0.03479 0 .0 3 4 9 399 3.913 3.793 0.190 1931 7 9 7 .1 4 9 797 413 3.99 3 .9 9 0 0.004 13991 9 1 9 .0 3 5 919 49S 4.774 4 .7 5 4 o.oao 3433 2 7 4 4 .1 9 2740 499 4.119 4 .1 4 9 0.030 94974 1 2 7 5 .3 0 1290 499 4.599 4 .1 4 9 0.430 12403 1 3 7 7 .4 0 1240 Cjn rci Cop]. '<' Original t p / f / .z-- iii a j Oafs 001.8S9 Report E02-0443 Data F lla : \\E t*ta rta t\ta r* tS c h a *S d u d jr.iS D 0 2 0 6 2 9 .b \D llD E 0 1 2 7 .D Tenn. River Valley Samples Pata 2 20 PFHS (3 99) :T,Vi ' 2 / / 'j /o? qo l $60 Report E02-0443 Data F llat SSEtstarcat\tarc*tSchanSdudaJr.l\D0206294bM)UDE0127.D 21 PFOA <413) Tenn. River Valley Samples 22 FOSA <498) 23 PFOS <499) "V jt ^ -v, 1Oi'.'giii: S-klOC. -il/to/i- ilaJ D f 001861 Report E02-0443 Tenn. River Valley Samples Data File: DUDE0089.D Report Date: 27-Aug-2002 11:06 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file Lab Smp Id \S\LE-t3s. taWrBg-e1t\target\chem\dudejr.i\D020702 (D20702).b\DUDE0089.D Inj Date 03-JUL-2002 07:02 Operator mla Inst ID: dudejr.i Sng? Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020702(D20702),b\D020702.m Meth Date 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD Cal Date 03-JUL-2002 01:21 Cal File: DUDE0058.D Als bottle 72 Dil Factor 1 .0 0 00 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Confound Variable Compound ia PPBS (3> 30 W H S (3) 21 PPOA (13 aa FOSA (43*) 23 PPO* (433) QUANT SIS MASS 290 299 299 399 399 413 49* 499 499 C0HCBMTIUXI3NS ON-COLONS FINAL RT BXP RT DLT RT RBSP0MS8 (ng/nL) (rjg/mL) 3.324 3.113 3.777 3.025 3.545 4.010 4.003 4.194 4.591 3.307 3.307 3.307 3.791 3.791 3.909 4.740 4.147 4.147 -0.041 -0.204 0.390 0.034 -0.244 0.021 0.055 0.027 0.414 25327 3225 490 7077 937 14443 5535 02445 22937 1219.50 1220.47 1220.50 0.25045 0.12420 795.103 2054.35 1323.02 1324.24 1230 1220 1220 0.25ft 0.124 7.8(11) 2150(H) 1320 1220 QC Flag Legend M - Compound response manually integrated. Exact Copy of Grig:r..v P in t Enttiai Dato 001862 Report E02-0443 Tenn. River Valley Samples ta t* F ilas SSEt*tart*tStarc*tSohSdud*jr. 1SD020702<S20702>.bSIHJDE0089.D PC 2 20 PFHS (399> Exact Copy of Criginal Initiai ;3te 001S63 Report E02-0443 Tenn. River Valley Samples Data F ila: SSEtatvt*tStars*tSeh*nSdud*Jr.iMK>20702(020702>.bSDU])EO89.D 21 PFOA <413> 22 FOSA <490) 23 PFOS <499) cicict Cupy of Origmai % < - . L 2 /o x - 001864 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 Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0064.D Lab Smp Id: SL-1. C-l-3 Inj Date : 30-JUN-2002 23:51 Operator mla Inst ID: dudejr.i Smp Info : Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m Meth Date : 27-Aug-200209:59 dudejr.i Quant Type: ESTD Cal Date : 30-JUN-2002 22:45 Cal File: DUDE0058.D Als bottle: 28 Dii Factor: 1 .0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 C o n c e n t r a t io n F o rm u la : A m t * D F * C p n d V a r ia b le Cpnd Variable Local Compound Variable Conpoundo IB PFBS (299) 20 PFH8 (299) 21 PPOA (413) 22 POSA (491) 23 ppoa (499) QUANT a m HASS 299 299 299 399 413 49B 499 499 499 CONCENTRAT] ONS ON-COLUMN PINAL RT KXP RT DLT RT R85POK5R (ng/mL) (ng/oL) 3.3BB 3.17 3.7S1 3.79B 3.997 4.754 4.175 4.434 4.409 3.311 3.3B1 3.3B1 3.792 3.990 4.75C 4.145 4.1*4 4.149 0.007 -0.305 0.370 0.004 0.007 0.000 0.007 0.2CC 0.437 12710 3939 2S5S 71B2 23937 140C25 4&0BC4 4774 19939 1333.84 1224.34 1224.42 0.13435 0.3B2S9 5.2038B 10.0242 1277.40 1177.17 1220 1220 1220 0.134(H) 0.343 (N) 5.30 (N) 10.0 12 BQ 1190 QC Flag Legend M - Compound response manually integrated. Eact Copy or Odern;: & L C . IZ U & lo i- feirsaj 00186S Report E02-0443 Data F ilas NSEt*UrjatStartatSchaSludajr.iSD02<S2S.bSDUDE006*.D Tenn. River Valley Samples Paca 2 20 PFHS (3 9 9 ) Bacttte# -?WC if?iaj L l/lo fb X -- 'MV:. 01866 Report E02-0443 Data Filai SSEt*targat\tarf*tSch*Sdu6jr.i\D020629 .b\BUDE0C64,D 21 PFOft <413) Tenn. River Valley Samples ps, 3 22 POSA <498) 23 PFOS <499) 0 00 C o.O ,i: r _ J 2 -/io / o2s fcit'ai rjofc 001S67 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 Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0065.D Lab Smp Id SL-1. C-2-1 Inj Date 01-JUL-2002 00:02 Operator mla Inst ID: dudejr.i Snip Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\Etstarget\target\chem\dudejr.i\D020629.b\D020629 .m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date 30-JUN-2002 22:46 Cal File: DDE0058.D Als bottle 29 Dil Factor 1 .0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound IB m s (a>) 30 FFHS (3>> 31 pro* (413) SB POSA (4M) 33 pros <499) QUANT SIG NASS 299 299 299 299 299 299 413 493 4 93 499 499 CONCENTRATIONS ON-COLUMN FINAL RT BXP RT DLT RT RISFOM8B (ng/nli) (ng/L) 3.3BB 3-1 3.751 3.791 3.402 3.531 3.997 4.7S3 4.171 3.792 4.COS 3.331 3.331 3.331 3.793 3.792 3.792 3.990 4.751 4.144 4.151 4.lit 0.007 -0.212 0.370 0.005 -0.390 -0.253 0.007 0.007 0.007 -0.375 0.437 13C24 2305 1(21 10531 1005 2533 25775 122304 473QS7 2335 21371 1223.79 1224.40 1224.47 0.23151 797.194 0.00404 0.54153 4.44735 9.74111 1377.70 1277.14 1220 1220 1220 0.232 797 0.00404 0.542(N> 4.45 9.74 1210 1230 QC Flag Legend M - Compound response manually integrated. Dat.3 001868 Report E02-0443 Tenn. River Valley Samples Data F ila: SSElstar*atStartatSehSdudJr.l\D020629.bSDUDE005.I) SSEtstartatSbarctSchanSdudajr.iS0020&29.bSIlUI00S.D Pa( 2 18 PFBS <299) 20 PFHS <399) Exact Ccpy of Originai y*i< 17-1/o f ai. Initiai Date 0169 Report E02-0443 Data F il t S\EUtar*at\taritSch\*jdajr.iSD020629.bSIIUl>E0C68.]) 21 PfOA (413) Tenn. River Valley Samples Pa 3 22 FDSft <498) 23 PFOS (499) Exa c tC c jy a :'! ,4dni_ jlc* initia} 0i6 Q1670 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE007L.D Page 1 Report Date: 27-Aug-2002 10:05 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE007l.D Led> Smp Id SL-1. C-3-2 Inj Date 01-JUL-2002 01:08 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\Etstarget\target\chem\dudejr.i\D020S29.b\D020629.m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: BSTD Cal Date 30-JDN-2002 22:46 Cal File: DUDE0058.D Als bottle 34 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Coapoundi 14 P P M Us) i t 30 r a s U> 31 n oA (413) * 32 roSA (4SI) 1 <4 23 r o s (4SS) QUANT sia hass 299 299 299 399 413 499 491 499 499 CONCENTRATIONS OH-COLOHN 92MAL sa SX RT DLT RT RESPONSI (ng/m L ) (ng/mL) 3.394 3.174 3.750 3.794 3.997 4.752 S. 009 4.174 a.es 3.341 3.341 3.341 3.792 3.990 4.754 4.75 4.144 4 .1 4 0.007 -0.205 0.349 0.004 0.007 0.004 0.253 0.005 0.437 1530S 2054 1430 12444 20244 145959 9741 742237 0017 1233.49 1224.45 1234.44 0.34719 0.17434 7.07743 2743.92 17.9441 1277.17 1220 1220 1220 0.2.7IM) 0.17SIM) 7.04 2740 17.9 120 QC Flag Legend M - Compound response manually integrated. 'S cxaciCopyofi L ta lL -- /2 / j o / r > i , Initiai Dais 00X87X Report E02-0443 Sata F i t a : S S E ts ta ria tS ta r{ t\c h a n S d iid a jr.l>vS020S29.bSIUDE0071.B Tenn. River Valley Samples Paa 2 20 PFHS (399> Sect Copy nfiaj bfU: 001872 Report E02-0443 Data Fila: SSEttartMarttSch*Sdudjr.lM20629.bM)UDE0071.D 21 PFOA (413) Tenn. River Valley Samples Paca 3 22 FOSA (496) 23 PFOS (499) ilC Copy... OcjiiTcl fniSaJ {feta 2 U d g L - OOI073 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 Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0076.D Lab Smp Id SL-1. C-4-2 Inj Date 01-JUL-2002 02:03 Operator mla Inst ID: dudejr.i Snip Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date 30-JN-2002 22:46 Cal File: DUDE0058.D Als bottle 37 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula.- Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 11 PFBS (2> 20 m U ) posa21 proA (413) 22 (4M) 22 9900 (49) qu a k t aia HASS 299 299 299 299 413 49t 499 499 41* 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSI (ng/L) (r.g/*L) 3 .311 3.391 3.224 3.311 3.750 3.3ftl 3.792 3.792 3.997 3.990 4.749 4.754 3.71S4.174 4.149 4.149 4.434 4.100 4.COC 4.159 0.000 -0.1S7 0.359 0.000 0.007 0.013 0.005 -0.393 0.200 0.437 13243 2*13 429 5712 11747 103537 594549 514 11440 20929 1223.91 1224.40 1234.53 0.09444 919.097 3.47245 14.1974 1277.75 1277.43 1277.15 1220 1220 1220 0.0944<M) 19(H) 2.57 14.2 1290 1290 1290 QC Flag Legend M - Compound response manually integrated. CM C lO -lio / t- initial 001874 S iS T o o C. Report E02-0443 Data Fil; SSEtstarttStare*tSchmSdud*Jr.i\l)02629.bSIIUOE0076.D 21 PFOft <413) Tenn. River Valley Samples Pag 3 22 FOSA <4 9 8) 23 PFOS (499) E ra# Cop., Q n _ is m U 0X87G Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0097.D Page l Report Date: 27-Aug-2002 10:06 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0097.D Leib Smp Id SL-2. C-l-3 Inj Date 01-JUL-2002 05:53 Operator mia Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020629.b\D020629.m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle 54 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 10* o1 Compounds is m s ( 099) 21 PPOA (411) aa s o s a <) 23 proa (4> quant a io HASS 299 299 299 399 399 399 399 413 4M 499 499 CONCBRKATIONS OH-COLUMN PINAL RT HXP XT DLT RT RB8PORSI (ng/.L) (ng/mL) 3.3S7 3.119 3*750 3.79S 3.394 3.SSS 3.952 3 *994 4.7M 4.110 4.11 3.311 3.311 3.311 3.792 3.792 3.792 3.792 3.990 4.71 4.1! 4.ICO 0.00 *0.212 0.319 0.001 *0.391 -0.234 0.190 0.001 0.00 0.012 0.443 1134$ 2159 1134 3192 1197 till 1579 12700 14*14 121153 113C1 1223.92 1224.44 1224.50 0.03700 797.111 0.17119 797.119 19.045 o.oaaoi 1374.02 1277.43 1220 1220 1220 0.0370 797 0.177 797 1 9 (N) o.oaio(K) 1270 1210 QC Flag Legend M - Compound response manually integrated. Exact Copy r.: 4~- laj'e/ai. 001877 Report E02-0443 Tenn. River Valley Samples Data Fila: SSEtstargat\targatSchanSdudajr.i\D020629.bM)UDE0097.D S\Et*tart*tVtrtatSchai*SdudaJr. iMK>20i29.b\DUDeo097,D Paca 2 18 PFBS <299) 2 PFHS <399) BxzCor.- - - .. /mXfff ~2-- ,p;'73 0 0 *5 7 8 Report E02-0443 Data Filai S\Ettar*atStar*at\ehiSdudajr.i\B020629,bSDUDE0097.D 21 PFOA <413) Tenn. River Valley Samples Paj* 3 22 FOSA <498) 23 PFOS <499) tacf Copy o f Original Oste 001879 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 Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0105.D Lab Smp Id SL-2. C-3-2 Inj Date 01-JUL-2002 07:21 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020629.b\D020629 .m Meth Date 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD Cal Date 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle 60 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable (a>Compounds 1ft PFBS ao PFHS (3S) 31 PPOA (413) 33 POSA (*) 23 PFOfl (4) G U M R 31G MASS 299 39ft 299 399 399 399 413 49ft 49ft 499 49 499 ot-couamG0NCSNTRAT1ON8 PIMM. RT EXP RT DLT RT RSSPONSB (ng/mL) (ng/mL) 3.3ftft 3.1(2 3.7S0 3.79ft 3.S4S 3.97ft 3.99 4.7C9 4.437 4.174 4.434 4.SOS 3.3ft! 3.391 3.311 3.792 3.792 3.792 3.990 4.75ft 4.7SS 4.14ft 4.1ft 4.14ft 0.007 -0.219 0.349 0.004 -0.247 0.1*4 0.004 0.013 -0.329 0.004 0.244 0.437 923ft 149 243 329 4903 3370 771 20521 14C4 179402 5700 19533 1224.04 1224.47 1224.41 0.02579 0.07143 0.02704 919.244 0.25210 3744.34 0.99442 1375.24 1277.19 1220 1220 1220 0.025ft 0.0714 w0.027ft 1 0.252 2740 0.9B7 1290 1200 QC Flag Legend M - Compound response manually integrated. Exact Copy oiO t'c'rt- .C k L - S j/ fo L - initiai Of-tr. ^ v > iS g o Report E02-0443 Bat F lit ! t*tSt*rt*tSchSdud*Jr. i SD020629.bSDUBE01.05. B Tenn. River Valley Samples P *t 2 20 PFHS <3 9 9) , f c t Cop; Oaii 001881 Report E02-0443 Data Fila: YsEtatartatStarft\cha\dud*Jr.iM>020629.bSDUDE0105.D 2 t PFOA <413> Tenn. River Valley Samples P a ja 3 22 FOSA <49S> 23 PF08 <499> &actCcpj/j-.:.. .,sl U ltP h u U 01bS 2 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0ll7.D Page 1 Report Date: 27-Aug-2002 10:07 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020629.b\DUDE0117.D Lab Smp Id SL-2. C-6-1 Inj Date 01-JUL-2002 09:33 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method Meth Date Cal Date \\Etstarget\target\chem\dudejr.i\D020629.b\D020629 .m 27-Aug-2002 09:59 dudejr.i Quant Type: ESTD 30-JUN-2002 22:46 Cal File: DUDE0058.D Als bottle 69 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound li PPBS (29) 20 PPKfl () 21 PPOA <13> 22 POSA (> 23 ppoa <> QUANT SIG NASS 299 299 299 399 413 490 499 499 CONCENTRATIONS ON-COLUMN PINAL RT BXP RT DXiT RT RESPONSO (ng/mL) <ng/mL) 3.301 3.170 3.7S0 3.790 3.990 4.709 4.101 4. COB 3.301 3.301 3.301 3.792 3.990 4.750 4.100 4.100 0.007 -0.205 0.309 0.000 0.000 0.013 0.013 0.437 9473 141B 545 2433 100 32417 221203 22005 1224.03 1224.41 1224.53 0.00120 19.302 0.33013 2.2003S 1277.10 1220 1220 1220 0.00120(H) 1(H) 0.330 2.20 1200 QC Flag Legend M - Compound response manually integrated. & a ct Copy or Gr.~?n:: C JlIL. IlkLijl-- iiiat Ost;- 001 3 Report E02-0443 Bat Filet SS E lt*rj t\t -t# t'sch N *Jd *4 r.iM )0 2 0 i2 9 .b M )U D E 0 1 1 7 ,D Tenn. River Valley Samples Pace 2 20 PFHS (399> Exact Copy of Original Clt2C- iJ//tn Ort. U014 Report E02-0443 Data Fila: \\EtitarcatStartat\eh**\dudajr.iSD020629.bSDUDE117.D 21 PFOA (413) Tenn. River Valley Samples 22 FOSA (49S> 23 PFOS <499) .