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BACK TO MAIN Study Title Soil Adsorption/Desorption Study of Potassium Perfluorooctanesulfonate (PFOS) Data Requirement Based on OECD 106 Author Mark E. Ellefson Study Initiation Date October 17,2000 Study Completion Date Date of Signing Performing Laboratory 3M Environmental Laboratory Building 2-3E-09,935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Laboratory Report No: E00-13 11 Total Number of Pages 703 BACK TO MAIN This page has been reserved for specific country requirements. 3M Environmental Laboratory Page 2 of 703 BACK TO MAIN GLP Compliance Statement Study Title: Soil AdsorptiodDesorption Study of Potassium Perfluorooctanesulfonate (PFOS) Study Identification Number: EOO-1311 This study was conducted in compliance with Toxic Substances Control Act (TSCA) Good Laboratory Practice (GLP) Standards with the exceptions listed below: Exceptions to GLP compliance: 40 CFR 972.130(e): There is not an electronic audit trail of corrections. The authenticated hardcopy printouts are considered the original raw data. William K. Reagen, Testing Facility Management Date 3M Environmental Laboratory Page 3 of 703 BACK TO MAIN Quality Assurance Statement Study Title: Soil AdsorptiodDesorption of Potassium Perfluorooctanesulfonate (PFOS) Study Identification Number: E00-13 11 This study was audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), as indicated in the following table. The findings were reported to the study director and laboratory management. Inspection Dates 911 9/00 ~ ~~~ ~ 11/07/00 4/18/01 511 1/01 ~ ~ ~~ ~ 5/14/01 5/17/01 5/22/01 512510 1 Phase Protocol ~~ In-phase Data (Tier I) Data (Tier II&III) ~~ Data (Tier II&III) Data (Tier II&III) Data (Tier II&III) Final Report Date Reported to Management Study Director 9/20/00 ~ 11/07/00 9/20/00 11/07/00 411810 1 4/18/01 511 1/01 ~ 5/14/01 511 1/01 5/14/01 5/17/01 512210 1 5/17/01 ~ 512210 1 512510 1 512510 1 QAU Repvesedative 6-"/-a1 Date 3M Environmental Laboratory Page 4 of 703 BACK TO MAIN Table of Contents GLP Compliance Statement ...................................................................................................... 3 Quality Assurance Statement..................................................................................................... 4 List of Tables ........................................................................................................................... 6 Study Personnel and Contributors .............................................................................................. 6 Location of Archives ................................................................................................................ 7 Summary ................................................................................................................................. 7 Introduction ............................................................................................................................. 8 Purpose ........................................................................................................................................... 8 Materials and Methods.............................................................................................................. 1 0 Chemical Characterization ............................................................................................................... 10 Method Summaries .......................................................................................................................... 11 Specimen Collection and Analysis .................................................................................................... 1 4 Results and Discussion ............................................................................................................. 16 Data Quality Objectives ................................................................................................................... 16 Statistical Methods and Calculations ................................................................................................. 17 Data Summary and Discussion ......................................................................................................... 17 Conclusions ............................................................................................................................. 23 References ............................................................................................................................... 23 Signatures ................................................................................................................................ 24 Appendix A: Study Protocol EOO- 1311- ..................................................................................... 25 Appendix B: Analytical Methods ............................................................................................... 26 ETS-8-159 "Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicals as the Test Substance"...................................................................................................................... 51 ETS-8-160 "Preparation of Soil Samples for Screening (Tier 11) and Advanced (Tier 111) Sorption Studies for Fluorochemicals as the Test Substance"............................................................................ 74 OECD 106 "Adsorption - Desorption Using a Batch Equilibrium Method" ......................................... 89 ETS-8-155 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream of Water Extracts Using HPLC-Electrospraylhlass Spectrometry" ........................................... 133 ETS-8-110 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Water Extracts Using HPLC-ElectrosprayiMass Spectrometry/Mass Spectrometry" ....................................... 142 Appendix C: Sample Preparation Sheets .................................................................................... 27 Appendix D: Indi.vi.dual Sample Data................................................................................................ 28 Appendix E: Quality Control Sample Data ................................................................................. 29 Appendix F: Notes to File and Deviation forms.......................................................................... 30 Appendix G: Chromatograms .................................................................................................... 31 Appendix H: Raw Data Summaries............................................................................................ 32 Appendix I: Traceability Information......................................................................................... 33 3M Environmental Laboratory Page 5 of 703 BACK TO MAIN List of Tables Table 1. Summary Table of PFOS Adsorb/Desorb Tier I Studies..................................................... 7 Table 2. Summary Table of PFOS Adsorb/Desorb Tier I1 Studies ................................................... 8 Table 3. Summary Table of PFOS AdsorbDesorb Tier I11 Studies.................................................. 8 Table 4. Characterization of the Test Substance, Test System, and Analytical Reference Substances .............................................................................. ........................................... 10 Table 5 . Test System Distribution for Study LRN-E00-1311 ........................................................... 13 Table 6. Sample Collection and Preparation for Study LRN-EOO- 1311...........................................14 Table 7. Suitable Analytical Method Determination......................................................................... 17 Table 8. Suitable Test Vessel Determination..................................................................................... 17 Table 9. Equilibrium Time for Adsorption of PFOS......................................................................... 18 Table 10: Suitable Desorb Solvent, Methanol ................................................................................... 19 Table 11. Stability of PFOS during the Study Period....................................................................... 20 Table 12. Adsorption Kinetics of PFOS, 1 5 Soi1:Solution Ratio, 48 hour Time Point .................... 20 Table 13. Desorption Kinetics of PFOS, 1:5 Soi1:Solution Ratio, 48 hour Time Point ....................2 1 Table 14. Adsorption Isotherms......................................................................................................... 22 Table 15. Desorption Isotherms.........................................................................................................23 Study Personnel and Contributors Study Director Mark E. Ellefson 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Sponsor William K. Reagan, Laboratory Manager 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 3M Environmental Laboratory and Professional Services Contributing Personnel Cindy M. Carlson (Pace Analytical Services, Inc., 1700 Elm St., Minneapolis, MN 55144) Linda A. Goodspeed (Braun Intertec Corporation, 6875 Washington Ave. South, Minneapolis, MN 55439) Kristin L. Terrell (Braun Intertec Corporation, 6875 Washington Ave. South, Minneapolis, MN 55439) Mark L. Anderson (Braun Intertec Corporation, 6875 Washington Ave. South, Minneapolis, MN 55439) 3M Environmental Laboratory Page 6 of 703 BACK TO MAIN Location of Archives All original raw data and the report have been archived at the 3M Environmental Laboratory. The test materials and analytical reference standard reserve samples, as well as the samples pertaining to the analytical phase of this study are archived at the 3M Environmental Laboratory. Reserve samples, digital copies of original data and all original paper data will be retained in the archives of 3M Environmental Laboratory for a period of at least 10 years following the effective date of the applicable final test rule. Summary A preliminary, screening, and advanced study of the soil adsorptioddesorption of Potassium Perfluorooctanesulfonate was performed to better understand partitioning under a variety of environmental conditions. Specifically, three types of soil, one sediment, and one sludge were tested. Analyses were conducted as described by 3M Environmental L,aboratory Analytical Methods ETS-8-159 "Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicals as the Test Substance" and ETS-8-160 "Preparation of Soil Samples for Screening (Tier 11)and Advanced (Tier 111) Sorption Studies for Fluorochemicals as the Test Substance" (Appendix A), according to OECD Guideline 106 "Adsorption - Desorption Using a Batch Equilibrium Method". Results of the study are presented in the following tables: Table 1. Summary Table of PFOS AdsorbDesorb Tier I Studies Question Is the analytical method appropriatehdequate for the study? What is the best test vessel to use? What is the equilibrium time and amount adsorbed at equilibriuiii`? 1 What is a suitable desorption solvent? What is the optimal soi1:solution ratio? Conclusion The 1 :5 soil:solution ratio shows a >50% adsorption for both soils tested. The equilibrium time is 48 hours. 1 II Methanol is a suitable desorption solvent. The optimal soi1:solution Is the test substance sufficiently stable during the study period? The test substance is stable during the course of the study. 3M Environmental Laboratory Page 7 of 703 BACK TO MAIN Table 2. Summary Table of PFOS AdsorbDesorb Tier 11 Studies I Clay (ST-1) I Clay Loam (ST-2) Sandy Loam (ST-3) River Sedimcnt (STSed) I Domestic Sludge (ST-Slg) I 0.0183 I 2.6 I 70.4 0.00972 2.6 31.4 0.0353 2.8 126 0.00742 1.3 57.1 <0.120 I NA I NA Table 3. Summary Table of PFOS AdsorbDesorb Tier III Studies I ~aiidy~oarn I River Seditiieiit Doinestic Sludge 0.0349 0.047 1 0.0100 < 0.237 0.0919 0.0421 0.0560 0.0094 0.0568 0.104 0.082 0.222 0.039 29.5 Introduction F -F FF F. F -F POTASSIUMPERFLUOROOCTANESULFO(PNFAOTSE) CAS Number: 2795-39-3 Chemical Formula: CgF17S03K Molecular Weight: 538.22 g/mol Purpose Adsorption/desorption studies are useful for generating essential information on the mobility of chemicals and their distribution in the soil, water, and air compartments of our biosphere. They can be used in the prediction or estimation of the availability of a chemical for degradation, transformation and uptake by organisms; soil leaching profile; volatility from soil; and run-off from land surfaces into natural waters. Adsorption data can also be used for comparative and modeling purposes. 3M Environmental Laboratory Page 8 of 703 BACK TO MAIN The distribution of a chemical between soil and aqueous phases is a complex process depending on a number of different factors: the chemical nature of the substance, the characteristics of the soil, and climatic factors such as rainfall, temperature, sunlight and wind. Thus, the numerous phenomena and mechanisms involved in the process of adsorption of a chemical by soil cannot be completely defined by a simplified laboratory model such as the present guideline. However, even if this attempt cannot cover all of the environmental possibilities cases, it provides valuable information on the environmental relevance of the adsorption of a cheinical.1 OECD guideline 106 is aimed at estimating the adsorptiorddesorption behavior of a substance on soils. The goal is to obtain a sorption value that can be used to predict partitioning under a variety of environmental conditions. Therefore, equilibrium adsorption coefficients for a chemical onto various soils are determined as a function of soil characteristics. Different soil types must be used in order to emulate the interactions of a given substance with naturally occurring soils. The soil parameters that are believed most important for adsorption are pH, organic carbon content, clay content, and soil texture. The procedures outlined in the guideline are designed to evaluate the adsorption of a chemical on different soil types that have a varying range of pH, organic carbon content, and soil texture. The guideline is comprised of three tiers: 1.1 Tier I: The Preliminary Study 1.1.1 The preliminary study is designed to determine: a) a suitable analytical method b) the adsorption of the test substance onto the surfaces of the test vessels c) the equilibration time for adsorption and the amount of test substance adsorbed at equilibrium d) a suitable desorption solvent e) the soi1:aqueous solution ratio f) the stability of the test substance during the study period 1.1.2 The preparatory methodology for Tier I is described in the 3M Environmental Laboratory Method ETS-8- 159: Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicals as the Test Substance (based on OECD Guideline 106). 1.2 Tier 11: Screening Study: 1.2.1 The screening study is designed to study the adsorption of the test substance in three different soil systems, one sediment, and one dried sludge by means of: a) adsorption kinetics at a single concentration b) determination of distribution coefficients Kd and Koc 1.2.2 The preparatory methodology for Tier I1 is described in the 3M Environmental Laboratory Method ETS-8-160: Preparation of Soil Samples for Screening (Tier 11) and Advanced (Tier 111) Sorption Studies for Fluorochemicals as the Test Substance (based on OECD Guideline 106). 1.3 Tier 111: Adsorption Isotherms and Desorption Kinetics/Desorption Isotherms 1.3.1 The advanced study is designed to: a) determine the Freundlich adsorption isotherms that, in turn, determine the influence of concentration on the extent of adsorption onto the soils, sediment ' According to OECD Guideline 106 3M Environmental Laboratory Page 9 of 703 BACK TO MAIN 1.3.2 and sludge. b) study desorption by means of determining desorption kinetics/Freundlich desorption isotherms The preparatory methodology for Tier 111is described in the 3M Environmental Laboratory Method ETS-8-160: Preparation of Soil Samples for Screening (Tier 11) and Advanced (Tier 111) Sorption Studies for Fluorochemicals as the Test Substance (based on OECD Guideline 106). Materials and Methods Chemical Characterization Table 4. Characterization of the Test Substance, Test System, and Analytical Reference Substances Test Substance I PFOS I THPFOS 1 Source 3M SpecialtyChemicals, Bldg. 236IB-10 SynQuest Labs I Expiration Date 1 8/31/2001 1 none I I Storage Conditions I Frozen I Frozen I I TCR Identification Number I Physical Description 1 TCR-00017-046 I White Powder I TCR-00017-047 I I Whitepowder I I 97.9% 1 TBD I ASTM Type I Water Natural Seawater Aqucous Solution of 3.5% Sodium Chloride n-Octanol 12.7uglnlz, ** 20.2 u g l d ** 56.0 udmL *** 3M Environmental Laboratory Page 10 of 703 BACK TO MAIN Soil Type Source Expiration Date Storage I I Agvise 1:2/31/2015 I I LotNumber I 1 Description 00-2407 Driedand sieved %Organic Carbon I %Sand 2.6% 1 16% Barnes I I Agvise 12/31/2015 Room Temperature I 00-2404 1 Driedand sieved 4.9% I 39% I Clay Loam I Agvise I 12/31/2015 Room 1. Temperature 00-2405 Dried and sieved 2.6% I 21% Sandy Loam River Sediment Agvise 1 Aevise Domestic Sludge 1 NIST -1 811I20 15 12/3 1/20 15 1013 1I2005 99-2564 Dried and 2.8% 5 8% 22% I 00-2046 Dried and I 2781 I Dried and 1.3% I 39% 1 42% NIA I I1 NIA N/A Method Summaries 0 ETS-8-159 "Preparation of Soil Samples for Preliminary (Tier I)Sorption Studies for Fluorochemicals as the Test Substance" 0 Suitable Analytical Method: A soil of high adsorbability (high organic carbon and clay content) is agitated with an appropriate volume of 0.01 M CaC12 solution at a 1 3 (w:v) ratio for a minimum of 4 hours. The mixture is centrifuged and the aqueous phase filtered, if necessary. This "matrix solution" is then prepared by adding lOOuL of 5OOmg/L PFOS in a lOml volumetric flask to reach a nominal concentration within the concentration range that is likely to occur during the test. This "study sample" is then analyzed using HPLCMS. After the study sample has been analyzed, a determination is made as to whether HPLCMS is a suitable analytical method for the test substance. 0 Suitable (Minimally Adsorbing) Container Up to five containers comprising a variety of materials are exposed to a 0.01 M CaC12 aqueous solution dosed with the test substance at a concentration of O.lOmg/L and 1.Omg/L for a minimum of 24 hours. The resulting solution is analyzed for the test substance using HPLCMS. In addition, an extraction of the container walls is made with methanol. This extract is analyzed as well. Any container that adsorbs less than 10% of the test substance onto its walls is considered suitable for use as a study container. Alternatively, the container demonstrating the least amount of test substance absorption is chosen from those tested. 0 Selection of Optimal Soil: Aqueous Solution Ratio, Determination of Equilibration Time, and Stability of the Test Substance Under the Conditions of the Study 3M Environmental Laboratory Page 11 of 703 BACK TO MAIN The optimal soil: aqueous ratio is determined by using two types of soils and three soil: solution ratios. An aqueous solution in contact with the soil is spiked with 125uL of 5OOmg/L PFOS to a concentration of 5 .Omg/L. Sufficient tubes are prepared such that tubes can be removed at intervals (spanning 0 to 48 hr) and the aqueous portion analyzed. Equilibrium is determined by plotting the adsorption of the test substance over time. The optimal soil: solution ratio is determined by comparing of the amount of adsorption of the test substance at equilibrium for the various soil: solution ratio study samples. Acceptable values are soil: solution ratios that give a depletion of the test chemical greater than 20% and preferably greater than 50% at equilibrium. Stability is determined by a mass balance determination following a methanol extraction of the soil. The mass balance determination is conducted on the one soi1:solutionratio per soil that gives a depletion of the test chemical above 20% and preferably above 50% at equilibrium. Suitable Desorption Solvent: Methanol was investigated as the suitable desorption solvent for the test substance. A high clay content soil was dosed with the test substance at two levels (0.75 pg, 7.5 pg). The test substance was then extracted from the study samples three times with methanol. The combined methanol extracts are then prepared for analysis by HPLC/MS. In all cases, adequate quality assurance samples were prepared and analyzed. The equilibration steps were performed at 19 to 30 degrees C. ETS-8-160 "Preparation of Soil Samples for Screening (Tier 11) and Advanced (Tier 111) Sorption Studies for Fluorochemicals as the Test Substance" Tier 11: Adsorption Kinetics (One concentration): Appropriate soils and/or sediments and/or sludges were selected for the study. Replicate study samples containing the soils (or sediments or sludges) are equilibrated by shaking for at least 12 hours at room temperature with 0.01 M CaC12. Study samples are dosed with the test substance at approximately 0.5 mg/L and placed on an orbital shaker. Replicate sets of these study samples are removed at designated time points throughout a 48 hour time period. Study samples are then prepared and analyzed for the target analyte. The adsorption kinetics are determined using this data. The last set of study samples (48 hour) are saved and used for the desorption kinetics portion of the method. Tier 111: Desorption Kinetics (One concentration): After the adsorption kinetics experiment, the 48 hour study samples are centrifuged and the aqueous phase removed. The volume of solution removed is replaced by an equal volume of 0.01 M CaC12 without test substance. The new mixture is agitated until the desorption equilibrium is reached. During a 48 hour period, at defined time intervals, small aliquots of the aqueous phase are removed and analyzed for the target analyte. The experiment then continues with the original mixture. The desorption kinetics are determined using this data. 0 Tier 111: Adsorption Isotherms (Five concentrations): Five test substance concentrations are used, covering two orders of magnitude. Study samples containing soil (or sediments or sludges) in contact with 0.01 M CaC12 are equilibrated for a minimum of 12 hours. After equilibration, the study samples are dosed 3M Environmental Laboratory Page 12 of 703 BACK TO MAIN with test substance. The samples are then gently agitated until adsorption equilibrium is reached. Sample sets are removed from the orbital shaker at designated time intervals. The study samples are then prepared and analyzed for the target analyte. The adsorption isotherms are calculated using this data. The study samples from the last time interval are saved for the desorption isotherm study. 0 Tier 111: Desorption Isotherms: The study samples from the adsorption isotherm study are used for the desorption isotherm study. These samples are centrifuged and the aqueous layer removed. An equal volume of fresh 0.01 M CaC12 solution containing no test substance is added to each sample. The samples are placed in the orbital shaker and equilibrated for 48 hours. The samples are then prepared and analyzed for the target analyte. (These study samples are saved and used to determine mass balance.) The desorption isotherms are determined using this data. Tier 111: Mass Balance: The study samples from the desorption isotherm study are used for the mass balance study. The study samples are centrifuged and the aqueous layer removed. Three portions of methanol are added to the study samples. With each addition of methanol, the study samples are agitated, centrifuged, and the methanol removed and placed in a second container. These subsequent (methanol) study samples are then prepared and analyzed for the target analyte. Mass balance is determined using this data. In all cases, adequate quality control samples are prepared and analyzed. Additionally, the equilibration steps were carried out at between 19 and 30 degrees C. Table 5. Test System Distribution for Study LRN-E00-1311 Tier I "Suitable Analytical Method" Tier I "Suitable Desorption Solvent" Tier I "Suitable (Minimally Adsorbing) Container" Tier I "Selection of Optimal Soil: Solution Ratios" Tier I1 "Adsorption Kinetics" Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks 45 15 18 + 6 Matrix Spikes 9 + 3 matrix spikes 60 + 16 Matrix Spikes 30 + 8 matrix spikes 171 + 57 Matrix Spikes 63 + 21 matrix I I spikes I 1 144+S4p8ikMesatrix 36 + 12 matrix spikes 45 15 18 + 6 Matnx Spikes 9 + 3 matrix spikes 60 + 16 Matrix Spikes 29 + 8 matrix spikes 171 + 57 Matrix Spikes I 139 +48 Matrix Spikes 36 + 12 matrix spikes 3M Environmental Laboratory Page 13 of 703 BACK TO MAIN Tier I11 "Desorption Test Substance 126 + 42 Matrix Kinetics" Solutions Spikes Control Blanks 126 + 42 Matrix Spikes Tier I11 "Adsorption Test Substance 180 + 60 Matrix Isotherms" Solutions Spikes Control Blanks 36 + 12 matrix spikes Tier I11 "Desorption Test Substance 90 + 30 Matrix Isotherms" Solutions Spikes Control Blanks 18 + 6 matrix spikes Tier I11 "Mass Test Substance 90 + 30 Matrix Balance" Solutions Suikes I Control Blanks 1 18 + 6 matrix spikes 1 115 + 42 Matrix Spikes 126 + 42 Matnx Spikes 180 + 60 Matrix Spikes 36 + 12 matrix spikes 89 + 30 Matrix Spikes 18 + 6 matrix spikes 89 + 30 Matrix Spikes 18 + 6 matrix spikes I Specimen Collection and Analysis During the course of the study, aliquots of the test systems were collected at predetermined time intervals. Some sample aliquots were diluted with methanol. The following table describes the sampling regimen information: Table 6. Sample Collection and Preparation for Study LRN-E00-1311 Tier I "Suitable Analytical Work" Tier I "Suitable Container" Tier I "Suitable Desorption Solvent" Each of the three soils, the sediment, and the sludge are equilibrated with 0.01M CaC1, in triplicate. This "matrix solution" is then removed and dosed with the test substance, and the resulting solution analyzed. Four types of test vessels, each of a different material, are exposed to the test substance for 24 hours. The resulting solution is analyzed for the test substance to measure any loss to the container. The test vessel is then extracted to measure any test substance that may have adsorbed onto the sides if the container. Two types of soil are dosed with the test substance, and the soil is extracted with methanol three times. The extracts are combined and analyzed to measure the suitability of the solvent. Each "matnx solution" is dosed in triplicate, and one control sample is prepared. Each type of container is dosed at two concentrations, and a set of controls is also prepared. Every vessel is extracted with methanol after the test substance has been removed. Each type of soil is dosed at two concentrations, and a set of controls is also prepared. Samples aliquotted 11/02/00 Aqueous samples aliquotted 11/14/00 Methanol extractions aliquotted 11/15/00 Methanol extractions aliquotted 1122101 3M Environmental Laboratory Page 14 of 703 BACK TO MAIN Tier I "Selection of Optimal Soil: Solution Ratios and Mass Balance" Tier I1 "Adsoiption Kinetics" Tier 111 "Desorption Kinetics" Tier 111 "Adsorption Isotherms" Tier 111 "Desoiption Isotherms" Tier I11 "Mass Balance Determination Two types of soil are prepared in three soi1:solutionratios to determinethe optimal ratio to use in the remainder of the study. Samplesare prepared at several time points to determine the time required for the solution to reach equilibrium, and a mass balance calculation is performed. Three soils, one sediment, and one sludge are prepared in the soi1:solutionratio indicated in the Tier I study. The samples are dosed with the test substance and placed on a shaker, samples are then pulled at several time points. The aqueous layer is removed from the 48 hour samples from the above step. Fresh CaC1, is added to the test vessel and the vessel is placed on a shaker. Small samples are taken at several time points, and additional aqueous solution is added to replace the sample taken. Three soils, one sediment, and one sludge are prepared in the soi1:solution ratio indcated in the Tier 1study. The samples are dosedwith the test substance (at one of 5 concentrations) and equilibrated for either 0 or 48 hours. The aqueous layer is removed from the 48 hour samples from the above step. Fresh aqueous CaC1, solution is added to the test vessel and the vessel is placed on a shaker for 48 hours. The aqueous solution is removed from the 48 hour samples in the above step. The remaining soil is then extracted with three pofions of methanol, each time the solution is decanted into the same vessel. ~ Each soillratioltime combination is prepared in triplicate, one matrix spike is performed, and one control is prepared. Each soilltime combination is prepared in triplicate, one matrix spike is performed, and a set of controls is prepared. Each 48 hour sample vessel from the above step produces 9 samples over the course of the desorption (seven time points and two matrix splkes). Each soillconcentratiodtime point combination is prepared in triplicate, one matrix spike is performed. Each 48 hour vessel ~ produces one sample, and every third sample is also prepared as a matrix spike. Each 48 hour vessel produces one sample, and every third sample is also prepared as a maisix spike. Aqueous samples aliquotted 11/29/00- 12/4/00 Methanol extractions aliquotted 12/7/00 Aqueous samples aliquotted 2/1/01- 21710 1 Aqueous samples aliquotted 2/13/01- 2/15/01 Aqueous samples aliquotted 2114101- 211 510 1 AqueousGmplesaliquotted 2121101 Methanol extractions aliquotted 2122101- 212610 1 Diluted samples (1.e. sample extracts) containing 250 ng/mL THPFOS as internal standard were analyzed using high-performance liquid chromatography/mass spectrometry (HPLC/MS) in the negative ion mode. PFOS levels were evaluated versus standard curves ranging in concentration from 2.5-1000 ng/mL PFOS and 250 ng/mL THPFOS. Internal Standard quantification was used to best fit and report the data. Target ions were deprotonated PFOS (m!z = 499), and deprotonated THPFOS (m/z = 427). Analytical details are included in the file for this study that is maintained by the 3M Environmental Laboratory; the study folder is located in the 3M archives. All study samples were generated and analyzed at the 3M Environmental Laboratory. No chain of custody forms were generated or required. Reserve samples of reference materials from the 3M Environmental Laboratory will be stored at the 3M Environmental Laboratory for a period not less than 10 years following the effective date of the final test rule, or until the quality of the preparation no longer affords evaluation. Reserve 3M Environmental Laboratory Page 15 of 703 BACK TO MAIN samples of the reference materials from the contract laboratory will be returned to the 3M Environmental laboratory for retention and archiving. Results and Discussion Data Quality Objectives The following data quality objectives are from the methods used in the present study. The data quality objectives were met, except as documented in raw data. Coefficient of Determination (r2). The coefficients of determination (r2) for the calibration curves were 0.985 or greater. The curves were examined closely for accuracy of quantitation at the low and high ends of the curve. Quadratic curve fit was applied to calibration standards and sample data to improve quantitation over the concentration range appropriate to the data. Method Blanks. Method blanks (applicable sample matrix taken through the entire sample preparation, dilution, and analysis process) provided a measure of laboratory contamination. Acceptable values for the blanks were less than 50% of the limit of quantitation (LOQ), defined herein as the concentration of the lowest standard. Matrix Spike Recoveries. A post-preparatory matrix spike sample for each of the sample groups used in the study was prepared by adding aliquots of test-analyte solution according to 3M Method ETS-8-159 and 160. The spike recoveries for >80% of the samples were acceptable (100 k 30%). Instances where spike recoveries outside of the control range were observed are indicated in Appendix E. Sample Triplicates. The Relative Standard Deviations of triplicate samples were acceptable when at least 80% of them were less than or equal to 30%. Q-tests were used to exclude outliers in data sets. Continuing Calibration Verification. If the percent difference for the amount of quantitated analyte was greater than 30% from the true value relative to the initial standard curve, only those samples analyzed before the last acceptable calibration check standard were used. The remaining samples were analyzed with a new curve. Limit of Quantitation (LOQ). The LOQ was equal to the lowest acceptable standard in the calibration curve. Calibration Standards. Eleven standards ranging in concentration from approximately 2.5 to 1000ng PFOS/mL methanol were used for the calibration curves. Calibration curves were run before and after every analytical sequence. Solvent Blanks. Solvent (Methanol) blanks provide a measure of instrumental contamination. Acceptable values for the blanks were less than 50% of the limit of quantitation, defined herein as the lowest calibration standard. System Suitability. Without performing a method validation, system suitability was demonstrated by acceptable instrumental checks (e.g abbreviated m/z check-tune, or full auto-tune routines). 3M Environmental Laboratory Page 16 of 703 BACK TO MAIN Statistical Methods and Calculations Means and standard deviations were calculated using functions provided in Microsoft@ Excel@ software. Calculations with the raw data were made using the equations described in the OECD Method 106 (see Appendix B). Data Summary and Discussion Appendices D and E summarize individual sample data. Representative chromatograms are presented in Appendix G. All concentrations and calculations can be found in the data tables, along with the log plots used to determine the isotherm values. These data are used in all subsequent tables and figures in this report. Results of the Tier I study are presented in table 7 through 11: Table 7. Suitable Analytical Method Determination I%arneLs oam (ST-1) Clay Loam (ST-2) Clay (ST-3) River Sediment(STSed) Domestic Sludge (STSlg) E00-131 1-0001,-0002,-0003 E00-1311-0004, -0005, -0006 EOO-13 1 1-0007, -0008, -0009 E00-1311-0010,-0011,-0012 EOO-1311-0013, -0014, -0015 Table 8. Suitable Test Vessel Determination 115% 1 IS% 99.8% 116% 88.3% 21.81 8.88 15.97 I Polypropylene I Polystyrene Glass Teflon 96.19% 94.51% 96.74% 89.49% I I I 244.36ppb 116.18% ~ 172.43ppb 203.04% 397.75ppb 206.69% 94.37ppb 170.45% It was determined that the polypropylene centrifuge tubes were suitable for this study. These tubes had the least amount of extractable PFOS, and were the only tubes with acceptable matrix spike recoveries. 3M Environmental Laboratory Page 17 of 703 BACK TO MAIN Table 9. Equilibrium Time for Adsorption of PFOS Clay ~ ~~ Sediment 1:l 1.5 1 :25 1:l 1.5 1: 2 5 I 36 I 20.98% 48 12.74% 24 21 3 3 % 23.51% 19.71% 24 57.42% 36 60.15% 48 66.80% 24 I 1.04% 36 14.32% I 48 I 10.63%1 I 24 I 45.85% 36 45.010/;, 48 42.19%) 65.34% 67.310/;, I 48 I 6X.00% 100.00 r' .0- 80.00 U 0 v) 60.00 U Q 40.00 ' ? m I U r 20.00 a 2 a a 0.00 0 Adsorption Equilibrium Plot -- - --t 1:IRatio (clay) 1.5Ratio (clay) +-1:25 Ratio (clay) 20 40 60 Equilibrium Time, hours 3M Environmental Laboratory Page 18 of 703 BACK TO MAIN ~ ~_.._______ _-____ I Adsorption Equilibrium Plot I ~ 100.00 80.00 s 60.00 40.00 I --e 1:l Ratio (Sediment) 1:5 Ratio (sediment) 1 2 5 Ratio (sediment) ~ 20.00 0.00 0 20 40 60 EquilibriumTime, hours 1- I I I ____~ The test substance appeared to reach equilibrium after 24 hours in all of the soi1:solution ratios. The clay appeared to take more time to reach equilibrium, therefore the 48 hour time point was used as the equilibrium time for the remainder of the study. This ensured that all five of the soils were given ample time to equilibrate. Table 10: Suitable Desorb Solvent, Methanol Clay I Sediment 1 - 0.0 < 25.0 100 71.2 71.2% 1000 591 59.1% 0.0 I < 25.0 - 1 1 7 100 1000 60 1 60.1% Despite using methanol, an excellent solvent for PFOS, the average percent recovery of PFOS ranged from zero to 96%. It is unlikely that a different solvent would yield better recovery. Previous results in this study have indicated that the test substance is readily and rapidly adsorbed on the soil, and is not likely to be completely extracted from it. . The optimal soi1:solution ratio was determined to be 1:5 (refer to Table 9 for applicable data). This ratio demonstrated average adsorption percentages of PFOS ranging from approximately 75% in clay to 55% in sediment. 3M Environmentaf Laboratory Page 19 of 703 Table 11. Stability of PFOS during the Study Period Clay BACK TO MAIN Sediiiient According to OECD guideline 106, the mass balance calculation should show at least 90% recovery of the test substance for the test substance to be considered stable over the course of the study. The recovery of the test substance was lower than the OECD guideline, likely due to the incomplete desorption of the test substance from the soil. Hydrolysis studies of PFOS conducted at the 3M Environmental Laboratory have demonstrated test substance stability in aqueous matrices. The results of the Tier I1 study are presented in Table 12: Table 12. Adsorption Kinetics of PFOS, 1:5 SoikSolution Ratio, 48 Hour Time Point I 1 ClayLoam(ST-2) I I Sandy Loam (ST-3) River Sediment (ST-Sed) Domestic Sludge (ST-Slg) 0.00972 0.00742 <0.120 26 I 2.6 I 1.3 NA I 70 4 37.4 I 3M Environmental Laboratory Page 20 of 703 BACK TO MAIN 100 90 80 70 60 50 40 30 20 10 0 0 ___________________~. Adsorption Percentage as a Function of Time +Sandy Loam -W-River Sediment 10 20 30 40 50 Time, hours All of the soil/sediment/sludge matrices adsorbed the test substance strongly. The sludge samples, in the adsorption portion of the kinetics study, demonstrated very strong adsorption (>96%) and PFOS was not detected in the samples. The data indicates that adsorption occurred within the first few hours of exposure and the test substance concentration does not vary significantly after the 16 hour time point. The results of the Tier I11 study are presented in Tables 13 through 15: Table 13. Desorption Kinetics of PFOS, 1:5 Soi1:Solution Ratio, 48 hour Time Point Barnes h a i n (ST-I) Clay Loam (ST-2) Clay (ST-3) River Sediment (ST-Sed) Domestic Sludge (STSlg) 0.047 1 0.0158 0.0349 0.0100 < 0.237 3M Environmental Laboratory Page 21 of 703 BACK TO MAIN I , 80.00 70.00 60.00 .'. ' 50.00 18 '=52 40.00 0 $ 30.00 0 20.00 10.00 0.00 0 Desorption Percentage as a Function of Time ~-A- Sandy Loam +River Sediment 10 20 30 40 50 Time, hours The test substance was poorly desorbed from the soil/sediment/sludge matrices during the 48-hour study period. The river sediment displayed the most desorption at only 39% after 48 hours. The sludge samples did not desorb a detectable amount of test substance. Desorption that did occur was accomplished rather quickly, after the 8 hour time point the test substance concentration did not vary significantly. Table 14. Adsorption Isotherms Clay Loam Domestic Sludge -1.2515 -1.3762 - 1.0369 -2.0261 -1.246 0.0560 0.0421 0.0919 0.0094 0.0568 0.884 0.841 0.829 0.989 1.2581 1.13 1.19 1.21 1.01 0.795 3M Environmental Laboratory Page 22 of 703 BACK TO MAIN Table 15. Desorption Isotherms Clay Clay Loam Sandy Loam River Sediment Domestic Sludge -0.653 -1.084 -0.981 -1.41 1.47 ~ 0.222 0.082 0.104 0.039 29.5 0.935 0.954 1.01 1.02 0.327 1.07 1.05 0.988 0.984 3.06 Freundlich isotherms relate the amount of test substance adsorbed on the soil to the amount present in the aqueous solution at equilibrium. The values calculated for the regression constant indicate that the data obtained for the test substance over two orders of magnitude is slightly nonlinear. Conclusions Perfluorooctanesulfonate (PFOS) strongly adsorbs to all of the soil/sediment/sludge matrices tested. The test substance, once adsorbed, does not desorb readily, even when extracted with an organic solvent. In either case, adsorption or desorption, an equilibrium is achieved in less than 24 hours, with substantial adsorption (>50%) occurring in some of the time 0 samples. The low recoveries demonstrated by the mass balance calculations are likely the result of the test substance being strongly adsorbed, since it is unlikely that the test substance degraded during the course of this study. References 1. Adsorption-Desorption Using a Batch Equilibrium Method (OECD 106), January 2000. 3M Environmental Laboratory Page 23 of 703 BACK TO MAIN The final draft of this report is a true representation of the data developed in this study. It has been issued by: Mark E. hllefson, Study Director Management Dhe ' 3M Environmental Laboratory Page 24 of 703 Appendix A: Study Protocol E00-1311- Soil AdsorptionLDesorptionStudy of Potassium Perfluorooctanesulfonate BACK TO MAIN 3M Environmental Laboratory Page 25 of 703 BACK TO MAIN -- STUDY PROTOCOL STUDY TITLE Soil AdsorptiodDesorptionStudy of Perfluorooctanesulfonate(PFOS) SPONSOR William K. Reagen, Ph.D. TESTING FACILITY 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St Paul, MN 55106 LABORATORY STUDY IDENTIFICATION Laboratory Request Number (LRN)-EOO- 1311 3M Environmental Laboratory BACK TO MAIN 4 Laboratory Request Number (LRN)--E00-13111 Protocol Signatures Study Director: 3M Environmental Laboratoh Protocol Approval Sponsor: William K. Reagen, Ph.D. 3M Environmental Laboratory /cl//ir/uo Date: 3M Environmental Laboratory I Page 2 of 19 I I 4 BACK TO MAIN - Laboratory Request Number (LRN)-E00-1311 I STUDY IDENTIFICATION Soil Adsorption/DesorptionStudy of Perfluorooctanesulfonate(PFOS) TESTSUBSTANCE SPONSOR SPONSOR EPRESENTATIVE STUDYDIRECTOR TESTFACILITY PROPOSESDTUDYTIMETABLE Perfluorooctanesulfonate (PFOS) 3M Environmental Laboratory 935 Bush Avenue, Building 2-3E-09 St. Paul, MN 55106 William Reagen, Ph.D. 3M Environmental Laboratory 935 Bush Avenue, Building 2-3E-09 St. Paul, MN 55 106 (65 1)778-6565 Mark E. Ellefson 3M Environmental Laboratory 935 Bush Avenue, Building 2-3E-09 St. Paul, MN 55106 (65 1)778-5405 3M Environmental Laboratory 935 Bush Avenue, Building 2-3E-09 St. Paul, MN 55106 Experimental Start Date Experimental Termination Date 18 October 2000 15 December 2000 BACK TO MAIN I I Laboratory Request Number (LRN)-E00-1311 1.O Introduction and Purpose/Objective 1.1 Adsorptioddesorption studies are useful for generating essential information on the mobility of chemicals and their distribution in the soil, water and air compartments of our biosphere. They can be used in the prediction or estimation of the availability of a chemical for degradation, transformation and uptake by organisms; leaching through the soil profile; volatility from soil; and run-off from land surfaces into natural waters. Adsorption data can also be used for comparativeand modeling purposes.' The distribution of a chemical between soil and aqueous phases is a complex process depending on a number of different factors: the chemical nature of the substance, the characteristics of the soil, and climatic factors such as rainfall, temperature, sunlight and wind. Thus, the numerous phenomena and mechanisms involved in the process of adsorption of a chemical by soil cannot be completely defined by a simplified laboratory model such as the present guideline. However, even if this attempt cannot cover,all the environmentally possible cases, it provides valuable information on the environmental relevance of the adsorption of a chemical.' 1.2 The target substance for this study is presented in Table 1.1 Table 1.1 Target Substance Target Substance Perfluorooctanesulfonate PFOS CeFi7SO3' I 3M Environmental Laboratory identification Number TCR-00017-46 2.0 Regulatory Compliance 2.1 By complying with the requirements of OECDIOCDE Guideline 106, the data will meet the testing requirements of the European Community and Canada. The data will also be used to meet the testing requirements of the Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) and the Toxic Substances Control Act (TSCA) in the United States. 2.2 This study will be conducted in accordance with the United States Environmental Protection Agency TSCA Good Laboratory Practice (GLP) Standards 40CFR Part 792. 1According to OECD Guideline 106 3M Environmental Laboratory 3M Environmental Laboratory page 4 of 19 I Page 29 of 703 BACK TO MAIN . h Laboratory Request Number (LRN)-E00-1311 I 3.0 Test Substance ' 3.1 Identification: Perfluorooctanesulfonate,CsF17S03- (PFOS;) 3.2 Source: 3M Specialty Materials Division 3.3 Description: white powder 3.4 3M Environmental Laboratory ID#: TCR-00017-46 3.5 Storage Conditions:PFOS should be stored at ambient temperature or lower. 3.6 Purity: 97.3% 3.7 Expiration Date: 2010 3.8 Retention Sample: A retention sample of the test substance (0.34 g) has been taken and stored frozen at -20C doc.The sample will be archived for at least the period as required by the EPA GLPs, Section 792.195. 3.9 Safety Precautions: 3.9.1 Wear appropriate laboratory attire. 3.9.2 An MSDS sheet is available on this substance and is accessible using the 3M Environmental Laboratory Lotus Notes TCR database. 4.0 Control Substances 4.1 There are no control substances in this study. 5.0 Reference Substances 5.1 THPFOS 5.1.1 Zdentaficution: 1H, 1H, 2H, 2H-Perfluorooctane Sulphonic Acid, C~HsF1303S(THPFOS) 5.1.2 Source: SynQuest Labs 5.1.3 Description: Fluffy, white crystals 5.1.4 3M Environmental Laboratory ID#: TCR-00017-047 5.1.5 Storage Conditions: THPFOS should be stored at ambient temperature or lower 5.1.6 Expiration Date: 2010 5.1.7 Retention Sample: A retention sample of 0.27 g of THPFOS has been taken and stored frozen at -2OoC+_5"CT. he compound will be archived for at least the period as required by the EPA GLPs, Section 792.195. 5.1.8 Safety Precautions: 3M Environmental Laboratory Page 5 of 19 3M tnvironmental Laboratory Page 30 of 703 BACK TO MAIN I I Laboratory Request Number (LRN~--E00-1311 5.1.8.1 Wear appropriate laboratory attire. 5.1.8.2 An MSDS sheet is available on this substance and is accessible 1 using the 3M Environmental Lotus Notes TCR database. 5.2 PFOS 5.2.1 Identification: Perfluorooctanesulfonate,CsF17S03(-PFOS) 5.2.2 Source: 3M Specialty Materials Division 5.2.3 Description: White powder 5.2.4 3M Environmental Zdzboratory ID#: TCR-00017-46 5.2.5 Storage Conditions: PFOS should be stored at ambient temperature or lower 5.2.6 Purity: 97.3% 5.2.7 Expiration Date: 2010 5.2.8 Retention Sample: A retention sample of 0.34 g PFOS has been taken and stored frozen at -20C G"C. The compound will be archived for at least the period as required by'the EPA G u s , Section 792.195. 5.2.9 Safety Precautions: 5.2.9.1 Wear appropriate laboratory attire. 5.2.9.2 An MSDS sheet is available on this substance and is accessible using the 3M Environmental Lotus Notes TCR database. 6.0 Test System 6.1 The test system consists of three soil types, one sediment and one dried sludge in contact with a 0.01 M CaC12 aqueous solution. 6.2 The criteria for selection of the soils are based on Table 1 of the OECD Guidelines 106. 6.3 The soils used in this study were characterized using GLP guidelines. 6.4 Although not specified in OECD Guideline 106, one sediment was also selected as part of the test system. 6.5 Although not specified in OECD Guideline 106, one dried sludge was also selected as part of the test system. 7.0 Analytical Scheme and Control of Bias 7.1 OECD Guideline 106 is aimed at estimating the adsorptioddesorption behavior of a substance on soils. The goal is to obtain a sorption value that can be used to predict partitioning under a variety of environmental conditions. Therefore, equilibrium adsorption coefficients for a chemical onto various soils are determined as a function of soil characteristics. Different soi 1 types must be used 3M Environmental Laboratory Page 6 of 19 3 M tnvr.ronmenfal Laboratory Page 31 of 703 BACK TO MAIN 1 . I I Laboratory Request Number (LRN)-E00-1311] in order to cover as widely as possible the interactions of a @veri substance with naturally occurring soils. The soil parameters that are believed most important for t adsorption are pH, organic carbon content, clay content and soil texture. The procedures outlined in the guideline are designed to evaluate the adsorption of a chemical on different soil types that have a varying range of pH, organic carbon content, clay content and soil texture. The guideline is comprised of three tiers: 7.1.1 Tier I: The Preliminary Study 7.1.1.1 The preliminary study is designed to determine: a) a suitable analytical method b) the adsorption of the test substance onto the surfaces of the test vesse1s c) the equilibration time for adsorption and the amount of test substance adsorbed at equilibrium d) a suitable desorption solvent e) the soi1:aqueous solution ratio f) 7.1.1.2 the stability of the test substance during the study period The preparatory methodology for Tier I is described in the 3M Environmental Laboratory Method ETS-8- 159: Preparation of Soil Samplesfor Preliminary (Tier I ) Sorption Studiesfor Fluorochemicals as the Test Substance (based on OECD Guideline 106). 7.1.2 Tier 11: Screening Study: 7.1.2.1 The screening study is designed to study the adsorption of the test substance in three different soil systems, one sediment and one dried sludge by means of: a) adsorption kinetics at a single concentration b) determination of distribution coefficients & and GC 7.1.2.2 The preparatory methodology for Tier II is described in the 3M Environmental Laboratory Method ETS-8- 160: Preparation of Soil Samplesfor Screening (Tier II) and Advanced (Tier III) Sorption Studiesfor Fluorochemicalsas the Test Substance (based on OECD Guideline 106). 7.1.3 Tier 111: Adsorption Isotherms and Desorption Kinetics/Desorption Isotherms 7.1.3.1 The advanced study is designed to: a) determine the Freundlich adsorption isotherms that, in turn, determine the influence of concentration on the extent of 3M Environmental Laboratory Page 7 of 19 3M tnvironmental Laboratory Page 32 of 703 - 6 I BACK TO MAIN Laboratory Request Number (LRN)--E00-1311 I adsorption onto the soils, sediment and sludge. b) study desorption by means of determining desorption i kineticsFreundlich desorption isotherms 7.1.3.2 The preparatory methodology for Tier III is described in the 3M Environmental Laboratory Method ETS-8- 160: Preparation of Soil Samplesfor Screening (TierII) and Advanced (Tier III) Sorption Studiesfor Fluorochemicalsas the Test Substance (based on OECD Guideline 106). 7.2 The adsorptioddesorption studies will be conducted according to a modified version of the OECD Guideline for the Testing of Chemicals 106 "AdsorptionDesorption Using a Batch Equilibrium Method." 7.3 The preliminary section of OECD Guideline 106 (Tier I) refers to performancebased criteria. This document outlines minimally acceptable criteria to be met before actually beginning Tiers I1 and 111.The study plan outlined for Tier I is an attempt to meet these criteria. The procedures used in the 3M Environmental Laboratory for Tier 11and Tier 111will follow as closely as practical the procedures outlined in Guideline 106. However, fluorochemicals have unique properties that may prohibit the criteria being precisely met. In these instances, modifications to the criteria may be necessary. Where this is the case, the reason for the modification will be stated and documented. 7.4 Sufficient controls and blanks will be incorporated as part of this study to ensure control of bias. These controls and blanks are described in more detail within this protocol. 8.0 Preparatory Methods 8.1 The study sample numbering scheme will be as follows: 8.1.1 Each study sample, each control sample, each control blank and all of their aliquots throughout the course of the study will have a unique identifier. 8.1.2 When the initial study samples are set up, each will be given a number beginning with the designator "E00-1311"which is the Laboratory Study Identification Number for this Study Protocol. These initial study samples will then be numbered sequentially for each section by the addition of a four digit number. 8.1.3 Each section will have its own unique section number (e.g. 1000, 2000, etc.) unless that section does not generate any "new"study samples, but continues use of the study samples from a previous section. 8.1.4 If more than one aliquot is taken from a study sample during the course of a section, a designator of S 1, S2, S3, etc. will be included to uniquely identify that aliquot. 3M Environmental Laboratory 3M tnvwonmental Laboratory Page 33 of 703 BACK TO MAIN I . * Laboratory Request Number (LRN)--E00-1311] 8.1.5 A study sample that is used in a following section will maintain its original unique identifier, but will continue with the appropriate addition 1 of the S1, S2, S3 designators as described above. 8.1.6 Each spike sample will include all of the above designators as well as the additional designator of "-MS" added to it to identify is as a Matrix Spike. 8.1.7 Example Numbering Scheme: See Attachment A Section A: Tier I, Preliminary Study This section details the general methodology used to determinethe range-finding and method development aspects of OECD Guideline 106. 8.2 Suitable Analytical Method: 8.2.1 Previous work with the test substance in a variety of matrices have strongly indicated that the analysis of PFOS in the aqueous/soil matrix described in OECD Guideline 106 can be accomplished by dilution of a portion of the centrifuged aqueous portion with methanol in a 1:l ratio. The resulting aliquot can then be analyzed using HPLC/MS/MS. 8.2.2 Refer to 3M Environmental Laboratory Method ETS-8-159 for the preparation of the study samples to be used. Refer to 3M Environmental Laboratory Method ETS-8-110for the analytical methodology. 8.2.3 Acceptable analytical method performance criteria is identified in 3M EnvironmentalLaboratory Document ETS-8-005. Data generated from Section 8.2 will be evaluated using the criteria in the referenced document. If the analytical method meets these criteria, the method will be determined to be appropriate for this study. 8.2.4 If it is determined that a preparatory cleanup step is necessary, solid phase extraction may be used as described in 3M EnvironmentalLaboratory Method ETS-8-154. 8.3 Suitable Container: 8.3.1 A minimally adsorbing container for the test substance is desirable for Tiers 11and 111of the Adsorption/Desorption study in order to generate the most useful information possible. However, due to the unique properties of fluorochemicals, significant adsorption of the test substance to the container walls is possible. Therefore, it may only be possible to determine which container from a variety of those tested will demonstrate the least adsorption of the test substance to it. This study will generate documentation that the container material used for Tiers 11and 111is the most suitable container of those tested. 3M Environmental Laboratory 3M tnvrronmental Laboratory Page 9 of 19 Page 34 of 703 BACK TO MAIN . , 8. Laboratory Request Number (LRN)--E00-1311 I 8.3.2 Test a reasonable variety of materialskontainers. They may include, but are not limited to, the following: Teflon@centrifuge tubes, Pyrex@glass 1 centrifuge tubes, polypropylene centrifuge tubes, polystyrene centrifuge tubes, and styrene butadiene centrifuge tubes. (Use 15-mL centrifuge tubes whenever possible.) 8.3.3 Two concentrations of the test substance will be used (0.1 mg/L and 1 mgL). 8.3.4 Equilibrate 12.5 mL of a 0.01 M CaC12 aqueous solution containing the test substance (at concentrationsof 0.1 m g L and 1 m&) for approximately 24 hours with the container. After that time, dilute a portion of the aqueous solution with methanol and analyze using HPLCMSMS to determine the amount of adsorption by the container. In addition, extract the walls of the container with methanol and analyze the methanol for the test substance. 8.3.5 Refer to Method ETS-8-159 for more details of this procedure. 8.3.6 Calculate the amount of test substance adsorbed onto each container. 8.3.7 The most appropriate container (based on minimal adsorptivity, convenience and cost) will be selected for use in Tiers 11and III. 8.4 Suitable Desorption Solvent: 8.4.1 Previous work with the test substance has indicated that methanol will be a suitable solvent for the desorption steps described in OECD Guideline 106. This assumption will be further investigated and confirmed. 8.4.2 Dose the test substance (at 2 pg and 20 pg) onto 2.5 grams of a strongly adsorbing (high clay content) soil. 8.4.3 Extract the soils with three 2.5-mL portions of methanol to desorb the test substance back off the soil. 8.4.4 Refer to Method ETS-8-159 for more details of this procedure. 8.4.5 If this process cannot recover 80% or more of the test substance, investigate a minimum of three other solvents. (These alternative solvents will be chosen based on the experience and knowledge of the analytical team leader.) 8.4.6 Choose the most suitable solvent (based on maximum desorption, convenience and cost) of those tested. 8.5 Selection of Optimal Soi1:Aqueous Solution Ratio, Determination of Equilibration Time, and Stability of the Test Substance under Conditions of the Study 8.5.1 Use two soil types and three soi1:solution ratios (six experiments). One soil type should have a high organic carbon and low clay content, and the other soil should have a low organic carbon and high clay content. Prepare the following ratios of soil and test substance: 3M Environmental Laboratory page10of19 I 3M tnvlronmental Laboratory Page 35 of 703 BACK TO MAIN , I. . Laboratory Request Number (LRN)-E00-1311 I 8.5.1.1 Equal parts (w:v) of soil to aqueous solution containing test substance 8.5.1.2 A 1:5 ratio (w:v) of soil to aqueous solution containing test substance 8.5.1.3 A 1:25 ratio (w:v> of soil to aqueous solution containin-g test substance 8.5.2 Dose the test substance such that the final concentration of test substance in solution is approximately 1 mgL. 8.5.3 Prepare control samples containing only the test substance in 0.01 M CaC12 solution (no soil) in order to check the stability of the test substance in the 0.01M CaClz solution. 8.5.4 Prepare background control samples containing soil and aqueous 0.01M CaClz (no test substance) using the same soi1:solution ratios as part of the study. 8.5.5 Prepare and analyze all study samples and controls in triplicate. In addition, spike a portion of one replicate from each triplicate set with additionaltest substancein order to determine spike recoveries. 8.5.6 Prepare a sufficient number of individual containers of each series such that a (triplicate) set of vials can be removed according to the following approximate time intervals: 0 hr, 2 hr, 4 hr, 8 hr, 16 hr, 24 hr, 36 hr and 48 hr . 8.5.7 Refer to Method ETS-8-159 for further details of this procedure. 8.5.8 The data generated from these study samples allow the estimation of the equilibrium plateau. Calculate the & value at equilibrium. Based on this & value, select appropriate soi1:solution ratios such that the percentage adsorption is between 20% and 80%. 8.5.9 Based on the data generated from this section, determine the stability of the test substance under the conditions of the study. Section B: Tier ZZ Screening Study 8.6 Adsorption Kinetics at One Concentration of the Test Substance: 8.6.1 Prepare control samples containing only the test substance in 0.01 M CaC12 solution (no soil) in order to check the stability of the test substance in 0.01M CaC12solution. 8.6.2 Include background control samples containing soil and aqueous 0.01M CaC12 (no test substance) in the same soiksolution ratios. 8.6.3 Set up and analyze all study samples and controls in triplicate. In addition, spike a portion of one of each triplicate with additional test substance in order to determine spike recoveries. 1 3M Environmental Laboratory page 11 of 19 I 3 M tnvironmental Laboratory Page 36 of 703 BACK TO MAIN , .b . Laboratory Request Number (LRN)-E00-1311 I 8.6.4 Select three soil types using the guidance given in Table I of OECD method 106, one sediment and one dried sludge. 1 8.6.5 Prepare a sufficient number of individual containers of each series such that a (triplicate) set of vials can be removed according to the following approximate intervals: 0 hr, 2 hr, 4 hr, 8 hr, 16 hr, 24 hr,36 hr and 48 hr. 8.6.6 Refer to Method ETS-8-160 for further details of this procedure. 8.6.7 Calculate the percentage adsorption of the test substance onto the soil at each time point and/or time interval and plot % adsorption versus time. Calculate the distribution coefficient at equilibrium. 8.6.8 Calculate the organic carbon normalized adsorption coefficient. Section C: TierI l l 8.7 Desorption Kinetics-Serial Method: 8.7.1 Using the last set of sample vials (hour 48) from the Tier II Adsorption Kinetics study, centrifuge the vials and remove as much of the aqueous layer as possible. 8.7.2 Replace the volume of solution with an equal volume of fresh 0.01 M CaC12 solution containing no test substance. 8.7.3 Agitate the new mixture until the desorption equilibrium is reached (as determined in Section 8.5. 8.7.4 Throughout this time, at defined time intervals, prepare study sample aliquots for analysis. 8.7.5 Proposed time periods are: 2 hr, 4 hr, 8 hr, 16 hr, 24 hr, 36 hr and 48 hr. 8.7.6 Refer to Method ETS-8-160 for further details of this procedure. 8.7.7 Calculate the percentages of desorption at each time point and/or time interval and plot percentage desorption versus time. 8.7.8 Calculate the desorption coefficient at equilibrium. 8.8 Adsorption Isotherms: 8.8.1 Prepare control samples containing only the test substance at the same concentrations as the study samples in 0.01 M CaCh solution (no soil). 8.8.2 Prepare background control samples containing soil and aqueous 0.01M CaC12(no test substance) in the same soi1:solution ratios as part of the study. 8.8.3 Prepare and analyze all study samples and controls in triplicate. In addition, spike a portion of one of each triplicate with additional test substance in order to determine spike recoveries. 8.8.4 For the adsorption isotherm determination, prepare five sample sets with initial concentrations of approximately 0.05,0.2,0.5, 1.0,and 5.0 mgL for each of the selected three soil types, sediment and sludge. Use the 3M Environmental Laboratory 3M Environmental Laboratory Page 37 of 703 BACK TO MAIN , I. . Laboratory Request Number (LRN)-E00-1311 I same soi1:solution ratio as that used in the Tier II study. (Iftheamount of adsolption of the test substance onto the soils will produce concentrations in the adsorption solvent which would border on,or be below, the quantflcation limits of the test substance, the concentration levels may need to be increased. The criteria that should be met are that the concentration range should span two orders of magnitude.) 8.8.5 Samples are placed in an orbital shaker until equilibrium time is established (or for a maximum of 48 hours). 8.8.6 Refer to Method ETS-8-160 for further details of this procedure. 8.8.7 Analyze the aqueous portion to (indirectly) determine the amount of test substance adsorbed onto the soil. 8.8.8 Plot the adsorbed mass of test substance per unit mass of soil as a function of the equilibrium concentration of the test substance. 8.9 Desorption Isotherms: 8.9.1 Determine Freundlich desorption isotherms on the soils used in the adsorption isotherms study. 8.9.2 Using the last set of study samples generated from the Adsorption Isotherm Study (Section 8.8), perform the desorption test using 0.01M CaClz solution as described in the "Desorption Kinetics" section (exception: the aqueous phases will be analyzed only once, at desorption equilibrium.) 8.9.3 Refer to Method ETS-8-160 for further details of this procedure. 8.9.4 Calculate the amount of the test substance desorbed. 8.9.5 Plot the content of test substance remaining adsorbed on the soil at desorption equilibrium as a function of the equilibrium concentration of the test substance in solution. 8.9.6 In addition, determine a mass balance by finding the concentration of the substance desorbed using an organic solvent (methanol) from the soil for one concentration. 8.9.7 Refer to Method ETS-8-160 for further details of this procedure. 9.0 Analytical Methods 9.1 ETS-8-110. Analysis of Perfluorooctanesulfonateor Other Fluorochemicalsin Water Extracts Using HPLC-ElectrosprayMassSpectrometryMass Spectrometry 9.2 Additional methods may be developed at a later time and will be listed as protocol amendments. 3M Environmental Laboratory 3M tnvironmental Laboratory Page 38 of 703 BACK TO MAIN . .s . Laboratory Request Number (LRN)--E00-1311~ 10.0 Data Quality Objectives t 10.1 Tier Z only-Although the statistical data will be generated from the Tier study, the primary purposes of Tier I are to determine an appropriate container, analytical method, desorption solution, and soi1:solution ratio. Tier I is also for range-finding in order to successfully proceed to Tiers II and III of the adsorptioddesorption study. 