~ct Copy ( ; Ctiginni i & C l2.Ulo2- Qstf; 0188S Report E02-0443 Tenn. River Valley Samples Data File: DUDE0066.D Report Date: 27-Aug-2002 11:05 Page 1 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0066.E Lab Smp Id SL-3. C-2-2 Inj Date 03-JUL-2002 02:49 Operator rala Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Misc Info Comment Method \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\D020702.m Meth Date 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD Cal Date 03-JUL-2002 01:21 Cal File: DUDE0058.D Als bottle 55 Dil Factor 1.00000 Integrator Falcon Compound Sublist:all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound 1* PRBS (2M> 20 PPHS (1) 21 PROA Mil) 22 ROSA (4M) 23 PROS (4M) QUANT SIG HASS ass 399 ass ass 413 4SB 4SS 4SS CONCENTRATIONS ON-COLUMN PINAL RT EXP RT DLT RT RBSPOKS8 (ng/mL) (ng/uL) a.ass 3.113 3.75? a.ais 4.003 4.003 4.Ill 4.SSI 3.307 3.3*7 3.3*7 3.7S1 3.S*S 4.74* 4.147 4.1*7 0.00* 0.204 0.370 o.oa* 0.014 0.055 0.014 0.424 14173 3040 aaac soss 2254 2313* 1*3*14 23954 1220.00 1220.4* 1230.51 0.30394 0.37074 0.4310* 1.14537 1324.22 1320 1320 1220 0.204(H) 0.271(H) 0.431 1.14 1320 QC Flag Legend M - Compound response manually integrated. "-XM CopyofOriginal C i& ~ mtiv Date 001886 Report E02-0443 Tenn. River Valley Samples Data F l U i SSEtstarfatStartatl>ha*Vluda<jr.lM)020?02<D20702.bMXJDE0066.D Paca 2 20 PFHS (399> Exact Copy of Origina1 Ul U I p initial Oatr- t0 lS S 7 Report E02-0443 Tenn. River Valley Samples Data Flit: \SEtUrtttStrttSchaiSdudJr.iS0020702<H20702) .bMXOEEOOi.D 21 PFOA <413) Pat# 3 23 PFOS <499) Exact Copy of Original CiiL_ l2-//dfL. 'nffiai ox,-. 0Q88S Report E02-0443 Tenn. River Valley Samples Data Pile: DUDE0076.D Report Date: 27-Aug-2002 11:06 Paqe 1 a 3M Environmental Laboratory B02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020702 (D20702).b\DUDE0076.D Leib Smp Id SL-3. C-4-2 Inj Date 03-JUL-2002 04:39 Operator tnla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Btstarget\target\chem\dudejr.i\D020702 (D20702).b\D020702.m Meth Date 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD Cal Date 03-JL-2002 01:21 Cal File: DUDE0058 .D Als bottle 62 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound* it PPBS (2) 20 FFHS tt) 21 PFOA (4131 22 POSA (4M) 23 rros <499* QUANT SIQ MASS 29 299 299 399 399 399 413 49 499 499 499 CONCENTRATIONS OH-COLUMN FINAL RT BXF RT DLT RT RESPONSE (ng/oL) (ng/*L) 3.394 3.112 3.770 3.25 3.572 4.01O 4.010 4.749 4.147 3.911 4.591 3.347 3.347 3.347 3.791 3.711 3.791 3.949 4.74 4.147 4.1C7 4.147 0.007 -0.205 0.343 0.034 -0.219 0.219 0.031 0.031 0.030 -0.35 0.434 21375 2047 1244 39C5 331* 3391 9130 20947 307947 1347 20341 1219.74 1220.52 1220.55 0.14177 0.14954 0.15973 795.310 0.35235 3.40(47 1324.54 1324.29 1220 1220 1220 0.143 0.170 0.170 7*5 (N) 0.352 3.41 1320 1320 QC Flag Legend M - Compound response manually integrated. Bract Copy of Origina! /3 -//o fp i- 0018S9 Report E02-0443 Tenn. River Valley Samples Dt* Fllt SSEtsUrs*t\tarsttSchnNdud*Jr.lSD020702<S20702>.bSOUI007e.S PHI 2 20 PFHS (399) Exact Copy of Original .CJ}*- iZ(</i- initia! Dair. 001C90 Report E02-0443 Tenn. River Valley Samples S*ta F ila i SSEtstartkStart*tSch*aSdudjp. i\IK>20702<B20702>. b\DUDEOO?6. D a PF (413) 3 22 FOSA <496) 23 PFOS <499) i Copy o f Original OnC._ la ftc J l- Osta 001891 Report EQ2-Q443 Tenn. River Valley Samples Data File: DUDE0083.D Report Date: 27-Aug-2002 11:06 Page 1 3M Environmental Laboratory E02-0443, Term. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\DUDE0083.D Lab Smp Id SL-3. C-6-1 Inj Date 03-JUL-2002 05:56 Operator mla Inst ID: dudejr.i Smp Info Tenn. River Valley Fish. Prep-17 Jun 02. CMC/MLA. 20 Jun 02 Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020702(D20702).b\D020702.m Meth Date 27-Aug-2002 11:01 dudejr.i Quant Type: ESTD Cal Date 03-JUL-2002 01:21 Cal File: DUDE0058.D Als bottle 68 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compound* It m s (399) 20 m a <359) 21 PPOA (413) 22 POSA (495) 22 ppoa (499) QUANT3ia NASS 299 3) 413 491 499 CONCSNTRATIOKS ON-COLUMN PINAL RT BXP RT DLT AT RBSPOKS (ng/mL) (ng/L> Compound Hob Detected Compound Not Dotocbftd. Cowpound Hob Dotectod Compound Hob Detected. Compound Nob Detected, Copy of Original C i n e ^//a/rj.2Dste 001892 Report E02-0443 Tenn. River Valley Samples Sata F ilt \SEt*tars*tStartt\ch*n\dudaJr.AD020702<D20702>.bMXJX0083.D p* 2 fl 20 PFHS <399) (Unctotaotad) Exact Copy of Origina! C m... la-J j d p -ju 001893 Report E02-0443 Tenn. River Valley Samples ta ta F lU t S S E ts ta rc *tS ta re tS e h *n S d U d *J r. iS D 020702(D 20702) .b S K fl)E 0 0 83 .D 2 t PFOA (413> (UncMmtwl) Pe* 3 22 FOSA (498) <Uhd*taetad) 23 PFOS (499> < U n d *te c t*d > :\ 'u Copy o Crfgfna! C W L . I2jc&- `niL!ai Oats 001894 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0065.D Page l Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr. i\D020812A.b\DUDE0065.D Lab Smp Id: Water Blank-1 Inj Date : 12-AUG-2002 23:11 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443 Water Blank Water Samples; non-GLP; 6/20/02; OK Misc Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Als Date : bottle: 2102-AUG-2002 16:13 Cal Pile: DUDE0027.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist:all.sub Target Version: 4.12 <o 1 Compound 1 (J9S) 2 PFH3 (MS) 3 PPOX (413) s4 YOOA (4SI) pros (4>) q u a n t aia HABS 299 299 299 399 399 413 496 499 C0NCEWTRATZ0M8 OM-COLUXM PINAS RT BXP RT DLT RT RR8PONSB (ng/mL) (ng/aL) 3.353 3.10 4.301 3.04 3.565 4.016 4.609 4.301 3.394 1.394 3.394 3.791 3,791 3.963 4.766 4.160 0.041 Q.145 0.607 0.013 -0.326 0.034 0.041 0.041 29174 5546 1904 S192 1012 9179 3390 34010 0.54141 501.660 503.766 0.1546 0.02703 0.04921 6.10649 0.16996 0.541 504 504 0.155 0.0270 0.0492 0.105 0.170 Eiaci Co;j orOrg-iiw: A.' IrJUa! Date 001S95 Report E02-0443 to ta F ila : SSt*tartt\tapet\chnSdudjr. lM1020fll2A.bSDUDE006S.D Tenn. River Valley Samples P**a i Exact Copy o: C r.--. -C&t t'lj/d i-- tflltfal Or.t 001836 Report E02-0443 Dit* F il; SSEttar{tNtrgtt\chiiSdudjr.l\D0208i2fl,b\DUE0065.D 3 P F <413> Tenn. River Valley Samples 4 FOM <498> B PFOS (499> ECt Copy o; iJrfn i2u initiaj Date 001S97 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0066.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443, Term. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0066.D Lab Stop Id: Water Blank-2 Inj Date : 1 2 -AUG-2002 23:22 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443 Water Blank Water Samples; non-GLP; 7/17/02; OK Misc Info : Comment Method : \\Etstarget\target\chem\dudejr.i\D0208l2A.b\D0208l2A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Typej ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 21 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compounds 1PFBS<2> 23PPPFOHSA((34131) 45PPOROSAS((443)) QUNAANSTSSIC RT BNPNT DLTRTRfiSPONSBONInG-CgOO/NaLCULBM)INTJUTXInPagNIN/SmALL) 299 299 299 299 2444411399339 333344444.......3..37103351491500140350150 333333344.........333399771999898988444343180--000000000.........01038003048440137404291471 511340133134158734183011740785110987890 154500005.00....0041121313332105...34.944477787978221828887703 0Q001....11124.555420510000355732454 c t C opy o f ergi:*; fnifiai 2- QZf 001S98 Report E02-0443 ta t F il : S\Etstr(tStargtSchSdudtJr. i\D02O8i2ft,b\DUDEOOM.D Tenn. River Valley Samples Pt 2 ExactCcpy Jt J o [ X Data 001S99 Report E02-0443 Data F ila: S\EfcatarcatStarsatSchMSdudajr.iSl)020ei2A.bMIUI)E0066.9 3 PFtM (413) Tenn. River Valley Samples Pata 3 4 FOSA <498> B PFOS (499) 'S .. W ( 001900 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0076.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443 Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudej r .i\D020812A.b\DUDE0076.D Lab Smp Id: 38032 Inj Date 13-AUG-2002 01:12 Operator : mia Inst ID: dudejr.i Smp Info : E02-0443-38032; Water Samples; non-GLP; 6/20/02; OK Misc Info : Comment Method : \\Etstarget\target\chem\dudejr.i\D0208l2A.b\D0208l2A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Queuit Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 26 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Coapound 1 FTBS 2 PTHfl (39J) 2 4 FVOX POSA l(U90) () iM QUANT SIS NASS 299 29 2 a2 2399 444199390 RT 2XF RT OUT RT RESPONSE 3.401 2.540 33..339944 0.007 -0.054 3.203 3.394 -0.191 34..004140 33..339944 00..442540 34,,021055 33..379941 0.021 0.014 444,.,71000031 434...197055200 0.0...00a22x11' 19351 147211 195 2975503 157279770 04190 130473 190157 CONCRNTRATCCMS ON-COLUMN (ng/mL) PINAL (ng/ab) a 0.19454 0.197 4.72522 4.73 303.706 504 550033..705219 550044 540.035.003070 45.0054 44..9544495220 44..9547 5.10901 5.19 Exact Copy n.! O-ip:; Uni. Urjih- Lnitia! 0*V: 001901 Report E02-0443 Dt* Filet 'sNEtitrt;tSUrttSchiSdu<iJr.SB020812.bVtlBE007t.D Tenn. River Valley Samples P *t Z Z PFHS <399) Exact Copy of Origina! CimC M -f/oloi- initial Date 0 0 1 .9 0 2 Report E02-0443 Data m a : \\EtttartatStartat\cha*Sduel9jr.i'J20eia).bSDUDE0076.D 3 PFOfi <413) Tenn. River Valley Samples P *(t 3 4 POSA <498) B PFOS <499) fc.tacCopy,-0Vf/:.^ ijx/o'i- 001903 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0073.D Page l Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0073.D Lab Smp Id 38029 Inj Date 13-AUG-2002 00:39 Operator mla Inst ID: dudejr.i Smp Info E02-0443-38029; Water Samples; non-GLP; 6/20/02; OK .Misc Info Comment Method Meth Date Cal Date \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD 12-AUG-2002 16:13 -C-a-l -F-ile: DUDE0027.D Als bottle 25 Dil Factor 1.00000 Integrator Falcon Compound Sublist : all.sub Target Version: 4.12 Compounde a 1 CPU (JJ> a PFHS (1*9) 3 PPA (413) 4 POSA (4*0 s proa (4) 1 i QOAMT 91 MAAS 399 39* 413 499 499 499 RT ax? RT 3.40* 3.111 4.00 4.19 4.197 4.447 3.394 3.791 3.943 4.74* 4.140 4.140 DLT RT RBSPORflB 0.014 0.030 0.037 0.034 0.037 0.307 19093 353177 3301*1 34000 31300 131570 c o N c n m u s io iu ON-COLON* FINAL (ng/L) (ng/aL) 3.45491 7.05310 31.0431 1.11439 30.1041 3.3904 a.c(N) 7.05 31.0 1.11 (M) 30.3 3.39 QC Flag Legend M - Compound response manually integrated. B o c i Cop/ of O rirJrr l/o/ km U01S04 Report E02-0443 Date F ile t Vtstar{tSt4rs*tSch*ASduc(*4rtMtt20812A.bM)UK0073,!l Tenn. River Valley Samples Pf* 2 2 PFHS <399) E e c t C o p y r .f -'. M l C. Il !/*{&- Initiai . 001905 Report E02-0443 Bata Filas \SEtstartetStarjat\cheiSdudaJi-,i\D020812ft.bMIUZ)E0073.I> 3 PFOA <4131 Tenn. River Vaitey Samples Pas 3 4 FOSA (498) B FFOS <4991 Exact Copy of Cn'!)'! l 'i l l o i - initial Date 001906 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02O8'2B.b\DUDE0l30.D Page l Report Date: 29-Aug-2002 07:12 3M Environmental Laboratory E02-0443, Term. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0130.D Lab Snip Id: 38030 Inj Date : 13-AUG-2002 11:08 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443-3&030; Water Samples; non-GLP; 7/17/02; OK Misc Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m Meth Date : 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD Cal Date : 13-AUG-2002 06:44 Cal File: DUDE0106.D Als bottle: 42 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compounds i PBS (a> 2 ras (3> 3 ?roA (411) 4 POSA (4*1) S PFOS (441) QUANT Slfr NASS 39 39 29 29 399 413 49 49 CONCENTRATIONS OM-CQliUKN PINAL RT RXP RT DLT RT R85P0NSK (ng/mL) (ng/ali) 3.3? 2.49 3.303 3.777 3.777 3.941 4.741 4.13 3.394 3.394 3.394 3.394 3.791 3.992 4.7 4.ICO 0.007 0.994 0.191 0.393 0.014 0.014 0.027 -0.021 197441 1231 2244 112C9 307299 4152125 7940357 991442 3934.50 2935.44 2935.42 2935.20 424.445 427.440 300.224 423.473 2930 2940 2940 2940 425 42 300 424 i Exact Copy a - G ri^ ir; UJjjrfamitlal Dsta' 001907 Report E02-0443 Hat F ilar \\EUUrs*tStare*tSchMSdud*jr.lM>020812B.bSIIUIIE0130.0 Tenn. River Valley Samples P j* 2 2 FFHS <399) East Copy 001908 Report E02-0443 D a ta F iU : S S E ts ta ri t\U r* l\c h tia \d u d * 1ir.iS D 020812B .bS IIU D E 130.II 3 PFOA <413) Tenn. River Valley Samples 4 FOSA <496) B PFOS <499) Exact Copy Or`r;.v . U o |s G 9 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0092.D Page 1 Report Date: 27-Aug-2002 14:12 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0092.D Lab Smp Id 38043 Inj Date 13-AUG-2002 04:09 Operator mla Inst ID: dudejr.i Smp Info E02-0443-38043; Water Samples; non-GLP; 6/20/02; OK Mise Info Comment Method Meth Date Cal Date \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m 27-Aug-2002 14:OS dudejr.i Quant Type: ESTD 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle 34 Dii Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Ooapeund* 1 p p b s (21) 3 m a (211) 3 PFOA (413) 4 POSA (4M) 5 proa (4M) QUANT S2Q MASS 299 299 299 299 299 299 413 4M 4M CONCENTRATIOMS OW-COLONN PXNAXi RT EXP RT DLT RT RESPONSE (ng/aL) (ng/aL) 3.354 a.4SI 3 .210 3 .IS 4.037 3.M3 4.010 4.7*5 4.195 3.3*4 3.3*4 3.3*4 3.3*4 3.3*4 3.791 3. a 4.75 4. ISO *0.040 -0.943 *0.1*4 0.424 0.443 0.171 0.020 o.oaa 0.035 3214 739 C2 1344 1953 15543 *4*1 5471 30*51 0.57051 503.29 503.534 503.511 503.7*5 0.S0173 0.0406a 0.2049 0.07297 0.571 504 504 504 504 0.502 0.05*7 0.207 0.0720 ;rracfCcpyofOr^ir-' Initiai n-j.. ' 001910 Report E02-0443 Sata F ila: SSEtitartatStarjat\ehaSdudajr. iND020812A. b\DUDE0C92. D Tenn. River Valley Samples Paca 2 Io n 299.00 6 .0 < 8 .8 -j r 5ri 8.0-1 4.8-1 4.0 -! ? 