10.2 Linearify-The measure of fit of the calibration curve, as measured by the coefficient of determination (r2)will be 0.980 or greater. The curve may include the origin, but should not be "forced" through the origin. 10.3 Limits of Detection/Quuntitatn-The LOQ is estimated at 5 pg/L at the instrument level. This would result in a Limit of Quantitation of 10 pg/L for the sample (1 :1 dilution in the preparation procedure). However, during the study, the LOQ will be equal to the lowest calibration standard used in the calibration curve and that is greater than two times the background "noise". 10.4 Matrix Spike Frequency-An aliquot of one replicate from each triplicate set will be spiked with a known amount of substance, except as noted in the referenced methods. 10.5 Acceptable Recoveries-Upon completion of the analytical method validation portion of the study, an amendment to the protocol will be written defining acceptable criteria based on the validation results. 10.6 Use of Reference Materials- 10.6.1 THPFOS-The reference material THPFOS will be used to determine gross instrument failure when using HPLC/MS/MS. Gross instrument failure is defined by a G O % deviation in standards and calibration checks. THPFOS is not used for quantitative purposes because the magnitude of response may not be consistent between standards and samples, although the response among a single group is expected to be consistent. THPFOS will be added to samples as the last step of the preparatory procedure. An equivalent concentration of the reference material will also be added to the calibration standards. 10.6.2 PFOS (TCR-00017-46)will be used to make the calibration standards, as well as being used as the test substance. Since commercial standards of known purity are unavailable for each isomer and since the isomer ratios of PFOS very from lot to lot, using the same lot number for the calibration standards provides the most accurate measure of the concentration of PFOS in the analyzed samples. 10.7 Use of Confirmatory Methods-No confirmatory methods will be used. The analytical method uses a very selective detector (mass spectrometer) with a chromatographicseparation method. 3M Environmental Laboratory 3M Environmental Laboratory Page 39 of 703 BACK TO MAIN . I* . Laboratory Request Number (LRN)-E00-1311 I 10.8 Demonstration of Specificity- 10.8.1 HPLC/MS/MS-Unique and characteristic product ions are monitored for 1 each analyte. In addition, a chromatographic separation method is employed. 10.9 Precision- 10.9.1 Precision will be measured by determining the relative Standard Deviation of triplicate samples. 10.9.2 Upon completion of the analytical method validation portion of the study, an amendment to the protocol will be written defining acceptable criteria , based on the validation results. 10.10 Quality Control Blanks-The area count of the peak of the test substance will be no more than half the area count of the average of the area counts (from the opening and closing curves) of the test substance in the lowest standard used in making the calibration standards. 10.1 1 Laboratory Controls-Laboratory control samples will be used throughout the study to ensure reliable results are achieved. Laboratory control data will be collected and compared to the data collected from the study samples. The report will include appropriate calculations based on the differences between the controls and the study samples. The final report will also include any appropriate tables, information or observations pertaining to the control samples. 11.O Subcontracted Analysis 11.1 Not Applicable. 12.0 Statistical Methods and Calculations 12.1 Statistical methods for the analytical results will be limited to the calculations of means, standard deviations, relative standard deviations, and percent recoveries (as appropriate). 12.2 Percent recoveries will be calculated using the following equation: [(A-B)/C] * 100 where: A = analyzed concentration of the spiked replicate sample B = analyzed concentration of the replicate sample (without spike) C = true concentration of the spike 12.3 Calculations will be made using the appropriate equations from the OECD Guideline 106 (pages 14-18). 3M Environmental Laboratory 3M Environmental Laboratory Page 15 of 19 Page 40 of 703 BACK TO MAIN . I. . Laboratory Request Number (LRN)-E00-1311 I 12.4 Report ~ A report of the results of the study will be prepared by 3M Environmental Laboratory. The report will include, but not be limited to, the following, when applicable: 12.4.1 Name and address of the facilities performingthe study, 12.4.2 Dates upon which the study was initiated and completed. 12.4.3 A statement of compliance by the Study Director addressing any exceptions to Good Laboratory Practice Standards. 12.4.4 A copy of the protocol, and any amendments and deviations. 12.4.5 The identification of the test substance (PFOS) and the results of composition analyses. 12.4.6 A description of the methods used to conduct the test(s). The report will contain updated methods incorporating any changes or improvements. 12.4.7 A description of the test system. 12.4.8 A description of any circumstances that may have affected the quality or the integrity of the data. 12.4.9 The name of the Study Director and the names of other scientists, professionals, and supervisory personnel involved in the study. 2.4. OA description of the transformations, calculations, or operations performed on the data, a summary and analysis of the analytical chemistry data, and a statement of the conclusions drawn from the analyses. 2.4. lstatistical methods used to evaluate the data, if applicable. 2.4. 2The signed and dated reports of each of the individual scientists or other professionals involved in the study, if applicable. 12.4.13The location where raw data and the final report are to be stored. 12.4.14A statement prepared by the quality assurance unit listing the dates that study inspections and audits were made and the dates of any findings reported to the Study Director and Management. 12.5 If it is necessary to make corrections or additions to a final report after it has been accepted, the changes will be made in the form of an amendment issued by the Study Director. The amendment will clearly identify the part of the final report that is being amended, provide the reasons for the amendment, and will be signed by the Study Director. 13.0 Quality Assurance 13.1 The 3M EnvironmentalLaboratory Quality Assurance Unit will audit this protocol, the study conduct, and the final report in accordancewith GLP regulations and 3M Environmental Laboratory standard operating procedures. 3M Environmental Laboratory Page 16 of 19 Y M tnvironmental Laboratory ~ Page 41 of 703 BACK TO MAIN . It * Laboratory Request Number (LRN)-E00-1311 I 14.0 Location of Raw Data, Records, and Final Report 1 14.1 Original data or copies thereof, will be available at 3M Environmental Laboratory. When the final report is completed (Tiers 11and III), all original paper data, including those items listed below, will be retained in the archives of 3M EnvironmentalLaboratory following signing of the final report. 14.2 The following raw data and records will be retained in the study folder in the archives according to 3M Environmental Laboratory SOPs. 14.2.1 Approved protocol and amendments 14.2.2 Study correspondence 14.2.3 Shipping records 14.2.4 Raw data 14.2.5 Approved final report (original signed copy) 14.2.6 Electronic copies of data 14.3 The following supporting records will be retained separately from the study folder in the archives according to 3M Environmental Laboratory SOPs: 14.3.1 Training records 14.3.2 Calibration records 14.3.3 Instrument maintenance logs for LCMS 14.3.4 Standard operating procedures, equipment procedures, and methods 15.0 Sample Retention 15.1 A portion of the test substance used in the study will be retained in the laboratory for a period of not less than 2 years after a report is issued. 15.2 Tier I is used for preliminary purposes only. The study samples generated from this portion of the study will be retained for a minimum of two weeks after the Tier I data has been reviewed by the Quality Assurance unit and the issuance of a QA audit report. 15.3 Tier I1 and Tier 111study samples will be maintained in the laboratory for a period of time as specified by regulation or as long as the quality of the preparation affords evaluation. However, samples will not be maintained more than 10 years after the effective date of the final test rule (if applicable). 3M Environmental Laboratory standard operating procedures also apply to sample retention times. 15.4 Tier I1 and Tier III study samples of the prepared HPLC/MS/MS sample vials will be retained and refrigerated for a period of not less than six months from the time of analysis. - 3M Environmental Laboratory 3M tnvironmental Laboratory Page 42 of (03 BACK TO MAIN .It c Laboratory Request Number (LRN)--E00-1311 I 16.0 Protocol Amendments and Deviations 1 16.1 Amendments and deviations to the protocol will be in the form of written amendments signed by the Study Director and the Sponsor Representative. Amendments will be considered as part of the protocol and will be attached to the final protocol. All changes to the protocol will be indicated in the final report. Any other changes will be in the form of written deviations, signed by the Study Director and filed with the raw data. 17.0 References 17.1 Organization of Economic Cooperation and Development. OECD Guideline for the Testing of Chemicals. "Adsorption-DesorptionUsing a Batch Equilibrium Method," OECD Guideline 106 Adopted 21 January 2000 17.2 United States Environmental Protection Agency. OPPTS 835.1220 Sediment and Soil AdsorptionDesorption Isotherm. Prevention, Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-C-98048.1998 17.3 United States Environmental Protection Agency. OPPTS 835.1110Activated Sludge Sorption Isotherm. Prevention, Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 7 12-C-98-298. January 1998 17.4 3M Environmental Laboratory Method ETS-8- 159: Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicals as the Test Substance 17.5 3M Environmental Laboratory Method ETS-8- 160: Preparation of Soil Samples for Screening and Advanced (Tier 11and Tier 111)Sorption Studies for Fluorochemicals as the Test Substance 17.6 3M Environmental Laboratory Method ETS-8-110: Analysis of Perfluorooctanesulfonateor Other Fluorochemicalsin Water Extracts Using HPLC-Electrosprayblass Spectrometryblass Spectrometry 17.7 3M Environmental Laboratory Method ETS-8- 154: Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane Sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water by Liquid-Solid Extraction and HighPerformance Liquid Chromatographymandem Mass Spectrometry (HPLC/MS/MS) 18.0 Attachments 18.1 Attachment A : Eample Numbering Scheme 3M Environmental Laboratory Page 18 of 19 3M Environmental Laboratory Page 43 of 703 BACK TO MAIN ' 3 . :. Laboratory Request Number (LRN)-E00-1311 I Attachment A: Example Numbering Scheme Matrix Solutions 1 E00-13 11-0001 E00-13 11-0002 E00-1311-0003 Analytical Samples made from Matrix Solutions EOO- 13 11-0004 E00-13 11-0005 EOO- 1 3 11 -0006 Suitable Container E00-1311-1016 --- S1 S2 E00-1311-1017 --- S1 S2 E00-1311-1018 --- S1 S2 E00-1311-1018 MS S1 S2 Suitable Desorption Solvent E00-1311-2010 --- S1 E00-1311-2011 --- S1 E00-1311-2012 --- S I E00-1311-2012 MS S1 Optimal Ratio E00-1311-3094 --- SI E00-1311-3095 --- S1 E00-1311-3096 --- S1 E00-1311-3096 MS S1 Optimal Ratio-Mass Balance E00-1311-3094 --- S2 EOO-1311-3095 --- s 2 E00-1311-3096 --- S2 E00-1311-3096 MS S2 Adsorption Kinetics-OneConcentration E00-1311-4031 --- S1 E00-1311-4032 --- S1 E00-1311-4033 --- S1 E00-1311-4033 MS S1 Desorption Kinetics-One Concentration --- E00-13114031 --- S2 S3 S4 S5 S6 S7 S8 E O - 1311-4032 S2 S3 S4 S5 S6 S7 S8 E00-1311-4033 --- S2 S3 S4 S5 S6 SI S8 E00-1311-4033 MS S2 S3 S4 S5 S6 S7 S8 Adsorption Isotherms-Multipleconcentrations E00-1311-5058 --- S1 E00-1311-5059 --- S1 E00-1311-5060 --- s1 E00-1311-5060 MS S1 Desorption Isotherms-Multiple concentrations E00-1311-5058 --- S2 S3 E00-1311-5059 --- S2 S3 E00-1311-5060 --- s 2 s 3 E00-1311-5060 MS S2 S3 3M Environmental Laboratory Attachment A: Example NumberingScheme =Page19of 19 3M Environmental Laboratory Page 44 of 703 BACK TO MAIN Study Title :, Soil AdsorptiodDesorption Study of Perfluorooctanesulfonate(PFOS) - Test Control Reference #TCR-00017-46 PROTOCOL AMENDMENT NO. I Amendment Date: October 30,2000 Performing Laboratory 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55144-1000 Laboratory Project Identification 3M EnvironmentalLaboratory Study LIMS #E00-1311 3M Environmental Laboratory 3M Environmental Laboratory Page 45 of 703 BACK TO MAIN Protocol #E00-I31 I Amendment I T h i s amendment modifies the following portion(s) of the protocol: `:, 1. PROTOCORLEADS: SECTION 8.2.1: Previous work with the test substance in a variety of matrices have strongly indicated that the analysis of PFOS in the aqueous/soil matrix described in OECD Guideline 106 can be accomplished by a dilution of a portion of the centrifuged aqueous portion with methanol in a 1:1 ratio. AMENDTO READ: Previous work with the test substance in a variety of matrices has strongly indicated that the analysis of PFOS in the aqueous/soil matrix described in OECD Guideline 106 can be accomplished by a dilution of a portion of the centrifuged aqueous portion with methanol in at least a 1:l ratio. REASON:Some of the samples in this study were diluted at a level other than 1:1. 2. PROTOCORLEADS: SECT~ON8.2.1:The resulting aliquot can then be analyzed using HPLC/MS/MS. AMENDTO,READ: The resulting aliquot can then be analyzed using HPLC/MS. REASON:Samples in this study were analyzed by single and triple quadrupole instruments, as well as MSD's. The '! term "LC/MS" encompasses all these instruments. 3. PROTOCOL READS:SECTION 8.4.2: Dose the test substance (at 2ug and 20ug) onto 2.5 grams of a strongly adsorbing (high clay content) soil. AMENDTO READ: Dose the test substance (at 0.75ug and 7.5ug) onto 2.5 grams of a strongly adsorbing (high clay content) soil. REASONT: he test substance concentrations were modified to more closely resemble the concentrations used in the rest of the study. 4. PROTOCORLEADS:SECTIO8N.4.5 If this process cannot recover 80% or more of the test substance, investigate a minimum of three other solvents. AMENDTO READ: If this process cannot recover 80% or more of the test substance up to three other solvents may be investigated. However, the test substance in question may be so strongly bound to the soil that no solvent will yield ideal recoveries. If one or more of the ratios tested in the "Optimal Soi1:Solution Ratio" portion of the experiment shows greater that 80% adsorption onto the high clay content soil at equilibrium this may be assumed to be the case. In this case no further solvent testing will be needed. REASON:The test substance demonstrated a very strong adsorption onto the high clay content soils. Based on previous experience it was reasoned that alternative solvents were unlikely to yield acceptable recoveries. 3M Environmental Laboratory 3M Environmental Laboratory Page 46 of 703 BACK TO MAIN Protocol #EOO-13I I Amendment 1 5. PROTOCOL READS: SECTION 8.5.2 Dose the test substance such that the final concentration of test substance is approximately 1mg/L. C AMEND TO READ:Dose the test substance such that the fmal concentration of test substance is approximately 5mg/L. REASONT: he test substance showed strong adsorption in earlier portions of the study, and it was necessary to increase the concentration. 6. PROTOCORLEADS:SECTIO9N.2 Additional methods may be developed at a later time and will be listed as protocol amendments. AMENDTO READ:ETS-S- 155. Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Wastestream or Water Extracts Using HPLC-ElectrosprayMass Spectrometry. REASON:This method was also used in the analysis of the study samples. 7. PROTOCORLEADS:SECTIO1N0.5 Upon completion of the analytical method validation portion of the study, an amendment to the protocol will be written defining acceptable criteria based on the validation results. AMEND TO READ: Matrix spikes and laboratory control sample recoveries will be acceptable if at least 80% of them are within f30% of the theoretical value. REASONA: cceptable criteria were decided upon after the signing of the protocol. 8. PROTOCOL READS: SECTION 10.8.1 HPLC/MS/MS AMENDTO READ: HPLC/MS. REASON:Samples in this study were analyzed by single and triple quadrupole instruments, as well as MSD's. The term "LCIMS" encompasses ail these instruments. 9. PROTOCOL READS:SECTIO1N0.9.2Upon completion of the analytical method validation portion of the study, an amendment to the protocol will be written defining acceptable criteria based on the validation standards. AMENDTO READ:The Relative Standard Deviations of triplicate samples will be acceptable if at least 80% of them are less than or equal to 30%. In addition, a Q-test may be used to exclude outliers in data sets. 3M Environmental Laboratory 3M Environmental Laboratory Page 47 of 703 BACK TO MAIN REASONA: cceptable criteria were decided upon affer the signing of the protocol. Protocol #OO- 7377 Amendment 7 ` 10. PROTOCORLEADS:SECTION12.2 Percent recoveries will be calculated using the following equation: [(A- B)/C]* 100 where: A = analyzed concentration of the spiked replicate sample B = analyzed concentration of the replicate sample (without spike) C = true concentration of the spike AMENDTO READ:Percent recoveries will be calculated using the following equation: [(A-B)/C]* 100 where: , A = analyzed concentration of the spiked replicate sample B = analyzed concentration of the replicate sample (without spike)** C = theoretical concentration of the spike **If the replicate sample is below the LOQ it will not be subtracted from the concentration of the spikes replicate sample. REASONC: larification of the term "true" concentration, and explanation of the formula. Since nothing can be said about a sample that is below the LOQ it should not be used in any calculations. 11. PROTOCOL READS: SECTION 15.4 HPLC/MS/MS AMENDTOREAD: HPLC/MS. REASON:Samples in this study were analyzed by single and triple quadrupole instruments, as well as MSD's. The term "LCMS" encompasses all these instruments, 12. PROTOCOLREADS: SECTION 17.8 N/A (there was no previous section 17.8) AMENDTO READ:3M Environmental Laboratory Method ETS-8- 155: Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Wastestream or Water Extracts Using HPLCElectrospraylMass Spectrometry. REASONT: his method was not referenced in the protocol, but was used in the analysis of the study samples. 3M EnvironmentalLaboratory 3M Environmental Laboratory Page 48 of 703 BACK TO MAIN Amendment Approval Protocol #E00-131I Amendment I William K. Reagen, Sponsor Representative --- o s - / 7 / ,c3/ Date .<I7// v . ' Date 3M Environmental Laboratory 3M Environmental Laboratory Page 49 of 703 BACK TO MAIN 1` Appendix B: Analytical Methods This amendix mesents the analvtical methods used in the mesent studv: ETS-8-159 "Preparation of Soil Samples for Prelimmiry (Tier I) Sorption Studies for Fluorochemicals as the Test Substance" ETS-8-160 "Preparation of Soil Samples for Screening (Tier II) and Advanced (Tier III) Sorption Studies for Fluorochemicals as the Test Substance" OECD 106 "Adsorption - Desorption Using a Batch Equilibrium Method" ETS-8-155 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream of Water Extracts Using WLC-Electrospray/Mass Spectrometryyy ETS-8-110 "Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Water Extracts Using HPLC-ElectrospmyMass Spectrometry/Mass Spectrometry" 3M Environmental Laboratory Page 50 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY METHOD PREPARATION OF SOIL SAMPLES FOR PRELIMINARY (TIERI) SORPTION STUDIES FOR FLUOROCHEMICAASLTSJ3E TESTSUBSTANCE (BASEDON OECD GUIDELINE106) Method Number: ETS-8-159.0 Author: Linda Goodspeed, Cindy Car...Jn, Mark Elrefson Approved By: Laboratory Manager I Adoption Date: Revision Date: Date Techical Reviewer Date 3M Environmental Laboratory ETS-8-159.0 Tier I Sorption Studies Page 1 of 13 Page 51 of 703 BACK TO MAIN 1.o SCOPE AND APPLICATION 1.1 By complyingwith the requirements of the OECD Guideline 106. "Adsomtion- Desorption Using A Batch Equilibrium Method", the data will meet the te'sting $i 1.2 requirements of the European Community and Canada. This method complieswith OPPTS 835.1220 "Sediment and Soil Adsorbhlesorb Isotherm" and is also intended to meet testing requirements of the Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) and the Toxic Substances Control Act (TSCA) for the United States. 1.3 This method describes the procedures used to prepare method development study samples and subsequently analyze them in order to demonstrate applicability. This method precedes testing methods for the screening (Tier I) and the advanced (Tier 111) portions of the Sorption Studies. 1.4 This method is based on the "Preliminary" subsection of OECD Guideline 106: "Adsorption - DesorptionUsing A Batch Equilibrium Method". 1.5 The "Preliminary" portion of OECD Guideline 106 requires pre-testing done (method development) in order to insure applicability of the subsequent tiers of the Guideline (the "Screening" portion and the "Advanced" portion). The required pre-testing is designed to determine: 1.5.1 a suitable analytical method 1.5.2 the adsorption of the test substance on the surfaces of the test vessels 1.5.3 the equilibration time for adsorption and the amount of test substance adsorbed at equilibrium 1.5.4 a suitable desorption solvent 1.5.5 the soi1:aqueous ratio 1.5.6 the stability of the test substance during the study period 1.6 In addition, this internal 3M method (ETS-8-159) will address determination of an approximationof the statistical variance of precision and accuracy data that may be expected fiom the continuation of the procedure to the screening and advanced tiers of OECD Guideline 106. 1.7 This method is applicable to the testing of fluorochemical substances manufacturedor distributed by 3M. I 1.8 An approximate solubility concentration of the test substance in water should be established prior to the commencement of this method, so that appropriate concentrations of the test substance in the study samples are used throughout. 2.0 SUMMARY OF METHOD 2.1 Suitable Analytical Method: 2.1.1 A soil of high adsorbability (high organic carbon and clay content) is agitated with an appropriate volume of 0.01 M CaC12 solution at cz 1:5 (w:v) ratio for a minimum of 4 hours. The mixture is centrifuged and the aqueous phase filtered, if necessary. A certain volume of the test substance stock solution is added to the latter to reach a nominal concentration within the concentration range that is likely to occur during the test. This "study sample" is then prepared for later analysis using HPLCMS. After the study sample has been analyzed, a determination is made as to whether HPLC/MS is a suitable analytical method for the test substance. ETS-8-159.0 Tier I Sorption Studies Page 2 of 13 3M Environmental Laboratory Page 52 of 703 BACK TO MAIN 2.2 i 2.3 2.4 2.5 3.0 3.1 3.2 3.3 Suitable Desorption Solvent: 2.2.1 Methanol is investigated as the first choice for a suitable desorption solvent for the test substance. A high clay content soil is dosed with the test substance at two levels (1 pg, 10 pg). The test substance is then extracted from the study samples three times with methanol. The combined methanol extracts are then prepared for analysis by HpLCiMS. 2.2.2 If the extraction results in a total of 280% desorption, no further testing of solvents is necessary. Otherwise, up to three other solvents will be investigated in a similar manner until the criteria (280% desorption) are met. 2.2.3 If the criteria are not met, the most suitable solvent among those tested will be chosen. Suitable (Minimally Adsorbing) Container 2.3.1 Up to five containers comprising a variety of materials are exposed to a 0.01 M CalClz aqueous solution dosed with the test substance for a minimum of 24 hours. The resulting solution is analyzed for the test substance using HPLC/MS. In addition, an extraction of the walls of the container with methanol is made. This extract is analyzed as well. Any container that adsorbs less than 10%of the test substance onto its walls is considered suitable for use as a study container. Alternatively, the container demonstrating the least amount of test substance absorption is chosen from those tested. Selection of Optimal Soil: Aqueous Solution Ratio, Determination of Equilibration Time, and Stability of the Test Substance under Conditions of the Study 2.4.1 The optimal soil: aqueous ratio is determined by using two types of soils and three soil: solution ratios. The test substance is dosed into an aqueous solution in contact with the soil. Sufficient tubes are prepared such that tubes can be removed after a period of time (spanning 0 to 48 hr) and the aqueous portion analyzed. Equilibrium is determined by plotting the adsorption of the test substance over time. The optimal soil: solution ratio is determined by a comparison of the amount of adsorption of the test substance at equilibrium for the various soil: solution ratio study samples. Acceptable values are soil: solution ratios that give a depletion of the test chemical above 20% and preferably above 50% at equilibrium. Stability is determined by a mass balance determination. The mass balance determination is conducted on both soils and on the one soi1:solution ratio per soil that gives a depletion of the test chemical above 20% and preferably above 50% at equilibrium. In all cases, adequate quality assurance samples are prepared and analyzed. DEFINITIONS Test Substance: Any substance (mixture or controlled compound) added or administered to the test system for the purpose of biological or chemical measurements. Target Analyte: In the analytical phase of a study, the chemical(s) singled out in the analyses is the target analyte. The target analyte may be identical to the test substance used in the in-life phase of the study, or a by-product of that chemical. Reference Substance: A material or substance, one or more properties or constituents of which are sufficiently well established for it to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to materials. ETS-8-159.0 Tier I Sorption Studies Page 3 of 13 3M Environmental Laboratory Page 53 of 703 BACK TO MAIN 3.4 .:<, 3.5 3.6 3.7 3.8 4.0 4.1 4.2 5.0 5.1 6.0 6.1 6.2 6.3 6.4 Test system: Any animal, plant, microorganism, chemical, or physical matrix (including soil or water) or any subpart thereof, to which the test, control, or reference substance is administered or added for study. Study sample: A sample containing the test substance in contact with the test system, or any of the subsequent samples generated from the initial set up. Control Sample: A sample containing the test substance, but which does not include the entire test system or any subsequent samples generated from the initial set up. In most, but not all cases, control samples go through all of the same processes as the study samples. Matrix Blank: A sample that has not been exposed to the test substance and/or target analyte. Matrix blanks may or may not include the entire test system. The term matrix blank also includes any subsequent samples generated from the initial matrix blank set up. In most, but not all cases, matrix blanks go through all of the same processes as the study samples. Solvent Blank: Aqueous or organic solvent that has not been exposed to the test substance and/or target analyte, and is analyzed to demonstrate the absence of target analytes in the solvent. WARNINGASND CAUTIONS Health and Safety Warnings: 4.1.1 Many of the fluorochemicals used in the laboratory are not completely characterized for toxicity and other health hazards. They should be treated as potential health hazards. Proper equipment such as gloves and safety glasses should be worn when working with these chemicals or any solvents. Skin contact and inhalation should be avoided. Preparation of the stock standards should be done under a hood. All spills should be wiped up immediately. Cautions: 4.2.1 Contaminationof glassware and equipment by the compounds of interest are an on-going issue within laboratories. Care must be taken to rinse any reusable glassware with appropriate solvents before and after the glassware is used. Triple rinsing with methanol or acetone is recommended to remove fluorochemicals from the glassware. Clean all spills immediately to avoid present or hture contamination. 4.2.2 Use disposable glassware whenever possible. INTERFERENCES Any compound that co-elutes with the test substance or the reference material during the HPLC/MS analysis can interfere with quantification. EQUIPMENT Balance capable of weighing to 0.1 mg, such as OHAUS Brand Model GA200 Centrifuge capable of maintaining 4,000 f 200 rpm, such as Jouan Brand Model C412 Orbital shaker capable of a gentle rotation and temperature controlled capable of maintaining 23 f 3 C, such as Lab-Line Model Environ-Shaker Vacuum Pump, such as Gast #DOA-P104-AA (Optional) ETS-8-159.0 Tier I Sorption Studies Page 4 of 13 3M Environmental Laboratory Page 54 of 703 BACK TO MAIN 7.0 SUPPLIES AND MATERIALS 7.1 15-mL polypropylene centrifuge tubes, such as VWRbrandQ Centrifuge Tubes, catalog number 21008-089 7.2 15-mL polystyrene centrifuge tubes such as VWRbrandQ Centrihge Tubes, catalog number 21008-202 7.3 15-mL styrene butadiene centrifuge tubes such as VWRbrandm Centrihge Tubes, catalog number 21008-226 7.4 15-mL glass centrifuge tubes 7.5 30-mL Teflon centrifuge tubes 7.6 50-mL plastic centrifuge tubes, such as VWRbrandcE 20171 7.7 Syringes, 10 uL, 25 uL, 1000UL 7.8 Volumetric flasks, 10-mL, lOO-mL, 1-L, 5-L, NalgeneB and/or glass 7.9 Automatic or manual dispenser, capable of dispensing liquid with *O. 1mL accuracy 7.10 250-1000 uL manual pipettor(s) and plastic pipette tips, or equivalent 7.11 Autosamplervials, 1.5 to 2 mL GC/HPLC, such as Kimble # 60820-1232 or equivalent 7.12 Autosamplervial caps, such as Wheaton # 224211-01 7.13 GC/HPLC autovial crimper(s) and decrimper(s) 7.14 Appropriately sized storage containers with tight-fitting caps for solutions i 7.15 Glassware, miscellaneous 7.16 150-mL NalgeneB bottles or equivalent 7.17 pH paper capable of distinguishing pH to k0.5 units. 8.0 REAGENTS, SOLUTIONS AND STANDARDS 8.1 Reagents 8.1.1 Methanol, HPLC grade, such as J.T. Baker #9093. 8.1.2 ASTM Type I water, 18.0 Mi2 or better. 8.1.3 CaC12, Anhydrous, to meet ACS specifications (>96% pure),'such as J.T. Baker #1311. 8.1.4 Soils: Appropriate soil types selected from Table 1 below. (Soils should be airdried at ambient temperature and sieved to a particle size 12 mm.) Table 1 Sandlloamy sand NOTE: It may not be possible to obtain soils that match all criteria. Soils will be used that match as closely as possible the parameters as listed. Exceptionswill be noted. ETS-8-159.0 Tier I Sorption Studies Page 5 of 13 3M Environmental Laboratory Page 55 of 703 BACK TO MAIN t 8.2 8.1.5 Sediment: NOTE: Sediment may be used in addition to the soil types listed, but is not required as part of this method. 8.1.6 Sludge: In addition to soil andor sediment, sludge may be used as appropriate to achieve the goals of the study in question. The use of sludge is not required by this method. 8.1.7 Test Substance: Characterized by HPLCNS 8.1.8 Reference Material: THPFOS, lH, lH, 2H, 2H- perfluorooctanesulfonic Acid Solutions and Standards: NOTE: Different quantities of any of the solutions may be prepared, as long as solutions are documented as to how they were made. 8.2.1 Solution A: 0.01 M CaCl2 Solution 5.55k0.02 grams of CaC12 dissolved in 5.0 L of ASTM Type I water. This solution is may be stored for up to 100 days at room temperature, 8.2.2 Solution B: -50 mg/L test substance in 0.01 M CaC12 Solution Dissolve 0.050 f0.005 grams of test substance in 1.0 liter of 0.01 M CaC12. Use volumetric flask and record weight. Immediately transfer into a NalgeneB container(s). This solution is may be stored for up to 35 days at room temperature. However, it is good practice to take an aliquot of this solution and prepare it to run along with samples prepared at the same time to monitor for any possible degradation andor adsorption to the container. 9.0 SAMPLEHANDLING 9.1 All study samples generated and prepared for analysis by HPLC/MS may be left at room temperature for a maximum of 15 days, or refkigerated for a maximum of six months. 9.2 The autovial study samples may be reanalyzed at any time throughout the study. However, autovials whose caps have been pierced should have the caps replaced within 3 days. 10.0 QUALITYCONTROL 10.1 Matrix Blanks consisting of the following types will be prepared for the study: 10.1.1 0.01 M CaClz in contact with each of the selected soil types 10.2 Matrix Spikes (MS): One matrix spike will be prepared for each sample set, except as noted in the method 10.3 Solvent Blanks will be prepared for the study: 10.3.1 0.01 M CaC12 and No Soil 10.3.2 Methanol and No Soil (in some sections) 10.4 Control Samples: Control Samples per following type will be prepared for the study: 10.4.1 Test substance in 0.01 M CaCl2 only 10.4.2 Test substance in Methanol only (in some sections) 10.5 Sample Replicates: Sample sets will consist of a "sample," "duplicate," and "triplicate," except as noted in the method 10.6 Surrogate(s): No surrogate will be used in this study. 10.7 Reference Material: THPFOS will be used as the reference material. ETS-8- 159.0 Tier I Sorption Studies Page 6 of 13 3M Environmental Laboratory Page 56 of 703 BACK TO MAIN 11.0 CALIBRATIOANND STANDARDIZATION 11.1 This section is outside the application of this method. 12.0 PROCEDURES 12.1 Labeling of Samples (Centrifuge Tubes) and Autovials-Centrifuge tubes and autovials should be prelabeled, according to the following scheme: 12.1.1 The study project should be given a unique Lab request number from 3M's EnvironmentalLaboratory Sample Control Numbering system. 12.1.2 Study Samples,Labeling of Centrifuge Tubes: Each individual sample and QC sample that is set up in the Suitable Analytical Work section will have a unique identifier. 12.1.3 If necessary, aliquots taken from the study samples will be uniquely identified by using the initial study sample ID and then adding an additional designator for each aliquot removed from the study sample. 12.1.4 All autovials will clearly identify any "extra" dilution made of its contents. 12.1.5 All Matrix Spike samples will contain all of the above information, as well as the designator "MS." 12.2 Suitable Analytical Work i 12.2.1 Each soil used in this study must be tested for the suitability of the proposed analytical work. Cany each soil to be used through the analysis described in this section. 12.2.2 Weigh 20 grams of soil into a vessel and record the weight. (Do this in triplicate.) 12.2.3 Add 100 mL of 0.01 M CaC12 solution. 12.2.4 Place the soil: aqueous solution in an orbital shaker with gentle rotation at ambient temperature for a minimum of four hours. 12.2.5 Centrifuge the contents until the aqueous portion is clear (transfer into smaller centrifuge tubes if necessary). 12.2.6 Transfer this solution into a clean container, label as "Matrix Solution" and give a unique ID number to it. Store under refrigeration. 12.2.7 Matrix Blanks: 12.2.7.1 Prepare by aliquotting 1.00mL of the Matrix Solution directly into an autovial. Prepare one Matrix Blank for each Matrix Solution. 12.2.8 Study Samples: 12.2.8.1 Add 100 pL of stock test substance solution (Solution B) to a 10 mL volumetric flask. (Volume of stock solution added may be adjusted. Final concentration should be approximately 0.500 mg/L). Dilute each flask to the mark with the Matrix Solution. Do this in triplicate for each Matrix Solution (a total of nine flasks). 12.2.8.2 Label with unique ID number. 12.2.8.3 Continue by withdrawing 1.0 mL of the study sample and dispensing into the same prelabeled autovial. 12.2.9 Add THPFOS internal standard prior to analysis. 12.2.10Analyze autovials using appropriate methodology to determine concentration of test substance. 12.2.11Calculate percent test substance of theoretical as described in the Calculations section. ETS-8- 159.0 Tier I Sorption Studies Page 7 of 13 3M Environmental Laboratory Page 57 of 703 BACK TO MAIN 12.3 Suitable Container 12.3.1 Select the typedmaterials of centrifuge tubes to use in the study from the Supplies and Materials section of the method (up to 5). 12.3.2 Prepare 100mL of each of the following solutions: 12.3.2.1 0.0 mg/L of test substance in 0.01 M CaC12 (i.e., Solution A). 12.3.2.2 -0.05 mg/L of test substance in 0.01 M CaC12. (Dilute 100 ULof Solution B to 100 mL with Solution A in a NalgeneB volumetric flask.) 12.3.2.3 -0.50 mg/L of test substance in 0.01 M CaC12. (Dilute 1000 ULof Solution B to 100 mL with Solution A in a NalgeneB volumetric flask.) 12.3.3 Prepare Time "0 hr" samples: 12.3.3.1 Dispense 1.OOmL of each of the three solutions listed in section 12.3.2 directly into labeled autovials. Do this four times for each solution (triplicate samples and one matrix spike). 12.3.3.2 Spiking: Refer to section 12.6. 12.3.4 Prepare Time "24 hr" samples: 12.3.4.1 Aliquot lOmL of solution into each centrifuge tube, according to the following Study Sample grid (Table 2): Table 2 Conc. Test Substance, mglL 0.0 -0.05 -0.50 I No. of tubes Solution Cent. Tube, Type 1 12.3.2.1 3 12.3.2.2 3 12.3.2.3 I 3 No. of tubes Cent. Tube, Type 2 3 3 3 No. of tubes Cent. Tube, Type 3 3 3 3 No. of tubes Cent. Tube, Type 4 3 3 3 No. of tubes Cent. Tube, Type 5 3 3 3 12.3.4.2 Equilibrate the tubes for 24 hours at room temperature in an orbital shaker set to gently rotate. Record start and stop times on the appropriate data form. 12.3.4.3 Transfer 1.OOmL of the study sample into a labeled autovial. 12.3.4.4 Spiking: Refer to section 12.6 for spiking. 12.3.4.5 Empty contents of the tubes. (Contents may be discarded.) 12.3.4.6 Add 2.0 mL of Methanol to the empty tube. 12.3.4.7 After recapping the tube, thoroughly rinse the sides and cap of the centrihge tube. 12.3.4.8 Transfer 1.0mL of the rinse solution from 12.3.4.6 to an autovial and cap tightly. 12.3.4.9 Spiking: Refer to section 12.6 for spiking. 12.3.5 Add THPFOS internal standard prior to analysis. 12.3.6 Analyze all autovials using appropriate methodology to determine concentration of test substance. 12.3.7 Calculate percent test substance of theoretical as described in the Calculations section. ETS-8-159.0 Tier I Sorption Studies Page 8 of 13 3M Environmental Laboratory Page 58 of 703 BACK TO MAIN 12.4 t 12.3.8 Choose the most appropriate container based on minimal adsorption as well as convenienceand cost. Suitable Desorption Solvent 12.4.1 Two amounts (1 ug and 10 ug total) of test substance will be used, as well as a blank control. 12.4.2 Select a soil with high clay content from the list of soil types in section 8.1.4 for use in this study. 12.4.3 Use the centrifuge tubes determined from section 12.3 of this method. 12.4.4 Using the following Study Sample grid (Table 3), prepare the following (replicate) sample sets: Table 3 Total pg of Test Substance 0.0 -1 PS -10 P9 Matrix Soil only Soil only Soil only VLof Stock Test Substance 0.0 20 200 Amount of Soil (grams) 2.50 k 0.05 2.50 f 0.05 2.50 k 0.05 # of Tubes with Soil 3 w#iOthfTNuobSeosil I 3 31 3 3 12.4.5 Weigh soil amounts as indicated and record weights on the appropriate data form. 12.4.6 Add the test substance onto the soil as indicated in Table 3. 12.4.7 Mix the soil contents thoroughly and then allow the tubes to sit for a minimum of 10 minutes to insure adsorption of the test substance onto the soil. 12.4.8 Add 2.5 mL of methanol to each tube and cap tightly. 12.4.9 Vortex for 1 minute. (Alternatively, place tubes horizontally on a shaker and mix for 10 minutes.) 12.4.10Centrifuge the tubes and remove as much of the solvent layer as possible, without disturbing the solids layer. 12.4.11Place the solvent layer into a second prelabeled centrifuge tube. 12.4.12Repeat steps 12.4.8 through 12.4.12 twice more, adding the solvent portion to the same tube each time. 12.4.13Withdraw 1.00mL of the study sample and dispense into a prelabeled autovial. 12.4.14Spiking: Refer to section 12.6 for spiking. 12.4.15Add THPFOS internal standard prior to analysis. 12.4.16Analyze autovials using appropriate methodology to determine concentration of test substance. 12.4.17Calculate percent test substance of theoretical as described in the Calculations section. 12.4.18If the total test substance recovery from the soil is S O % , no further testing of solvent is necessary. 12.4.19If the test substance recovery from the soil is <SO%, investigate other solvents, using the same procedural steps. ETS-8-159.0 Tier I Sorption Studies Page 9 of 13 3M Environmental Laboratory Page 59 of 703 BACK TO MAIN 12.5 i t Selection of Optimal Soil: Solution Ratios 12.5.1 Select two soils from the soils listed in section 8.1.4. 12.5.1.1 One soil type with high organic carbon and low clay content. 12.5.1.2 One soil type with low organic carbon and high clay content. 12.5.2 Using the centrifuge tube type determined for use from section 12.3, set up the following study sample grid (Table 4). Control blanks are set up for only two time points (0 hr and 48 hour). All other samples are set up for eight time points, Table 4 12.5.3 12.5.4 12.5.5 12.5.6 12.5.7 Document the pH of the stock test substance solution, using pH paper. Record to k0.5 pH units. The study samples are equilibrated with the 0.01 M CaC12 solution for a minimum of 12 hours by placing the tubes on an orbital shaker at 23 f3 O C using a gentle rotation. Record start and stop timeddates on appropriate data forms. Remove the tubes after the 12 hours and add the Stock Test Substance Solution (Solution B) in the amounts as specified in Table 4 (grayed section). For Time "0 hr" study samples only, gently mix and proceed directly to 12.5.10. The rest of the study samples are then placed back on the orbital shaker 23 +_ 3 "C using a gentle rotation. Record start timeddates on appropriate data forms. ETS-8-159.0 Tier I Sorption Studies Page 10 of 13 3M Environmental Laboratory Page 60 of 703 BACK TO MAIN 12.5.8 Remove (replicate) sample sets at the following time points and record the date(s)/time(s) of removal. 2 hr 4 hr 8 hr 16 hr 24 hr 36 hr 48 hr 12.5.9 For the Time "48 hr" study samples only, weigh the tube + Contents and record on the appropriate data forms. 12.5.10Centrifuge until the aqueous layer appears clear. 12.5.11Document the pH for one of each sample set per time point. Record to k0.5 pH units. 12.5.12Withdraw 1.OOmL of the study sample and dispense into a prelabeled autovial. 12.5.13Spiking: Refer to section 12.6 for spiking. 12.5.14Continue to pull the (replicate) timed study sample sets at the designated time points and repeat steps 12.5.10 through 12.5.13, as appropriate. 12.5.15Continue with the procedure using the "Time 48 hr" set of tubes only. 12.5.16Remove as much of the aqueous layer as possible without removing any of the solids layer (discard the aqueous layer). 12.5.17Weigh the tube + contents and record on the appropriate data form. 12.5.18Methanol addition 12.5.18.1 Add 2.0 mL of methanol to tubes containing 3 or less grams of soils (this include all blank controls). 12.5.18.2 Add 3.0 mL of methanol to tubes containing more than 3 grams of soil. 12.5.19Vortex for 1 minute. (Alternatively, place tubes horizontally on a shaker and mix for 10 minutes.) 12.5.20Centrifuge the tubes and remove as much of the solvent layer as possible. 12.5.21Place the solvent layer into a second prelabeled centrifuge tube. 12.5.22Repeat steps 12.5.18 through 12.5.21 twice more, adding the solvent portion to the same tube each time. 12.5.23After all three portions of methanol extract have been added to the centrifuge tube, centrifuge the solution until it is clear. 12.5.24Transfer 1.OOmL of the study sample solution into the sane autovial. 12.5.25Spiking: Refer to section 12.6 for spiking. 12.5.26After all study samples have been pulled, prepped, and the internal standard added, analyze autovials using appropriate methodology to determine concentration of test substance. 12.5.27Make appropriate calculations as defined in the Calculations section. 12.5.28Determine the optimal soiksolution ratio based the following two factors: 12.5.28.1 Adsorption of the test substance should be between 20% and 80% onto the soil. 12.5.28.2 If possible, a soil: solution ratio that enables the use of 15-mL centrifuge tubes is highly preferred. (The weight of the soil can be adjusted down to a minimum of 1.0 k 0.05 grams. The aqueous ratio would be adjusted accordingly.) ETS-8-159.0 Tier I Sorption Studies Page 11 of 13 3M Environmental Laboratory Page 61 of 703 BACK TO MAIN 12.6 t Spiking 12.6.1 Only one replicate per study sample set will be spiked with a known amount of the test substance. 12.6.2 Spiking will be done whenever any aliquoted study sample is generated. 12.6.3 Dilute samples to the appropriate level for analysis (if necessary) with methanol. 12.6.4 Add an appropriate amount of spiking solution to provide a spike concentration of approximately 200ppb (or as deemed appropriate). 13.0 DATAANALYSIS AND CALCULATIONS 13.1 Data analysis and calculations should be done using the templates provided from OECD Guideline 106. 14.0 METHODPERFORMANCE There are no previously defined method performance criteria for this method. However, this method will generate statistical data that may be used as a guideline for monitoring performance for Method ETS-8-160. 14.1 Accuracy 14.1.1 Matrix Spikes (MS): One matrix spike per study sample set will be generated. The matrix spikes will be calculated by using the following equation: (MS conc. analytical - Sample conc. analytical) x 100 (MS Spike conc. theoretical) 14.2 Precision 14.2.1 Replicates: Triplicate study samples will be generated using this method. Relative Standard Deviations (RSD) will be calculated from the triplicate samples. In the cases, where there are only two replicates, the Relative Percent Difference (RPD) will be calculated. 15.0 POLLUTION PREVENTION AND WASTE MANAGEMENT 15.1 Dispose of sample waste by placing in high or low BTU containers as appropriate. 15.2 Use broken glass containers to dispose of any empty glass containers, pipettes, etc. 16.0 RECORDS 16.1 Laboratory data forms will be generated and filled out during the course of this study. These data forms will be archived according to standard laboratory protocols. 17.0 ATTACHMENTS 17.1 Example data forms: 17.1.1 Suitable Analytical Method Data Form 17.1.2 Suitable Container Data Form 17.1.3 Suitable Desorption Solvent Data Form 17.1.4 Soil: Aqueous Optimal Ratio Data Form 18.0 REFERENCES ETS-8-159.0 Tier I Sorption Studies Page 12 of 13 3M Environmental Laboratory Page 62 of 703 BACK TO MAIN 18.1 c 18.2 Organization of Economic Cooperation and Development, OECD Guideline for the Testing of chemicals. "Adsorption-Desorption Using a Batch Equilibrium Method: OECD Guideline 106 Adopted 21 January 2000. EPA Fate, Transport and Transformation Test Guidelines: OPPTS 835.1220 Sediment and Soil Adsorptiodllesorption Isotherm, EPA 712-C-98-048, January 1998. 19.0 AFFECTEDOCUMENTS 19.1 ETS-8-160.0 Preparation of Soil Samples for Screening (Tier 11) and Advanced (Tier 111) Sorption Studies for Fluorochemicals as the Test Substance (Based on OECD Guideline 106). 20.0 REVISIONS Revision Number. Reason For Revision Revision - Date 3M EnvironmentalLaboratory ETS-8-159.0 Tier I Sorption Studies Page 13 of 13 Page 63 of 703 BACK TO MAIN Suitable Analytical c,G 5 - 0 0 P i 1 -0 g0 .sz 5.- I % 09 2 EOO-W-OOOI E00-~-0002 EW-W-WO~ , ETS-8-159 Section 12.2 &m .sooe! 3 A .?m wr 4 5 6 Test Substance: -u) 5 E 5 0 7 I 0 E00-~-0004 E00-aca-0001 1 EOO-xca4001 1 EOO-XXX-OW~ 1 E00-xm-0002 1 E00-m-0003 1 EOO-XXX-OOO~ 1 E00-aca-0003 1 Col. 4 Test Substance = TlDll ID #: -/-I - Col. 5 Col. 6 Matrix Solution ID #: --- TIDll --- TIDll I I I I Internal Standard ID Number GLP Study Number: 3M Environmental Laboratory Page 64 of 703 Suitable Analytical ETS-8-159 Section 12.2 BACK TO MAIN Test Substance: Col. 2 Col. 3 Col. 4 Col. 5 Col. 6 Soil ID #: Balance ID TIDII -1-1- 0.01 M CaC12 Soln ID #: TIDll Inc. ID Start TIDII Stop TIDll TIDII 1- -I-/ -I-I - 1- Col. 4 Test Substance = ID #: TIDII -I-1- Col. 5 Matrix Solution ID #: TIDII Col. 6 TIDII Internal Standard ID Number -I-1 -I -1 - TIDll 1- GLP Study Number: 3M Environmental Laboratory Page 65 of 703 Suitable Container !a2 CT-1 CTd CT-2 CTJ CTJ ETS-8-159Section 12.3 BACK TO MAIN Test Substance: -. I I-IS2I I I I I GLP Study Number: 3M Environmental Laboratory Page 66 of 703 BACK TO MAIN Desorption Solvent C o l 4 Soil ID 1 Soil ID 2 C o l 6 Batanem ID Tmn--/-/- CoI 7 Test Subst Soh 10# T/D/l / I Co1.8 MeOH ID # rnIl--/-/- ETS-8-159 Section 12.4 C~ O~l 9~. TIDII C o l 10 M e O H ID # TID/I COl11 T/DA C o l 1 2 MeOH ID# T/D/l / I / / I I I I Test Substance COl I 3 T/D/l / Col 15 Study Sample Tmn--/-/Col 16 Spike soh ID # TimelDate/lnitials Internal Standard ID # TimelDatellnitials I II I / GLP Study Number: 3M EnvironmentalLaboratory Page 67 of 703 Optimal Ratio t ETS-8-159 Section 12.5 BACK TO MAIN Test Substance GLP Study Number: 3M EnvironmentalLaboratory lof5 Page 68 of 703 Optimal Ratio ETS-8-159 Section 12.5 BACK TO MAIN Test Substance GLP Study Number: 3M Environmental Laboratory Zof 5 Page 69 of 703 Optimal Ratio ETS-8-159 Section 12.5 BACK TO MAIN Test Substance GLP Study Number 3M Environmental Laboratory 30f 5 Page 70 of 703 Optimal Ratio ETS-8-159 Section 12.5 BACK TO MAIN Test Substance GLP Study Number: 3M Environmental Laboratory 40f 5 Page 71 of 703 Optimal Ratio ETS-8-159 Section 12.5 BACK TO MAIN Test Substance GLP Study Number: 3M Environmental Laboratory 50f 5 Page 72 of 703 Optimal RatitiolMarsBalsncn BACK TO MAIN ETS-8.159 Section 12 5 (cont) Test Substance: . I , , GLP Study Number: 3M Environmental Laboratory Page 73 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY t METHOD PREPARATION OF SOIL SAMPLES FOR SCREENING(TIER11) AND ADVANCED (TIER111) SORPTION STUDIES FOR FLUOROCHEMICALSAS THE TESTSUBSTANCE (BASEDON OECD GUIDELIN1E06) Method Number: ETS-8-160.1 Author: Cindy Carlson, Mark Elrefson Approved By: W- Ld- Laboratory Manager Adoption Date: I I 3 i IOu Revision Date: s / ,7 / 0 Date ETS-8- 160.1 Tiers I1 and 111 Sorption Studies 3M Environmental Laboratory Page 1 of IS Page 74 of 703 BACK TO MAIN 1.0 1.1 `d 1.2 1.3 1.4 1.5 2.0 2.1 2.2 2.3 - SCOPE AND APPLICATION By complying with the requirements of the OECD Guideline 106, "Adsorption Desorption Using A Batch Equilibrium Method",the data will meet the testing requirements of the European Community and Canada. This method complies with OPPTS 835.1220 "Sediment and Soil Adsorbmesorb Isotherm" and is also intended to meet testing requirements of both the Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) and the Toxic Substances Control Act (TSCA) for the United States. This method is applicable to test systems using soils, sediments or similar matrices as the adsorptive material. This method is applicable to the testing of fluorochemical substances manufactured or distributed by 3M. An approximate solubility concentration of the test substance in water should be established prior to the commencement of this method, so that appropriate concentrations of the test substance in the study samples are used throughout. SUMMARY OF METHOD Tier 11: Adsorption Kinetics (One concentration): 2.1.1 Appropriate soils andor sediments andor sludges are selected for the study. Replicate study samples containing the soils (or sediments or sludges) are equilibrated by shaking for at least 12 hours at room temperature with 0.01 M CaC12. These study samples are then dosed with the test substance and placed back on an orbital shaker. Aliquots of these study samples are removed at designated time points throughout a 48-hour time period. These study samples are then prepared and analyzed for the target analyte. The adsorption kinetics are then determined using this data. After the last aliquot is taken (48 hour time point) the study samples are saved and used for the desorption kinetics portion of the method. Tier 111: Desorption Kinetics (One concentration): 2.2.1 After the adsorption kinetics experiment, the study samples are centrifuged and the aqueous phase removed. The volume of solution removed is replaced by an equal volume of 0.01 M CaCl2 without test substance. The new mixture is agitated until the desorption equilibrium is reached. During a 48-hour period, at defined time intervals, aliquots of the aqueous phase are removed and analyzed for the target analyte. The experiment then continues with the original mixture. The desorption kinetics are determined using this data. Tier 111: AdsorptionIsotherms (Five concentrations): 2.3.1 Five test substance concentrations are used covering two orders of magnitude (if the solubility of the test substance permits). Study samples containing soil (or sediments or sludges) in contact with 0.01 M CaC12 are equilibrated for a minimum of 12 hours. After this, the study samples are dosed with test substance. The samples are then gently agitated until adsorption equilibrium is reached. Sample sets are removed from the orbital shaker at designated time intervals. The study samples are then prepared and analyzed for the target analyte. The adsorption isotherms are calculated using this data. The study samples fiom the last time interval are saved for the desorption isotherm study. ETS-I- 160.1 Tiers I1 and I11 Sorption Studies Page 2 of 15 3M Environmental Laboratory Page 75 of 703 BACK TO MAIN 2.4 i 2.5 2.6 3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 Tier 111: Desorption Isotherms: 2.4.1 The study samples from the adsorption isotherm study are used for the desorption isotherm study. These samples are centrifuged and the iiqueous layer removed. An equal volume of fresh 0.01 M CaCl2 solution containing no test substance is added to each sample. The samples are placed back in the orbital shaker and equilibrated for 48 hours. These new study samples are then prepared and analyzed for the target analyte. (These study samples are saved and used to determine mass balance.) The desorption isotherms are determined using this data. Tier 111: Mass Balance: 2.5.1 The study samples from the desorption isotherm study are used for the mass balance study. The study samples are centrifuged and the aqueous layer removed. Three portions of methanol are added to the study samples. With each addition of methanol, the study samples are agitated, centrifuged, and the methanol removed and placed in a second container. These subsequent (methanol) study samples are then prepared and analyzed for the target analyte. Mass balance is determined using this data. In all cases, adequate quality assurance samples are prepared and analyzed. DEFINITIONS Test Substance: Any substance (mixture or controlled compound) added or administered to the test system for the purpose of biological or chemical measurements. Target Analyte: In the analytical phase of a study, the chemical(s) singled out in analyses is the target analyte. The target analyte may be identical to the test substance used in the in-life phase of the study, or a by-product of that chemical. Reference Substance: A material or substance, one or more properties or constituents of which are sufficiently well established for it to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to materials. Test system: Any animal, plant, microorganism, chemical, or physical matrix (including soil or water) or any subpart thereof, to which the test, control, or reference substance is administered or added for study. Study sample: A sample containing the test substance in contact with the test system, or any of the subsequent samples generated from the initial set up. Control Sample:A sample containing the test substance, but which does not include the entire test system or any subsequent samples generated from the initial set up. In most, but not all cases, control samples go through all of the same processes as the study samples. Matrix Blank: A sample that has not been exposed to the test substance and/or target analyte. Matrix blanks may or may not include the entire test system. The term matrix blank also includes any subsequent samples generated from the initial matrix blank set up. In most, but not all cases, matrix blanks go through all of the same processes as the study samples. Solvent Blank: Aqueous or organic solvent that has not been exposed to the test substance and/or target analyte, and is analyzed to demonstrate the absence of target analytes in the solvent. ETS-8-160.1 Tiers I1 and I11 Sorption Studies 3M Environmental Laboratory Page 3 of 15 Page 76 of 703 BACK TO MAIN 4.0 4.1 i. t 4.2 WARNINGASND CAUTIONS Health and Safety Warnings: 4.1.1 Many of the test substances used in the laboratory are not completely characterized for toxicity and other health hazards. They should be treated as potential health hazards. Proper equipment such as gloves and safety glasses , should be worn when working with these chemicals or any solvents. Skin contact and inhalation should be avoided. Preparation of the stock standards should be done under a hood. All spills should be wiped up immediately. Cautions: 4.2.1 Contamination of glassware and equipment by the compounds of interest are an on-going issue within laboratories. Care must be taken to rinse any reusable glassware with appropriate solvents before and after the glassware is used. Triple rinsing with methanol or acetone is recommended to remove background contamination fiom the glassware. Clean all spills immediately to avoid present or future contamination. 4.2.2 Use disposable glassware whenever possible. 5.0 INTERFERENCES 5.1 Any compound that co-elutes with the target analyte(s) or the re.ference material during the HPLCMS analysis can interfere with quantification. 6.0 EQUIPMENT 6.1 Balance capable of weighing to 0.1 mg, such as OHAUS Brand Model GA200 6.2 Centrifuge capable of maintaining 4,000 f 200 rpm, such as Jouan Brand Model C412 6.3 Orbital shaker capable of a gentle rotation and temperature controlled capable of maintaining 23 f 3"C, such as Lab-Line Model Environ-Shaker 6.4 Vacuum Pump, such as Gast #DOA-P104-AA (Optional) 7.0 SUPPLIES AND MATERIALS 7.1 15-mL polypropylene centrifuge tubes, such as VWRbrandB Centrifuge Tubes, catalog number 2 1008-089 7.2 15-mL polystyrene centrifuge tubes, such as VWRbrandB Centrifuge Tubes, catalog number 21008-202 7.3 15-mL styrene butadiene centrifuge tubes, such as VWRbrandB Centrifuge Tubes, catalog number 21008-226 7.4 15-mL glass centrifuge tubes 7.5 30-mL Teflon centrifuge tubes 7.6 50-mL plastic centrifuge tubes, such as VWRbrandB 20171 7.7 Syringes, 10-pL, 25-pL, 1000-pL 7.8 Volumetric flasks, 10-mL, 100-mL, I-L, 5-L, NalgeneB and/or glass 7.9 Automatic or manual dispenser, capable of dispensing liquid with h0.1 mL accuracy 7.10 250-pL 1000-pL manual pipettor(s) and plastic pipette tips, or equivalent 7.11 Autosampler vials, 1.5 to 2 mL GC/HPLC, such as Kimble # 60820-1232 or equivalent 7.12 Autosampler vial caps, such as Wheaton # 22421 1-01 7.13 GC/HPLC autovial crimper(s) and decrimper(s) 7.14 Appropriately sized storage containers with tight-fitting caps for solutions ETS-8-160.1 Tiers I1 and 111 Sorption Studies Page 4 of 15 3M Environmental Laboratory Page 77 of 703 BACK TO MAIN 7.15 Glassware, miscellaneous 7.16 150-mL NalgeneB bottles or equivalent 7.17 pH paper capable of distinguishing pH to k0.5units t 8.0 8.1 REAGENTS, SOLUTIOANNSD STANDARDS Reagents 8.1.1 Methanol, HPLC grade, such as J.T. Baker #9093. 8.1.2 ASTM Type I water, 18.0 M a or greater. 8.1.3 CaC12, Anhydrous, to meet ACS specifications (>96% pure), such as J.T. Baker #1311. 8.1.4 Soils: Appropriate soil types selected from Table 1 below. (Soils should be air- dried at ambient temperature and sieved to a particle size 52 mm.) Table 1 2 >7.5 3.5-5.0 20-40 Clay loam 3 5.5-7.0 1.5-3.0 15-25 Silt loam 4 4.0-5.5 3.0-4.0 15-30 Loam 5 <4.0-6.0 <0.5-1.5 <10-15 6 >7.0 <0.5-1.O 40-65 Clay loamlclay NOTE: It may not be possible to obtain soils that match all criteria. Soils will be used that match as closely as possible the parameters as listed. Exceptionswill be noted. 8.1.5 Sediment: Sediment may be used in addition to the soil types listed, but is not required as part of this method. 8.1.6 Sludge: In addition to soil and/or sediment, sludge may be used as appropriate to achieve the goals of the study in question. The use of sludge is not required by this method. 8.1.7 Test Substance: Characterized by appropriate analytical technique 8.1.8 Reference Material: THPFOS, lH, lH, 2H, 2H-perfluorooctanesulfonic Acid, and/or PFBS, Potassium Peduorobutanesulfonate. 8.2 Solutions and Standards: NOTE: Different quantities of any of the solutions may be prepared, as long as solutions are documented as to how they were made. 8.2.1 Solution A: 0.01 M CaC12 Solution: 5.55k0.02 grams of CaC12 dissolved in 5.0 L of ASTM Type I water (or as appropriate for other volumes). This solution may be stored for up to 6 months at room temperature. 8.2.2 Solution B: An appropriate concentration of stock test substance in 0.01 M CaC12 Solution: Prepare an appropriate concentration of test substance in 0.01 M CaC12 in sufficient quantity to be used through out the study. Use volumetric flask and ETS-8-160.1 Tiers I1 and 111 Sorption Studies Page 5 of 15 3M Environmental Laboratory Page 78 of 703 BACK TO MAIN record weight. Immediately transfer into a NalgeneB container(s). This solution may be stored for up to 6 months at room temperature. However, it is good practice to take an aliquot of this solution and prepare it to run along with samples prepared at the same time to monitor for any possible degradation and/or adsorption to the container. 8.2.2.1 NOTE: If there is concern about the solubility of'the test substance in aqueous solutions the stock solution may be made in an appropriate solvent. 9.0 SAMPLHEANDLING 9.1 All study samples generated and prepared for analysis by HPLCYMS (in tightly capped vials) may be left at room temperature for a maximum of 15 days, or refrigerated for a maximum of six months. 9.2 The autovial study samples may be reanalyzed at any time throughout the study. However, autovials whose caps have been pierced should have the caps replaced within 3 days. 10.0 QUALITYCONTROL 10.1 Matrix Blanks consisting of the following types will be prepared for the study: 10.1.1 0.01 M CaC12 in contact with each ofthe selected soil types 10.2 Matrix Spikes (MS): One matrix spike will be prepared for each sample set, except as noted in the method. 10.3 Solvent Blanks will be prepared for the study: 10.3.1 0.01 M CaC12 and no soil 10.3.2 Methanol and no soil (in some sections) 10.4 Control Samples: Control Samples per following type will be prepared for the study: 10.4.1 Test substance in 0.01 M CaC12 only 10.4.2 Test substance in methanol only (in some sections) 10.5 Sample Replicates: Sample sets will consist of a "sample," "duplicate," and "triplicate," except as noted in the method 10.6 Surrogate(s): No surrogate will be used in this study. 10.7 Reference Substance: THPFOS and/or PFBS will be used as the reference substance. 11.0 CALIBRATION AND STANDARDIZATION 11.1 This section is outside the application of this method. 12.0 PROCEDURES 12.1 Labeling of Samples (Centrifuge Tubes) and Autovials-Centrifuge tubes and autovials should be prelabeled, according to the following scheme: 12.1.1 The study project should be given a unique Lab request number from 3Ms Environmental Laboratory Sample Control Numbering system. 12.1.2 Study Samples, Labeling of Centrifuge Tubes: Each individual sample and QC sample that is set up will have a unique identifier. 12.1.3 If necessary, aliquots taken from the study samples will be uniquely identified by using the initial study sample ID and then adding an additional designator for each aliquot removed from the study sample. ETS-8-160.1 Tiers I1 and III Sorption Studies Page 6 of 15 3M Environmenfal Laboratory Page 79 of 703 BACK TO MAIN 12.1.4 All autovials will clearly identify any "extra" dilution made of its contents. 12.1.5 All Matrix Spike samples will contain all of the above information, as well as the designator "MS." 'i 12.2 Adsomtion Kinetics at One Concentration of the Test Substance 12.2.1 Select appropriate soils and/or sediments and/or sludges using the soils/sediments/sludges listed in section 8.1. Use the centrifuge tube materialhype determined for use from Method ETS-8- 159. 