3 .8 ) 1 3 .0 j 2 .8 -i o * M Al A o. b-A /L -- lJ J - US s " *k. .^J _____2_._4___2_._8__B3.i2n. 3.4 4.0 2 PFHS <399) -f -r'Original CMJL / io/o^ 'i'rai Daa 00X311 Report E02-0443 Data F ila: \SEtstarcatStarsatSchmSdud*Jr.iM)020912A>bM)U])E0092>D 3 PFOA (413) Tenn. River Valley Samples 4 FOSA (4W> B PFOS (4 9 9 ) 001912 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 Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDB0067.D Lab Smp Id: 38025 Inj Date : 12-AUG-2002 23:33 Operator : mla Inst ID: dudejr.i Smp Info : E02-0443-38025; Water Sandies; non-GLP; 6/20/02; OK Misc Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D AlS bottle: 22 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compounds a1 a ms PFHS PROA, Um ) O (*!*) 4 POSA (4M) S PPOS (4M) QCANT SIO NASS 399 399 413 494 49 499 CONCENTRATIONS OH-COLOHM PINAL RT EXP RT DLT RT RBSPORSI (ng/mL) tng/L) 3.401 3. aia 4.003 4.794 4.141 4.464 3.394 3.791 3.931 4.764 4.160 4.160 0.007 0.031 Q.031 0.014 0.031 0.304 9453 247750 33164 39344 643(51 135043 3.99306 7.71X34 31.319 0.96234 14.4924 3.40254 3 . M (N) 7.71 31.3 S.M2M) 14. S 3.40 QC Flag Legend M - Compound response manually integrated. EiaciCopv C- D L . U/y fe iia i 001913 Report E02-0443 Data F ilt S\EttarttStartt\eha*SdudJr.i\D020812A.b\IWIIE0067.D Tenn. River Valley Samples Pat a 2 PFHS <399) WoO\ 001914 Report E02-0443 Data Fi lat SSEtstartatStar*lScha\du<ra,Jr.i\D020812A.bMIUDE0067,D 3 PFOA C4t3> Tenn. River Valley Samples ptgt 3 4 FOSA <498) 8 PFOS <49> C-0 1 9 1 5 Report E02-0443 Tenn. Rivet Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0069.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory- B02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0069.D Lab Smp Id 38026 Inj Date 12-ADG-2002 23:55 Operator mla Inst ID: dudejr.i Smp Info E02-0443-38026; Water Samples; non-GLP; 7/17/02; OK Misc Info Comment Method \\Etstarget\target\chem\dudejr.i\D020812A.b\D0208l2A.m Meth Date 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle 23 Dil Factor 1.00000 Integrator Falcon Compound Sublist : all.sub Target Version: 4.12 1 i i CONCSNTRATXONS QUANT SXG ON-COLUMN PINAL Qmapounds NAJS m r t DLT RT RBSPOMS8 (ng/aL) (ng/aL) 1 PFBB 2 PPKfl 3 PPOA 4 POSA 5 PPOS (299) <299) (413) (494) (499) 299 3.401 3.394 0.007 114547 3.70420 3.70{lt) 399 3.411 3.791 0.020 2S5IC4 7.94944 7.97 M 4.003 3.942 0.031 340041 22.4S24 22.4 49t 4.749 4.744 0.021 31142 1.02079 1.0i (H) 99 4.140 4.140 0.020 444455 20.7904 20.4 499 4.497 4.140 0.307 140144 3.54101 3.57 QC Flag Legend M - Compound response manually integrated. Cos, Ci/ic i j j /0{ i_ 00916 Report E02-0443 Tenn. River Valley Samples i PFBS <299 2 PFHS <399) 00191? Report E02-0443 Hat F ila t S\EtstargatStarcatSchaMSdudaJr.i'a>O2OB12fl.bsgUIE009.D 3 PPM <413> Tenn. River Valley Samples Paca 3 4 FOSA <498> S PFOS <499> ^Ca^ya;Cr!:in.y M L u U (* /n - 0 0 9 1 S Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DUDE0071.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0071.D Lab Smp Id: 38027 Inj Date : 13-AUG-2002 00:17 Operator : mla Inst ID: dudejr.i Stnp Info : E02-0443-38027; Water Samples; non-GLP; 7/17/02; OK Mise Info : Comment : Method \\Etstarget\target\chem\dudejr.i\D0208l2A.b\D0208l2A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 24 Dii Factor: 1.00000 Integrator: Falcon Compound. Sublist : all.sub Target Version: 4.12 Compound* 1 PVBS U s s ) 2 PFHS (is > 3 PPOA (413) 4 POSA (4SI) 5 p ro s (4SI) QUANT 8Xa NASa 139 399 413 49 499 499 499 COWCBmUZIOHS ON-COLUMN PINAL RT EXP RT DUT XT RESPONSE (ng/mL) (ng/aL) 3.401 3.911 4.002 4.794 4.190 3.944 4.447 3.394 3.791 3.993 4.749 4.140 4.140 4.140 0.007 0.020 0.020 0.02 0.020 -0.294 0.307 102929 405593 412129 121332 909339 410 S093 3.14444 12.7977 27.9472 4.0011S 24.5743 379.797 1.79743 3*1. (It) 12.9 29.0 4.00 24.4 390 l.0 QC Flag Legend M - Compound response manually integrated. < 0Q1919 Report E02-0443 Oats F ilet \\Ett*rtt\tarj*t\ehw\dudjr,lM020812A.b\DUDE0071.D Tenn. River Valley Samples Fit 2 2 PFHS <399) '^COC; ,CMr_ ii'a;" w/il 001920 Report E02-0443 Data Fil! SSEtstarjatNtarj*t\eh*a\dud#jr, iSD020812A. b\DUBE0071. D 3 PFCK < 413) Tenn. River Valley Samples 4 FOSA <496) B PFOS <499) Chy /xht/oi. 001921 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082A.b\DDE0078.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0078.D Lab Smp Id: 38033 Inj Date : 13-AUG-2002 01:34 Operator : mla Inst ID: dudejr.i Smp Info E02-0443-38033; Water Samples; non-GLP; 6/20/02; OK Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:05 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 27 Dii Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compounds 1 m a (3) a PIHS (3*) a PPOA (413) 4 POSA (4**) s PPOS (43) QUANT SZG MASS 299 295 29 299 39 399 413 49ft 499 CONCSNTKATJOtKi ON-COLUMN PINAL RT BXF RT DLT RT RB5F0MS8 (ng/*L) (ng/nlj) 3.3CO a.aio 3.10 4.OSS 3.412 3.969 4.010 4.796 4.194 3.394 3.394 3.394 3.394 3.791 3.791 3.992 4.76 4.160 -0.034 -0.14 0.424 0.664 0.021 0.17 0.02 0.02 0.034 26600 4236 1671 634 S6S 5436 11637 5467 S0it 0.45093 503.706 503.796 503.632 0.16974 0.16313 0.20126 0.17456 0.20349 0.451 504 504 504 0.170 0.162 0.201 0.174 0.203 t 001922 Report E02-0443 D*U F i l e SSEtstr(tStar(tNchmSdud*jri SD020B12A. bMUDE0078. S Tenn. River Valley Samples <*n* 2 2 PFHS <3S9> ..CiiiC J ii /o k . 001923 Report E02-0443 Data F ilt \\Ettar*t\t*rxtSchw\dudjr.iSI02ei2A.bSDUDE0<>78.D 3 P FM (413> Tenn. River Valley Samples Pjp 3 B PFOS <499> Ciyu"Ju, l^l//2001924 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr .i\D020812A.b\DUDEQ080.D Pacre 1 Report Date: 27-Aug-2002 14:11 a 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file \\Etstarget\target\chem\dudej r .i\D020812A .b\DUDE0080.D Lab Smp Id 38034 Inj Date 13-AUG-2002 01:57 Operator mla Inst ID: dudejr.i Smp Info E02-0443-38034; Water Samples; non-GLP; 6/20/02; OK Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date 12-AUG-2002 16:13 Cal File: DDE0027.D Als bottle 28 Dil Factor 1.00000 Integrator Falcon Compound Sublist : all.sub Target Version: 4.12 Compound 1 PPBS (a> a PPHS (3l 3 SPOA U V D 4 POSA (4M) 5 p ros (4M) QUANT SIO HASS 299 399 413 492 492 499 COMCBHTftATIOHS ON-COLUMN PINAL RT BXP RT DLT RT RESPONSI (ng/mL) (ng/aL) 3.401 3.212 4.010 4.79 5.090 4.194 3.394 3.791 3.922 4.752 4.742 4.150 0.007 0.021 0.022 0.022 0.322 0.034 21015 2573 17031 5747 275 51049 0.50070 0.25104 0.55503 0.21507 0.00294 0.71127 0.501(M) 0.251 0.555 0.215 0.00294 0.711 QC Flag Legend M - Compound response manually integrated. J On' / j / , a/ c. *> 0 1 9 2 5 Report E02-0443 Data F lla: SSEtatarc*tStar(tSehmSdiidaJr.:SD020S12A.bMIUDE0ee.D Tenn. River Valley Samples Paj 2 2 PFHS <399> UJJtiC\ k '& a i L2lteJ.2Jrcw.u- i9 2 e Report E02-Q443 B a t* F l U t \S E ts ta rt t\ta rt tS c h m S d u d J r. L\D 02 0 8 i2 .b \D U D E 0 O e o .r 3 PFOA <413) Tenn. River Valley Samples 4 FOSA <498) 8 PFOS (4 9 9 ) r x i c i iJc^y ; Original feiraJ Date 001927 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0084.D Page 1 Report Date: 27-Aug-2002 14:11 3M Environmental Laboratory E02-0443, Terni. River Valley Samples Data file : \\Etstarget\target\chem\dudej r .i\D020812A.b\DDE0084.D Lab Smp Id: 38037 Znj Date : 13-AUG-2002 02:41 Operator : mia Inst ID: dudejr.i Smp Info E02-0443-38037; Water Samples; non-GLP; 6/20/02; OK Mise Info : Comment Method \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date : 27-Aug-2002 14:06 dudejr.i Quant Type: ESTD Cal Date : 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle: 30 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Coapoundfl 1 m s > 2 PVHS <34) 3 PPQA <413) 4 POSA <44) S vos (449) QUANT 81G NASS 299 399 413 499 499 CONCENTRATIONS ON-COLOHM VINAI* RT KXP RT DLT RT R8SPOMSB (ng/L) tng/aL) 3.3S3 3.90S 4.010 4.79C 4.199 3.394 3.791 3.992 4.769 4.160 -0.041 0.014 0.029 0.029 0.029 32546 12979 14081 6547 43CS1 0.65999 0.39267 0.36547 0.20949 0.47606 0.660(N> 0.393 0.365 0.209 0.476 QC Flag Legend M - Compound response manually integrated. 001928 Report E02-0443 D a ta F i la t S S E tsta rja tS ta rja tS ch a S d u d a Jr.iS D 0 2 4 8 1 2 ft.b \D U D E O O S 4 .B Tenn. River Valley Samples P a ja 2 2 PFHS <399) `^^yofO iigfnai C1 3t3 001929 Report E02-0443 D a ta F ila S \E U ta r t t\ta r fr tS e h M \* jd a J r . iS B 0 8 1 2 fl.b M U B E 0 0 8 4 .a 3 PFOA <413> Tenn. River Valley Samples Pe 3 4 FOSA (4 9 8 ) B PFOS (499) 001930 Report E02-0443 ' Tenn. River Valley Samples Data File-. \\Etstarget\target\chem\dudejr.i\D020812A.b\DUDE0086.D Page 1 Report Date: 27-Aug-2002 14:12 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Btstarget\target\chem\dudejr.i\D0208l2A.b\DUDE0086.D Lab Stnp Id 38038 Inj Date 13-AUG-2002 03:03 Operator Smp Info mia Inst ID: dudejr.i E02-0443-38038; Water Samples; non-GLP; 6/20/02? OK Mise Info Comment Method \\Etstarget\target\chem\dudejr.i\D020812A.b\D020812A.m Meth Date 27-Aug-2002 14:06 dudejr.i Quant Type: ESTO Cal Date 12-AUG-2002 16:13 Cal File: DUDE0027.D Als bottle 31 Dil Factor 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compound* 1 PFBS (2M> 2 pphs (IS 2 PTC* (41 4 POSA (4M) % pros (4M) QUART SII MASS 299 39* 413 49 4 OOHCBHTRArtOtB OM-COLUNN PINAL KT BXP RT DLT RT RESPONSI (ng/nL) (ng/L) 3.353 3.12 4.003 4.794 4.111 3.394 3,791 3.992 4.74 4.140 >0.041 0.021 0.021 0.02 0.02 34994 214 1S139 3453 44194 0.74244 0.24701 0.43379 0.10754 0.4933 0.743(H) 0.247 0.434 0.10 0.493 QC Flag Legend M - Compound response manually integrated. <act Copy of 0ri3,,,a! ''i ( Date 001931 Report E02-0443 Data F ila i S\EttarttStartt\chSduci*jr. lSD020ei2A.bMJUDE0084.fl Tenn. River Valley Samples Pa( 2 2 PFHS <3OT> fmcoi'PyofOrigin# CsL tm T '--'niS 0X332 \ Report 02-0443 F il*: \SEtstarg*t\t*rttSc)wSdtid*,ir.iM)OZO812A.bMUl)E0O86.9 3 PFOA <413) Tenn. River Valley Samples Pat* 3 4 FOSA (498) B PFCS <499) ftn c i Copy o; Origyihn,ci n ( LllLiT- Fn;t!a! iteto 001933 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D0208l2B.b\DUDE0l27.D Page l Report Date: 29-Aug-2002 07:12 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Btstarget\target\chem\dudejr.i\D020812B.b\DUDE0127.D Lab Smp Id: 38028 Inj Date : 13-AUG-2002 10:35 Operator : cmc Inst ID: dudejr.i Smp Info : E02-0443-38028; Water Samples; non-GLP; 7/17/02; OK Misc Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020812B.b\D020812B.m Meth Date : 29-Aug-2002 07:08 dudejr.i Quant Type: ESTD Cal Date : 13-AUG-2002 06:44 Cal File: DUDE0106.D Als bottle: 41 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Ooapoundi 1 SPSS <i> 2 PPH3 (]>*) 3 p f o a (411) 4 POSA (4*1) S pros (4*1) QUANT SIO NASS 299 299 299 299 299 299 299 413 494 499 CONCENTRATIONS QN-COLUMN PXNAb RT BXP RT DLT RT R8SMNSI (ng/aL) (ng/aL) 3.31 2.497 3.073 3.777 4. OIS 4.249 3.777 3.942 4.741 4.140 3.394 3.394 3.394 3.394 3.394 3.394 3.791 3.9S2 4.744 4.140 -0.004 -0.497 -0.321 0.3S3 0.491 0.454 -0.014 -0.020 -0.027 -0.020 195304 943 9274 1440 402 439 7474701 34 4 43 02 4025349 7427444 2924.40 2934.44 2935.29 3935.33 2935.49 2935.70 392.549 314.424 302.105 341.743 3930 2940 2940 2940 2940 2940 392 344 302 342 !:>FIGVCti c#* 001934 Report E02-0443 Data F ila: SSEfcfcar{t\tarjt\ch*Sdudjr.l\D020812B.bMUDE0127,D Tenn. River Valley Samples Paja 2 2 FFHS (399) -.aut Cos j o; CiiginaJ Date 0193S Report E02-0443 Data F ila : S\Ettare#t\tarcttSchaaNdudtjr. 1SD020812B. b\DUDE0127. S 3 PFOft <4131 Tenn. River Valley Samples Pact 3 4 FOSA <4901 B FFOS <499) .'.VaICt LOfjy ;17Oriofngl fa/io/?-- 00X93G Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudej r .i\D02082B.b\DUDE0133.D Page 1 Report Date: 29-Aug-2002 07:12 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0133.D Lab Smp Id: 38036 Inj Date : 13-AU6-2002 11:41 Operator Smp Info : : mla E02-0443-38036; Water Inst ID: dudejr.i Samples; non-GLP; 6/20/02; OK Mise Info : Comment : Method : \\Etstarget\target\chem\dudejr.i\D020Sl2B.b\D0203l2B.m Meth Date : 29-Aug-2002 07:08 dudejr.i Quant Type.