12.2.2 Prepare a sufficient number of individual containers of each series such that a (triplicate) set of tubes can be removed according to the following approximate time intervals: 0 hr, 2 hr, 4 hr, 8 hr, 16 hr, 24 hr, 36 hr and 48 hr. 12.2.2.1 NOTE: I f the soi1:solution ratio permits one set of (triplicate) tubes may be prepared for each soil, and aliquots taken out at each time point rather than preparing a separate set of tubes for each time point (serial method). The volume of the aliquot must not exceed 2.5% of the total volume in the test vessel. In this case matrix spikes will only be performed for two time points rather than all of them. 12.2.3 Using the soil: solution ratio determined from Method ETS-8-159, set up the appropriate study sample grid using Table 2. Table 2 E h Onlyneed one from this set one from this set. 12.2.4 Weigh the soil and record on the appropriate data form. 12.2.5 Add the appropriate volume of 0.01 M CaC12 solution (Solution A) to each tube and record the volume on the appropriate data form. 12.2.6 Document the pH of the stock test substance solution, using pH paper. Record to f0.5pH units. 12.2.7 The study samples are equilibrated for a minimum of 12 hours by placing the tubes on an orbital shaker at 23 +3 "C using a gentle rotation. Record start and stop timeddates on appropriate data forms. 12.2.8 Remove the tubes after the 12 hours. Add the stock test substance solution. 12.2.8.1 NOTE: The test substance concentrations specified in Table 2 (grayed section) are meant as a guide only. The final concentration of the test substance can be changed to better accommodate the analytical objectives of the study. ETS-8-160.1 Tiers I1 and I11 Sorption Studies Page 7 of 15 3M Environmental Laboratory Page 80 of 703 BACK TO MAIN 12.2.9 All but the "0 hr" study samples are then placed back on the orbital shaker for designated time intervals at 23 rt3 "C using a gentle rotation. The "0hr"study samplesproceed directly to 12.2.12. 12.2.9.1 NOTE: If using the serial method centrifuge the tubes after the addition of t the test substance and take the 0 hour aliquot, then place the tubes on the shaker. 12.2.10Remove study sample sets at the following approximate time points and record the datehime. 2hr 16hr 48hr 4hr 24hr 8hr 36hr 12.2.10.1 Note: If using the serial method remove the sample tubes at each time point, follow steps 12.2.11 through 12.2.15. Add an amount of fresh CaClz equal to the amount taken out as an aliquot. Then vortex and return the tube to the shaker. 12.2.11For the "48 hr" study samples only, weigh the container + contents and record - on the proper data form. Document the pH for one of each sample set. Record to 50.5 pH units. 12.2.12.Centrifuge until the aqueous layer appears clear 12.2.13Withdraw an aliquot of the study sample and dispense into a prelabeled autovial. Dilute as needed. 12.2.14Spiking: Refer to section 12.7 for spiking. 12.2.15Continue to pull the timed study sample sets at the designated time points and repeat steps 12.2.11 through 12.2.15, as appropriate. 12.2.16Do not discard the "48 hr" study sample tubes. 12.2.17Add THPFOS and/or PFBS internal standard prior to analysis. 12.2.18After all the study samples have been pulled and prepared, analyze autovials using appropriate methodology to determine concentration of target analyte. 12.2.19Make the appropriate calculations as defined in the calculations section. 12.2.20Determine the Adsorption Kinetics. 12.3 Desorption KineticsCerial Method 12.3.1 Desorption Kinetics Study Samples will be generated according to the following grid (Table 3). Table 3 12.3.2 This section uses the last set of sample tubes ("48 hr") from Method ETS-8160.0 Section 12.2 (Adsorption Kinetics Study). ETS-8-160.1 Tiers I1 and 111 Sorption Studies Page 8 of 15 3M Environmental Laboratory Page 81 of 703 BACK TO MAIN 12.3.3 Centrifuge the tubes until the aqueous layer appears clear. Remove as much of the aqueous layer as possible, taking care not to remove any of the solids. 12.3.4 Replace the volume of solution removed with an equal volume of fresh 0.01 M CaC12 solution containing no test substance. This is done by refilling with fresh t Solution A until the weight of the container + contents is equal to the weight (+O. 1 g) recorded in step 12.2.11. Record this new weight on the appropriate data form. 12.3.5 Place the study samples back into the orbital shaker and continue the gentle agitation for a total of 48 hours, during which aliquots of the aqueous phase will be taken at the following approximate times: 2 hr, 4 hr, 8 hr, 16 hr, 24 hr, 32 hr and 48 hour. (Times may be varied depending on results from Section 12.1.) Record the actual times on the appropriate data forms. Prepare each aliquot by following the steps given in 12.3.6 through 12.3.7. NOTE:Maximum sample volume removal is limited to approximately 1% - 2% per time point, thus limiting sample volume removal. 12.3.6 Draw two aliquots of the study sample from the 24-hour and 48-hour time points (for matrix spike); draw only one aliquot of the study sample for the other time points. Transfer the contents into a prelabeled autovial and cap. 12.3.6.1 Spiking: Important! Only two time points will be spiked for this series of study samples: 24 hr and 48 hr due to limited volume I removal constraints. See section 12.7 for spiking. 12.3.7 Replacement of 0.01 M CaClz solution to study samples: Add an equal amount of fresh 0.01 M CaC12 solution (Solution A) to the centrifuge tubes after the withdrawal of the sample aliquots. 12.3.8 At each time point, follow steps 12.3.5 through 12.3.8 until the last time point has been sampled. Note: step 12.3.8 is not repeated for the final time point. 12.3.9 Add THPFOS and/or PFBS internal standard prior to analysis. 12.3.10After all the study samples have been pulled and prepared, analyze autovials using appropriate methodology to determine concentration of target analyte. 12.3.1 1Make the appropriate calculations as defined in the calculations section. 12.3.12Determine the Desorption Kinetics. 12.4 Determination of Freundlich Adsorption Isotherms 12.4.1 Select appropriate soils and/or sediments and/or sludges using the soils/sediments/sludges listed in section 8.1. Use the centrifuge tube materialhype and soi1:solution ratio determined for use from Method E;TS-8-159. 12.4.2 Prepare a sufficient number of individual containers of each series such that a (triplicate) set of tubes exists for each soil/concentrationcombination 12.4.3 Set up the study sample grid, according to Table 4. Remember that only one of these ratios will be selected for use in this part of the study! Table 4 ETS-8-160. I Tiers I1 and 111 Sorption Studies 3M Environmental Laboratory Page 9 of 15 Page 82 of 703 BACK TO MAIN Only need one from this set 1.1 5.00 f 0 05 5 0 f 0.1 2 NA 3 (X5) o.oo* 1 :5 2.50 f0.05 12.5 k 0.1 2 NA 3 (x 5) 0.00' 125 1.OO f 0 05 25.0 f 0.2 2 NA 3 (x 5) 0.00' one from this set. one from this set this set. * To be added in afterthe study samples have equilibrated for 12 hours. 12.4.4 Weigh the soil and record on the appropriate data form. 12.4.5 Add the appropriate volume of 0.01 M CaC12 solution (Solution A) to each tube and record the volume on the appropriate data form. 12.4.6 Document the pH of the stock test substance solution, using pH paper. Record to + _ O SpH units. 12.4.7 The study samples are equilibrated with 0.01 M CaC12 for a minimum of 12 hours by placing the tubes on an orbital shaker at 23 +3 "C using a gentle rotation. Record start and stop timeddates on appropriate data forms. 12.4.8 Remove the tubes after the 12 hours and add the stock test substance solution. 12.4.8.1 NOTE: The test substance concentrations specified in Table 4 (grayed section) are meant as a guide only. The final concentration of the test substance can be changed to better accommodate the analytical objectives of the study. Fewer concentrations may be used if there is a solubility limitation as long as the reasons for doing so are documented in the final report. 12.4.9 Steps for "0 hr" study samples: 12.4.9.1 Gently shake to mix the contents of the test vessels. 12.4.9.2 Centrifuge until the aqueous layer appears clear. 12.4.9.3 Document the pH for one of each sample set per time point. ETS-8-160.1 Tiers I1 and 111 Sorption Studies Page 10 of 15 3M Environmental Laborafory Page 83 of 703 BACK TO MAIN 12.4.9.4 Withdraw an aliquot from the test vessel and dispense into a prelabeled autovial. Replace the amount aliquotted G t h fresh 0.01M CaC12 solution. Dilute as needed. 12.4.9.5 Spiking: Refer to Section 12.7 for spiking. 12.4.10Steps for "48 hour" study samples: 12.4.10.1 The test vessels are placed back on the orbital shaker for 48 hours at 23 +.3 "C using a gentle rotation. Record start and stop fimeddateson appropriate data forms. 12.4.10.2 Remove sample sets after 48 hours and record the datehime. 12.4.10.3 Weigh each container + contents and record on the appropriate data form. 12.4.10.4 Centrifuge until the aqueous layer appears clear. 12.4.10.5 Document the pH for one of each sample set. 12.4.10.6 Withdraw an aliquot of the study sample and dispense into a prelabeled autovial. Dilute as needed. 12.4.10.7 Spiking: Refer to Section 12.7 for spiking. 12.4.11Do not discard the "48 hr" set of study samples. These will be used in Section 12.5. 12.4.12Add THPFOS and/or PFBS internal standard prior to analysis. 12.4.13After all study samples have been pulled and prepared, analyze autovials using appropriate methodology to determine concentration of target analyte. 12.4.14Make appropriate calculations as defined in the Calculations section. 12.4.15Determine the Freundlich Adsorption Isotherms 12.5 Desorption Isotherms 12.5.1 Use the test vessels generated from ETS-8-160 Section 12.4, Adsorption Isotherms. (Refer to Table 5) Table 5 12.5.2 12.5.3 12.5.4 12.5.5 Centrifuge the tubes until the aqueous layer appears clear. Remove as much of the aqueous layer as possible, taking care not to remove any of the solid layer. Replace the volume of solution removed with an equal volume of fresh 0.01 M CaC12 solution containing no test substance. This is done by refilling with the aqueous solution until the weight of the container + contents is equal to (+O. 1 g) what it was in step 12.4.10.3 (before removal of the aqueous portion). Record this new weight on the appropriate data form. Place the tubes back in the orbital shaker and gently rotate at 23 +3 OC for 48 hours. Record datehime on the appropriate data form. Remove the tubes from the shaker after 48 hours and record datehime. ETS-8-160.1 Tiers I1 and 111 Sorption Studies Page 11 of 15 3M Environmental Laboratory Page 84 of 703 BACK TO MAIN 12.5.6 Centrifuge until the aqueous layer appears clear. 12.5.7 Withdraw an aliquot of the study sample and dispense into a prelabeled autovial. Dilute as needed. i. 12.5.8 Spiking: Refer to Section 12.7 for spiking. i 12.5.9 Do not discard the "48 hr" set of study samples. These will be used in Section 12.6 12.5.10Add THPFOS andor PFBS internal standard prior to analysis. 12.5.11After all study samples have been pulled and prepared, analyze autovials using appropriate methodology to determine concentration of target analyte. 12.6 Mass Balance Determination 12.6.1 Continue using the test vessels from Section 12.5, Desorption Isotherms 12.6.2 Centrifuge the tubes until the aqueous layer appears clear. 12.6.3 Remove as much of the aqueous layer as possible, taking care not to remove any of the solids layer (the aqueous layer may be discarded). 12.6.4 Add the amount of methanol appropriate to the amount of soil in each tube by referring to the following table: Table 6 12.6.5 Vortex the tubes for -1 minute. (Alternatively,tubes may be placed horizontally in a shaker and shaken for -5 minutes.) 12.6.6 Centrifuge until the solvent layer appears clear. Remove as much of the solvent (methanol) layer as possible without removing the solids layer. 12.6.7 Place the solvent in a second prelabeled centrifuge tube. 12.6.8 Repeat steps 12.6.4 through 12.6.7, using the same prelabeled centrifuge tube for each extraction. 12.6.9 Mix the contents of the second centrifuge tube after the last extraction volume is added. Centrihge the solvent to remove particulates if needed. 12.6.10If it is anticipated that the concentration of the test substance will be near or below the limit of quantification, a concentration step should be performed prior to continuing with step 12.6.11. 12.6.11Withdraw an aliquot ofthe study sample from step 12.6.LO and dispense into a prelabeled autovial. Dilute as needed. 12.6.12Spiking: Refer to Section 12.7 for spiking. 12.6.13Add THPFOS and/or PFBS internal standard prior to analysis. 12.6.14After all study samples have been pulled and prepared, analyze autovials using appropriate methodology to determine concentration of target analyte. 12.6.15Make appropriate calculations as defined in the Calculations section. 12.6.16Determine mass balance. ETS-8-160.1 Tiers I1 and 111 Sorption Studies Page 12 of 15 3M Environmenfal Laboratory Page 85 of 703 BACK TO MAIN 12.7 1 Spiking 12.7.1 Only one replicate per study sample set will be spiked with a known amount of the test substance. 12.7.2 Spiking will be done whenever any aliquoted study sample is generated. 12.7.3 Dilute samples to the appropriate level for analysis (if necessary) with methanol. 12.7.4 Add an appropriate amount of spiking solution to provide a spike concentration of approximately 200ppb (or as deemed appropriate). 13.0 DATAANALYSIASND CALCULATIONS 13.1 Data analysis and calculations should be done using the templates provided from OECD Guideline 106. 14.0 METHODPERFORMANCE There are no previously defined method performance criteria for this method. However, this method will generate statistical data that may be used as a guideline for monitoring performance for Method ETS-8-160. i 14.1 Accuracy 14.1.1 Matrix Spikes (MS): One matrix spike per study sample set will be generated. The matrix spikes will be calculated by using the following equation: (MS conc. analytical - Sample conc. analytical) x 100 (MS Spike conc. theoretical) 14.2 Precision 14.2.1 Replicates: Triplicate study samples will be generated using this method. Relative Standard Deviations (RSD) will be calculated from the triplicate samples. In the cases, where there are only two replicates, the Relative Percent Difference (RPD) will be calculated. 15.0 POLLUTION PREVENTION AND WASTE MANAGEMENT 15.1 Dispose of sample waste by placing in high or low BTU containers as appropriate. 15.2 Use broken glass containers to dispose of any empty glass containers, pipettes, etc. 16.0 RECORDS 16.1 Laboratory data forms will be generated and filled out during the course of this study. These data forms will be archived according to standard laboratory protocols. 17.0 ATTACHMENTS 17.1 Example data forms: 17.1.1 Suitable Analytical Method Data Form 17.1.2 Suitable Container Data Form 17.1.3 Suitable Desorption Solvent Data Form 17.1.4 Soi1:Aqueous Optimal Ratio Data Form ETS-8- 160.1 Tiers I1 and 111 Sorption Studies Page 13 of 15 3M Environmental Laboratory Page 86 of 703 BACK TO MAIN 18.0 REFERENCES 18.1 Organization of Economic Cooperation and Development, OECD Guideline for the Testing of chemicals. "Adsorption-Desorption Using a Batch Equilibrium Method: ;c. OECD Guideline 106 Adopted 21 January 2000. 18.2 EPA Fate, Transport and Transformation Test Guidelines: OPPTS 835.1220 Sediment and Soil AdsorptiodDesorption Isotherm, EPA 712-C-98-048, January 1998. 19.0 AFFECTEDDOCUMENTS 19.1 ETS-8-159 Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicalsas the Test Substance (Based on OECD Guideline 106) ETS-8-160.1 Tiers I1 and 111Sorption Studies 3M Environmental Laboratory Page 14 of 15 Page 87 of 703 BACK TO MAIN 20.0 REVISIONS Revision % Number. Reason For Revision 160.1 Requirements for specific test substance concentrations were taken out to accommodate less soluble species and matrix effects. The I .OO mL sample size was eliminated to accommodate dilutions of the original sample. The 1 5 ratio sample size was adjusted to be consistent with the ETS-8-19.0 sample size. The adsorption kinetics section was revised to accommodate a serial sample preparation rather than just the parallel method. Revision - Date ETS-8- 160.1 Tiers I1 and 111 Sorption Studies 3M Environmental Laboratory Page 15 of 15 Page 88 of 703 BACK TO MAIN OECD/OCDE 106 Adopted : 2 1I' January 2000 OECD GUIDELINE FOR THE TESTING OF CHEMICALS Adsorption - DesorDtion Usiw a Batch EauilibEium Method INTRODUCTION 1. This Guideline is based on the proposal submitted by the European Commission in 1993 and takes into account the comments on that proposal submitted by the Member countries. Several activities undertaken in the European Union bore on the development of an adsorption test. These included an extensive investigation due to the collaboration of the German UmweltbundesamtW A ) , the University of Gel, and the European Commission and its Joint Research Centre at Ispra, Italy (1)(2). In 1988 UBA organised a ring-test in which 27 laboratories in EU Member Statesparticipated(3). An OECD Workshop on Soil Selection was held at Belgirate, Italy, in 1995 (4). The Woikshop agreed on the main elements of the updated Test Guideline 106 for an adsorptioddesorption test and, in particular, on the characterisation and selection of the soil types for use in the test. 2. Other guidelines concerning adsorptioddesorption exist only at national level and are mainly focused on pesticides testing (5)(6)(7)(8)(9)( lo)( 11). These documents as well as an extensive relevant literature were considered when developingthis Guideline. SIGNIFICANCE AND USE 3. Adsorptioddesorption studies are useful for generating essential information on the mobility of chemicals and their distribution in the soil, water and air compartments of our biosphere (12)(13)(14)(15)(16)(17)(18)(19)(20)(21). They can be used in the prediction or estimation,for example, of the availability of a chemical for degradation (22)(23), transformation and uptake by organisms (24); leaching through the soil profile (16)(18)(19)(21)(25)(26)(27)(28); volatility from soil (21)(29)(30); and run-off from land surfaces into natural waters (18)(31)(32). Adsorption data can also be used for comparative and modelling purposes (19)(33)(34)(35). 4. The distributionof a chemical between soil and aqueous phases is a comple_xprocess depending on a number of different factors: the chemical nature of the substance (12)(36)(37)(38)(39)(40), the characteristics of the soil (4)( 12)(13)(14)(41)(42)(43)(44)(45)(46)(47)(48)(49), and climatic factors such as rainfall, temperature, sunlight and wind. Thus, the numerous phenomena and mechanisms involved in the process of adsorption of a chemical by soil cannot be completely defined by a simplified laboratory model such as the present Guideline. However, even if this attempt cannot cover all the environmentally possible cases, it provides valuable information on the environmental relevance of the adsorptionof a chemical. SCOPE 5. This Guideline is aimed at estimating the adsorptioddesorption behaviour of a substance on soils. The goal is to obtain a sorption value which can be used to predict partitioning under a variety of environmental conditions; to this end, equilibrium adsorption coefficients for a chemical on various soils are determined as a fbnction of soil characteristics (e.g. organic carbon content, clay content, soil texture, and 1/45 3M Environmental Laboratory Page 89 of 703 BACK TO MAIN 106 OECD/OCDE pH). Different soil types have to be used in order to cover as widely as possible the interactions of a given i substance with naturally occurring soils. 6. In this Guideline,adsorptionrepresents the process of the binding of a chemical to surfaces ofsoils; it does not distinguish between different adsorption processes (physical and chemical adsorption) and such processes as surface catalysed degradation,bulk adsorption or chemical reaction. Adsorption that will occur on colloids particles(diameter < 0.2 pn)generatedby the soils is not fklly-taken into account. 7. The soil parameters that are believed most important for adsorption are: organic carbon content (3)(4)( 12)(13)(14)(41)(43)(44)(45)(46)(47)(48); clay content and soil texture (3)(4)(41)(42)(43)(44)(45)(46) (47)(48); and pH for ionisable compounds (3)(4)(42). Other soil parameters which may have an impact on the adsorptioddesorption of a particular substance are the effective cation exchange capacity (ECEC), the content of amorphous iron and aluminium oxides, particularly for volcanic and tropical soils (4), as well as the specific surface -(49). 8. The test is designed to evaluate the adsorption of a chemical on different soil types with a varying range of organic carbon content, clay contentand soil texture, and pH. It comprisesthree tiers: - Tierl: Preliminarv study in order to determine: - the soillsolution ratio; - the equilibration time for adsorption and the amount of test substance adsorbed at equilibrium; - the adsorption of the test substance on the surfaces of the test vessels and the stability of the test substance during the test period. Tier2: Screeninv test: the adsorption is studied in five different soil types by means of adsorption kinetics at a single concentration and determination of distribution coefficients K, and K,. Tier 3: Determination of Freundlich adsomtion isotherms to determine the influence of concentration on the extent of adsorption on soils. Study of desomtion by means of desomtion kineticflreundlich desomtion isotherms (Annex 1). DEFINITIONS AND UNITS 9. Definitions and units are set out in the Data and Reporting section and Annex 2. The weight of soil samples as mentioned in the equations of the Guideline refer to the oven dry weight. PRINCIPLEOF THE METHOD - 10. Known volumes of solutions of the test substance, non-labelled or radiolabelled, at known concentrations in 0.01 M CaC1, are added to soil samples of known dry weight which have been pre- equilibrated in 0.01 M CaCI,. The mixture is agitated for an appropriate time. The soil suspensions are then separated by centrihgation and, if so wished, filtration and the aqueous phase is analysed. The amount of test substance adsorbed on the soil sample is calculated as the difference between the amount of test substance initially present in solution and the amount remaining at the end of the experiment (indirect method). 11. As an option, the amount of the test substance adsorbed can also be directly determined by analysis of soil (direct method). Although this makes the analytical procedure more tedious, involving stepwise soil extraction with an appropriate solvent, it is recommended in cases where the difference in the solution concentration of the substance cannot be accurately determined. Examples of such cases are: adsorption of 2/45 3M Environmental Laboratory Page 90 of 703 BACK TO MAIN OECD/OCDE 106 the test substance on surfaces of the test vessels, instability of the test substance in the time scale of the experiment, weak adsorption giving only small concentration change in the solution; and strong adsorption yielding low concentration which cannot be accurately determined. If radiolabelled substance is used, the soil extraction may be avoided by analysis of the soil phase by combustion and liquid scintillationcounting. However, liquid scintillationcounting is an unspecific technique which Cannot differentiate between the test chemical and its transformation products; thereforeit should be used onlyif the test chemical is stable for the duration of the study. INFORMATIONON THE TEST SUBSTANCE 12. Chemical reagents should be of analytical grade. The use of non-labelled test substances with known composition and preferably at least 95% purity or of radiolabelled test substances with known co be mpositio applied. n a n d - radio-purity, is recommended. In the case of short half-life tracers, decay corrections should 13. Before carrying out a test for adsorption-desorption, the following information on the test substance should be available: (a) solubility in water [OECD Guideline 1051; (b) vapour pressure [OECD Guideline 1041orland fienry's law constant; (c) abiotic hydrolysis as a function of pH [OECD Guideline 1111; (d) n-octanol/waterpartition coefficient [OECD Guidelines 107 and 1171; (e) ready biodegradability [OECD Guideline 3011 or aerobic and anaerobictransformation in soil; (0 pKa of ionisable substances; (g) direct photolysis in water (Le. UV-Vis absorptionspectruminwater, quantum yield) and photodegradationon soil. APPLlCABlLlTY OF THE TEST 14. The test is applicable to chemical substances for which an analytical method with sufficient accurancy is available. An important parameter that can influence the reliability of the results, especially when the indirect method is followed (see paragraph lo), is the stability of the test substance in the time scale of the test. Thus, it is a prerequisite to check the stability in a preliminruy study; if a transformation in the time scale of the test is observed, it is recommen&d that the main study be performed by analysing both soil and aqueous phases. 15. Difficulties m a y arise in conducting this test for test substances with low water solubility (Sw -=IO4 8 1-I), as well as for highly charged substances, due to the fact that the concentration in the aqueous phase cannot be measured analytically with sufficient accuracy. In these cases, additional steps have to be taken. Guidance on how to deal with these problems is given in the relevant sections of this Guideline. 16. When testing volatile substances, care should be taken to avoid losses during the study. DESCRIPTION OF THE METHOD Apparatus and chemical reapents 17. Standard laboratory equipment, especially the following: (a) Tubes or vessels to conduct the experiments. It is important that these tubes or vessels: - fit directly in the centrifuge apparatus in order to minimise handling and transfer errors; 3/45 3M Environmental Laboratory Page 91 of 703 BACK TO MAIN 106 OECDlOCDE - be made of an inert material, which minimises adsorption of the test substance on its surface. (b) Agitation device: overhead shaker or equivalent equipment; the agitation device should keep the soil in suspension during shaking. (c) Centrifuge: preferably high-speed, e.g. centrifugation forces > 3000g, temperature controlled, capable of removing particles with a diameter greater than 0.2 p n from aqueous solution. The containersihould be capped during agitationand centrifugationio avoid volatility and water losses. To minimise adsorptionon them, deactivated caps such as PTFE (Teflon? lined screw caps should be used. (d) Optional: filtration device; filters of 0.2 pn porosity, sterile, single use. Special care should be taken in the choice of the filter material, to avoid any losses of the test substance on it; for poorly soluble test substances, organic filter material is not recommended. (e) Analytical -instrumentation,suitable for measuring the concentration of the test chemical. (0 Laboratory oven, capable of maintaining a temperature of 103 O to 110 O C . Characterisationand selectionof soils 18. The soils should be characterised by three paraineters considered to be largely responsible for the adsorptive capacity: organic carbon, clay content and soil texture, and pH. As already mentioned in paragraph 7, other physico-chemical properties of the soil may have an impact on the adsorptioddesorption of a particular substance and should be considered in such cases. 19. The methods used for soil characterisation are very important and can have a significant influence on the results. Therefore, it is recommended that soil pH should be measured in a solution of 0.01 M CaCl, (that is the solution used in adsorptioddesorption testing) according to the correspondingIS0 method (IS0 10390-1). It is also recommended that the other relevant soil properties be determined according to standard methods (for example IS0 "Handbook of Soil Analysis"); this permits the analyses of sorption data to be based on globally standardised soil parameters. Some guidance for existing standard methods of soil analysis and characterisation is given in references 50-52. For calibration of soil test methods, the use of reference soils might be considered. 20. Guidance for selection of soils for adsorptioddesorption experiments is given in Table 1. The seven selected soils cover soil types typically encountered in temperate geographical zones. For ionisable test substances, the selected soils should cover a wide range of pH, in order to evaluate the adsorption of the substance in its ionised and unionised forms. Guidance on how many different soils to use at the various stages of the test is given under the heading "Performanceofthe test". * 21. Other soil types may sometimes be necessary to represent cooler, temperate and tropical regions within the OECD Countries. Therefore, if other soil types are preferred, they should be characterisedby the same parameters and should have similar variations in properties to those described in Table 1, even if they do not match the criteria exactly. 4/45 3M Environmental Laboratory Page 92 of 703 BACK TO MAIN OECD/OCDE 106 Table 1: Guidance for selection of soil samples for adsorption-desorption t I Organic carbon content 1 Clay content 1 Soil texture* 1 /II II 4.5-5.5' I > 7.5 5.5-7.0 4 4.0-5.5 5 < 4.0-6.0' 6 > 7.0 7 < 4.5 I 1.0-2.0 1 3.5-5.0 I 1.5-3.0 3.0-4.0 < 0.5-1.5'' < 0.5-1.0'' > 10 1I 1 65-80- I 20-40 1 15-25 I clay - 1 clay loam 1 silt loam 15-30 loam < 10-158 loamy sand 40-65 clay loadclay < 10 sandloamy sand Collection and storage of soil samoles Collection 22. No specific soil sampling techniques or tools are recommended; the sampling technique depends on the purpose of the study (53)(54)(55)(56)(57)(58). 23. The following should be considered (a) detailed information on the history of the field site is necessary; this includes location, vegetation cover, treatments with pesticides and/or fertilisers, biological additions or accidental contamination. Recommendations of the IS0 standard on soil sampling ( I S 0 10381-6) should be followed with respect to the description of the sampling site; @) the sampling site has to be exactly defined by UTM (Universal Transversal Mercator- ProjectionEuropean Horizontal Datum) or geographical co-ordinates; this could allow re- collection o f a particular soil in the future or could help in defining soil under various classification systems used in different countries. Also, only A horizon up to a maximum depth of 20 cm should be collected. Especially for included in the sampling. the soil no. 7, if a 0, horizon is present as -part of the soil, it should be 24. The soil samples should be transported using containers and under temperature conditions which guarantee that the initial soil properties are not significantly altered. Storage 25. The use of soils freshly taken from the field is preferred. Only if this is not possible soil can be stored at ambient temperatures and should be kept air-dried. No limit on the storage time is recommended, but soils stored for more than three years should be re-analysed prior to the use with respect to their organic carbon content, pH and CEC. Handling and Dreoaration of soil samoles for the test 5145 3M Environmental Laboratory Page 93 of 703 BACK TO MAIN 106 OECD/OCDE 26. The soils are air-dried at ambient temperature (preferably between 20-25 "C). Disaggregation should be performed with minimal force, so that the original texture of the soil will be changed as little as i possible. The soils are sieved to a particle size 12 mm; recommendations of the IS0 standard on soil sampling (IS0 10381- 6) should be followed with respect to the sieving process. Careful homogenisation is recommended, as this enhances the reproducibility of the results. 27. The moist3e content of each soil is determined on three aliquoswith heating at 105C until there is no significant change in weight (approx. 12h). For all calculations the mass of soil refers to oven dry mass, i.e. the weight of soil corrected for moisture content. Preoaration of the test substance for amlication to soil .28. The test substance is dissolved in a 0.01 M solution of calcium chloride (CaClJ in distilled or de- ionised water; the CaCl, solution is used as the aqueous solvent phase to improve centrifugation and minimise cation exchange. The concentration of the stock solution should preferably be three orders of magnitude higher than the detection limit of the analytical method used. This threshold safeguards accurate measurements with respect to the methodology followed in this Guideline (paragraphs 52-58); additionally, the stock solution concentration should be below water solubility of the test substance. 