- ESTD Cal Date 13-AUG-2002 06:44 Cal File: DUDE0106.D Al s bottle: 43 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Cofound 1 m a (a> 2 anta (>) 2 PFQA (413) 4 POSA <> 5 p r o s (.) QUANT 813 HASS 399 299 399 399 399 399 413 499 499 499 CONC8NTRATXON8 ON-COLUMN FINAL AT SXP RT DLT RT HRSPONS8 (ng/aL) (ng/mL) 3.399 3.073 3.777 4 095 4.342 3.771 3.9C3 4.735 4.133 3.932 3.394 3.394 3.394 3.394 3.394 3.791 3.993 4.799 4.190 4.190 >0.009 -0.321 0.393 0.991 0.949 -0.020 -0.020 -0.033 -0.027 -0.339 302053 19005 9501 930 917 9071912 3927039 9559553 71*0357 909 2929.29 2934.99 2935.39 2935.99 2935.99 404.170 399.497 324.535 395.295 3071.35 2930 2930 2940 2940 2940 405 399 324 395 3070 Braci Copy or C 'jir-.. .XJLC initial 001937 Report E02-0443 Qt* F il : \\Ettar-t*tSt*rt*lSch**\du<iJr.iMW20812S.bM)UDE0133.D Tenn. River Valley Samples P*C*Z 1 PFBS (299> 2 PFHS <3> B cbctCopy of Orfclna' ! L LOi/joJfru 001938 Report E02-0443 Bata F it: S\EUtar*atVtarjtSc*aa\dudajr.iVJ>030812B.b\DUI>e0133.D 3 PFOA (413) Tenn. River Valley Samples B PFOS (499) CuiL. /^((isu .W; 001939 Report E02-O443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\dudejr.i\D02082B.b\DUDE0136.D Page 1 Report Date: 29-Aug-2002 07:12 3M Environmental Laboratory E02-0443, Tenn. River Valley Samples Data file : \\Etstarget\target\chem\dudejr.i\D020812B.b\DUDE0l3S.D Lab Smp Id: 38040 I.nj Date : 13-AUG-2002 12:14 Operator Smp Info : : mla E02-0443-38040; Water Inst ID: dudejr.i Samples; non-GLP; 6/20/02; OK Mise Info : Comment : Method : \\Etstarget\tarcet\chem\dudejr.i\D020812B.b\D020812B.m Meth Date Cal Date : : 29-Aug-2002 13-AUG-2002 07:C8 06:44 dudejr.i Quant Type: ESTD Cal File: DUDE0106.D Als bottle: 44 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist:all.sub Target Version: 4.12 Compound* 1 PFBfl Iasi) 2 FFH9 (3) 3 PPOA (411) 4 POSA (4SI) 5 pros (4*4) QUART 9H3 MA99 399 299 299 299 299 299 413 499 499 C0NCRNTRATX0M9 OR-COLORI* FINAL XT KXP RT DXiT RT R U PORSI (ng/aL) (ng/aL) 3.297 3.936 3.073 3.932 4.023 3.777 3.991 4.741 4.132 3.394 3.394 3.394 3.394 3.394 3.791 3.9ta 4.74 4.140 -0.007 -0.454 -0.331 0.434 0.439 -0.014 -0.021 -0.037 0.024 200230 5435 13145 10649 44$ 4244279 3997S4S 795SS92 776002S 2926.37 2936.47 2935.11 2935.33 2935.70 416.475 407.549 299.205 354.040 2930 2940 2940 2940 2940 416 404 299 354 issaci- Ccpy of Origina.' fox* fcs] Oato 0019^ Report E02-0443 D*ta F lit: SSEttarcttSttrcttSehtnSdudtlJr.lS0020812B*bSDUlOt36D Tenn. River Valley Samples p*gv 2 i 1t i ii t 1 PFBS <299) 'J;2CU/p vilgii^ teaj jai.- 001941 Report E02-0443 Seta F il t SSEtstarsetStarfat\ehe*SdudaJriSD024812BbSDUDE0136.D 3 PFOA (413) Tenn. River Valley Samples Pag 3 4 FOSA (498) 8 PFOS (499) BaciCo,'-;-.-.: f:-;- 001942 Report E02-0443 : ^ Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\l021112.b\ITCHY034.D Page l Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\1021112.b\ITCHY034 ,D Lab Smp Id: 0443-WB-l Inj Date : 12-NOV-2002 13:40 Operator Smp Info : mla : E02-0443-WB-l; Water Blank; Inst ID: itchy.i MeOH Extract; 21 Oct 02; MLA. Misc Info : Comment : Method : \\Etstarget\targBt\chem\itchy.i\I021ll2.b\I0211l2.m Meth Date : 13-NOV-2002 09:IS itchy.i Quant Type: ESTD Cal Date 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle: 21 Dil Factor: 1.00000 .Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compound* i 1 pros U*J 2 PFH8 <3> 3 PPOA (411) 4 TOSA (>> S PPOS (4) Q vw r axe HASS 39 399 399 399 413 413 49 499 GOMCmZIUiTZONS OM-OOUJMM fimi RT RXP RT DLT RT RESPONSI ing/mh) (ng/mL) 3.421 3.353 4.129 3.940 4.039 4.341 4.157 4.209 3.422 3.422 3.422 3.130 4.020 4.020 4.157 4.199 -0.001 -0.170 0.707 0.010 0.019 0.320 0.000 0.010 37974 7025 7365 2S41 13412 10374 1927 70922 0.55035 932.500 933.490 0.13306 744.74 745.050 0.17215 1.09119 0.560 933 933 0.133 746 745 0.172 1.09 ~T/r ClttL jj/tnSfia] 001943 Report E02-0443 Data Fila: \\Efc*tarct\tarefc\ch'atchy.M021112.h\ITCHY034,D Tenn. River Valley Samples 2 PFHS <399> Ion 399,00 i 1.00 I/rl l "1A 0 .9 0 11 / g .SO %$F0,70 ( \ a / > 0.60 // ^ 0 .5 0 -3-.4-0---3-.6-0 Hi3n_.80__4.0_0__4.20--- wacrcupy:;.- _j; is ir V *f ' 01(1944 Report E02-0443 Sa ta F ila i S\E ttariatStarcatSehai\lte*m ,i\IM 1112.bSITCH Y034.D 3 PFOA (413) Tenn. River Valley Samples Pag 3 4 FOSA (499) B PFOS (4 9 9 ) 4 . ^ lief6101*4345 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\1021112.b\ITCHY035.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file \\Etstarget\target\chem\itchy.i\l02iii2.b\ITCHY035.D Lab Smp Id 0443-WB-2 Inj Date 12-NOV-2002 13:51 Operator mla Inst ID: itchy.i Smp Info E02-0443-WB-2; Water Blank; MeOH Extract; 21 Oct 02; MLA. Misc Info Comment Method \\Etstarget\target\chem\itchy.i\I021ll2.b\I021112.m Meth Date 1 3 -Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle 22 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all,sub Target Version: 4.12 Cowpound* 1 ? n a la) a PPHS <> a PPGA (413) 4 POSA (491) S PPOS (499) q u a n t sicNASS 39 39 399 399 39 413 413 49 49 coN cnm urxoM S O N -counuf FINAL RT RXP RT DLT RT RESPONSI (ng/nL) (ng/mL) 3.411 3 .353 4.119 3.930 3.491 4.039 4.34 4 .47 4.319 3.433 3.433 3.423 3.930 3.930 4.030 4.020 4.997 4.199 -0.011 -0.170 0.997 0.000 -0.33 0.009 0.32 0.000 0.020 -32544 5959 3295 3529 1344 14593 12055 3453 42341 0.39735 933.530 933.507 0.15642 0.10734 0.04324 744.949 0.19434 0.23530 0.397 934 934 0.155 0.107 0.0432 745 0.194 0.236 001946 Report E02-0443 Data F ila t \ \E ttarja tS tar*atSch aa SI tehy. 1S1021112.bSITCHY03S. D Tenn. River Valley Samples Paca 2 2 PFHS <399) & a ci Copy x Odgi J t 001947 Report E02-0443 Data F ila : S \ E t * t * r tchy, iSI021112.bSITCHY03B.D 3 PFOA (413> Tenn. River Valley Samples Pat* 3 4 FOSA <496> H<acf Copy of Original 001948 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\itchy.i\I021l2.b\ITCHY038.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\l021112.b\lTCHY038 .D Lab Smp Id: 0443-38044-1 Inj Date 12- NOV-2002 14:23 Operator : mla Inst ID: itchy.i Smp Info : E02-0443-38044-1; SL-1; MeOH Extract; 21 Oct 02; MLA Mise Info : Comment : Method \\Etstarget\target\chem\itchy.i\l02lll2 .b\I021H2 ,m Meth Date : 13-Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date : 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle: 25 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub v** Target Version: 4.12 Compound* 3 t 1 m a (299) 2 PPHfl (399) 3 PPOA (413) 4 POSA (494) 5 PPOS (499) QOJU9T 813 NWB 299 299 299 399 399 413 413 491 499 a a 1 a a a a a !1 a> 1 ; a RT BXP RT DLT RT RiaPOMSR a a a : a 11 a a 3.511 3.970 4.309 3.940 3.432 4.040 3.701 4.997 4.219 3.422 3.422 3.422 3.930 3.430 4.020 4.020 4.4C7 4.199 0.049 0.544 0.447 0.010 -0.394 0.020 -0.319 0.020 0.020 313459 2S93 4144 132C3S 14909 295590 4211 1250415 2745277 COMCSMIMTIONB N-C01HN PINAL (ng/aL) (ns/b) ....... 10.5974 933.427 932.592 2.71999 0.49492 14.1949 745.144 10.4 934 934 2.73 0.445 14.2 745 29.4711 47.4542 29.7(1*) 47.4(H) QC Flag Legend M - C o m p o u n d re s p o n s e m a n u a lly in t e g r a t e d . B a c i Copy or Original 001949 Report E02-0443 Sata Fil*; S\Et*fcarffcSfcart*tXeh\itchy,l'\lG2111.2.bMTCHY038,D Tenn. River Valley Samples Pat* 2 1 PFBS <299) 2 PFHS <399) wtOWKOrsi 001950 Report E02-0443 lu t * Pi U t SSEt*t*rt*tSt*rtt\ch*nSi teTia.iSI*2H12.b\ITCHY038.D Tenn. River Valley Samples P l{ 3 4 FOSA (4 9 8 ) B PFOS (499) oeci Ccay of Orig na* C `'mna-:j x 'M--j:.;- p -' U01S51 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\l021ll2.b\ITCHY040.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\l02lll2.b\ITCHY040 .D Lab Smp Id: 0443-38044-2 Inj Date : 12-NOV-2002 14:45 Operator : mia Inst ID: itchy.i Smp Info : E02-0443-38044-2; SL-1; MeOH Extract; 21 Oct 02; MIA Mise Info : Comment : Method : \\Etstarget\target\chem\itchy.i\I021112.b\l021112.m Meth Date : 13-Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date : 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle: 26 Dii Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub 4II Target Version: 4.12 COtKBRMTIOMS QOAMT SZG OM-COLONM PIMM. Compound MASS K t BXP RT DLT RT RSSFOS08 (ng/ab) (ng/aL) l pros <2l 2 PFHS (3M> 3 p p o a (413) 4 POSA (4M) S PPOS (4M) 299 3.432 3.422 0.010 393409 10,5904 10.4 299 3.970 3.432 0.549 1970 933.945 934 299 4.309 3.422 0.447 <2491 1.29471 1.27 399 3.940 3.930 0.010 111901 2.93937 2.94 399 3.432 3.430 -0.394 13479 0.37475 0.377 413 4.040 4.020 0.030 290003 14.1091 14.1 413 3.711 4.020 -0.309 9504 745.093 745 494 4.9S7 4.497 0.020 1341450 32.3550 32.4 499 4.219 4.199 0.020 2445124 70.2517 70.2(H) QC Flag Legend 3 M - Compound response manually integrated. 43 ../icfiru 001952 Report E02-0443 Dt F i U s SSEt*fcarstNfciri*fc\ch*Mtehy.l\I02ill2.bMTCHV040.J) Tenn. River Valley Samples PH 2 2 PFHS <399) Exact Copy o; Origini. > fffifeaJ fe T 001953 Report E02-0443 D a ta F ila : S S ts ta rc a tS ta rta tS c h a a M te h y .lS I0 2 1 1 1 2 .b M T C H Y 0 4 0 .D 3 PFOft <413 Tenn. River Valley Samples Pac* 3 4 FOSA <498 B PFOS (4 9 9 ) ' i-V v ;>? Orfgna C M C ljiU u 0019jp4 Report EQ2-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021ll2.b\ITCHY042.D Page 1 Report Date: 19-NOV-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\I02ili2.b\lTCHY042.D Lab Smp Id: 0443-38044-3 Inj Date : 12- NOV-2002 15:07 Operator : mla Inst ID: itchy.i Smp Info : E02-0443-38044-3; SL-1; MeOH Extract; 21 Oct 02; MLA Mise Info : Comment : Method : \\Etstarget\target\chem\itchy. i\I02H12.b\I021H2 .m Meth Date Cal Date : 13-NOV-2002 : 12-NOV-2002 09:16 12:14 itchy.i Quant Type: ESTD C-al- File: ITCHY026.D Als bottle: 27 Dii Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 i t A Oompounda 1 m a (3) 2 FFHS ( 3 * 9 ) 3 n o A (4X3) 4 POSA (4 9 ) 1 5 ppoa (499) QUANT IO MAS 3 299 399 399 413 413 494 499 CONCBMmXXONS oH -counm RT BXP XT DXiT XT KX S90N 8I (ng/*L) v in a l (ng/.L) 3 .5 3 1 4 .2 3 .5 4 0 3 .4 3 2 4 .0 4 0 3 .7 0 1 4 .5 5 7 4 .2 1 3 .4 2 2 3 .4 2 2 3 .5 3 0 3 .5 3 0 4 .0 2 0 4 .0 2 0 4 .5 7 4 .1 9 0 .1 0 9 Q .577 0 .0 1 0 -0 .3 9 5 0 .0 2 0 -0 .3 1 0 .0 2 0 0 .0 2 0 452034 50024 111724 19590 253343 5515 1033771 2109105 13.4994 0.59957 2.45445 0 .4 9 9 5 7 13.7201 7 4 5 .1 4 9 34.4535 50.3521 13.S 0 .9 0 0 2 .4 5 0 .5 0 0 1 3 .7 745 24.9(H ) 5 0 .4 QC Flag Legend M - Compound response manually integrated. feast &jpv ::: u*rOii-. Cvnc /j/./.fu 0019S 1 Report E02-0443 Sat* Fila: SSEtt*rjt\t*rjet\oh*nSitchy.lSI021112.bSlTCHY042.D Tenn. River Valley Samples PH Z 2 PFH8 <399> ^ O ricin a] L m ( ll/jAJt* 0019(16 Report E02-0443 Data F ile : V \ E t*t` t*tStr{tSch*\ltcha.l''I02 1il2 .b M ;T C H Y O 4 2.I> 3 PFOA <413) Tenn. River Valley Samples 4 POSO <49B> B PFOS <499) ; '.* V.'lw'lli, n c ^ IS-J&lsi* t;ll :?*! 001957 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Etstarget\target\chem\itchy.i\I021l2.b\ITCHY046.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\l021ll2.b\lTCHY046.D Lab Sirro Id: 0453-38045-1 Inj Date : 12-NOV-2002 15:50 Operator : mla Inat ID: itchy.i Smp Info : E02-0443-38045-1; SL-3; MeOH Extract; 21 Oct 02; MLA Misc Info : Comment Method \\Etstarget\target\chem\itchy.i\l0211l2.b\l02ili2.m Meth Date 13-Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle 31 Dii Factor 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 1 PPBS *> 2 PPHS (3> 3 PPOA (413) 4 P O M (4M) 5 PP09 (433) QOMfT SIG NASA 39 39 399 39 39 413 413 413 499 49ft 499 49 CONCBNIMSlOm OH-COLOMM PINAL RT BXP RT OUT RT RtSPOtlH (ng/aU (ng/*M 3.413 3.950 4.30 3.940 3.443 4.040 3.711 4.37 4.ft>7 4.59ft 4.31 4 569 3.433 3.422 3.422 3.030 3.930 4.020 4.020 4.020 4.947 4.967 4.199 4.199 >0.010 0.529 0.997 0.010 >0.399 0.020 -0.309 0.359 0.020 -0.26 0.020 0.369 325254 2272 17131 13341 750 49049 9113 7941 49310 5113 4194S4 11902 9.99037 933.634 933.210 0.36520 0.26651 1.92935 745.115 745.191 1.24672 0.24754 9.07917 1354.25 9.ft 934 933 0.365 0.266 1.93 745 745 1.25 0.249 9.09 13S0 Gre. llltl-- ,.:a T fe o 001958 Report E02-0443 Data F ila i SSEfctarcatStartatSehai\itchy,iM02U2.bM.TCHY046,I> Tenn. River Valley Samples Paca 2 2 PFHS <399) an" -^nsl ) 001959 Report E02-0443 Hat F lU t V sE tlw ttS trtt\ ch **Slte h a.lM 0 2 1 il2 .b SIT C H Y 0 4 t.B Tenn. River Valley Samples P l( 3 4 F08A (498> S PFOS (499> SZ2 j-ir; n, 001960 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\lTCHY048.D Page 1 Report Date: 19-NOV-2002 14:49 3M Environmental Laboratory Data file \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY048.D Lab Smp Id 0453-38045-2 Inj Date 12- NOV-2002 16:12 Operator mla Inst ID: itchy.i Smp Info E02-0443-38045-2; SL-3; MeOH Extract; 21 Oct 02; MLA Misc Info Comment Method \\Etstarget\target\chem\itchy.i\l021112.b\I021112 .m Meth Date 13- Nov-2002 09:16 itchy.i Quant Type: ESTD Cad. Date 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle 32 Dil Factor 1.00000 integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Compounds 1 PFBS (2*1) 2 PFHS **) 3 PPOA (411) 4 POSA (41) s p ro s (411) QUANT SXQ NASS 399 399 399 399 399 399 413 413 493 499 499 cohcbwiraxxons ON-COUMN FINAL RT EXP RT DOT RT RBSFONS8 (ng/L) (ng/aL) 3.431 3.940 4.31 3.940 3.441 4.039 4.049 3.710 4.334 4.417 4.339 4.543 3.433 3.433 3.433 3.330 3.930 3.930 4.030 4.030 4.447 4.367 4.199 4.199 0.001 0.633 0.396 0.010 0.399 0.199 0.039 -0.310 0.019 0.350 0.030 0.369 305101 7199 12339 11469 19109 10665 60331 754 44173 4067 323943 6925 9.29129 933.495 933.333 0.33496 0.46773 0.30767 2.61356 745.135 1.19716 0.22171 6.94S39 1354.37 9.29 933 933 0.335 0.469 0.309 3.62 745 1.30 0.322 6.34 1350 UQ1961 Report E02-0443 Data Fllaj SNEtatar|atStartat\ehMSitchy.lM021112.bSITCHV048.9 Tenn. River Valley Samples Pt2 2 PFHS <399) CM . liHH j 001962 Report E02-0443 Data Fil.! S\Etit*ret\UrttSchnMtcha.iM021112.bSITCHV048.D 3 PFOA (413) Tenn. River Valley Samples 3 4 FOSfl (49S) C PFOS (499) C Jt '/cfi 001963 Report E02-0443 Tenn. River Valley Samples Data Pile: \\Btstarget\target\chera\itchy.i\I02lll2.b\lTCHY05l.D Page 1 Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\l02lll2.b\ITCHY05l.D Lab Snip Id: 0453-38045-3 Inj Date : 12-NOV-2002 16:44 Operator : mla Inst ID: itchy, i Strip Info : E02-0443-38045-3; SL-3; MeOH Extract; 21 Oct 02; MLA Misc Info : Comment Method : \\Etstarget\target\chem\itchy.i\I0211l2.b\I02lll2.m Meth Date : 13-NOV-200209:16 itchy.i Quant Type: ESTD Cal Date : 12-NOV-2002 12:14 CalFile:ITCHY026.D AlS bottle: 33 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Oowpomid* 1 PPB3 ttll) a p p H s (31*) 3 PPQA (33) 4 POSA (4*1) 5 PP03 (**) QUANT SID NASS -- 239 239 299 399 399 399 413 413 413 499 499 499 499 11 81aa 1 1 11t RT -- 3.402 3.950 4.309 3.720 3.431 4.039 4.049 3.711 4.319 4.997 4.599 4.229 3.930 BXF NT 3.422 3.423 3.422 3.130 3.930 3.930 4.020 4.020 4.020 4.967 4.967 4.199 4.199 OLT ST -0.020 0.529 0.997 -0.110 -0.299 0.209 0.029 -0.309 0.3S9 0.030 -0.279 0.030 -0.2C9 RESPONSE ........ 