29. The stock solution should preferably be prepareh just before application to soil samples and should i be kept closed in the dark at 4C. The storage time depends on the stability of the test substance and its concentration in the solution. 30. Only for poorly soluble substances ( S , < 10` g l'), an appropriate solubilising agent may be needed when it is difficult to dissolve the test substance. This solubilising agent: (a) should be miscible with water such as methanol or acetonitrile; (b) its concentration should not exceed 1% of the total volume of the stock solution and should constitute less than that in the solution of the test substance which will come in contact with the soil (preferably less than O.l"/o); and (c) should not be a surfactant or undergo solvolytic reactions with the test chemical. The use of a solubilising agent should be stipulated and justified in the reporting of the data. 31. Another alternative for poorly soluble substances is to add the test substance to the test system by spiking: the test substance is dissolved in an organic solvent, an aliquot of which is added to the system of soil and 0.01 M solution of CaCZ in distilled or .de-ionised water. The content of organic solvent in the aqueous phase should be kept as low as possible, normally not exceeding 0.1%. However, the experimenter should have in mind that spiking from an organic solution may suffer from volume unreproducibility. Consequently, an additional error may be introduced as +e test substance and co-solvent concentration would not be exactly the same in all tests. - PREREOUISITES FOR PERFORMING THE ADSORPTIONlDESORPTION TEST The analytical method 32. The key parameters that can influence the accurancy of sorption measurements include the accuracy of the analytical method in analysis of both the solution and adsorbed phases, the stability and purity of the test substance, the attainment of sorption equilibrium, the magnitude of the solution concentration change, the soil/solution ratio and changes in the soil structure during the equilibration process (35, 59-62). Some examples bearing upon the accuracy issues are given in Annex 3.33. 6/45 3M Environmental Laboratory Page 94 of 703 BACK TO MAIN OECD/OCDE 106 The reliability of the analytical method used must be checked at the concentration range which is likely to occur during the test. The experimenter should feel free to develop an appropriate method with appropriate accuracy, precision, reproducibility, detection limits and recovery. Some guidance on how to perform such a test is given by the experiment below. 34. An approppate volume of 0.01 M CaCl,, e.g. 100 cm', is agitated during 4 h with a weight of soil, e.g. 20 g, of high adsorbability, i.e. with high organic carbon and clay content; these weights and volumes may vary depending on analytical needs, but a soiholution ratio of 1:s is a convenient starting point. The mixture is centrifuged and the aqueous phase may be filtrated. A certain volume of the test substance stock solution is added to the latter to reach a nominal concentration within the concentration range which is likely to occur during the test. This volume should not exceed 10% of the final volume of the aqueous phase, in order to change as little as possible the nature of the pre-equilibrationsolution. The solution is analysed. 35. One blank F n consisting of the system soil + CaCl, solution (without test substance) must be included, in order to check for artifacts in the analy!kal method and for matrix effects caused by the soil. 36. The analytical methods which can be used for sorption measurements include gas-liquid chromatography (GLC), high-performance liquid chromatography (HPLC), spectrometry (e.g. GC/mass spectrometry, HPLC/mass spectrometry) and liquid scintillation counting (for radiolabelled substances). Independent of the analytical method used, it is considered suitable if the recoveries are between 90% and 110% of the nominal value. In order to allow for detection and evaluation after partitioning has taken place, the detection limits of the analytical method should be at least two orders of magnitude below the nominal concentration. 37. The characteristics and detection limits of the analytical method available for c a v i n g out adsorption studies play an important role in defining the test conditions and the whole experimental performance of the test. This Guideline follows a general experimental path and provides recommendations and guidance for alternative solutions where the analytical method and laboratory facilities may impose limitations. The selection of optimal soiUsolution ratios 38. Selection of appropriate soil to solution ratios for sorption studies depends on the distribution coefficient K,and the relative degree of adsorption.desired. The change of the substance concentration in the solution determines the statistical accuracy of the measurement based on the form of adsorption equation and the limit of the analytical methodology, in detecting the concentration of the chemical in solution. Therefore, in general practice it is useful to settle on a few fixed ratios, for which the percentage adsorbed is above 20%, and preferably >50% (62), while care should be taken to keep the test substance concentration in the aqueous phase high enough to be measured accurately. This is particularly important in the case of high adsorption percentages. 39. With respect to the above remarks, a convenient approach to selecting the appropriate soil/water ratios, is based on an estimate. of the K, value either by preliminary studies or by established estimation techniques (Annex 4). Selection of an appropriate ratio can then be made based on a plot of soil/solution ratio versus K,, for fixed percentages of adsorption (Fig.1). In this plot it is assumed that the adsorption equation is linear'. The applicable relationship is obtained by rearranging equation (4) of the K,in the form ofequation (1): 1/45 3M Environmental Laboratory Page 95 of 703 106 OECD/OCDE - mnds(eq) or in its logarithmic form assuming that R = m J V oand Ag%/IOO = : m0 BACK TO MAIN Distribution coefficient Kd (cm3 g-1) Fig. 1 Relationship between soil to solution ratios and K,at various percentages of adsorbed test substance 40. Fig. 1 shows soiVsolutionratios required as a b c t i o n of K, for different levels of adsorption. For example, with a soiVsolution ratio of 1:5 and a K, of 20, approximately 80% adsorption would occur. To obtain 50% adsorption for the same K,, a 1:25ratio must be used. This approach to selecting the appropriate soiVsolutionratios gives the investigator the flexibilityto meet experimentalneeds. 41. Areas which are more difficult to deal with are those where the chemical is very slightly or highly adsorbed. Where low adsorption occurs, a 1:l soil/solution ratio is recommended, although for some very organic soil types smaller ratios may be necessary to obtain a sluny. In any case, care must be taken with the analytical methodology to measure small changes in solution concentration; otherwise the adsorption measurement will be inaccurate. On the other hand, at very high distribution coefficients K,, one can go up to a 1:100 soiVsolutionratio in order to leave a significant amount of chemical in solution. However, care must be taken to ensure good mixing, and adequate time must be allowed for the system to equilibrate. An alternative approach to deal with these extreme cases when adequate analytical methodology is missing, is to predict the K, value applying estimation techniques based, for example, on Pa,,values (Annex 4). This could be useful especially for low adsorbedpolar chemicals with Pa,,< 20 and for lipaphilichighly sorptive chemicals with Pew> 10'. 8/45 3M Environmental Laboratory Page 96 of 703 BACK TO MAIN OECD/OCDE 106 PERFORMANCE OF THE TEST t Test conditions 42. All experiments are done at laboratory ambient temperature and, if possible, at a constant temperature betweea20 "C and 25 "C. 43. Centrifugation conditions should allow the removal of particles larger than 0.2 pm from the solution. This value triggers the smallest sized particle that is considered as a solid particle, and is the limit between solid and colloid particles. Guidance on how to determine the centrifigation conditions is given in Annex 5. 44. If the centrifugation facilities cannot guarantee the removal of particles larger than 0.2 w, a combination of centrifugation and filtrationwith 0.2 p n filters could be used. These filters should be made of a suitable inert material to avoid any losses of the test substance on them. In any case, it should be proven that no losses of the test substance occur during filtration. Tier 1- Preliminary study 45. The purpose of conducting a preliminary study has already been given in paragraph 8 in the Scope section. Guidance for setting up such a test is given with the experiment suggested below. Selection of optimal soiVsolution ratios 46. Two soil types and three soil/solution ratios (six experiments) are used. One soil type has high organic carbon and low clay content, and the other low organic carbon and high clay content. The following soil to solution ratios are suggested. However, the absolute mass of soil and volume of aqueous solution correspondingto these ratios can be different with respect to laboratory facilities: -- SO g soil and 50 cm' aqueous solution of the test substance (ratio l/l); 10 g soil and 50 cm' aqueous solution of the test substance (ratio 1/5); - 2 g soil and 50 cm' aqueous solution of the test substance (ratio 1/25). 47. The minimum amount of soil on which tile experiment can be carried out depends on the laboratory facilities and the performance of analytical method used. However, it is recommended to use at least 1 g, and preferably 2 g, in order to obtain reliable results from the test. 48. One control sample with only the test substance in 0.01 M CaC1, solution (no soil) is subjected to precisely the same steps as the test systems, in order to check the stability of the +est substance in CaC4 solution and its possible adsorption on the surfaces of the test vessels. ' 49. A blank run per soil with the same amount of soil and total volume of SO cm' 0.01 M CaC1, solution (without test substance) is subjected to the same test procedure. This serves as a background control during the analysis to detect interfering compounds or contaminated soils. 50. All the experiments, including controls and blanks, should be performed at least in duplicate. The total number of the samples which should be prepared for the study can be calculated with respect to the methodology which will be followed (paragraphs 57-58). 51. Methods for the preliminary study and the main study are generally the same, exceptions are mentioned where relevant. 9145 3M Environmental Laboratory Page 97 of 703 BACK TO MAIN 106 OECD/OCDE 52. The air-dried soil samples are equilibrated by shaking with a minimum volume of 45 cm' of 0.01M CaC1, overnight (12 h) before the day of the experiment. Afterwards, a certain volume of the stock solution t of the test substance is added in order to adjust the final volume to 50 cm'. This volume of the stock solution added: (a) should not exceed 10% of the final 50 cm' volume of the aqueous phase in order to change as little as possible the nature of the pre-equilibration solution; and @) should preferably result in an initial concentration of the test substance being in contact with the soil (CJ at least two orders of magnitude higher than the detection l i s t of the analytical method; this threshold safegudrds the ability to perform accurate measurements even when strong adsorption occurs (> 90%) and to determine later the adsorption isotherms. It is also recommended, if possible, that the initial substance concentration (CJ not exceed half of its solubility limit. 53. An example of how to calculate the concentration of the stock solution (CJ is given below. A detection limit of 0.01 pg cmJ and 90% adsorption are assumed; thus, the initial concentration of the test substance in contact with the soil should preferably be 1 pg cm" (two orders of magnitude higher than the detection limit). Suppbing that the maximum recommended volume of the stock solution is added, i.e. 5 to 45 cm' 0.01 M CaCl, equilibration solution (= 10% of the stock solution to 50 cm' total volume of aqueous phase), the concentration of the stock solution should be 10 pg cm"; this is three orders of magnitude higher than the detection limit of the analytical method. 54. The pH of the aqueous phase should be measured before and after contact with the soil since it plays an important role in the whole adsorption process, especially for ionisable substances. 55. The mixture is shaken until adsorption equilibrium is reached. The equilibrium time in soils is highly variable, depending on the chemical and the soil; a period of 24 h is generally sufficient (77). In the preliminary study, samples may be collected sequentially over a 48 h period of mixing (for example at 4,8, 24,48h). However, times of analysis should be considered with flexibilitywith respect to the work schedule of the laboratory. 56. There are two options for the analysis of the test substance in the aqueous solution: (a) the parallel method and (b) the serial method. It should be stressed that, although the parallel method is experimentally more tedious, the mathematical treatment of the results is simpler (Annex 6). However, the choice of the methodology to be followed, is left to the experimenter who will need to consider the available laboratory facilities and resources. 57. fa) Parallel method Samples with the same soUsolution ratio are prepared, as many as the time intervals at which it is desired to study the adsorption kinetics. After centrifugation and if so wished ' filtration, the aqueous phase of the first tube is recovered as completelyas possible and is measured after, for example, 4 h, that of the second tube after 8 h, that of the third after 24 h, etc. 58. QJ)Serial method: Only a duplicate sample is prepared for each soil/solution ratio. At defined time intervals the mixture is centrifuged to separate the phases. A small aliquot of the aqueous phase is immediately analysed for the test substance; then the experiment continues with the original mixture. If filtration is applied after centrifugation, the laboratory should have facilities to handle filtration of small aqueous aliquots. It is recommended that the total volume of the aliquots taken not exceed 1% of the total volume of the solution, in order not to change significantly the soil/solution ratio and to decrease the mass of solute available for adsorption during the test. 59. The percentage adsorption A , is calculated at each time point (t,) on the basis of the nominal initial concentration and the measured concentration at the sampling time((), corrected for the value of the blank. Plots of the Ati versus time (Fig. 1, Annex 6) are generated in order to estimate the achievement of 10/45 3M Environmental Laboratory Page 98 of 703 BACK TO MAIN OECD/OCDE 106 equilibrium plateau'. The K, value at equilibrium is also calculated. Based on this K, value, appropriate E soil/solution ratios are selected from Fig.1, so that the percentage adsorption reaches above 20% and i preferably >50% (61). All the applicable equations and principles of plotting are given in the Data and Reporting section and in Annex 6. Determination of adsorption equilibration time and of the amount of test substance adsorbed at equilibrium 60. As already mentioned in paragraph 59, plots of At, or C z t versus time permit estimation of the achievement of the adsorption equilibrium and the amount of test substance adsorbed at equilibrium. Figs. 1 and 2 in Annex 6 show examples of such plots. Equilibration time is the time the system needs to reach a plateau. 6 1. If, with a particular soil, no plateau but a steady increase is found, this may be due to complicating factors such as biodegradation or slow diffusion. Biodegradation can be shown by repeating the experiment with a sterilised sample of the soil. Ifno plateau is achieved even in this case, the experimenter should search for other phenomena that could be involved in his specific studies; this could be done with appropriate modifications of the experiment conditions (temperature,.shaking times, soil/solution ratios). It is left to the experimenter to decide whether to continue the test procedure in spite of a possible failure to achieve an equilibrium. Adsorption on the surface of the test vessel and stability of the test substance 62. Some information on the adsorption of the test substance on the surface of test vessels, as well as its stability, can be derived by analysing the control samples. If a depletion more than the standard error of the analytical method is observed, abiotic degradation andor adsorption on the surface of the test vessel could be involved. Distinction between these two phenomena could be achieved by thoroughly washing the walls of the vessel with a known volume of an appropriate solvent and subjecting the wash solution to analysis for the test substance. If no adsorption on the surface of the test vessels is observed, the depletion demonstrates abiotic unstability of the test substance. If adsorption is found, changing the material of the test vessels is necessary. However, data on the adsorption on the surface of the test vessels gained from this experiment cannot be directly extrapolated to soillsolution experiment. The presence of soil will generally reduce this adsorption. 63. Additional information on the stability of the test substance can be derived by determination of the parental mass balance over time. This means that the aqueous phase and extracts of the soil and test vessel walls are analysed for the test substance. The difference between the mass ofthe test chemical added and the sum of the test chemical masses in the aqueous phase and extracts of the soil and test-vessel walls is equal to the mass degraded and/or volatilized and/or not extracted. In order to perform a mass balance determination, the adsorption equilibrium should have been reached within the time period of the experiment. 64. The mass balance is carried out on both soils and for one soil/solution ratio per soil that gives a depletion above 20% and preferably >50% at equilibrium. When the ratio-finding experiment is completed with the analysis of the last sample of the aqueous phase after 48 h, the phases are separated by centrifugation and, if so wished, filtration. The aqueous phase is recovered as much as possible, and a suitable extraction solvent (extraction coefficient of at least 95%) is added to the soil to extract the test substance. At least two successive extractionsare recommended. The amount of test substance in the soil and test vessel extracts is determined and the mass balance is calculated (equation 10, Data and Reporting section). If it is less than Plots of the concentration of the test substance in the aqueous phase ( C$ ) versus time could also be used to estimate the achievement of the equilibriumplateau (see Fig. 2 in Annex 6). 11/45 3M Environmental Laboratory Page 99 of 703 BACK TO MAIN 106 OECD/OCDE 90%, the test substance is considered to be unstable in the time scale of the test. However, studies could still be continued, taking into account the unstability of the test substance; in this case it is recommended to i analyse both phases in the main study. Tier 2 - Adsorption kinetics at one concentration of the test substance - 65. Five soils are used, selected using the guidance given in TCble 1. There is an advantage to including some or all of the soils used in the preliminary study, if appropriate, among these five soils. In this case, Tier 2 has not to be repeated for the soils used in preliminary study. 66. The equilibration time, the soilkohtion ratio, the weight of the soil sample, the volume of the aqueous phase in contact with the soil and the concentration of the test substance in the solution are chosen based on the preliminary study results. Analysis should preferably be done approximately after 2, 4, 6, 8 (possibly also IO) and 24 h contact time; the agitation time may be extended to a maximum of 48 h in case a chemical requires longer equilibration time with respect to ratio-finding results. However, times of analysis could be considered with flexibility. 67. Each experiment (one soil and one solution) is done at least in duplicate to allow estimation of the variance of the results. In every experiment one blank. is run. It consists of the soil and 0.01 M CaCI, solution, without test substance, and of weight and volume, respectively, identical to those of the experiment. A control sample with only the test substance in 0.01 M CaCJ solution (without soil) is subjected to the same test procedure, serving to safeguard against the unexpected. The test runs as described in paragraph 52-59. 68. The percentage adsorption is calculated at each time point At,and/or time interval AAt, (according to the needs of the study) and is plotted versus time. The distribution coefficient K, at equilibrium, as well as the organic carbon normalized adsorption coefficient Knc(for non-polar organic chemicals), are also calculated. Results and discussion of the adsomtion kinetics test 69. The linear K, value is generally accurate to describe sorptive behaviour in soil (35)(78) and represents an expression of inherent mobility of chemicals in soil. For example, in general chemicals with K,, 5 1 cin' g" are considered to be qualitatively mobile. Similarly, a mobility classification scheme based on K, values has been developed by McCall et al. (16). Additionally, leaching classification schemes exist based on a relationship between K, and DT-50' (32)(79). 70. Also, according to error analysis studies (61), K, values below 0.3 cm' g ' cannot be estimated accurately from a decrease in concentration in the aqueous phase, even when the mosrfavourable (from point of view of accurancy) soiYsolution ratio is applied, Le. 1:l. In this case analysis of both phases, soil and solution, is recommended. 71. With respect to the above remarks, it is recommended that the study of the adsorptive behaviour of a chemical in soil and its potential mobility be continued by determining Freundlich adsorption isotherms for these systems, for which an accurate determination of K,, is possible with the experimental protocol followed in this Guideline. Accurate determination is possible if the value which results by multiplying the K,,with the soiVsolution ratio is > 0.3, when measurements are based on concentration decreasein the aqueous phase (indirect method), or > 0.1, when both phases are analysed (direct method) (61). Tier 3 - Adsorption isotherms and desorption kineticsldesoration isotherms 'DT-50:degradation time for 50% of the test substance. 12/45 3M Environmental Laboratory Page 100 of 703 BACK TO MAIN OECD/OCDE 106 i. Adsorption isotherms t 72. Five test substance concentrations are used, covering preferably two orders of magnitude; in the choice of these concentrations the water solubility and the resulting aqueous equilibrium concentrations should be taken intq account. The same soil/solution ratio per soil should be kept along the study. The adsorption test is performed as described in paragraphs 47-58, with the only difference that the aqueous phase is analysed only once at the time necessary to reach equilibrium as determined before in Tier 2. The equilibrium concentrations in the solution are determined and the amount adsorbed is calculated from the depletion of the test substance in the solution or with the direct method. The adsorbed mass per unit mass of soil is plotted as a function of the equilibrium concenkation of the test substance (see Data and Reporting). Results from the adsorption isotherms experiment 73. Among the mathematical adsorption models proposed so far, the Freundlich isotherm is the one most frequently used to describe adsorption processes. More detailed information on the interpretation and importance of adsorption models is provided in the references (41)(45)(80)(81)(82). - Note: It should be mentioned that a comparison of K,. (Freundlich adsorption coefficient) values for different substances is only possible if these K , values are expressed in the same units (83). Desorption kinetics 74. The purpose of this experiment is to investigate whether a chemical is reversibly or irreversibly adsorbed on a soil. This information is important, since the desorptionprocess also plays an important role in the behaviour of a chemical in field soil. Moreover, desorption data are usehl inputs in the computer modelling of leaching and dissolved run-off simulation. If a desorption study is desired, it is recommended that the study described below be carried out on each system for which an accurate determination of K, in the preceding adsorption kinetics experiment was possible. 75. Likewise with the adsorption kinetics study, there are two options to proceed with the desorption kinetics experiment: (a) the parallel method and (b) the serial method. The choice of the methodology to be followed, is left to the experimenter who will need to consider the available laboratory facilities and resourses, keeping in mind the remarks made in paragraph 56. 76. {a) Parallel method: For each soil which is chosen to proceed with the desorption study, samples with the same soWsolution ratio are prepared, as many as the time intervals at which it is desired to study the desorption kinetics. Preferably, the same time intervals as in the adsorption kinetics experiment should be used; however, the total time may be extended as appropriate in order the systzm to reach desorption equilibrium. In every experiment (one soil, one solution) one blank is run. It consists of the soil and 0.01 M CaCl, solution, without test substance, and of weight and volume, respectively, identical to those of the experiment. As a control sample the test substance in 0.01 M CaCl, solution (without soil) is subjected to the same test procedure. All the mixtures of the soil with the solution is agitating until to reach adsorption equilibrium (as determined before in Tier 2). Then, the phases are separated by centrifugation and the aqueous phases are removed as much as possible. The volume of solution removed is replaced by an equal volume of 0.01 M CaC1, without test substance and the new mixtures are agitated again. The aqueous phase of the first tube is recovered as completely as possible and is measured after, for example, 2 h, that of the second tube after 4 h, that of the third after 6 h, etc until the desorption equilibrium is reached. 77. [bl Serial method: After the adsorption kinetics experiment, the mixture is centrifuged and the aqueous phase is removed as much as possible. The volume of solution removed is replaced by an equal volume of 0.01 M CaCI, without test substance. The new mixture is agitated until the desorption equilibrium 13/45 3M Environmental Laboratory Page 101 of 703 BACK TO MAIN 106 OECD/OCDE is reached. During this time period, at defmed time intervals, the mixture is centrifuged to separate the phases. A small aliquot of the aqueous phase is immediately analysed for the test substance; then, the i experiment continues with the original mixture. The volume of each individual aliquot should be less than 1% of the total volume. The same quantity of fresh 0.01 M CaCl, solution is added to the mixture to maintain the soil to solution ratio, and the agitation continues until the next time interval. 78. The percehage desorption is calculated at each time poinf D t j andor time interval DAt, (according to the needs of the study) and is plotted versus time. The desorption coefficient of K, at equilibrium is also calculated. All applicable equations are given in Data and Reporting Section and Annex 6. Results from desomtion kinetics exueriment 79. Common plqts of the percentage desorption Dtjand adsorption A , versus time, allow estimation of the reversibility of the adsorption process. If the desorption equilibrium is attained even within twice the time of the adsorption equilibrium, and the total desorption is more than 75% of the amount adsorbed ,the adsorption is considered to be reversible. Desorption isotherms 80. Freundlich desorption isotherms are determined on the soils.used in the adsorption isotherms experiment. The desorption test is performed as described in the section "Desorption kinetics" (paragraph 76 or 77), with the only difference that the aqueous phase is analysed only once, at desorption equilibrium. The amount of the test substance desorbed is calculated. The content of test substance remaining adsorbed on soil at desorption equilibrium is plotted as a function of the equilibrium concentration of the test substance in solution (see Data and Reporting and Annex 6). DATA AND REPORTING 81. The analytical data are presented in tabular form (see Annex 7). Individual measurements and averages calculated are given. Graphical representations of adsorption isotherms are provided. The calculations are made as described in paragraphs 83-86. 82. For the purpose of the test, it is considered that the weight of 1 cm'of aqueous solution is lg. The soillsolution ratio may be expressed in units of w/w or who1 with the same figure. Adsorotion - 83. The adsorption Atj is defined as the percentage of substance adsorbed on the soil related to the quantity present at the beginning of the test, under the test conditions. If the test substance is stable and does not adsorb significantly to the container wall, Ati is calculated at each time point ti, according to the equation: m:d`(ti) ' 100 (3) At, = mo ("A) where: A, = adsorption percentage at the time point (%); , m:"' (ti) "0 = mass of test substance adsorbed on the soil at the time ti (pg); = mass of test substance in the test tube, at the beginning of the test (pg). 14/45 3M Environmental Laboratory Page 102 of 703 BACK TO MAIN OECD/OCDE 186 Detailed information how to calculatethe percentage of adsorption A, for the parallel and serial methods is 4 t given in Annex 6. 84. The distribution coefficient K,, is the ratio between the content of the substance in the soil phase and the mass concentration of the substance in the aqueous solution, under the test conditions, when adsorption equilibrium is reached. where: C ; ~ J(eq) cz(eq) my m;: (eq) m.au V" = content of the substanceadsorbed on the soil at adsorption equilibrium(pg g-I); -= mass concentration of the substance in the aqueous phase at adsorption equilibrium (pgcm"); this concentration is analytically determined taking into account the values given by the blanks. = mass of the test substanceadsorbed on the soil at adsorption equilibrium(pg); = mass of the test substancein the-solutionat adsorptionequilibrium(pg); = quantity of the soil phase, expressed in dry mass of soil (g); = initial volume of the aqueous phase in contact with the soil (cm'). 85. The relation between 4,and K, is given by: - Kd = A,, 100 A,, vo (cm' g') mWi, .where: Act! = percentage of adsorption at adsorption equilibrium, %. 