364599 2069 19956 12125 2424 11470 54999 12405 12569 65769 4044 420495 4S04 C0MC8MTRATI0N9 ON*COLUMN PINAL (ng/aL) (ng/aL) as s ....... 10.0353 10.0 933.642 0.00434 934 0.00434 0.33906 0.339 0.13055 0.130 0.32499 0.32S 2.32242 744.930 2.32 74S 744.915 1.65159 745 1.65 0.22117 9.12623 1354.43 0.221 9.13 1350 i Jr: 001964 Report E02-0443 Data Filai S\EttarcatStarcptSch*MMtchy.iSI021112.bSITCHY061.D Tenn. River Valley Samples P*C 2 2 PFHS <3995 '/-/h / t u __ 001965 Report E02-0443 Data Filt SSEtstarc*tStarc*tSehMSitcy.iSI021112.bSiyCHY081.D 3 FFOA <413) Tenn. River Valley Samples 4 POSA <498> 8 PFOS <499) Q01966 Report E02-0443 Tenn. Rive'Valley Samples Data Pile: \\Etstarget\target\chem\itchy.i\I02lll2.b\ITCHY053.D Page l Report Date: 19-Nov-2002 14:49 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\l02lll2.b\lTCHY053.D Lab Smp Id: 0453-38045-MS(3) Inj Date : 12-NOV-2002 17:05 Operator : mla Inst ID: itchy.i Smp Info E02-0443-38045-MS(3); SL-3; MeOH Extract; 21 Oct 02; MLA Mise Info : Comment Method \\Etstarget\target\chem\itchy.i\l021112.b\I021112 .m Meth Date 13-Nov-2002 09:15 itchy.i Quant Type: ESTD Cal Date 12-NOV-2002 12:14 Cal Pile: ITCHY026.D Als bottle 34 Dii Factor 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 Compounds 1 P P M (299) 2 PPHS (399) 3 PPOA (413) 4 POSA (49) 5 PROS (499) QUANT 310 NASS 299 299 299 399 413 413 499 499 499 CONCENTRATIONS ON-COLUNN PINAL RT EXP RT OIiT RT RESPONSE (ng/uL) (ng/aiL) 3.422 3.940 4.299 3.920 4.020 3.991 4.947 4.199 3.920 3.422 3.422 3.422 3.930 4.020 4.020 4.997 4.199 4.199 H Ml e 0.000 0.997 -0.010 0.000 -0.329 0.000 0.000 -0.279 1540799 9713 119799 1995S5A 991399 9719 1092919 1295395 2917 45.9349 933.509 2.99093 37.9097 40.2752 745.250 25.9793 29.9191 1354.45 45.9 934 2.95 37. 40.3 745 25.9 29.9 1350 001967 Report E02-0443 SaU F il : NNEtatarjtStartt\chSitchy, iS 1021112.b\lTCH053. B Tenn. River Valley Samples P a (* 2 2 PFHS <3W > ' ''" `k O C Oriain! 001$68 Report E02-0443 Data Fila$ SSEtstarc*tStiPt*tSchMMtehy.iM021112.bSITCHY0S3.D 3 PFOft (413) Tenn. River Valley Samples Pag* 3 9 PFOS < 4 > 001969 Report E02-0443 Tenn. River Valley Samples Data File: \\Etstarget\target\chem\itchy.i\I021112.b\lTCHY05S.D Page l Report Date: 19-Nov-2002 14:50 3M Environmental Laboratory Data file : \\Etstarget\target\chem\itchy.i\l021112.b\ITCHY055.D Lab Smp d: 0463-38046-1 Inj Date : 12- NOV-2002 17:28 Operator : mla Inst ID: itchy.i Smp Info E02-0443-38046-1; SL-2; MeOH Extract; 21 Oct 02; MLA Mise Info : Comment : Method : \\Etstarget\target\chem\ itchy.i\I021H2 .b\I021H2 .m Meth Date : 13- Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date : 12-NOV-2002 12:14 Cal File: ITCHY026.D Al s bottle: 41 Dii Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.12 R11 I Compounds i pros (39) 2 pros (399) 2 PPQA (413) 4 POSA <49) 5 PPOS (499) QfOHr SIG HASS 293 299 299 799 299 413 413 411 49 49 . H. .T. 3.S31 4.01 4.319 3. 40 3.423 4.040 3.711 4.97 4.219 3.930 HXP KT 3.422 3.422 3.422 3.930 3.930 4.029 4.020 4.997 4.199 4.19 DLT HT 0.109 0.CS7 0.997 0.010 -0.409 Q.Q2Q -0.309 0.020 0.020 -0.299 RSSPOtfSB 327390 SO09 043 173S3 14192 5337S 72S9 120497 417239 11992 C O M C BN T O A rXO N S OM-C0L0HN PINAL Ing/mL) Ing/mL) 9.9425 933.959 33.471 0.4514 0.39350 2.23055 745.219 2.92155 9.04935 1354.25 9.94 934 933 0.451 0.393 2.23 74S 2.92 9.05 1350 001970 4 0} Report E02-0443 Data F il; \\EttaritStart*t\ohiSitcha.iM21112.b\lTCHY058.D Tenn. River Valley Samples Paca 2 J i r 001971 Report E02-0443 lUt* FU *t VsEtst*rt*t\tM>ttSohM>Sitehy.tsI021112.bSITaQe.S 3 PFQft (413) Tenn. River Valley Samples P** 3 4 FOSA <498) B PFCS (499) ?%' WO 001972 Report E02-0443 Tenn. River Valley Samples Data File: \\Btstarget\target\chem\itchy.i\I021112.b\lTCHY057.D Page 1 Report Date: 19-Nov-2002 14-.50 3M Environmental Laboratory Data file \\Etstarget\target\chem\itchy.i\I021112.b\ITCHY057.D Lab Strip Id 0463-38046-2 Inj Date 12- NOV-2002 17:50 Operator mla Inst ID: itchy.i Smp Info E02-0443-38046-2; SL-2; MeOH Extract; 21 Oct 02; MLA Misc Info Comment Method \\Etstarget\target\chem\itchy.i\l0211l2.b\I02lll2.m Meth Date 13-Nov-2002 09:16 itchy.i Quant Type: ESTD Cal Date 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle 42 Dil Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.12 Coapounds i w na ( 3 WHa (3**) 3 PPOA (413) 4 FOflA (4M) 5 w o a (4> QOJun s i a Musa 39 299 299 299 399 399 413 413 413 494 499 499 CONCENTRATIONS ON-COLUMN fin a l RT XXP XT DLT RT X B S N M a i (ng/aL) (ng/t) 3.511 3.940 4.019 4.319 3.440 3.432 4.040 3.711 4.349 4.447 4.229 3.930 3.422 3.422 3.422 3.423 3.430 3.430 4.020 4.020 4.020 4.447 4.19 4.199 0.049 0.534 0.447 0.497 0.010 -0.394 0.020 -0.309 0.349 0.020 0.030 -0.249 232749 2454 S27Q 7437 14434 10544 35197 7429 12091 103403 393450 12974 4.14254 933.425 933.550 933.444 0.47471 0.30507 1.20373 745.199 744.944 3.52745 4.49144 1354.23 4.14 34 934 933 0.47S 0.305 1.30 745 74S a . 53(H) 4.49 1350 QC Flag Legend M - Compound response manually integrated. o. V |jf . ' J '"f v r/giriai Ja& 001973 Report E 02-0443 Sata F ilt SSEtstargatNtargatSchaaSitchy.iM421112.bMTCHY057'B Tenn. River V alley Samples Pa 2 C n i 001974 Report E 02-0443 Bata F ila : SSEtstargatStar(atSchmSit6hy.iM021112.bMTCHY0S7.D 3 PFOft (413) Tenn. River Valley Sam ples Pag 3 4 FOSA C498) B PFOS (499) 'vCiCWoiOr}3ina! 0019^5 Report E 02-0443 Tenn. River Valley Sam ples Data File: \\Etstarget\target\chera\itchy.i\I02lll2.b\rrCHY059.D Page 1 Report Date: 19-NOV-2002 14:50 3M Environmental Laboratory Data file \\Etstarget\target\chem\itchy.i\I021ll2.b\ITCHY059 .D Lab Strip Id 0463-38046-3 Inj Date 12- NOV-2002 18:12 Operator mla Inst ID: itchy.i Smp Info E02-0443-38046-3; SL-2; MeOH Extract; 21 Oct 02; MLA Misc Info Comment Method \\Etstarget\target\chem\itchy.i\I021ll2.b\I021ll2.m Meth Date 13- NOV-2002 09:16 itchy.i Quant Type: ESTD Cal Date 12-NOV-2002 12:14 Cal File: ITCHY026.D Als bottle 43 Dil Factor 1.00000 Integrator Falcon Compound Sublist:all.sub Target Version: 4.12 Compound 1 m s US 3 PFHS U s > 3 PFA (413) 4 POSA (4M) s p r o s (4SS) QUANT SZ6 HASS 39 399 399 399 399 413 413 413 490 499 49 coM cra nuT ione ON-COLUMN PINAL RT EXP RT DLT RT RESPONSE (ng/aL) (ng/aL) 3.541 4.090 4.319 3.050 3.433 4.040 3.711 4.369 4.007 4.339 3.930 3.433 3.423 3.423 3.030 3.030 4.030 4.020 4.030 4.067 4.199 4.199 0.119 0.660 0.097 0.030 >0.390 0.020 -0.309 0.349 0.020 0.030 -0.26 420079 6904 11502 25494 17014 40917 ' 0500 11004 133252 470507 14760 11.6624 933.503 933.369 0.62654 0.44417 1.52653 745.145 744.964 3.21070 10.5037 1354.1 11.7 934 933 0.626 0.444 1.53 745 745 3.22 10.5 13S0 B ract Copy x w . --.; mL Dfssu 00^976 Report E02-0443 Data F ila : S\EtstarcatStartatSchaaSitehy,iM0211t2.bSITCHY059,D Tenn. River Valley Samples Pa(t 2 2 PFHS <399) t 001977 Report E02-0443 Tenn. River Valley Samples IUU F ilt SSEUtar?at\tarstSchmSltchu.tSI0ailia.bSITCHY0S9.S 3 PFOA (413) pe 3 4 FOSA <496> 8 PFOS <499> 1' (ki',y f; Orioii1?' 001978 Report E02-0443 Tenn. River Valtey Sam ples Attachment D: Sample Prep Sheets, Test Substance, and Test System Information 001979 Report E02-0443 Tenn. River Valley Samples coi s tid/i 7 _l j / y H3- gy^C Ter,:Cvntrifuo* >0: RCF/PRM Readouti3coo 3 --- Temp " C A Z L c o n T/Q ji? .3 o < w i (a i l Y i t d - C t t t Col 7 Spiking Standard 1 0 * ~~l7 _ Approxim ate Cone. 1 p jd rv * Am ount added ^ 0 C. T/ori n - o a . t m (p / H ; /t f k i : w Col i ' T hi*-Mbs' ^ l ^ J a U sio9' a ^ c G e B^RM Readout ^ 0 .*^ Minute IT S _______Temp *C /Q O coin i? n? /{fl-CW l l coi iaTmnlf.giki. It nX i o i f j vtc WaterID M ill. -fr^ W ^lll? 001980 Col 13 T/DP I n ICi ColH T/DPO.AT/W. fa I lOl . MeOH10: TN-A 4 5 3 f t \fil ^n f iff? Q Tf.flmi/*i-'y/f> jrr.-Ttr+JrJ cil`1 Page 1ote'(y^.1l>Anr C-itT' -*1W- !!<>*>&) . /* . (LiD'fM ` ** IlfttPi *'''V Report E02-0443 Tenn. River Valley Samples Lab Request i Tennessee River Valley Samples Sample Location 1, Catfish VI. MaMKlige at SOMrcf1er 9 I 1 SL-1. C-1-1 SL-1. C-1-2 S l-1 . C-1-3 n I 1 i X I k s1 5 . 5 /V -- 7 5 T 3 ii 1 ! illl i j li 3 7L A _r _ i Is I ill| i i l 7 j i ii i 1__!S _ A is /t r / / - L r r_ I is ii 14 \ ,1 $ Hs SL-1.C-2-1 $ , < p s r SL-1. C-2-2 SL-1, C-2-3 SL-1. C-2-MS L -- n u .. , a SL-1. C-3-1 A. S L-1.C -U T 3 \ ES 1 H S L -1 ,C -3 -y \ S L-1.C -4-7 SL-1. CM -J -- iZ 1 "1 J .O D .'i -S c B 1 _s: H ir N _ SL-1, C-4 ~ t .____. S L-1.C M -M S SL-1. C-S-1 > d ? 3 0 fe ! i V X ^3 Ki "< SL-1. C-5-2 _ V SL-1. C-5-3 -- ~V 53 .3 SL-1. CM-1 li r 1 11 l . l_ > m Wt _ > A s. 2 VJ \ 4 " 53 . 2 " T . ^. .1 d/ 5 z X rv V 4: s [C 4 " --s .2 _ _ 4 . -L- 3: -L S T] . Z _w ^3 O V _ a i. 1 3 _. 1 1 . IEL / M/ . 5 . __5 ___ !9 SL-1, C-8-2 SL-1. C-6-3 SL-1. C-e-MS SL-1. WB-1 SL-1. WB-2 SL-1, SB-1 SL-1. SB-2 I j --- -- n.-- , n 7-- 3 2 . J )- s IZ-- t Lia i2A i- NL -- ~ t \U - 0 --- ___ j '.A r~ ' "3 ^e r r [n 1 ---- r~ r -- V - r-- ~ _ - IlZ - - 50*coi2Tfl m n lOoo >fi*i./*T**-.n*!f l i . j . ,, Vji>rCiA\A ' . Balance ID t t 9 / H Tube tvoe/slza f V y f r y / <- C ol Shaker ID J X L S L C _______ Equj Start I/ J f r ^ L ^ C cd 3T/tmp'.^ffyvr. /a 11 iO-LAA-C Equil Stop T r t M jllS a r liia ' fm t 11 * i W ater ID M U V . - f o T f i C ^ i A col 4 ___von l-.l'pmh ttl SX. ( f h --wHmL Cois nonT to . > I f t en. CMC. Centrifuge 10:, 3RCF/PRM Readout ccd Col non*?.' V/Vrv ( a l i i iC D r.t '~ 'c Tno*C f~7 C o l7 n n iw in ^a ie n rt.n lm e r~VJ6 3 ~ 7 7 Approximate Clone f ^ Amount added__ICOy L , non n.ocn-v la ; /T ) C o l? : T M A -W ^ S ' SM Environmental laboratory Col to non h n r lO.a-rnng. CenklkiaeIpT T "Q ~ 2 -__________ 0^PR M R6doul3 C fil^ I i _____ __Temp c 5 3 co in n o n (j >iy >^ y rC. co tnnontMip.vx, h in 2 (_ waterIDIU'iU i-pi T H wAift Col 13 T lD flMO|'i<n f r r l cl iC X -O ^ cot14nonl',to^iv IcAc\ il, 001981 MeOHID: TN-A, 4 3 - 0 Mi! O u d - ^ n"(U //J(J^) L i t t rr7ry-/i(fJ.'J f t i ft ! Y "+'L < *r - * 0 4 - 0 1 O tt 0 1 Page 20160) A f ' 7*1,1r, V V } -/* 'X , < \ _ . T r . '_ t A * , , . V H f t t t y !/ ;/ t * - V "W y v ;* ft Report E02-0443 Tenn. River Valley Samples Lab Request: Tennessee River Valley Samples Sample Location 2- Large Mouth & Location 3-Small Mouth 9 ! 1 SL-2. LM-1-1 SL-2. LM-1-2 SL-2. LM-1-3 w I t 1 i i 1 *, \ J i. . l i 1 2 9 4s W `` J A * "7q r MS -------- . !fi li 1 Jl y V il il 1r 1 %1 s II 9 ]B T II S f li i l li J ii l i 1 i 10 11 12 19 14 t _J_ vr " 7 ~ r v /< i .! 19 SL-2. LM-2-1 J i g V h } I J SL-2. LM-2-2 _ __ 1 _ ! SL-2. LM-2-3 SL-2. LM-2-MS __ -- si i 3 ._ 4 r? _ .3 .X _J SL-2. LM-3-1 J a t J T j SL-2, LM-3-72 SL-2. LM-3-/J -- SL-2, LM-1-1 C. OTtfo7 SL-2. LM-4 -2 rv. s n SL-2, LM-4 - SL-2. LM-4-MS -- -- - /oUHc1SL-3?&?1-1 SL-3?Jhft-2 __ a JC - c" i ~ 1 \3 tv " _ vV 7<t3 1-- S'S, ",," s 0 J oV l ^5 T\** _ i . 1 5 2 z V 3 Tn _ ~ 313 33 %' "3 3 _*S_ 0 . o I P I >5 -aJX t- -S TZ IE I ' 3 O I j V . m i . 1 ? ~_s - L S ~ m m i i L 3 'S t, s^! SL-3,^M ^-3 rS L-3.^lt-M S __ ----. SP L iL d L Irp L HT ! \ l> L 3 P 3 Z3M y. V 'r5TM f *\fS*i7j* yc L < C o l2 T / D / l fa / n / G - ir X f Col 9 Shaker ID O S T -- Balance ID ^ lO O __________ Tube tvne/tee \tn \l -Vi | 5?s. L EquM Start T/O /l IK U fr, lb / f r T X l x A C ol 3 T im U M d /h v f t l 1 1 I O X C/ r l WaterID H ; 'ii; - a T h e B u s Equil S lop T/DA/ r cU vw L / IV / > fl-L > v J C ol 10 T/D /l iJ lS s jh ^ t i H ^ I h Q ftV C . c o la t /d /i ft'.O Q ^ Irv U / O fS l * rJ I^ M d /M llln a ^ 0 CentnfuoelO: 1 t 2 - . c o i s Tim 7 - l a i l X i D 3 ct v \( rfCF/^RM ReadoutA D Minuta L Q Tamo *C 3 o t Centrifuga ID: | C l C o in T/D /i k?` s te / I t \ X Ch rC RCF/PRM Readout: Ulnute 0?._______ Temp *C / 7 C ol 12 T /D /l t i r I 2 / f iA C ol 6 T/D /l 9 .` 3 0 tte n ( i ! i K l tT)- CK* < W ater ID H \ U > T r r ^ lu & Col 7 Spiking Standard ID # 0 . 3 l ) ^ . i - 7 1 C ol ? T/D /l l l g L / / a J C - / / 4 w Approxim ate Cone. Am ount added; t*3L)<A -L- Col fp TM , /! / f 9 r a _ M r A * i4 T/D/l is /I ST / flL - C lK / 1 Cr-LC tf/n/oi l T T W A - W i f `'a/tnn L/t XO)- 3M Environm ental Laboratory M eO H ID : TN-A A p ' - I j L ' , . / j ^ C ^ Q O ( P L v A iiT ry^ ^ t | | /t f J y / ^ l/ i /IH- (flUfiBX (^J ) L j f t t* T yyt, r~p d tttb j 9h4ofl^1! *('' ,(<Mr rt "- ^ .3 *0 0 * 1 /.^ S fv ? tv Report E02-0443 Tenn. River Valley Samples LabRoquoU: M Tennessee River Valley Samples S a m p la L o c a tio n 2 , C a tfis h fi i t SL-Z 0 1 -1 SL-2. C-1-2 SL-2. 0 1 -3 I 5T 1 1 1 1 1 li i ili 7I li 23 li 41 li .1 3 o * 3 -fc > -A - V 1 -- SL-2. C-2-1 3 e & T j SL-2, C-2-2 SL-2. 0 2 -3 -- SL-2. 02-M S -- -- 1 SL-2. 0 3-1 i f l l l l q C - SL-2. C - l- r j SL-2. C -3 -/ -- -- Ve_ IN. S L -2.C -4 -/ A o m SL-2. C -4-J -- SL-2.C-4 -1 ------ SL-2. C-4-US -- ^_ . 7" '- - \ ^-- V. \ X SL-2. 05-1 SL-2. C-5-2 co tti -------- d '5 V .^ N s. SL-2. C-5-3 -- _v _ : > a '^ 5 ' SL-2. C-S-1 J S W f' SL-2. 0 6 -2 v< " SL-Z 0 8 -3 SL-2. C-6-MS ---- F -I I v ~ -4 - . il SL-2, 07-1 U 1 T S L . 1 w A t l: jH K 3E _ ~__- i. V. p 3 0 SL-Z 0 7 -2 SL-Z 0 7 -3 SL-ZW B-1 SL-Z WB-2 SL-2. SB-1 SL-2. S8-2 -----a -------- -- /V O r-- ti ir T JI " "1 13 -- ~t EVL T i 1 1 ?1 li l IliI I i l Wl i a ta T HI ti * 12 13 14 rA 1 * 1 t . --{ - e Iy * fR f S is 5 r q ~T I s '3 .1 2 M 1 S _ -q / l( . . 2 'N HI J S i1 -o 1 - : j s _ ._ a 3 % !1 7 HJ -1 ~n X_ r " s IF . 5 T j ' L" X 1 P> '_____ > ~ L v "1 il A \_ A \__ NP ---- ^ . 1 3 5,__r * ~" ,, ~ T i P 1T i C o U T flM .U-iD-f& .C&'K C ol ShakarIP O S ~ ~ J _______ ! 12 Satanca ID P C D ________ Tub * Equi Start T/DB U ` W n / It T / - O - X , c o t s t /o/i jy ^ Q p n n [ f i h i C iX C K ^ - W aterID ~G -T C C ^ - l^ Col 4 T /O /ljfC P ^ V rt 1 0 / H / C kO ^S Q aadH aiH na ( j Col 5 T/OB i ( V i C O - C**-C. Equi Stop T/O BlfATfr , Ip i li7f i ) - 0 \.l Otrv.b-nw. c o n o t/db II iS jv n j f u fi; m i C iW CanUUuoi IH; \ f\~Z--___________ (bCjVrMRaadoutSCCO Mtaaaa\Q _Tamp *C, CarrtrAjoaID RCF/PRM B m a * >2________ Mirm laa _______ Tamp *C c o in t /db f P fV W / IK~< IS ^ - C n n C CO112 T/O/l I V O 6 l/T l 0 1 A * ili u*it . * 's1 j "?e ^ > c N^ J 4 -1 " V* *r-b7t* VO _'r>ITja?^S jS1i ^X <5^3 C o l# T IP tf t . X W ( d l l X l f r ' l - Lj * ~ _ Col 7 Spiking Standard 10 f " 77 Approximata Cone 1 ^ 1 I V t Amount addad IC O T/O/I U .lP A + i f t ' Col5: TA/yt-^-r V: 3i-\Tvt b h t u iv-c^c 3M Enwonmerwat laboratory . v o ta r ID K x V V \ - f a T C l I ^ V jS Col 13 T/DB - ) 0 r ^ .. I f / y> *1 00*983 Col 14 T/DB > j 5 f - < !j,. 1 v y fH MaOH IO: TH -A c4 5 ~ c ? t^ V i i Q t -3 ^ - `" 'r' J (T ) L t / ^ t< y. /fl>Ol aJJUr JhJrJhisp^ (idilli? X--) - MIr/ . Y&Sl ^ Ji'L Report E02-0443 Tenn. River Valley Samples Lab Request , Tennessee River Valley Samples Sample Location 3, Large Mouth lu ip ItB 1 !1 1L 1 S9 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 lJlc 1 V --r Aonu ~ "T 1 SL-3, LM-2-3 ---- . SL-3. LM-2-MS -- SL-3. LM-3-1 0 i 17 i l j ! i| ! il! ! i 48 8 7 hi ._ L 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. IM-5-3 SL-3. LM-S-1 -- -_r OWlo 1 --q - "" n i > .1 . --> V L-- ^T " S. n. ientfio \ N. --a 3 N o -- h/.< ? % U SL-3. LM-6-2 SL-3. LM--3 --j SL-3, LM-6-MS -- VJ \ <S s *; a IJ p4 ^3 >3 c SL-3. IM-7-1 > 0 1 ^ SL-3. LM-7-2 SL-3. LM-7-3 -- - A - J f --N L' Ni ' i 1 jl P i I as !i ! il ili l a i i\ S h Ui ! i il! ii B 8 10 i 12 .JL_ Z / k ..JJLL \13 U / i\ 1 r> . -4 - . 5. rA rj k -O l -X. JL JS .3 \ ! s. V0 cJ N 'V 4 1' 'S s n " tw S i \ \ J V S \ \ 1 i 1 i 1 '1 ' L > t! -L- .J l Col 2 1Ip i n 0 ,3 C U C C ol 9 Shaker ID 03L3.U ^iD bBalance ID ________ Tube type/sizej) Equ Start T/Q /l If {, I l Y l h ) /h q t , 11 c o i j t /d/i ( ill i O - L ^ Equil Stop TMfrx b iV v t i / Y fi 6 l - i f f d w a te r ID t u ; i r . - & T t t : M u s C ol 10 T/Pfl /WS^kM /p / ItC I P X O V iC C o te t / d / i T o ti* ia ;/ V / O'L Q l'Z L tc a n o t/> Col s von T.JStV* (o i l l r i (12 O n . c Cantrtbg ___ Centrifuge ID: | C \~2~ jic )/P R M Readaufc ^ C filN Minute / P Tem o*C^ - 3 C o in von t / Hr/ 03-CtviC RCF/PRM Readout I d M Minute X L C o l* T /D /l9 '? tV n i n I I f f I ffXC ol 7 S p ikin g Standard 10 i f t Tamp "Cj [ f i C ol 12T/O/l / ?/S _____ _/_Z/ 0 -3 Water IP M U k-ft 7PC P/o--> C ol 13 T/D/t ) 5 i O I 9 , J * V t 'J s u t 001984 Approxim ate Cone. I Amount added T/D /l \ V. Iv / 1^ C d Uq- ^DWv b/t'ifcn- rwv_ 3M Environmental Laboratory C ol 14 T/D/I /y /X n /^ X ^ vvoA m -m * - d ) C l "- r t S * wer* ip'.lff ii S f p f t V - 1 ?t (2) ~ \,7.n-/ f>7rykhu-~i1 wr/-f W~ H ht !l kJ Trr-- hi'/r`u7? Page Sois Report E02-0443 Tenn. River Valley Samples Lab Request ; Tennessee River Valley Samples Sample Location 3, Catfish a 1 1 SL-3. C-1-1 SL-3, C-1-2 SL-3, C-1-3 f 1 2 l.'W lo 3 1 w !i 1? 3 k1 i l l i 3 4$ A _ k ,i. I / if P i72a j l i il II ilii l I l i i i l i 11 il y i t 10 11 12 13 14 _ L 7 7 k " r / s. 7 \ feLe s rtu . 0< zZ __ n SL-3. C-2-1 'TirSVf 1 SL-3. C-2-2 I SL-3.C-2-3 -- SL-3. C-2-MS -- 1 1y I SL-3, C-3-1 SL-3.C-3-1 SL-3. C-3-1 sua.c-4 SL-3.C-4 SL-3. C-4 SL-3, C-4-MS Sc-3. C-5-1 SL-3. C-S-2 SL-3, C-5-3 SL-3. C-S-t SL-3, C-S-2 SL-3, C-6-3 /.W /r & ---- __ J s -- i \ .A . l_ mVlAi . 4 -VA _ j - X .- S - I S Se -- aiM W ij *r x "S ` ' " t" 1I _J v! A O w X ~>5 7* *3 jla 1-- * _ -3 '.Kola ___ 7 - ..3 --- ~~ s. ~ 1-- . 3 _c 3 .1 5 * 75 --j--. 3 V- ; _1. N *N 5 - L_ rA i 4 f- s .3 !_ Ti L- i 7] _ c .s !_ " " TS .Io __ :- 1 - 4 777 >v -- 7J SL-3. C-6-MS ----- . SL-3, WB-1 -- SL-3.WB-2 -- 5 y |u 2 1 3 r>r vD SL-3, SB-1 SL-3. SB-2 "" __ i i i i 1 L L !__ > [ 711 rJ__n__ ____ I "i C1 -X M iE 2 1, > XT' C o l2 ( / i 11 IO O C C o is Shaker ID _ - o a & L Balancs ID ^ lO Q ________Tuba typelsizaj E qui Start T/D41l ' J c fta ( j //& / (S > -f IW C ! 10 . Col 3 T/DIt I 3 & 0 f i ( { / |1 l O -- M lWater ID 111 T C H mS c o i4 t/d h T .O Q v * fc L> EquIIStop T/Dfl I I ' W f . / t ^ r f L C - ^ C o lio TIDft? .U J p *i / f i 0 > 4*1 ( - CenlrihKM IP: Ig t8*_______ Col S T/Ofl l i t I OX-c* - c. ( r CF^RM RaeflouL 3 tp Q Mtaul. ( A Te m e *C _ 3 5 -- CantritUo*10:. < T c . t ~ C o lli T/DO J c y u (g / I t i c o _ g ^ . e RCFJPRMRaadout^ O U ^ Minuta z-3-- Tu li *C. Q - Q C o l* TIPif l ' t f l i t I f i A - C tV -C Col 12Tm o/ ? l9 a ! T l3vl 0 J WWater ID ri;!h 0 P/,,K Toc a 001985 Col 7 Spiking Standard ID # *1 ^ Approximate Cone.. ) p p W * \ Amount rid* n \ l l l T/O/lU a i ^ x _ U . / J L 6 1 K 3U E nw ranm tnui Laboratory Col 13 TIPO Col 14 T ID I0 9 & 0 ) 6 l 7 * ' ' l M S ix 9 fl' MeOH IO: TN-A 5 ^ 7) / V j Us ti) } " i^ lP c ,0 i Q U & oitiyW- Wton **? p/f/rv* - /**n 'tK/i7'! V PlQaSoft 5 c V y ' - / V i - ' s - y - s jy , . S ty ? f. .. fi 986T00 Tenn. River Valley Sample mmausimsomiuo u'**Q*uSo3c-a1n1p3o9u-tHi3-trcH0a064ntVWI ww oootj 301 iwanpaid '1-0OC6 =P1 H i 1 i"ft** --CIIPM*Mi8<uuttlie3 JWWOPmUa 01**0 *1Tivilursml"t'm*a*uu'm*ynefmA*mU"u"iUT'Tv1OoouOUoouWOocO*WoenoOoOmosO*LWftiilnlUun'ImtsIfo6sHMOr-iu6nanH+O0QaoomOOar13riIrirfufwH1ktwMHna8OooMo0oMOamsM*1ts-4w'aOM0aail>tslB^hin-MKM>mMe'uiI1illi133sMT*3KK3XennnWninIMmuMuruMuSsssSSssSs! 1 1 n T f / O O t l (J)*1*L|03 hJfUi9fTH--fI7'`0v,VfgPlfwAwiuJ-uitfilwernaiu.al -tiwjfy'f/'PUit.T"7f";"*,~S<>',,.w/i;io V/~4>y<W2VM"Lti'?"Jj)'Ht.Un'ryV3I1Huiu~MIswiao - n ! \ lix im b ^ V)S0V'*VrC/Vitf vati *0" -- '""fKfe'HfWfg2wf>t0o* aw=pBMm*n3*g t j * yssA--S-A"Aanm-'1tan'n%>T9*niismnU>ni**tv^`KaS-S/S^SArSS/AsC**T99/7ttLT2'*T77/)^ct^x--i****'7*970-7*>9at7~SssffSASAusSfft~7fLAA*l*lt/tAiLllw*l7">T Ij 1 !** f S l l1 rl f l i ' i t * I t i ' u >f / i A F'/ ra a ^ w o 'Kj<...V'OTT/'"117 anun lim/Kr iKiJVJStl'm. 4ot- /WJ*utvMiiywn s*j*M/?tc|)W/-7"ysf-Q-XimiWfiYMipotapuuo*Q**pMvWpmVs u*Wgr ^^Wi'H^VSH-rta wu. fl f1l sA ffASlnlTt *1ASfSffAAfHSSfllll*il n If li s\ A *ffAAS/Sl1lt\1 AffSsll ----AA5flTl----A ti* %1 i f.'l'9/ *"? 1SAfASfAAfnSftAAAsAAslli.ll. j i ""A~AfffAsATf/ASSA7ff>Sl/nlltlll-ri~-"l"TSrsSfAAAfAAAAnff1AfAi.i1?Al.llll't*rrWTiTfU<SIhJ>PiTiffref&r(*ITrrl<fiAr!T"f3kr:7VifA--fn~m*i}ifhTUlu?mlle.3-7-----T---i-J5Tt-cBinTuTr>AiLiW7TMfnCmY7w--sKt1FiTff--A^3TtlMwgt*i*.ft3u->TTWTiT"-r<-'H'T'JJrJiJT?TfJP?fTWttiT-t- tMSSS'wVPHNVMiiWWMPu>ItmmMiulmHIwiUUUOiiuUWUuiCMdoHu8WnuMBWswMMNnacsVpIFipZnPPifpPWuwMMioMHAliS*Wm*po*ugg'lSSnNU9SuASSoA'*T''A8AAAAaAMAoA'0AAAAo'AAaTA3oHHWn~HHTMUMuHIMoI*iu9Vlr)Mr*I*'''i''TA1111iiliil1ll1iliiimIWB`WmetZM-HnCMntfiiLt*i--^Hincimw>-iMo-mMMpsOrt*Mr-swwt-WaoO3o-fOtoWaOOmwotOtio1lwa>vIeeMKtAtHtn-tTCCC-tceAvcr-ecWwtKm-L-Ct-*W<--CtcMwcmtocCt-zCcCmtw--^wm*ttwwoM>tLM>ocMOt>OuwoW0oK0-0Lowoocw-pooh0-OzZ-->^f-c8-ZO-aCnCZOt8zrtZ0oc^oioWooDoo000l0osmo0n003a3a338a3a3aa3333a33a3i i r6 ^'>1 :pnuum(O3|0PdAi u&|^ij)X3 dos ttW K03 _Mqiun(4*P"IS O -P O -S l ~:pcy*l9PQ Report E02-0443 Raport E02-0443 '8 1 i C O 33 O i U1l 1 to 1 '} i 6 1 1 >1 I fi 19 B 0 Tann. River VaHey Samples 1 '<*.h33 ** 1 "V Report E02-0443 Tenn. River Valley Samples Balana ID 900 C ol J TOM (? & > _ Tuba type/alze. Z )l7 . U (S i M tl fq d il S tart TOM fd tfil S lop TOM J i lX ./iU -# h. J I I . V A /> */ ^ 0* fJ lV S ^ , {V P ? ' W ater ID A : l l i ' U T0\ C o l4 TOM ( ? V S S P /u \_________ ff (fit 7S petd/uttinfl C ol ST/Dfl IQOQ M ___ C ol 10 T/D /l l l T ^ l X / l tTh Centrifuga ID: T 4 (^C{>PRM Readout: ^ 0 0 0 Mlnirtaa /iO '" ^ yS ^ Tamo *C Cantrifuga IP: O o t l / % ~ S' ^ C ol 11 TOM / 5 V 3 j / / J a / y? -- tR CF/^R SR .adoutK t * C ol 6 TOM l / O O /) Minula >.01" r f lA- Tamp c_ A ,< t O t i ) C ol 1J TOM f."*a^e> ' W ater ID 3 / /J ^ ' l (S iV fH T Q P )^ J C ol 7 S p ikin g S tandard ID O l O P ' O 1 4 f O i C 1 J h/' Approxim ate Cone. V _ _ _ _ A m o u n t added___________ Q l 0 0*1 0 > J O S i , C 5 V " O S S TOM / H O )) 1 7 .-i / & " 0 ( j ( Z 1 / b / J /JH L - iL / -V iH S L t T 4 (,v id , tv - 4 * / lt 6$ - 3M Erwanmotal laborMory COM3 TOM J > lX a f `'I C ol 14 TOM M eO H ID : TN.A / ) 6 t ) 0 6 / V '. '/ l/ 'p J O " ^ d.J Pagatoli 001988 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 ETS 8Afrfcfr 4 0 1*14-Ititi Vi E02-0443 Volume of 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 mi 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 cotumn used 1g, 6 m l, C1B lo t 2057B2 1g, 6m l, C 18 W 2057B2 1g, 6 m l, C 18 to t 20S7B2 1g, 6m l, C1B kX2057B2 1g, 6m l, C 18 Io t2 0 5 7 8 2 1g, 6 m l,C 1 8 lo t 2057B2 1g, 8m l, C 18 lo t 2057B2 1g, 6 m l, C 18 lo t 205782 1 g .6 m l.C 1 8 to t 205782 1g, 6m l, C 18 to t 205782 1g, 6m l. C 18 lo t 205782 1g, 6 m l, C18 lo t 205782 1g, 6m l, C a M 2057B2 1g, 6 m l, C 18 lo t 205782 1g, 6 m l, C18 M 2057B2 1 g .6 m l.C 1 8 to t 2057B2 1g, 6 m l, C 18 lo t 205782 1g .6m l,C ia lo t 2057B2 1g, Bm l, C 18 k it 205782 1g, 6m l, C 18 lo t 2057B2 -- 14- ! t Amount and Elution solvent and spike mix used volume NA M oOH T N -A -6116 2m l N A M oOH T N -A -6116 2m l NA M oOH T N -A -6116 2m l NA M oO H T N -A -6116 2m l N A M oOH T N -A -6116 2m l NA MoOH T N A - 6116 2m l NA MoOH T N -A -8116 2m l NA MoOH T N -A -6116 2m l NA MeOH T N -A -6116 2m l NA MoOH T N A - 8116 2m l NA M eOH TN -A -6116 2m l N A M eOH T N -A -6116 2m l NA MeOH T N A -6118 2m l MeOH T N -A -6116 NA 2m l NA M eOH T N -A -6116 2m l M oOH T N -A -6116 NA 2m l M eOH T N -A -6116 NA 2m l NA MeOH T N A -6 11 6 2m l MeOH T N A -6 11 6 NA 2m l NA MeOH T N A -6 11 6 2m l Comments Extraction Steps (initial when/if done): C*i,' condition column with MeOH; wash with milliq; filter sample; r K . vacuum dry the column; c K elute column with solvent; o K transfer extract into an autovial Additional comments: -If! ,Uc,'f ofe'C - P .cp t iy&czfj vT-v/ii-j ,>@ 6 b t * r j = n ,'1 < ~ r 'i b '1 .1 cv .o j y u i , J $ ,fA' GtCop'J jD k - Report E02-0443 Tenn. River Valley Samples Non GLP SPE Columns Extraction W orksheet Prep Date: 7/17/2002 Analysts initials: OK Method Revision: BFS*r15rO- <> .\a litr/t, Study Number E02-0443 volume ot 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 V Type of column used Ig , 6 m l. C16 lo t 2057B2 Ig , 6 m l, C 18 lo t 2057B2 1g, 6 m l, C 18 lo t 2057B2 Ig , 6 m l, C18 lo t 2057B2 Ig , 6 m l, C IS lo t 2057B2 Amount and Elution solvent and spike mix used volume 2NA M eO H T N -A -fiM O tC ml { 2NA M e O H T N -A - ttfl 1 ml I 2NA M e O H T H A -S H fl ml 2NA M eOH T N -A -.6 4 ml 2NA M eOH T N -A -U M . ml Comments ' S s s ''v \ \ Extraction Steps (initial when/if done): :ondition column with MeOH; CM wash with milliq: p ^ filter sample; vacuum dry the column; /P K elute column with solvent; pK . transfer extract into an autovial Additional comments: g g ) TXi-fw-eao? r e -`& c h cK ? b 'c tA ._ ___ 7 ^02. S>. E-octCopyc'Ci: / r _ J 2 & l Initial nL/ui<3 Q ^ fr.ct,^ Wi 1 ** ^ T5 M I** ^ ' / ^ J * ' 001990 Report E02-0443 D escrip tion : Date Prepared: Prepared By: I La I ( , * j< <m__________ _____________ Storage Location: Expiration Date: 3, f& i M U LTI-LEVEL PREPARATION LOG Book No. 02 003 ________ _____ Solvent: / I t f i HPa_g_e_N_o_.