86. The organic carbon normalized adsomtion coefficient K, relates the distribution coefficient K, to the content of organic carbon of the soil sample: where: %oc = percentage of organic carbon in the soil sample (g g ' ) . K, coefficient represents a single value which characterizes the partitioning mainly of non-polar organic chemicals between the organic carbon in the soil or sediment and water. The adsorption of these compounds is correlated with the organic content of the sorbing solid (7); thus, K, values depend on the specific characteristics of the humic fractions which differ considerably in sorption capacity, due to differences in origin, genesis, etc. Adsorption isotherms 87. The Freundlich adsomtion isotherms equation relates the amount of the test Substance adsorbed to the concentrationof the test substancein solutionat equilibrium (equation 8). The data are treated as under "Adsorption"and, for each test tube, the content of the test substance adsorbed on the soil after the adsorption test (CtdS(eq) , elsewhere denoted as d m ) is calculated. It is assumed that equilibrium has been attained and that C y (eq) represents the equilibrium value: 15/45 3M Environmental Laboratory Page 103 of 703 106 OECD/OCDE BACK TO MAIN The Freundlich adsorption equation is shown in (8): c:*(es> = K? .C::(eq)l'" (pgg.') or in the linear form: logCzd'(eq) = l o g K T + l/n .logC::(eq) (9) where: KadS F n = Freudlich adsorption coefficient; its dimension is cm' g' only if lln = 1; in all other cases, the slope l/n is introduced in the dimension of K F (Fg I."" (cm')'" g.'); = regression constant; l/n generally ranges between 0.7-1.0, indicating that sorption data is frequently slightly nonlinear. Equations (8) and (9) are plotted and the values of K P and I/n are calculated by regression analysis using the equation 9. The correlation coefficient r2of the log equation is also calculated. An example of such plots is given in Fig.2. Fig. 2 Freundlich Adsorption Plot, normal and linearized Mass balance 88. The mass balance (MB) is defined as,the percentage of substance which can be analytically recovered after an adsorption test versus the nominal amount of substance at the beginning of the test. 89. The treatment of data will differ if the solvent is completely miscible with water. In the case of water-miscible solvent, the treatment of data described under "Desolption"may be applied to determine the amount of substance recovered by solvent extraction. If the solvent is less miscible with water, the determination of the amount recovered has to be made. 90. The mass balance MB for the adsorption is calculated as follows; it is assumed that the term (ma corresponds to the sum of the test chemical masses extracted from the soil and surface of the test vessel with an organic solvent: where: MB m.. CrJ = mass balance (%); = total mass of test substance extracted from the soil and walls of the test vessel in two steps (pg); = initial mass concentration of the test solution in contact with the soil (pg cm"); 16/45 3M Environmental Laboratory Page 104 of 703 BACK TO MAIN OECD/OCDE 106 Vre = volume of the supernatant recovered after the adsorption equilibrium (cml). i t Desorption 91. The desomtion is defined as the percentage of the test substance which is desorbed, related to the quantity of substancepreviously adsorbed,under the test conditions: ' where: Dti = desorptionpercentage at a time point ti (YO); m;y (ti = mass of the test substancedesorbed from soil at a time point ti,(pg); m;ds (eq) =, mass of the test substance adsorbed on soil at adsorption equilibrium(pg). Detailed information on how to calculatethe percentage of desorption Dtifor the parallel and serial methods is given in Annex 6. 92. The apuarent desorption coefficient (KdJ is, under the test conditions, the ratio between the content of the substance remaining in the soil phase and the mass concentration of the desorbed substance in the aqueous solution, when desorption equilibrium is reached: where: K, mg(eq VT = desorption coefficient (cm' g.'); = total mass of the test substance desorbed from soil at desorption kquilibrium (pg); = total volume of the aqueous phase in contact with the soil during the desorption kinetics test (cm'). Guidance for calculatingthe m:;(eq) is given in Annex 6 under the heading "Desorption". Remark If the adsorption test which was preceded, was performed with the parallel method the volume V, in the equation (12) is considered to be equal to V,. Desorption isotherms . 93. The Freundlich desomtion isotherms equation relates the content of the test substance remaining adsorbed on the soil to the concentrationof the test substance in solution at desorption equilibrium (equation 16). 94. For each test tube, the content of the substance remaining adsorbed on the soil at desorption equilibriumis calculated as follows: m:r(eq) is defined as: 17/45 3M Environmental Laboratory Page 105 of 703 BACK TO MAIN 106 OECD/OCDE where: = ~,d-(~d m$(eq> = = m,A, m: (eq) = content of the test substance remaining adsorbed on the soil at desorption equilibrium (Pg g'>; mass of substance determined analytically in the aqueous phase at desorption equilibrium (pg); mass of the test substance left over from the adsorption equilibrium due to incomplete volume replacement (pg); mass of the substance in the solution at adsorption equilibrium (pg); -= volume of the solution taken from the tube for the measurement of the test substance, v: at desorption equilibrium (cm'); VR - volume of the supernatant removed from the tube after the attainement of adsorption equilibrium and replaced by the same volume of a 0.01 M CaCI, solution (cm'); The Freundlich desorption equation is shown in (16): c,"l(e9> = K? . CZ(eq)''" (pg g') or in the linear form: l o g C r ( e q ) = I o g K P + I/n . logCtr(eq) where: K;= n c:;(~~) = Freundlich desorption coefficient; = regression constant; = mass concentration of the substance in the aqueous phase at desorption equilibrium (pg cm"). The equations (16) and (17) can be plotted and the value of K r and l/n are calculated by regression analysis using the equation 17. Remark If the Freundlich adsorption or desorption exponent l/n is equal to 1, the Freundlich adsorption or desorption binding constant ( K F a n d K 2 ) will be equal to the adsorption ordesorption equilibrium constants (K,and &J respectively, and plots of C, vs C, will be linear. If the exponents are not equal to 1, plots of C, vs C,q will be nonlinear and the adsorption and desorption constants will vary along the isotherms. TEST REPORT 95. The test report should include the following information: - Complete identification of the soil samples used including: - geographical reference of the site (latitude, longitude); - date of sampling; - use pattern (e.g. agricultural soil, forest, etc.); - depth of sampling; 18/45 3M Environmental Laboratory Page 106 of 703 BACK TO MAIN OECD/OCDE 106 sand/silt/clay content; pH values (in 0.01 M CaCl,); organic carbon content; organic matter content; nitrogen content; C y ratio; Cation Exchange Capacity (mmolkg); all information relating to the collectionand storage of soil samples; where appropriate, all relevant information for the interpretation of the adsorption - desorption of the test substance; reference of the methods used for the determination of each parameter. information on the test substanceas appropriate; temperature of the experiments; centiifugation conditions; analyticalprocedure used to analyse the test substance; justificationfor any use of solubilizingagent for the preparation of the stock solution of the test substance; explanationsof correctionsmade in the Calculations,if relevant; data according to the form sheet (Annex 7) and graphical presentations; all information and observationshelpful for the interpretation of the test results. LITERATURE 1. H. Kukowski and G. Briimmer, (1987), Investigations on the Adsorption and Desorption of Selected Chemicals in Soils. UBA Report 106 02 045, Part II. 2. 0. F k l e , G. Kuhnt and L. Vetter, (1987), Selection of Representative Soils in the EC-Territory. UBA Report 10602 045, Part I. 3. G. Kuhnt and H. Muntau, (Eds.) EURO-Soils: Identification, Collection, Treatment, Characterisation. Special Publication no. 1.94.60, Joint Research Centre. European Commission, ISPRA, December 1994. 4. OECD Test Guidelines Programme, Final Report of the OECD Workshop on Selection of Soils/Sediments,Belgirate, Italy, 18-20 January 1995(June 1995). - 5. US-Environment Protection Agency: Pesticide Assessment Guidelines, Subdivision N, Chemistry: Environmental Fate, Series 163-1, Leaching and AdsorptiodDesorption Studies, Addendum 6 on Data Reporting, 540/09-88-026, Date: 1/1988. 6. 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BBA (1990), Guidelines for the Official Testing of Plant Protection Products, Biological Research Centre for Agriculture and Forestry, Braunschweig, Germany. 12. Calvet R., (1989), "Evaluation of adsorption coefficients and the prediction of the mobilities of pesticides i 6 soils", in Methodological Aspects of the Study of-Pesticide Behavior in Soil (ed. p. Jamet), INRA,Paris, (Review). 13. R. Calvet, (1980), "Adsorption-Desorption Phenomena" in Interactions between herbicides and the soil. (R.J. Hance ed.), Academic Press, London, pp. 83-122. 14. Hasset J.J., and Banwart W.L., (1989), "The sorption of nonpolar organics by soils and sediments" in Reactions and Movement of Organic Chemicalsin Soils. Soil Science Society of America (S.S.S.A), Special Publication no. 22, pp 31-44. 15. van GenuchtG M. Th., Davidson J.M., and Wierenga P.J., (1974), "An evaluation of kinetic and equilibrium equations for the prediction of pesticide movement through porous media". Soil Sci. SOC.Am. 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Chu-Huang Wu, N.Buehring, Davinson J.M., and Santelmann, (1979, "Napropamide Adsorption, i desorptionand Movement in soils". Weed Science, 23,454457. t 48. Haues M.H.B., Stacey M., and Thompson J.M., (1968) "Adsorption of s-triazine herbicides by soil organic preparations" in Isotopes and Radiation in Soil Organic Studies, p.75, International. Atomic Energy Agency, Vienna. 49. Pionke H.B:, and Deangelis R.J., (1980), "Methods for distributing pesticide loss in field run-off between the solution and adsorbed phase", CREAMS, in A Field Scale Model for Chemicals, Runoff and Erosion from Agricultural Management Systems, Chapter 19, Vol. III: Supporting Documentantion,USDA Conservation Research report. 50. IS0 Standard Compendium Environment: Soil Quality - General aspects; chemical and physical methods of analysis; biological methods of analysis. First Edition (1994). 51. Scheffer F., 1lth edition. -and Schachtschabel P., Lehrbuch der Bodenkunde, F. Enke Verlag, Stuttgart (1982), 52. 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Proc., 34,353-354. 60. Grover R, and Hance R.J. (1970), "Effept of ratio of soil to water on adsorption of linuron and atrazine". Soil Sci., 109-138. 61. Boesten, J.J.T.1, (1990), "Influence of soilhiquid ratio on the experimental error of sorption coefficients in pesticiddsoil system". Pest. Sci., 30,3 1 4 1 . 62. Boesten, J.J.T.I. " Influence of soilkquid ratio on the experimental error ofsorption coefficients in relation to OECD guideline 106" Proceedings of 5th international workshop on environmental behaviour of pesticides and regulatory aspects, Brussels, 26-29 April 1994. a, 63. Bastide J., Cantier J.M., and Coste C., (1980), " Comportement de substancesherbicides dans le sol en fonction de leur structure chimique". Weed Res., 227-231. 64. Brown D.S., sediments". m, and Flagg E.W., (1981), "Empirical J. Environ. Qual., 382-386. prediction of organic pollutants sorption in natural 65. w, Chiou C.T., Porter P.E., and Schmedding D.W., (1983), "Partition equilibria of nonionic compounds between soil organic matter and water". Environ. Sci. Technol., 227-23 1. organic 66. w, Gerstl Z., and Mingelgrin U., (1984), "Sorption Environm. Sci. Health, 297-312. of organic substances by soils and sediments". J. 22/45 3M Environmental Laboratory Page 110 of 703 BACK TO MAIN OECD/OCDE 106 67. Vowles P.D., and Mantoura R.F.C., (1987), "Sediment-water partition coefficient and HPLC retention factors of aromatic hydrocarbons". Chemosphere,M,JJ 103-116. t 68. Lyman W.J., Reehl W.F., and RosenbIatt D.H., (1990), Handbook of Chemical Property Estimation Methods. Environmental Behaviour of Organic Compounds. American Chemical Society, Washington DC. 69. Keniga E.E:, and Goring, C.A.I., (1980), "Relationship between water solubility, soil sorption, octanol-water partitioning and concentration of chemicals in the biota" in Aquatic Toxicology (e& J.G. Eaton, et al.), pp. 78-1 15, ASTM STP 707, Philadelphia. 70. Chiou C.T., Peters L.J., and Freed V.H., (1979), "A physical concept of soil-water equilibria for nonionic organic compounds". Science, l&83 1-832. 71. Hassett J.J., Banwart W.I., Wood S.G., and Means J.C., (1981), "Sorption of /-Naphtol: implications concerning the limits of hydrophobic sorption". Soil Sci. SOCA. m. J., 45,3842. 72. m, Karickhoff SYW., (1981), "Semi-empirical estimation of sorption natural sediments and soils". Chemosphere, 833-846. of hydrophobic pollutants on 73. - m, Moreale A., van Blade1 R., (1981), "Adsorption de 13 herbicides solubilitC reactivitk. Revue de l'Agric., 319-322. et insecticides par le sol. Relation 74. M. Muller, W. 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Cohen S.Z., Creeger S.M., Carsel R.F., and Enfield C.G., (1984), "Potential pesticide contamination of groundwater from agricultural uses", in Treatment and Disposal of Pesticide Wastes, pp.297-325, ACS Symp. Ser., 259, American Chemical Society,Washington,DC. 80. Giles C.H., (1970), "Interpretation and use of sorption isotherms" in Sorption and Transport Processes in Soils. S.C.I. Monograph No. 37, 14-32. * 81. Giles C.H., McEwan J.H., Nakhwa S.N., and Smith D., (1960), "Studies in adsorption: XI. A system of classification of solution adsorption isotherms and its use in the diagnosis of adsorption mechanisms and in measurements of pesticides surface areas of soils". J. Chem. SOC.3, 973-93. 82. Calvet R., Terc6 M., and Arvien J.C., (1980), "Adsorption des pesticides par les sols et leurs constituants: 3. CaractCristiques gtnCrales de l'adsorption". Ann. Agron., 31,239-25 1. 83. Bedbur E., (1996), "Anomalies in the Freundlich equation", Proc. COST 66 Workshop, Pesticides in soil and the environment, 13-15 May 1996, Stratford-upon-Avon, U.K. 84. Guth, J.A., (1989, "Adsorptioddesorption", in Joint International Symposium, Physicochemical Properties and their Role in Environmental Hazard Assessment, July 1-3, Canterbury, UK. 85. Soil Texture Classification (US and FA0 systems): Weed Science, 3,Suppl. 1 (1985) and Soil Sci. SOCA. mer. Proc., 26,305 (1962). 23/45 3M Environmental Laboratory Page 111 of 703 BACK TO MAIN 106 OECD/OCDE ANNEX 1 TESTING SCHEME - I,.Set up,ofa'suitable analytical method I + Available? @ 8*No hrther test [2] 4 .( W CI vessel surface Check of the stability by means of parental mass balance Equilibrium plateau is achieved? +@1 5 soils. I t / If mass balance < 90 %, test substance is unstable in the time scale of the test. The test can continue by analysing both phases if: Kd*(mm)V,>) 0.3 (indirect method: measurement of solutio K,*(m,/v,J > 0.1 (direct method measurement ofboth phases) m 1 as appropriate F,V D e s o r p t i 1 on kinetics. - - I 24/45 3M Environmental Laboratory Page 112 of 703 BACK TO MAIN OECD/OCDE 106 1 Svmbol A I m?(t,) m: (4 m, C CO c$(ti> c:d"es) C$ (e4 "0 V. A 11 K . K, K" Kiidr F I 1In Dt: %t$ , K, ANNEX 2 DEFINITIONS AND UNITS I Definition Units I adsorption percentage at the time point t, % 1 I I adsomtion uercentaw at adsomtion eauilibrium mass of the test substance adsorbed on the soil at the time t, % I mass of the test substance adsorbed on the soil during the time interval At mass of the substance adsorbed on the soil at adsorption emilihrium mass of the test substance in the test tube, at the beginning of the adsomtion test (rg1 mass of the substance measured in-an aliquot ( v,-" ) at the time point t, mass of the substance in the solution at adsorption equilibrium quantityof the soil phase,expressedin dry mass of soil mass concentrationof the stocksolutionof the substance initial mass concentration of the test solution in contact with the soil mass concentration of the substancein the aqueousphase at the time 6 that the analysis is performed content of the test substance adsorbed on soil at adsorption equilibrium an equilibrium mass concentration of the substance in the aqueous phase at adsorption equilibrium . initial volume of the aqueous phase in contact with the soil during the adsorption test volume of the aliquot in which the test substance is measured g pg cm" pg cm'] pg cm" Pg g.' pg cm" cm' cm' I distributioncoefficientfor adsomtion cm' i ` U organic carbon normalized adsorption coefficient organic matter normalized distribution coefficient Freundlich adsorption coefficient Freundlich exponent desorption percentage at a point time t, desorptionpercentage correspondingto a time interval At, apparent desorption coefficient %, LIE4 cm' g.' 25/45 3M Environmental Laboratory Page I 1 3 of 703 BACK TO MAIN 106 OECD/OCDE 1 t Symbol der I Definition 1 Freundlich desorption coefficient m z(ti) mass of the test substance desorbed from soil at the time t, m z (At i1 mF(eq) mf (eq mass of the test substance desorbed from soil during the time At mass of substance determined analytically in the aqueous phase I at desomtion equilibrium total mass of test substance desorbed at desorption equilibrium m,d- (At i ) mass of the substance remaining adsorbed on the soil after the time interval At, mass of the test substance left over from the adsorption equilibrium due to incomplete volume replacement content of the test substance remaining adsorbed on the soil at desomtion equilibrium c: (4 mass concentration of the substance in the aqueous phase at desorption equilibrium total volume of the aqueous phase in contact with the soil VT during the desorption kinetics experiment performed with the serial method volume of the supematant removed from the tube after the &+----- attainement of adsorption equilibrium and replaced by the same volume of a 0.01 M CaCl solution volume of the aliquot sampled for analytical purpose from the tume (i), during the desorption kinetics experiment performed with the serial method volume of the solution taken from the tube (i) for the measurement of the test substance, in desorption kinetics experiment (parallel method) . volume of the solution taken from the tube for the measurement of the test substance, at desorption equilibrium MB mass balance I ms total mass of test substance extracted from the soil and walls of the test vessel in two steps v, volume of the supernatant recovered after the adsorption equilibrium p, octanovwater partition coefficient I PKa dissociation constant sw water solubility w I cm' cm' cm' cm' cm' % " 1 26/45 3M Environmental Laboratory Page 1 14 of 703 BACK TO MAIN OECD/OCDE 106 AMVEX 3 Influence of Accuracy of Analytical Method and Concentration Change on Accuracy of Adsorption Results From the foJlowing table (part of ref. 84) it becomes obvious that when the difference between the initial mass (m,= 1I O pg) and equilibrium concentration (m:t(eq)= 100 pg) of the test substance in the solution is very small, an error of 5 % in the measurement of equilibrium concentration results in an error of 5 0 % in the calculation of the mass of the substance adsorbed in soil (mr(eq))and of 52.4%in the calculation of the K,. Amount of soil Volume of solution ma1 = log vo = 100 cm' m$(eq) 'Cg(eq) R (!%I cm.7 mZd(seq)* (PP) c:"'(eq) R' *(!% S') K,* R' 1.oo 0.90 0.50 0.10 truevalue 10% 50% 90% 1 0.89 1 0.476 0.092 10.9% 52.4% 90.8% truevalue 60.0 0.01111 1% 6.00 5.95 5.75 5.50 true value 0.8% 4.0% 8.3% 12.00 11.78 10.95 1 10.00 I1 10.88 0.01% 1.8% 8.8% 16.7% m?(eq) m$(eq) C?(e) c$ (e@ R R' = mass of the test substancein the soil phase at equilibrium,pg; = mass of the test substancein the aqueousphase at equilibrium,pg; = content of the test substancein the soil phase at equilibrium,pg g.'; * = mass concentrationof the test substancein the aqueousphase at equilibrium,pg cm" = analytical error in the determination of the m.,d,s(eq) ; = calculated error due to the analytical error R. 27/45 3M Environmental Laboratory Page 115 of 703 BACK TO MAIN 106 OECD/OCDE AMYEX 4 $4 t Estimation techniques for K, 1. Estimation techniques permit prediction of K, based on correlations with, for example, p_ values (12,39,63-68), water solubility data (12, 19,21,39,68-73), or polarity data derived by application of HPLC on reversed phase' (7'4-76). As shown in Tables 1 and 2, is the K, o r X m that are calculated from these equations and then, indirectly,the K,fiom the equations: 2. The concept of these correlations is based on two assumptions: (1) It is the organic matter of the soil that mainly influences the adsorption of a substance; and (2) The interactions involved are mainly non- polar. As a result, these correlations: (1) are not, or are only to some extent, applicable to polar substances, and (2) are not applicablein cases where the organicmatter content of the soil is very small (12). In addition, although satisfactory correlationshave been found between Pmand adsorption (19), the same cannot be said for the relationship between water solubility and extent of adsorption (19, 21); so far the studies are very contradictory. 3. Some examples of correlations between the adsorption coefficient and the octanol-water partition coefficient,as well as water solubilityare given in Tables 1 and 2, respectively. Table 1. Examples of correlations between the adsorption distribution coefficient and the octanol-water partition coefficient; for further examples see refs. 12 and 68. Various pesticides log K,, = 4.4 + 0.72 log P_ Authors Bnggs(1981) (Ref. 39) Chiou et al. (1983) (Ref. 65) Gerstl and Mingelgnn (1984) (Ref. 66) Vowles and Mantoura (1987) (Ref. 67) Table 2. Examples of correlations between the adsorption distribution coefficient and water solubility; for further examples see refs. 68 and 69. "ompounds Various pesticides Aliphatic, aromatic chlorinated substances a-naphtol Cyclic, aliphatic aromatic substances Various compounds Correlations - log Km=3.8 0.561 log S, - K = (4.040 +/- 0.038) (0.557 +/- 0.012) log Sw - lOgK_ = 4.273 0.686 log Sw - logK = - 1.405 0.921 log S - 0.00953 (mp-25) - K, = 2.75 0.45 log S , Authors Gerstl and Mingdgdn (1984) (Ref. 66) Chiou et aI.(1979) (Ref. 70) Hasset et al. (1981) (Ref. 71) Karickhoff (1981) (Ref. 72) Moreale van Blade (1982) (Ref. 73) DraR OECD Test Guideline "Estimation of Adsorption Coefficient (Koc) on Soil and on Sewage Sludge using High Performance Liquid Chromatography (HPLC) " , July 1997. 28/45 3M Environmental Laboratory Page 116 of 703 BACK TO MAIN OECD/OCDE 106 ANNEX 5 Calculations for Defining the Centrifugation Conditions 1. The centrfigation time is given by the following formula, assuming spherical particles: For simplificationpurposes, all parameters are described in non-SI units (8, an), where: w= rpm = q= rp = 2P. := %= %-R, = -rotational speed (=2 TC rpm/60), rad s"; revolutions per minute; viscosity of solution, g s-'cm"; particle radius, cm; soil density, g cmJ; solution density, g cm"; distance from the centre of centrifuge rotor to top of solution in centrifuge tube, cm; distance from the centre of centrifuge rotor to bottom in centrifuge tube, cm; length of the soilholution mixture in the centrifuge tube, cm. In general practice, double the calculated times is used to ensure complete separation. 2. The equation (1) can be simplified further if we consider the Viscosity (q) and the density (p ) of the solution as equal to the viscosity and density of water at 25 "C; thus, q = 8.95 x IO-'g s.'cm.'qand p, = 1.O g cm". Then, the centrifugation time is given by the equation (2): 3. From the equation (2) it becomes apparent that two parameters are important in defining the Centrifugation condition, Le. time (t) and speed (rpm), in order to achieve separation of particles with a specific size (in our case 0.1 prn radius): (1) the density of the soil and (2) the length of the mixture in the centrifuge tube (k-R,)L,e. the distance which a soil particle covers from the top of the solution to the bottom of the tube; obviously, for a fixed volume the length of the mixture in the tube will depend on the square of the radius of the tube. 4. Fig. 1 presents variations in the centrifugation time (t) versus centrifugation speed (rpm) for different soil densities (p,) (Fig. la) and different lengths of the mixture in the centrifuge tubes (Fig. 2a). From Fig. l a the influence of the soil density appears obvious; for example, for a classical centrifugation of 3000 rpm the centrifugation time is approx. 240 min for 1.2 g cm' soil density, while it is only 50 min for 2.0 g cm'. Similarly, from Fig lb, for a classical centrifugation of 3000 rpm the centrifugation time is approx. 50 rnin for a length of the mixture of 10 cm and only 7 min for a length of 1 cm. However, it is important to find an optimal relation between centrifugation which requires the less length possible and easy handling for the experimenter in separating the phases after centrifugation. 29/45 3M Environmental Laboratory Page 117 of 703 BACK TO MAIN 106 OECD/OCDE 5. Moreover, when defining the experimental conditions for the separation of soiVsolution phases, it is important to consider the possible existence of a third "pseudo-phase", the colloids. These particles, with a i size less than 0.2 p,can have an important impact on the whole adsorption mechanism of a substance in a soil suspension. When centrifugation is pedormed as descrbided above, colloids remain in the aqueous phase and are subjected to analysis together with the aqueous phase. Thus, the information about their impact is lost. If the conducting laboratory has ultracentrifugation or ultrafiltration facilities, the adsorptioddesorption of a substance in sbil could be studied more in depth, including information on the adsorption of the substance on the colloids. In this case, an ultracentrifugation at 60,000 .rpm or an ultrafiltration with filter porosity of 100,000 Daltons should be applied in order to separate the three phases soil, colloids, solution. The test protocol described in the following paragraphs should be also be modified accordingly, in order all three phases to be subjected to substance analysis. h 1000 .z-3Y +a 100 ! .-0 E . I 5 M 10 + E U 1 1000 10000 Centrifugation speed (rpm) Fig. l a Variations of centrifugation time (t) versus centrifugation speed (rpm) for different soil densities (p). R, = 10 cm, & -R, = 10 cm, q = 8.95 x 10'g s"cm" and p,= 1.0 g cm" at 25C. 30145 3M Environmental Laboratory Page 118 of 703 t 1000 OECD/OCDE BACK TO MAIN 106 mo iooa ioaoo Centrifugation speed (rpm) Fig. l b Variations of centrifugation time (t) versus centrifugationspeed (rpm)for different lengths of the mixture in the centrifuge tube (Rb -Rt) = L; R, = 10cm, q = 8.95 x 10'g s"cm",p, = 1.0 g cm" at 25C and p, = 2.0 g cm". 3M Environmental Laboratory 3 1/45 Page 119 of 703 BACK TO MAIN 106 OECDIOCDE ANNEX 6 CALCULATION OF ADSORPTION A (YOa)nd DESORPTJON D(%) 1. The time scheme of the procedure is: rn to tl ----------------- Atn-, At, I I t2 fn-2 tn-I t" b Time t 2. For all the calculations it is assumed that the test substance is stable and does not adsorb significantlyto the container walk. ADSORPTION A(%> a) Parallel method 3. The percentage adsorption is calculated for each test tube (i) at each time point (tJ, according to the equation: Ati = m:ds(ti> . IO0 (%I (1)$ mo The terms of this equation may be calculated as follows: r n o = Co . V, (pg) rn:"'(ti>= mo - c : t ( t i > * VO (pg) where: A ti = adsorption percentage (YO)at the time point ti; rn:d'(t, ) = mass of test substance on soil at the time t, that the analysis is performed (pg); mo = Cc"c(tl)== v, = mass of test substance in the test tube, at the beginning of the test (pg); initial mass concentration of the test solution in contact with the soil (pg cm"); mass concentration of the substance in the aqueous phase at the time t that the analysis is performed (pg cm-'); this concentration is analytically determined taking into account the values given by the blanks. initial volume of the test solution in contact with the soil (cm'). - The values of the adsorption percentage Atior C$(t,) are plotted versus time and the time after which the sorption equilibrium is attained is determined. Examples of such plots are given in Fig. 1 and Fig. 2 respectively. Equations applicableto both direct and indirect methods . All the other equations are applicable only to indirect method. 32/45 3M Environmental Laboratory Page 120 of 703 OECD/OCDE BACK TO MAIN 10s Equilibration time ti (h) Fig. 1 Adsorption Equilibrium Plot 100 90 M J 0 5 10 15 20 25 30 35 40 45 50 Equilibration time ti (h) - Fig. 2 Mass concentration of the test substance in the aqueous phase (C-) versus time b) Serial method 4. The following equations take into account that the adsorption procedure is carried out by measurements of the test substance in small aliquots of the aqueous phase at specific time intervals. During each time interval the amount of the substance adsorbed on thesoil is calculaied as follows: - for the first time interval At, = t, - to 33/45 3M Environmental Laboratory Page 121 of 703 BACK TO MAIN 106 OECD/OCDE - for the second time interval A5 = 5 - t, - for the third time interval At, = f - $ - for the n" &e interval Atn= tn- t,, a The percentage of adsorption at each time interval,AAt,iis calculated using the followingequation: mF(Ati) = .loo (%) (8) m0 2mF while the percentage of adsorption (A'i ) at a time point is given by the equation: (j) (9) A = j=At, .loo (%) ti m I The values of the adsorption At, or (with respect to the needs of the study) are plotted versus time and the time after which the sorptionequilibrium is attained is determined. At the equilibrationtime t,: - the mass of the test substanceadsorbed on the soil is: - the mass of the test substance in the solution is: m:$(eq) = mo - xm:"(Ati) Ati=l - and the percentageof adsorption at equilibriumis: * Equations applicable to both direct and indirect methods. All the other equations are applicable only to indirect method. 34/45 3M Environmental Laboratory Page 122 of 703 BACK TO MAIN OECD/OCDE 106 m:ds ( e 4 i A,, =-. 100 (%) t m0 The parameters used above are defined as : mass of the substance adsorbed on the soil during the time intervals At,, At2,...,Atn respectively (pg); mass of the substance measured in an aliquot (.," ) at the time points t,, 5,...,tnrespectively (pg); mass of the substance adsorbed on the soil at adsorption equilibrium (pg); mass of the substance in the solution at adsorption equilibrium (pg); volume of the aliquot in which the test substance is measured (cm'); percentage of adsorption corresponding at a time interval At, ("/.I; percentage of adsorption at adsorption equilibrium (%). 5. The time 6 that the desorption kinetics experiment begins, is considered as the moment that the maximal: recovered volume of the test substance solution (after that the adsorption equilibrium is attained) is replaced by an equal volume of 0.01 M CaCI, solution. a) Parallel method 6. At a time point t, ,the mass of the test substance is measured in the aqueous phase taken from the tube i (V;' ), and the mass desorbed is calculated according to the equation: At desorption equilibrium t, = t, and therefore mf'(t ,) = mg(es). The mass of the test substance desorbed during a time interval (At,) is given by the equ'ation: i-l mtT(Ati) = m ~ ~ ( t i ) - ~ m ~ ( i ) j= I 7. The percentage of desorption is calculated: at a time point ti from the equation: and during a time interval (At3 from the equation: 35/45 3M Environmental Laboratory Page 123 of 703 BACK TO MAIN 106 OECD/OCDE m::(Ati) it. DAli = .loo mtdr(4 (%) where: D ti = desorption percentage at a time point t,(%); DAti = desorptionpercentage corresponding to a time interval A\(%); m: (ti) mty(Ati) mF(ti> m: = mass of the test substance desorbed at a time point ti (pg); = mass of the test substance desorbed during a time intervals Ati (pg); = mass of the test substance analytically measured at a time ti in a solution volume V;`, which is taken for the analysis (pg); = mais of the test substance left over from the adsorption equilibrium due to incomplete volume replacement (Fg); mt: (eq) = mass of the test substance in the solution at adsorption equilibrium (pg); v, = volume of the supematant removed from the tube after the attainement of adsorption equilibriumand replaced by the same volume of a 0.01 M CaCl, solution (cm'); V;` = volume of the solution taken from the tube (i) for the measurement of the test substance, in desorption kinetics experiment (cm'). The values of the desorption Dti or Dbt, (accordingto the needs of the study) are plotted versus time and the time after which the desorption equilibriumis attained is determined. b) Serial method: vt 8. The following equations take into account that the adsorption pkocedure, which was preceded, was carried out by measurementsof the test substance in small aliquots ( ) of the aqueous phase (serial method, paragraph 58). It is assumed that: a) the v o l b e of the supernatant removed from the tube after the adsorption kinetics experiment was replaced by the same volume of 0.01 M CaCl, solution (V, ) and b) the total volume of the aqueous phase in contact with the soil (V,) during the desorption kinetics experiment remains constant and is given by the.equation: 9. At a time aoint ;t the mass of the test substance is measured in a small aliquot ( v r ) and the mass desorbed is calculated, according to the equation: At desorption equilibrium ti= tcqand therefore rn; ( t i )= m;(eq) The percentage of desorption Dl, is calculated, from the following equation: 3 6/45 3M Environmental Laboratory Page 124 of 703 BACK TO MAIN OECD/OCDE 106 10. At a time interval ( A t . During each tim(interva1 the amount of the substance desorbed is calcdated as follows: - for the first time interval At, = t, - to m:y(At,)= m p ( t l ) . D - m t and m F ( t , ) = m:q(eq)-mt7(At,) (21). - (3 - for the second time interval At, =t, - t, mF(t,) =m:" ( e q ) - [ m t ~ ( A t , ) + m ~ ~ ( A t 2 ) ] - for the nIhtime interval Atn= tn- tWi and m F ( t , ) = m:ds(eq) - ~ m ~ ( A t i ) i=l.n#l Finally, the percentage of desorption at each time interval,DAti, is calculated using the following equation: while the percentage of desorption D,,at a time point tiis given by the equation: At. where the above used parameters are defined as : m:"'(At,), mF(At2) ,... ,msJ"(Att.) m::(At,), mz(At,) ,... ,m:T(Att.) md,"(t,), m?