______5_2 ,f jU Ci } 3M Trace f t r3> Standard ID # 02003-12-1 lu O D M M 02003424 02003434 02003-52-8 02083-824 0200342-7 02003424 Description Cp f O Component Standard* D escription V e - 5/:i A lt ID # Cone ' rJ T C O iio ^ V it. . V f- E x p ira tio n Date li/J l/o i lOOnatK ft',1 ft / f / r tu e IQ O fft k /O i -- 1 1 3 .S Std 1 3 J-- -- Std 2 -- -- S 0 S 5> Am ount o f Com ponent Standard Added 6 0 dse S td 3 i& u . -- -- Std 4 3 0 1 /L -- -- Std 5 SOctL -- -- Std 6 IC & U -- -- Std 7 _ 3 , -- Sid 8 -- Sj L Final Vbltne 6 * ^ Final Coneartntk I 0 .S s 3 a. So1 0 3 5 i _ 5 0 D escription Standard ID # Description Component Standards ID # Core fffk ) E x p ira tio n Date 02003424 0208343-10 0200342-11 020034242 0200342-13 020034244 0200342-18 0200342-18 <00 7 5 l e v a 0. -- ------ Am ount o f Com ponent Standard Added Std 9 Std 10 Std 11 S td 12 Std 13 Std 14 Std 15 Std 16 IO O .,,t, % ;i. M l/ O io iW i lh * A Vo -- 1 0 t. -- S x /C -- ^ 0uL -- ---- ---- -- -- ---- -- -- -- ------ -- -- ---- -- ---- Final Volane (n 0 Final ConcatMien ( f f i) D 5C 0 0 * tooo 0 -- -> -- ---- "l^A^ir.*Cift/j*- Ravfewod itfLlOO SigntureJ DaiirJ61 Dai Tenn. River Valley Samples 001991 Report E02-0443 ascription: Cot K i i (tw r Storage Location: M ULTI-LEVEL PREPARATION LOO Book No. 02 003 Paga No. 54 S o lva n t s J r M Standard ID # 020QM4.1 02003-64-2 02003-044 0200144-4 02003444 2003444 0200344-7 02003444 Description Description Component Standards ID # Cono (ffi Expiration Date I Std 1 Std 2 5 Jo 2 5 5 o Amount ot Component Standard Added Std 3 Std 4 Std 5 Std 6 loo Std 7 So Std B Irtan ^tr^> MlY l M t 0 H Vati-r& t 1I f * 1o o f r Mir;-, iOH W Q -O tt iOOfmn -- "/u / 4 /li/c A -- 3t/ -- - 5oL -- -- fBoi >vt -- ---- S0vL -- - lkit -- -- >1 -- o t- -- FM Votum 6 L-) i o) i * FlraiConontratton {*$^0 I 3 .S 5 l <35 SO J <3J Standen! ID # D escription Description Component Standards ID # Cono E xp ira tio n Date lO O jpn lr f lif t M 'O t 0 0 M * Tr '/)/* > -- o o o fo o o -- --2003444 0200344-16 0200144-11 0200344-12 0200344-13 0200944-14 0034445 00344-1 S ?5 Q -- Am ount o f Component Standard Added Std 9 & u L -- Std 10 IS ^ L -- Std 11 -- S U 12 Q uL -------- SU 13 ---- --SU 14 -- --SU 15 -- SU 16 --- -- -- -- -- ------ -- ---- ---- FWaiVolume FndCorrartrattanl ^ 0 Tvon-LuS" uM. j[y| "i i m. /Ooo o lOiSf OtiB 2 Reviewed ---- ---- \'sWJlU -- ------ ------- Rhs-<kOK-_ Vr " *` VR~~ . . Term. River Valley Samples 001992 Report E02-0443 D escription: 'F is* Storage Location: M U LTILE V E L PREPARATION LOG Book No. 02 003 Page No. SO Solvent: M e o H Stnden! ID # 0200340-1 02003404 02003404 82003404 02003404 2003404 0200340-7 02001404 Com ponent Standards D escription _________<&)Ju i ID # Cone n io > -TR n a rm a -T l lo O y r* A - --------------- E xp ira tio n Date iirs lo v / fe v Std 1 IO ,u L . -------- j- s x tb J s . ~ u ^ > e ^ Am ount o f Com ponent Standard Added S td 2 5 ^ L -- Std 3 S O jtL -- Std 4 --tO O juL Std 5 Std 6 -- --SSOm U 5 c o > u Std 7 lOfiL- --Std 8 JS >L p m vouma Final Concantnton o n U _ L j2___ a s - go ----- V i sIO s o ID O a r o D escription Standard ID # Description Com oonent Standards ID # Cone E xp ira tio n Date o a o j a - i A - l i t s : __ / V U 3 . OJoaa-33 Fral Vokm FinalConantrmon. o n io s;82003404 0200340*10 0200340-11 0208340-12 0200340-13 B20034D-U 0200340-19 0200340-19 -7 S & * k 18 C Am ount o f C< m txw ent Standard Added \ -- -- --Std 9 S td 10 Std 11 S t 5Cy*<- i 5 * l IOOm L ISO300 -> \S&Qr S W l3 Std 14 ** S _ ------- /Std 15 Std 16I _4 ______ 3 _____ i r u BactCopyof Original S M &iD"91 M U Data R*viwedbyv Signatur, . _ Tenn. River Valley Samples 001993 Exact concentration of every point of every analyte Prao data: f Q T , vui____________ A nalyst F/WC SoFlivneanlVt &olTumOeAof:eMachr * p \K o in t TNA -_______f_\______________________ Target analytes: frp iAS. FOSA. _______________________________________ PBaoooek NNoo:: oaoo] 50 Report E02-0443 Tenn. River Valley Samples SectCopyof Original AtA- ONPita total otoi *3t Revtaradby: Signatur, 01994 Report E02-0443 Tenn. River Valley Samples r* I SINGLE COMPONENT PREPARATION LOG Date: 1 ) O t l I / O ______ Analyst: / v} i , 1 ____________ _ Book No. 02 050 Page No. 34 IDescription: A v ,Vt lJ ilts ; P i'ir 'i, Fo>4j p m . fpoj r* pPd s Stock Number, n Weight or Volume Used: Concentration or Purity: Corrected Weight F in a l V o lu m e : 1 , 0 "?,C Storage Location: Balance ID: A/A Other Correction Factors: Solvent and TN-A Number. d S T / f /v w i U i / T f r - ( M M r Q . TOC Final Concentration: I Expiration Date:_ I ExactCopyofOriginal Initial Caia Reviewed by: Signature, / k / L / k J ' IIA / ^ _ Date 001995 Report E02-0443 Tenn. River Valley Sam ples Description: Y t f'U . -So? E g Date Preoared: > ( \ K \ ' i -- Prepared By:_ C M C ___________ Storage Location:_ Expiration Date: il / ,3 .3 ) 3--* _MULTI-COMPONENT PREPARATION LOG Book No. 02 002 Page No. 33 Solvent' 3MTrace It. TN-A- fMiw Description P F dp. PPSS Standard ID * 02 002-33 H Component Standard ID# Cone, or Purity Expiration Weightor Corrected Weight Final Concentration Date Volume Balance ID O^CCI - n o a c c *-i^ 3na P frv' 471# V i lo - K V - 53/^ '/lt> )t> 3 Nft ?xsx* IO .0p |Q ^v\ osh.d i- o s 'S' 3 \ 1 3 L l\ x -U n m&2o pp* 03LOOI-&M 3 3 c t \ \ V > - . pprv a j j S '/ \ 1 06 ^ pp/Vn `m s ; \V ^ 9 .1 M pprrt ___ 1 tl ..... ^ Final Volume Exact Copy of Original /H/c Initial Dato Reviewed m Approximate Concentrationof the irix 1C x ) p p iV \ Signature. 0 0 1/9/ 3 8J u n 0 0 Report E02-0443 Tenn. River Valley Samples Date: Analyst fMl SINGLE COMPONENTPREPARATION LOG ____ Book No. 02022 Page No. 77 Description: I /vs S ii lL. M f X _______ StockNumber, m r ^ / l ~ 3=^-------------------- Weight orVolume Used: Concentration or Purity: CorrectedWeight S S O ^l M 'j' i f*', k w * ce ID: 1 - > > { / lD p p n rs_ *? *'' 1^ li tt M r 11 i~Q T r l uSolventamnd TN-A Number CL,V Final Volume:_ r S / n \ ~ Final Concentration: -ftpm. Storaga Location: ExpirationDate: Il j H f O l* -* Exact Copy ofOrigbid Ma ^MAM-i Cats Reviewed by: Signatura, Oata 001997 Report E02-0443 Tenn. River Valley Samples Date; SINGLE COMPONENT PREPARATION LOG I I S f p j 0 ^ ______ BookNo. 02 040 Pipe No. 80 Description: / % A r a i r e A a J h / l u b - Q ________ Stock Number ( Z Q & r n V T M 'J - lt l- Weight orVolume Usetfc__ Concentrationor Purity:_ <n Balance ID: A /A - OtherCorrection Factors: . sisA t CorrectedWeight _ //A . " " S T M - J } T o e p /u ^ _ Final Volume:_ 1) Final Concentration: i^ Storage Locatkm:_ y ^ F f r frrp___ ExpirationDate: G ty ) A / A ls f j & r Reviewed 001998 Report E02-0443 Tenn. River Valley Samples Date: SINGLE COMPONENT PREPARATION LOG | fOO_________ Analyst:________ OKJ______________ BooKNo. 02 001 PageNo. 17 Description: 7*4 H S Stock Number ` 0^>G WeightorVolume Used: Concentration or Purity: Corrected Weight: BalanceID: _____ ^ IM OtherCorrection Factors: iJA Solvent andTN-A Number H e O H W -A Final Volume: Storage Location: t L c t ja?l Final Concentration: 7 *5 fp A xj Expiration Date:______ f-JO-t? 3 ReportE02-0443 Tenn. River Valley Samples ! m 0 i Im \ a im Data:______ 1 - fO 'O S Analyst 06 Description: SINGLE COMPONENT PREPARATION LOG Book No. 02 001 Page No. 19 Stock Number -2 D o a q Weight orVolume Used: (p . / / 7 ? cl ---------------------- z r Concentration or Purity:__ M p a i. Corrected Weight M _____________ Balance ID: Other Correction Factors: Solvent and TN-A Number H e O n /m 'A - e s ^ - ^ Final Volume: cf c 5 u A . StorageLocatk>n:_ d u d jfcPC Final Concentration:_______t*-t- Expiratlon Date: //fr 0 3 002000 Report E02-0443 Tenn. River Valley Samples SINGLE COMPONENT PREPARATION LOG Analyst /j t/F_ _ _ _ _ _ _ _ _ FC K ?FQ5>Description: Book No. 02001 Page No. 84 Stock Number:_J M M jd -- w < w " v?r 0 ,. m Concentration or Purity: CorrectedWelght:_ ^ 5*7FinalVolume: C Storage Location: Other Correction Factors: Solvent and TN-A\ * t J Number f P f l i f I* 61 Final Concentration: 0 e/ ^ 3 0 3>Expiration Date: fe b Exact Copy of Original / WU U- Di a/tka i n Reviewed t / '/ o .I 003001 Report E02-0443 Tenn. River Valley Samples a SINGLE COMPONENT PREPARATION LOG Date: BookNo. 02001 4 Page No. 85 Analyst_ / V A ________V C - mDescription:_ jP T O A 'Hay*-mi S tock N um ber^ g> " w * " vs s ; 0 . 5 7 { 9- a Concentration or Purity: IS 3 & Corrected W eight Balance ID: m. Other Correction Factors: /I O M } 7A/'ASolventand TN-A Number p ~ 7~ Final Volume: .~? . h n L Final Concentration:_____ S to ra g e L o c a tio n : D f- Expiration Date: ,J?S? Exact Copy of Original A M - & 0 ib e c i # * - biitial Date Reviewed by: j [ x j- 002002 Report E02-0443 Tenn. River Valley Samples SINGLE COMPONENT PREPARATION LOG _ _ _ _ _1/4Analyst / t y Book N a 02022 Pig* No. 66 Description: / I. - T O t t . L s r Z (C s s ,< c O StockNumber. 7C.Q-Mf-}-e>?l / TCK - i i l CMew) WWghtorVotums Ueed: - _^ .5 > % 5 * Concentrationor Purilv: n --> o / y 7 .5 / 0 (7).^CorrectedWeight_____ f Final Volume: .Storage Location: V PI, Balance ID; Other Correction Factors; Solvent andTN-A m- Final Concentration: I1 ; ? f J Expiration Date: A 'f r J < 0 3 m Reviewed uy SignuM^uraJy'tL! P&JsA J' ?Oiatn*J7'L-> 002003 Report E02-0443 Tenn. River Valley Samples Oat: Analyst SIN G LE C O M PO NENT PR EPARA TIO N LO G V T tj r\& C~ C M C ___________ BookNo. 02022 PageNo. 79 Description: X ~ C . ( v \ 'v . ( p p y v \ _____ _______________________ __ Stock Number ( g p "O ie > e X - M * . i 0 J WeightorVolume Used:_____ lO a -- Concentration or Purity: p p ^ Corrected Weight Balance ID: W f i OtherCorrection Factors: Solvent andTN-A Number V-V OH . T N f l ~ 4 S J O Final Volume: ItV rL Storage Location: Final Concentratione:-----! ^ J 3 0 Expiration Date: Reviewed by. Signatura, 0X Data 002004 Report E 02-0443 Tenn. River Valley Samples TCR Receipt & General Information rcR# TCR-S3 Substance trade name or T B i reference*: Substance/chemlcal name: Parfluorohexancsulfonate Primary std Lot/batch *: Location of synthesis, fabrication, or derivation -acorda: Molecular Formula: C6F13S03-K+ Condition: white powder Expiration date: 10/18/3000 TCR Substance * SE038 Received from: George Moore Date Received: 09/03/1999 Amount received (wt orvol): 154 0,277.38 g gross w t Number/size of containers: Shipper MSOS (y/n) 1/150 mL glass container Courier Y <J N Purity: 98.6% LAC 01/17/01 3M # Entered by (Initials) LAC Std Location/Storage N B 120067-89 Date Entered 09/03/1999 Initials Records received: Checked By Date MSDS, NMR Characterization Request*69085 Interim final report bom Centra and Certificate of Analysis. LAC 04/26/01 Date Checked by (Initial/Dale) F19, Frozen Amount of Retain 0.3610 g Initials Date 10/19/1999 Checked by (Initial/Date) Comments Standard has been moved to Freezer 19 in room 347 KJD 06/08/00 Sent to Centre Analytical for Certificate of 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, 311 shipping ID 41-2700-4647-3. LAC 01/104)2 Attachments Date Checked By Date ase036m sds.pdf se036nmrreq59085. pd E00-1878-COA-SE036-PFHS-R "O Archlved/Substance Not Avajlablej 002005 Report E02-0443 Tenn. River Valley Samples rcR* Substance trade name or reference #: Substance/chemical name: lo t/b atch * Location of synthesis, fabrication, orderivation 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 # mi Perfluorooctane sulfonyl amide or Perfluorooctanesulfonamlda AC KJD 7/24/00 L-15709 Building 236 Received from: R. Buckanin Date Received: 04/20/1999 Amount received (w t or vol): 124.98g gross w t C0F17SO2NH2 Number/size of containers: light yellow waxy solid MCH 07/22/99 Shipper. 10/31/2006 MSDS (y/n) TBD, KJD 06/05/00 Records received: NA Data Entered Checked By 1/100 mLglass container Road Runner yon MSDS, summary page of FID analysis 57915 Date Initials Data Checked by (Inkial/Date) Initials Date 10/18/1999 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 10/25/01 Shipping Comments: NOT REGULATED, shipping code -LB-I000-1S70-S. L-15709. LAC01/08/02 Attachments Date Checked By Date sd029msds.pd sd029fid57915.p ;Ci rchlved/Substance NotAvailable 002006 / Report E02-0443 Tenn. River Valley Samples rcR# Substance trade name or reference#: Substance/chemical name: Lot/bateh#: Location of synthesis, fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M# Entered by (Initials) KJD Std Location/Storage F19, Frozen Amount of Retain 0.2737 g TCR Receipt & General Information TCR-123 PFOA (POAA) TCR Substance # TCR-ifigd-oSa FC-143 Ammonium Perfluorooctanoate (Primary Std) 332 3M Received from: N/A Date Received: 02/02/2000 Amount received (wL 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 of containers: Shipper USDS (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/Data) Date 02/17/2000 Checked by (Initial/Date) Comments Initials Was originally TN-A-2143, KJO 2121/00 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 10/03/OO.LAC 10/03/00 Shipping Codes: 98-02114)891-9/FC-S000-0192-0(00 g on dry Ice) LAC 08/14/01 Standard stored at room temperature prior to 6/6/00 LLAabCe-l1-2r/2e8c/o0r0ded-10/98 RVWV-11/8/01 Shipping comments: REGULATED-TOXIC Dangerous goods In excepted quantity of Class 8, 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 * EOO-1763-COA-99030-30-P FOA-R Archived/Substaiice Not Available | 002007 Report E02-0443 Tenn. River Valley Samples rcR* Substance trade name or reference #: Substance/chemlcal name: Lot/batch #: -ocatlon of synthesis, fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M * Entered by (Initials) KJD Std Location/Storage F19, Frozen Amount of Retain 0.18670 TCR Receipt & General information TCR-129 PFOS TCR Substance# TCR-fiOSJ-Od FC-98 Received from: Potassium perfluorooctansultanato N/A AC KJD 7/24/00 215 Date Received: 02/02/2000 N/A Amount received (w l or voi): 40.1441 g gross wL C8F17S03-K+ whit powder 12101(2010 TBD.KJD Sismo N/A Data Entered Initiate Initiate Number/size of containers: Shipper MSOS (y/n) Records received: 1/ 80ml nalgene bottle N/A yU n MSDS Checked By Date Date Checked by (Initial/Oate) Date 02/17/2000 Checked by (Initial/Date) Comments initials Was originally TN-A-2144, KJD 201/00 Standard has been moved to Freezer 19 In room 347 KJD 6/6/00 Shipping Codes: FC-SOOO-0185-6(<30 g on dry Ice) LAC 96/14/01 Standard wae stored at room temperature prior to 8/6/00 LAC 12/26/00 Received 5/96 RWW11/8/01 Shipping Comments: Dangerous goods in excepted quantity of Claes 6, UN2B11. REGULATED-TOXIC 98-0211-0808-6 (>30 g (1 oz tempi)) Not on dry lea. LAC 01/08/02 Mtachments Date Checked By Date tcr99030-36msds. pdf ,0 Archived/Substance NotAvailable j 002008 Report E02-0443 Tenn. River Valley Samples rcR# Substance trade name or rfrence#: Subetance/ehamical name: Lot/batch #: Location of synthesis, Fabrication, or derivation records: Molecular Formula: Condition: Expiration date: Purity: 3M # Entered by (Initials) KJD Std Locatkm/Storage Freezer F-19, frozen Amount of Retain 0.282 g TCR-ffiJ PFB3 TCR Receipt & General Information TCR Substance * TCR-00017-071 Potassium perfluorobutane sultanate 2 Wildlife Received from: Wildlife Data Received: 06/30/2000 Amount received (wt or vol): -100 g, 121.6288 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 MSOS (y/n) Records received: 1/ -100 mL plastic container unknown vO n MSDS Intarim final report from Centre and Certificate of Analysis. LAC 04/26/01 Checked By Date Date Checked by (Initial/Date) Data 06/30/2000 Checked by (InWal/Oatel Comments Wildlife International Number 8292 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 Centra Analytical for Certificate of Analysis Analysis on 07/08/00 LAC 07/31/00 By F-11926 process LAC 01/03/01 Shipping comments: NOT REGULATED, (based on shipping code of LB-1000-0703-8). LAC 01/10/02 A ttachm ents Initials Date Checked By Date tcr00017-71msds.pdf tcr00017-71Iotinfo. E00-1877-COA-00017-71-PFBS-R i^O' re h iw ^ u ^ n ' Ncrt. 03$ 0QS009 Report E02-0443 E N T- R O l- O th l S M fV j n -i Atlanta Goleta Wihninton Boston H ouston _ D ates Okemos Walnut Creek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Page - Gig Harbor Ventura ------------ " *----- Jw rjtant: _________ & * * 1 ------------------- - --y ------- ,-------------- ProtectKlo. I 7 Q 0 \ t w a l y t i o l V q u e s t ____________________ 1 Sample ID M .Q & W r Akbfll No ''Pi Data Time Comp Grab No. of Con Sample / 1 i i r l Meda / v j V / / i / li / / / / / / //// I / i / Commenta * bW O\ v jo i --0w 0 V s W O I- L ol/ A S W fll -M e ri P S C l -- Lid P S C o i-fja d 'fib rp v ii Sv o3a U II * h . h II I I II X i W^i' * fi i fi i Xi Xi 11 M . I L|3>C \\ II X i V/ yX/ j-- r . i i & r i VeA fio o X Total NumberofContainers \ V 'ig o z s i*o z & l& o x i3&Zg iK o z I 1XQ 2& 3SO 1 3 *0 3 2 t e r buyj viWHn ^ bhf Reinquiahed By Data Tima _ / RecabadBy *"***** ***** Dale Time w / (n _____________ - iSa ftJ + J 'C T ^ r - f n m -r- r \ ., V ? .. i ficto. FO R M * CNT-1S1 . _ Tenn. River Valley Samples 002010 Report E02-0443 Atlanta G Goleta Wilminton Boston n Houston Dallas Okemoa Walnut Creak i-- , S f M p J S ItsJ 0 2 - C 'V ' t 3 - Dearborn Olympia , East Greenwich Sacramento Edmond Tacoma K V.aie Gig Harbor Ventura C H A IN O F C U S T O D Y A N D A N A L Y T IC A L R E Q U E S T R E C O R D S r ^ fatm- j e . " 5 e i* L i 4 l Enti4.r^nMi-% u>rr-r ra i * ProiecINo. I " 7 ^ ^ 0 ) $ E 2 $ T L W , U M , \ iW Airbill No ANALYTICAL REQUEST WTTTTTTTT7*'1 3 'I*jotr 7s?/ Sample ID O at* Time Comp Grab No. o l Sample / ( J J C ent Media / s / j // Comments V J 03- D t.p s i " 0200 X 1 Weir C 7goy~t C , v J 01 " Loi~> $ W o l* M eJ Q moI l v /i/o a u i l> >030 X1 X1 X1 7to !> 3 o i y io z q - S w o 3 - u O 1 X1 os O s7 O ol - 1-0 uJ %l ZZO 'l*! S W o 'J -N ftJ F S C 0 3 - Lou *\ 1 - 'ito H -o 7&o<r> / - S C 0 ol " MccJ "Tr ; ^ t I^h K ^ ) n| / * 1/ X\ 1 'A' \y 3 yo tfx Total Number o f Container 10 TU M Relinquished By FORM I ENT*131 Data Time I3oo fktr-JL- Received By C .'3 ^ *r' 3r~> . * ' ' i.'. .-rt Date Time ty/iln. ucl a . . _ Tenn. River Valley Samples 002011 Report E02-0+43 Atlanta Goleta Wilmlnton Boston Dallas Houston Okemos ______ Walnut Creek . 0 2 - 0 r t 3 Dearborn Olympia East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura _ Tenn. R iver Valley Samples FOPM * E*fT>l9Y 00C 012 Report E02-0443 E OX-Oi^ Atlanta Golata Wilminton Boston H ouston _ a lia s Okamos W alnut C reek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD Paga Q G ig Harbor Ventura _j -o t_ 2 L -r O ta r ry "3 ^ , A, ) O Protect No. Alm a NO T S -tn -in # A N A L Y T IC A L R E Q U E S T 1 , \v/ l/ l / / l l / l I l I lI l I l I l I l / v/////////// Sample ID j S L o i- i- M o a J y S L O I-L in c i j SLC1 - l ^ O b Date ll Time Comp Grab X No. of Sample I J jY / C ant Media / k / / 1 T r . 1. \ h *pj /' / '/ /// // / / i 1 1 III// Comments p a 4 K W J ) >1. <5ev 3? 2 3 *1 1 I t l? C tt 3 :hu j M b 5 C - n ic 4 4 S ' n -ivi i t />. 12; . S . .u . } I ^ 1S C .I I - C A T o \ cA To& C, L e i - O T T o S ,i.o )-a ^ H x >1/ >1/ Total Number o l Containers . . 1 /o \y >1 t t f ? '4 / G A- # 20 'i f rs^ d Z f'.n , p . /t. / i l f l i . 6 / / '. j 3 a y 1 1 4 - u ., p , ib . si-. Relinquished By Date Time ^ / Received By Date Time 7 7 /'7/<q |3 V 0 ^ /z c / i / a t y lo h \7 '.& V FOWU t E JfT -U I Term. River Valley Samples 002013 Report E02-0443 J Atlanta Goleta G Wibninton E . Il I K ox- O Boston D allas Houston Okamos ______ Walnut Creek G Dearborn Olympia ' East Greenwich Sacramento Edmond Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD p^. 3 ^ 3 l` Tenn. R iver Valley Samples 002014  Atlanta Goteta Wilminton Boston Houston Dallas Okemos Wlnut Creek 1i i . rt Dearborn Olympia t0 Z '0 'j> tf-n East Greenwich Sacramento / Edmond Tacoma Gig Harbor Ventura CHAIN OF CUSTODY AND ANALYTICAL REQUEST RECORD ' p*ge_L-e<-i. Term. River Valley Samples >> 002015  Atlanta Goleta Wilminton N >r -R Boston n Houston Dallas Okemos P I Walnut Creek Dearborn Olympia East Greenwich Sacramento Edmond Tacoma C H A IN O F C U S TO D Y A N D A N A L Y T IC A L R E Q U E S T R E C O R D Pag Gig Harbor Ventura m S i' Tenn. River Valley Samples qO & 0 ( & - E - N - ~ R ~ - 1 - 0 3 (f Atlanta Goleta WHminton Boston Houston _____ Dallas Otemos Walnut Creek Dearborn Olympia Q East Greenwich Q Edmond Sacramento Tacoma Gig Harbor Ventura C H A IN O F C U S T O D Y A N D A N A L Y T IC A L R E Q U E S T R E C O R D P age___!___ o t-- kX . I oa m o I Tenn. River Valley Samples U0 2 0 1 7  Atlanta Golata Wilmlnton r - ' N V-T: R' boz-olu 7 D Boston Dallas Houston Okemos ______ Walnut Creek Dearborn Olympia' East Greenwich Sacram ento Edmond Tacoma Q G ig H arbor Ventura C H A IN O F C U S T O D Y A N D A N A L Y T IC A L R E Q U E S T R E C O R D PllB. 3 ,, ^ Tenn. River Valley Samples 1 (0 2 0 1 8 Report E02-0443 Attachment E: Notes to File Tenn. River Valley Samples 002019 Report E02-0443 Tenn. RK/er Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443 LIM S Number: NA________ ________________________________________ Affected Data: D020626Extracted, D020628, D020629, and D020702 (Fish Tissue) T1.he following samples were mislabeled in their respective sequences. They were all labeled as "-1-1" when they should have been labeled as "-1-2". The list is as follows: D020626Extracted: DUDE0055, D020628: DUDE0056 and DUDE0075, D020629: DUDE0063 andDUDE0096, and D020702: DUDE0062. 2A.ll o f the fish tissue sample preparation was done at the same time; therefore, Water Blanks (WB) and Solvent Blanks (SB) were done with each Sample Location, not with each different type of fish from each location. This was done since the WBs and SBs are for examining the sample preparation process and are independent of the 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. 3. Tcohnetafiisnherti(sCsuoelusmamn p2l)e,shwaderweaatnearlaydzdeeddin(Ctroilpulmicante3.),Eaancdhthfiesnhhtiosmsuoegpeanrieznedt s(aCmoplulemwna4s)fbiresftowreeiitgwheads oseupt ainratotead into triplicates. The weight are recorded in the "-1" rows of the Fish Tissue prep sheets. It is not until Column 6 that the triplicates are generated from the homogenate (MSs are also generated at this time). The samples that were labeled with "-MS" were spiked with the spike solution in Column 7. 4T.he fish tissue that was used in the extracted fish curves was from the fish tissue sample with the lowest amount o f endogenous analyte concentration. This was determined during a preliminary range-finding experiment. 5. The extracted fish tissue standard curves had a 0 ppb curve point. This point was part of the calibration curve and was "Enabled" in the quantitation software, but it was not calculated as part of the curve. T6.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. 002020 Date: Page i_ of fx- Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number; E02-Q443 LIM S 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 2T.he injection files from the sequence 1021112 that are after file Itchy062 are not part o f the reportable analyses. These samples were method development only. Recorded Date: 002021 Pave<D of Report E02-0443 Tenn. Rn/erVatey Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443________________ __________ LIM S Number; NA_______________________ Affected Data: D020812A and D020812B. A1.ll data that is in D020812A and D020812B are from one original sequence: D020812. The D020812 parent sequence is made up o f 161 injections/files. Files DUDE0001 to DUDE0096 are found in the sub-sequence 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. Low concentration samples that fall in the bottom end o f the standard calibration curve (0.1 ng/mL to SO ng/mL) are in sub-sequence D020812A. Very high concentration samples that required small injection volumes that fall in the top end of the curve (S ng/mL to 1000 ng/mL) are in sub-sequence D020812B. There are not any files that are contained in both sub-sequences. 2 There are two different extraction dates for the samples: 20 Jun 02 and 17 Jul 02. This is due to a re-extraction o f 5 samples whose results were questionable. 3. The following are the LIMS numbers and the sample names of the samples and their associated duplicates and matrix spikes: 38025 SW01 38026 SWOl-Dup 38027 SW01-Low SFWSC==SFaimelpdleSaWmaptleer(CSoamntprolel Location) FB= Field Blank 38028 SW01-Med Low=Low Field Spike 3388002390 F S C 0 1-Low FSCOl-Med Med=Medium Field Spike 38032 FB02 38033 SW03 38034 SW03-Dup 38035 SW03-Low 38036 SW03-Med 38037 SW02 38038 SW02-Dup 38039 SW02-LOW 38340 SW02-Med 38041 FCS02-LOW 38042 FCS02-Med 38043 Trip Blank #1 and 38047 Trip Blank #2 002022 Recorded Bv: Date: Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443 LIMS Number: NA Affected Data: D020626Extracted I1n. 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: 002023 M AT>____ - f Report E02-O443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443 LIMS Number; NA Affected Data: All Data Note: This is to explain how the quantitation wasperformed on the data. T1.he entire calibration curve was entered into the quantitation software and the curve was then analyzed. In many cases, high level curve points were "Disabled" in the software and were removed from the curve calculation. In all instances in which this was done, the disabled curve points show a recovery o f 0%. Low end curve points that had % Recoveries that exceeded the criteria or were <2X the solvent blanks levels were not used. These points were still included in the calibration curve calculations, however, they were not used in the determination of the LOQ. 2In. the raw data that comes from the Target software, concentrations that would normally be quantitated as a very alobwnoorrmaalnleyglaatrigvee vvaalluueesaarleoansgsiwgintehdvaenryexsmtreamll earpeoascitoivuentvs.aluTeh.esTehveasleuvesa,luaelosnagreweiathsilvyalnuoetsictehdatdaureetboetlhoewirthe limit o f quantitation, are changed to "BLOQ" to eliminate any possible confusion. Recorded By: Date: 0 OC0 2 4 SPase of . Report E02-0443 Tenn. River Valley Samples 3M ENVIRONMENTAL LABORATORY Note to File Project or Study Number: E02-0443 __________ LIM S Number: NA_______ Affected Data: Fish Tissue I1n. die sample preparation process o f the fish tissue, after the homogenization process (Step 4), the homogenate is centrifuged for a short time and then shaken (Step S). 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. OOC025 Page Cl. 0