(t,) ,... ,md,"(tn) = mass of the substance remaining adsorbed on the soil after the time intervals Ati, At2,...,Atnrespectively (gg); = mass of the test substance desorbed during the time intervals At,, At2,..., Atmrespectively (pg); = mass of the substance measured in an aliquot (v,") at tilne points t,, t,,...,tn,respectively (pg); 37/45 3M Environmental Laboratory Page 125 of 703 106 i 1 BACK TO MAIN OECD/OCDE = total volume of the aqueous phase in contact with the soil during the desorption kinetics experiment performed with theserial method (cm'); = mass of the test substance left over from the adsorption equilibrium due to incomplete volume replacement (Fg); = volume of the supernatant removed from the tube after the attainement of adsorption equilibrium and replaced by the same volume of a 0.01 M CaCI, solution (cm'); = volume of the aliquot sampled for analytical purpose from the tube (i), during the desorption kinetics experiment performed with the serial method (cm'); v." 5 0.02.. v, (27) 38/45 3M Environmental Laboratory Page 126 of 703 BACK TO MAIN OECD/OCDE 106 ANNEX 7 ADSORPTION-DESORPTIONIN SOILS: DATA REPORTmG SHEETS Substance tested: - Soil tested Dry mass content ofthe soil (105"C, 12 h): ........................................................................................................................... % Temperature: ......................................................................................................................................................................... c Suitability ofihe analytical method Analytical conc. final sol. Principle of the analyticalmethodused Calibrationof the analyticalmethod ~~ ~ 3M Environmental Laboratory 3 9/45 Page 127 of 703 BACK TO MAIN 106 OECDlOCDE Substance tested 0 n Soiltested i Dry mass content of the soil (105"C, 12 h): ............................................................................. .............................................. Temperature: ..............................................................,............................................,................"C Analytical methodology followed Indirect Parallel Serial Direct 0 Adsorption test: test samples Adsorption coefficient 1 K, Means 3M Environmental Laboratory 40145 H Page 128 of 703 BACK TO MAIN OECDIOCDE 106 d Substance tested: i Soil tested Dry mass contentofthe soil (105"C, 12 h):........................................................................................................................... % Temperature: .......................................................................................................................... .."C Adsorption test: blanks and control Water amount in weighed soil ncentrahon in aqueous Remark: Add columns if necessary 3M Environmental Laboratory 41/45 Page 129 of 703 BACK TO MAIN 106 OECDIOCDE Substance tested Soil tested i < Dry mass content of the soil (I05"C, 12h): ........................................................................................................................... % Temperature: ................................................................................................................................................................. "c Mass balance I I Svmbol I units I 1 TubeNo. U Weighed soil I I I B Soil: drymass ms,, g Water volume in weighed soil V, ml (calculated) Vol. 0.01 M CaCt sol.70 equilibratesoil ml 1 Volume of stock solution I 1 I Total vol. of aq. phase in contactwith soil V, 1 Initial concentration Test solution co I cm' I I I I I cm' I I-pgcm.' Eauilibration time I I 1 ~ I I II I I I I n i : eCqounilci.brteiusmt sbulbasnt.kacqo.rrpehcatisoenaint caldusdoerdption c ( 4 pg cm" I Removed volume aq. phase 1 Added volume of solvent I1 Signal analyzer in solvent I s., 1 Conc. test substance in solvent I c, II( Mass subst. extracted from soil &vesselwalls I m., 1 Removed volume of solvent 1 Added volume of solvent I I 1 Signal analyzer solvent phase s., \ Conc. test subst. in solvent I c., Mass subst.extractedfrom soil & vessel walls m, Total mass test subst. extracted in two m, steps Mass balance MB I cm' ] I cm' I I var. I I I wgcm'' I ue I I cm' I I cm' I I uecmJ I Pg P!3 % I I I I I II 1- 7 I I I I I 1 I I I I I I I I I I I I I 1 I I 1 I 42/45 3M Environmental Laboratory Page 130 of 703 OECD/OCDE Substance tested: Soil tested: Dry mass content of the sol1 (105"C, 12 h): ............................... Temperature: ......................................................... Adsorption isotherms BACK TO MAIN 106 ............................... % ......................... ."C ! Regression analysis: value of K? : - value of Wn: regression coefficient?: 3M Environmental Laboratory 43/45 Page 131 of 703 BACK TO MAIN 106 OECD/OCDE Substance tested: Soil tested t Dry mass content ofthe soil (105"C, 12 h): ........................................................................................................................ % Temperature: ............................................................................................................................. "C Analytical methodology followed: Indirect 0Parallel 0Serial [I Desorption test Symbol Units Tube No. coming - from adsorption step Time interval Time interval Time interval Time interval Mass of substance adsorbed on soil at adsorption equilibrium Removed volume aq. phase, replaced by 0.01 M CaC1, phase in contact with soil Mass test subst. left over the adsorption equilibrium due to incomplete volume replacement Desorption kinetics '0.t '' '-'. Measured mass of substance desorbed from soil at time f Volume of solution taken from the tube (i) for the measurement of the test substance Mass of substance desorbed from soil at timet, (calculated) Mass of substance desorbed from soil during time interval At, (calculated) .L Desorption percentage . 3 :,. ; ..,.(. , Desorption at time T Desorption at time interval A\ ADDarent desomtion coefficient K, 'M:Parallel method SM: Sc al method .. - ...t:.' . .. . ' . . . . :J . ; , . . , . I . .. . .. * - " ..: . ';*- :_'. . . . . . . : " (:L, 44/45 3M Environmental Laboratory Page 132 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY i METHOD ANALYSIS OF POTASSIUM PERnUOROOCTANESULFONATE OR OTHER FLUOROCHEMICIANLWSASTE STREAM OR WATER EXTRACTUSSING HPLC-ELECTROSPRAYDIASS SPECTROMETRY Method Number: ETS-8455.0 Author: Mark L. Anderson, Mark E. Ellefson Approved By: Laboratory Manager Adoption Date: /(/fO/m Revision Date: /!!/d,/i c) Date Word 97 ETS-8- 155.0 Page 1 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-ElectrosprayMass Spectrometry 3M Environmental Laboratory Page 133 of 703 BACK TO MAIN 1.0 SCOPE AND APPLICATION t 1.1 Scope: This method describes the analysis of waste stream or water extracts using HPLC- electrospray/mass spectrometry. 1.2 Applicable Compounds: Fluorochemicals or other electrospray ionizable compounds. 1.3 Matrices: Tap water, ground water, wastewater and other aqueous solutions. 2.0 SUMMARY OF METHOD 2.1 This method describes the analysis of fluorochemicals or other electrospray ionizable compounds extracted from water, using HPLC-electrospray mass spectrometry (HPLCES/MS). The analysis is performed by the mass selection of a single ion characteristic of a particular compound, such as the perfluorooctanesulfonate(PFOS) anion, m/z = 499 or perfluorooctanoate (PFOA), m/z = 4 13. 3.0 DEFINITIONS 3.1 Atmospheric Pressure Ionization (MI): The Micromass Platform LCZ singlequadrupole system and other commercially available LCMS systems allow for various methods of ionization by utilizing a variety of 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 of 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 of a strong electrical field. 3.3 Mass Spectrometer (MS): The Platform LCZ and other commercially manufactured ES/MS systems are equipped with a single quadrupole mass selectivedetector. Ions are selectivelydiscriminated by mass to charge ratio ( d z ) and subsequently detected. 3.4 Conventional vs. Z-spray probe interface: The Micromass Platform LCZ system utilizes a "Z-spray" conformation. The spray emitted from the probe is orthogonal to the cone aperture. In the conventional conformation it is aimed directly at the cone aperture, after passing through a tortuous pathway in the counter electrode. Though the configuration is different, the methods of operation, cleaning, and maintenance are the same. However, Zspray components and conventional components are not compatible with one another, but only with similar systems (i.e., Z-spray components are compatible with some other Z-spray systems, etc.). Other commercially manufactured ES/MS systems may have similar features. 3.5 Mass Lynx Software: System software designed for the specific operation of Micromass LCZ Mass spectrometer. Currently MassLynx has Windows 95 and WindowsNT 4.0 versions. All versions are similar. For more details see the manual specific to the instrument (MassLynx NT User's Guide or Micromass Platform LCZ User's Guide). ETS-8-155.0 Page 2 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M EnvironmentalLaboratory Page 134 of 703 BACK TO MAIN 4.0 WARNINGSAND CAUTIONS t 4.1 Health and Safety Warnings: 4.1.1 Use caution with the voltage cables for the probe. When engaged, the probe employs a voltage of approximately 5000 Volts. 4.1.2 When handling samples or solvents wear appropriate protective clothing, gloves, and eyewear. 4.2 Cautions: 4.2.1 Operate solvent pumps below a backpressure of 400 bar (5800 psi). If the backpressure exceeds 400 bar, the HPl 100 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 of 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 the raw data as method deviations. 6.1.1 Micromass Platform LCZ Mass Spectrometer equipped with an electrospray ionization source. 6.1.2 I-IPl 100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler. 7.0 SUPPLIESAND 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 analyticalcolumn, such as a Betasil C18 column (5Ox2mm, 5 pm particle size) or equivalent. 7.1.3 Capped autovials or capped 15 mL centrihge tubes. ETS-8-155.0 Page 3 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrosprayhlass Spectrometry 3M Environmental Laboratory Page 135 of 703 BACK TO MAIN 8.0 REAGENTS AND STANDARDS ii 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent. 8.1.2 Milli-QTMwater (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 other vendor. 8.1.3 Ammonium acetate, reagent grade or equivalent. 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.1.3.2 2.0 mM ammonium acetate solution: Weigh approximately0.300 g ammonium acetate. Pour into a 2000 L volumetric flask, add the appropriate volume of Milli-Q water, mix until all solids are dissolved. Store at room temperature. 8.2 Calibration Standards 8.2.1 Typically two method blanks (Milli-Q water), two matrix blanks, and solvent standards are prepared during the sample extraction procedure. 9.0 SAMPLHEANDLING 9.1 Standards and sample extracts are stored in capped autovials or capped 15 mL centrifbge tubes until analysis. 9.2 If analysis will be delayed, standards and sample extracts may be refkigerated at approximately 4" C until analyses can be performed. 10.0 QUALITY CONTROL 10.1 Solvent Blanks, Method Blanks and Matrix Blanks 10.1.1 Solvent blanks, method blanks, and matrix blanks are prepared and analyzed with each sample set to determine contamination or carryover. 10.1.2 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Matrix spikes are prepared for each sample set and analyzed to determine the matrix effect on the recovery efficiency. 10.2.2 Matrix spike duplicates are prepared periodicallyto 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 duplicateconcentrationsshould fall in the mid-range of the initial calibration curve or should be prepared at 1.5-4 times the endogenous ETS-8-155.0 Page 4 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochernicalsin Waste Stream or Water Extracts Using HPLC-ElectrosprayMass Spectrometry 3M Environmental Laboratory Page 136 of 703 BACK TO MAIN concentration of the analyte. Spike concentrations should fall in the low-range of the initial calibration curve if extremely low levels are expected. 10.3 Continuing Calibration Verifications 10.3.1 Continuingcalibration verifications(CCV) are analyzedto veri@the continued accuracy of the calibration curve. 10.3.2 Analyze a mid-range calibration standard after every tenth sample, with a minimum of one per sample set. 10.4 Internal StandardSurrogate Standard 10.4.1 An internal standard (IS) may be used to quanti@the target analytes by establishing a relationship between the ratio of analyte response to IS response and a known concentration of the analyte of interest. The IS should be spiked at an amount that will fall within the mid-range of 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 to fill within the low to mid-range of the calibration curve. 11.0 CALIBRATION AND STANDARDIZATION 11.1 Analyze the standard curves prior to and following each set of extracts. The average of two standard curves may be plotted by linear regression (y = mx + b) weighted l/x, or quadratic fit (y = ax2+ bx + c) using MassLynx or other suitable software. The calibration curves should not be forced through zero. 11.2 If the calibration curve does not meet acceptance criteria perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze. 11.3 For purposes of accuracy when quantitating low levels of analyte, it may be necessary to use the low end of the calibration curve rather than the full range. Example: when attempting to quantitate approximately 10 ppb of analyte, generate a calibration curve consisting of the standards from 5 ppb to 100 ppb rather than the fir11 range of the curve (5 ppb to 1000ppb). This will reduce inaccuracy attributed to linear regression weighting of high concentration standards. 12.0 PROCEDURES 12.1 Acquisition Set up 12.1.1 Set up the sample list. 12.1.1.1 Assign a sample list filename using the first letter of the name of the instrument (T for Tucker), the year (00 for 2000), the month (04 for April), and the day (TO01012 for October 12,2000). 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. ETS-8-155.0 Page 5 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrosprayhlass Spectrometry 3M Environmental Laboratory Page 137 of 703 BACK TO MAIN 12.1.1.2 Assign a method (MS) file. E 12.1.1.3 Assign an HPLC program (Inlet file). t 12.1.1.4 Type in sample descriptions and vial position numbers. 12.1.2 To create a method, click on method in the Acquisition control panel then mass spectrometer headings and select SIR. Set ionization mode as appropriate and 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. 12.1.3 Typically the analytical batch run sequence begins and ends with a set of 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. 12.2 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. 12.2.2 Attach the proper analytical column in the column heater compartment. If using the switching valve, make sure that the tubing is run to the appropriate ports. 12.3 Using the Inlet Editor 12.1.1 Set-up the H P l l O O using the following conditions or at conditionsthe analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.1.1.1 Sample size = 10 pL injection 12.1.1.2 Flow rate = 300 pL/min. 12.1.1.3 Cycle time = 10.0 minutes 12.1.1.4 Mobile phase components: Solvent A: 2.0 mM Ammonium Acetate Solvent B: Methanol (MeOH) Solvent Gradient: Time (min.) 0.00 1 .oo 4.50 8.00 8.50 10.0 - Yo B 5.00 Yo 5.00 % 95.0 ?h 95.0 ?h 5.00 !h stop ETS-8-155.0 Page 6 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrosprayhlass Spectrometry 3M Environmental Laboratory Page 138 of 703 BACK TO MAIN 12.4 Instrument Set-up 12.4.1 Refer to the Platform LCZ User's Guide, the MassLynx NT User's Guide or ETS- 1 t 9-36, "Operation and Maintenance of the Micromass Platform LCZ Electrospray/Mass Spectrometer". 12.4.2 Check the solvent level in reservoirs and refill if necessary. 12.4.3 Check the tip of the stainless steel capillary at the end of the probe with an eyepiece. The tip should be flat with no jagged edges. If the tip is found to be unsatishctory, 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 &e desoivation heaters. 12.4.6 Open the Inlet Editor. 12.4.5.1 Set HPLC pump to "On". 12.4.5.2 Set the solvent flow to the desired flow rate. 12.4.5.3 Observe droplets coming out of the tip of the probe. A fine mist should be expelled with no nebulizing gas leaking around the tip of the probe. i Readjust the tip of the probe if no mist is observed. 12.4.5.4 Allow to equilibrate for at least 10 minutes. 12.4.6 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.4.6.1 Drying gas 250-425 literdhour 12.4.6.2 ESI nebulizing gas 10-15 literdhow 12.4.6.3 HPLC constant flow mode, flow rate 10 - 500 pUmin 12.4.6.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.4.6.5 Source Block temperature 150'. 12.4.6.6 Desolvation temperature 250". 12.4.7 Print the tune page with its parameters, the Inlet page, sample list, mass spec information, and all other applicable information and store it.in the study binder with copies taped into the instrument run logbook. 12.4.7.1 All copies must be initialed and dated. 12.4.8 Click on start button on the MassLynx toolbar. Ensure start and end sample numbers include all samples to be analyzed. 13.0 DATAANALYSA~NSD CALCULATIONS 13.1 Calculations: 13.1.1 Calculate matrix spike percent recoveries using the following equation: ETS-8-155.0 Page 7 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/MassSpectrometry 3M Environmental Laboratory Page 139 of 703 BACK TO MAIN % Recovery = Observed Result - Backmound Result x 100 Expected Result i i 13.1.2 Calculate percent difference using the following equation: % Difference = Expected Conc. - Calculated Conc. x 100 Expected Conc. 13.1.3 Calculate actual concentration of analyte in matrix (pg/mL): On-Column Concentration (pg/mL) x Dilution Factors = Calculated Concentration 14.0 METHODPERFORMANCE 14.1 The Limit of Quantitation (LOQ) is method, analyte, and matrix specific. For many analytes, the LOQ concentration is selected as the lowest acceptable non-zero standard in the calibration curve. 14.2 Solvent and method blank values must be < 'h that of the lowest standard used in the calibration curve. 14.3 The coefficient of determination (rz)value for the calibration curve must be greater than or I equal to 0.980. 14.4 Continuing Calibration Verification (CCV) percent recoveries must be k 30% of the standard concentration. 14.5 Internal Standard recoveries should be within k 50% of 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 performancecriteria have not been met, the data must be footnoted on tables and discussed in the text of 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 containerslocated in the laboratory. 16.0 RECORDS 16.1 Each 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 the tune page, sample list, and acquisition method fiom MassLynx and other applicable information to include in the appropriate study folder. Copy these pages and tape into the instrument runlog. 16.3 Plot the calibration curve then print these graphs and store in the study folder. ETS-8-155.0 Page 8 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicalsin Waste Stream or Water Extracts Using HF'LC-ElectrosprayMass Spectrometry 3M Environmental Laboratory Page 140 of 703 BACK TO MAIN 16.4 Print data integration summary, integration method, and chromatograms, fiom MassLynx, and store in the study folder. 16.5 Summarize data using suitable software and store in the study folder. 16.6 Back up electronic data to appropriatemedium. Record in study notebook the file name and location of backup electronic data. 17.0 ATTACHMENTS 17.1 None 18.0 REFERENCES 18.1 Platform LCZ User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ;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. 18.3 MassLynx NT Guide To Data Acquisition, MicromassUK Limited, Tudor Road, Altrincham, WA14 5RZ;or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.4 ETS-9-36.0, "Operation and Maintenance of the Micromass Platform LCZ Electrospray/Mass Sprectrometer". 19.0 AFFECTED DOCUMENTS 19.1 None 20.0 REVISIONS Revision Number. Reason For Revision Revision Date ETS-8-155.0 Page 9 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicalsin Waste Stream or Water Extracts Using HF'LC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 141 of 703 BACK TO MAIN 3M ENVIRONMENTALLABORATORY METHOD ANALYSIOSF POTASSIUPMERFLUOROOCTANESULFONAOTREOTHER FLUOROCHEMICAINLWS ATEREXTRACTUSSING HPLC-ELECTROSPRAY~S~PAESCSTROMETRYB~SAPESSCTROMETRY Method Number: ETS-8-110.0 Author: Kris Hansen, Lisa Clemen Approved By: Adoption Date: b9\O'dah Revision Date: Group Leader CLe Technical Reviewer c,-- 9/8/54 Date 9 (Eky Date 1.0 SCOPE AND APPLICATION 1.1 Scope: This method describes the analysis of water extracts for fluorochemicals using HPLC-electrospray/mass spectrometry/mass spectrometry. 1.2 Applicable Compounds: Fluorochemicals or other fluorinated compounds, or other ionizable compounds. 1.3 Matrices: Tap water, ground water, and wastewaters Word 6/95 ETS-8-110.0 Analysis of Water Extract Using HPLC-ES/MS/MS Page 1 o f 9 3M Environmental Laboratory Page 142 of 703 BACK TO MAIN 2.0 SUMMARY OF METHOD , 2.1 *; This method describes the analysis of fluorochemicals extracted from water, using HPLCelectrospray tandem mass spectrometry (HPLC-ESMSMS). The analysis is performed by following mass selection of a single ion characteristic of a particular fluorochemical, such as the perfluorooctanesulfonate (PFOS) anion, m / ~ 4=99 or perfluorooctanoate (POAA), m/z = 413; a compound specific product ion is created through high-energy collisions, and + + creation of the product ion is monitored quantitatively. For example, the transition from 499 80 (characteristic of SO3-) is monitored for PFOS and the 413 119 (characteristic of C2F5-) transition is monitored for POAA. This selectivity afforded by this technique reduces background interferences and enhances analytical sensitivity. . __ 3.0 DEFINITIONS 3.1 Atmospheric Pressure Ionization (API): The Micromass Quattro II triple quadrupole systems and other commerciallyavailable LCMS and LC/MS/MS systems allow for various methods of ionization by utilizing various sources, probes, and interfaces. These include but are not limited to: Electrospray Ionization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ionization process in these techniques occurs at atmospheric pressure (i.e., not under a vacuum). 3.2 Electrospray Ionization ( E S , ESI): a method of ionization performed at atmospheric -- pressure, whereby ions in solution are transferred to the gas phase via tiny charged droplets. __ --Thesecharged droplets are produced-by-tkeapplicatiorrof a strong electrical field. --- -- . - - -- 3.3 Mass Spectrometry, Mass Spectrometer ( M S ) , Tandem Mass Spectrometer( M S / M S ) : The API Quattro I1 triple quadrupole systems and other commerciallymanufactured ES/MS/MS systems that are equipped with quadrupole mass selective detectors. Ions are selectively discriminated by mass to charge ratio ( d z ) and subsequently detected. A single MS may be employed for ion detection or a series (MS/MS) for more specific fiagmentation information. 3.4 Conventional vs. 2-spray probe interface: The latest models of Micromass Quattro 11 triple quadrupole systems (post 1998) utilize a "Z-spray" conformation. The spray emitted from a probe is orthogonal to the cone aperture. In the conventional conformation it is aimed directly at the cone aperture, after passing through a tortuous pathway in the counter electrode. Though the configuration is different, the methods of operation, cleaning, and maintenance are the same. However, Z-spray components and conventional components are not compatible with one another, but only with similar systems (ie., Z-spray components are compatible with some other Z-spray systems, etc.). Other commercially manufactured ES/MS/MS systems may have similar features. 3.5 Mass Lynx Software: System s o h a r e designed for the specific operation of the Quattro I1 triple quadrupole systems. Currently MassLynx has Windows 95 and WindowsNT 4.0 versions. All versions are similar. For more details see the manual specific to the instrument (Micromass Quattro I1 triple quadrupole MassLynx or MassLynx PJT User's Guide). ETS-8- 110.0 Analysis of Water Extract Using HPLC-EShlSIMS 3M Environmental Laboratory Page 2 of 9 Page 143 of 703 BACK TO MAIN 4.0 WARNINGANSD CAUTIONS 4.1 Health and Safety Warnings: 4.1.1 Use caution with the voltage cables for the probe. When engaged, the probe t. employs a voltage of approximately 5000 Volts. 4.1.2 When handling samples or solvents wear appropriate protective gloves, eyewear, and clothing. 4.2 Cautions: 4.2.1 Operate solvent pumps below a back pressure of 400 bar (5800 psi). If the back pressure 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 of instrumentation that comes in contact with the sample or extract. I 6.0 EOUIPMENT 6.1 Equipment listed below may be modified in order to optimize the system. Document any modificat_io_ ns in the ra-w_d_at_a as method deviations. - ^ I _ _ ~ 6.1.1 Micromass Quattro I1 triple quadrupole Mass Spectrometer equipped with an electrospray ionization source 6.1.2 HPl 100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler 7.0 SUPPLIES AND MATERIALS 7.1 Supplies 7.1.1 7.1.2 - High purity grade nitrogen gas regulated to approximately 100psi (House air system) High purity grade argon regulated to approximately 6 psi. 7.1.3 HPLC analytical column, such as a Betasil C18 column (SOx2mm, 5 pm particle) 7.1.4 Capped autovials or capped 15 mL centrifuge tubes 8.0 REAGENTS AND STANDARDS 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent 8.1.2 Milli-QTMwater (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 other vendor ETS-8-110.0 Analysis of Water Extract Using ES/MS/MS 3M EnvironmentalLaboratory Page 3 of 9 Page 144 of 703 BACK TO MAIN 8.1.3 Ammonium acetate, reagent grade or equivalent 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.1.3.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g ammonium acetate. Pour into a 2000 L volumetric flask containing 2000 mL Milli-Q water, mix until all solids are dissolved. Store at room temperature. 8.2 Standards 8.2.1 Typically two method (Milli-Q water) blanks, two matrix (tap water) blanks, and eighteen solvent standards are prepared during the extraction procedure. 9.0 SAMPLHEANDLING 9.1 Standards and sample extracts are stored in capped autovials or capped 15mL centrifige tubes until analysis. 9.2 If analysis will be delayed, standards and sample extracts may be refrigerated at approximately 4"C, or at room temperature, until analysis can be performed. 1 10.0 QUALITY CONTROL 10.1 Solvent Blanks, Method Blanks and Matrix Blanks -- 7 U X I - S d v e n t l Z a r i E s , method E i E i X s d - m i t i i i sare prepared aiil ahalyiZd-wiii---- each batch to determine contamination or carryover. 10.1.2 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Matrix spikes are prepared for each sample and analyzed to determine the matrix effect on the recovery efficiency. - 10.2.2 Matrix spike duplicates are prepared periodically to measure the precision associated with the analysis. 10.2.3 Analyze a 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 fall in the mid-range of the initial calibration curve or should be prepared at 1.5-5 times the endogenous concentration of the analyte. Spike concentrations should fall in the low-range of the initial calibration curve, if extremely low-levels are expected 10.3 Continuing Calibration Verifications 10.3.1 Continuing calibration verifications are analyzed to verify the continued accuracy of the calibration curve. 10.3.2 Analyze a mid-range calibration standard after every tenth sample, with a minimum of one per batch. ETS-8-110.0 Analysis of Water Extract Using ES/MS/MS 3M Environmental Laboratory Page 4 of 9 Page 145 of 703 BACK TO MAIN 11.0 CALIBRATION AND STANDARDIZATION 11.1 Analyze the standards prior to and following each set of extracts. The average of two standard curves will be plotted by linear regression (y = my + b), weighted l/x, not forced t: through zero, using MassLynx or other suitable s o h a r e . 11.2 If the curve does not meet requirements perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze. 11.3 For purposes of accuracy when quantitating low levels of analyte, it may be necessary to use the low end of the calibration curve rather than the full range of the standard curve. Example: when attempting to quantitate approximately 10 ppb of analyte, generate a calibration curve consisting of the standards from 5 ppb to 100 ppb rather than the full range of the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting of high concentration standards. 12.0 PROCEDURES 12.1 Acquisition Set up 12.1.1 Set up the sample list. 12.1.1.1 Assign a sample list filename using MO-DAY-last two digits of year- increasing letter of the alphabet starting with A - 12.1.1.2 Assign a method ( M S )--f-i-le - -__------ -__ - - - - _.__- - 12.1.1.3 Assign an I@LC program (Inlet file) 12.1.1.4 Type in sample descriptions and vial position numbers 12.1.2 To create a method click on method in the Acquisition control panel then mass spectrometer headings and select SIR (Single Ion Recording) or MRM (Multiple Reaction Monitoring). Set Ionization Mode as appropriate and mass to 499 or other appropriate masses. A full scan is usually collected along with the SIRS. Save acquisition method. If MSMS instruments are employed, additional product ion fragmentation information may be collected. See Micromass MassLynx GUIDE TO DATA ACQUISITION for additional information and MRM. 12.1.3 Typically the-analytical batch run sequence begins and ends with a set of solvent standards. 12.1.4 Samples are analyzed with a continuing calibration check injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor possible analyte carryover and are not considered samples but may be included as such. 12.2 Using the Autosampler 12.2.1 Set up sample tray according to the sample list prepared in Section 12.1.1. 12.2.2 Set-up the HP1 lOO/autosampler at the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.2.2.1 Sample size = 10 pL injection 12.2.2.2 Inject/sample = 1 ETS-8-110.0 Analysis of Water Extract Using E S N S N S Page 5 of 9 3M Environmental Laboratory Page 146 of 703 BACK TO MAIN 12.2.2.3 Cycle time = 9.0 minutes 12.2.2.4 Solvent ramp = 4 Time MeOH 2.0 mM Ammonium acetate 0.00 min. 40% 60% 1.OO min. 40% 60% 4.50 min. 95% 5% 6.50 min. 95% 5% 7.00 min. 40% 60% 9.00 min. 40% 60?4 12.2.2.5 Press the "Start" button. 12.3 Instrument Set-up 12.3.1 Refer to ETS-9-24, "Operation and Maintenance of the Micromass Quattro I1 Triple Quadrupole Mass Spectrometer Fitted with an AtmosphericPressure Ionization Source," for more details. 12.3.2 Check the solvent level in reservoirs and refill if necessary. 12.3.3 Check the stainless steel capillary at the end of the probe. Use an eyepiece to check -- tuhnestaipt.isfTah~eotripy,s-h~oiusladsbseemfla~tew-tithhpnrooajbangeT-gfeid1Sedcgeetsh.eIsfttahienlteipssisXfeo1ucnadptiollabrey. - -- 12.3.4 Turn on the nitrogen 12.3.5 Open the tune page. Click on operate to initiate source block and desolvation heaters. 12.3.6 Open the Inlet Editor. 12.3.6.1 Set HPLC pump to "On". 12.3.6.2 Set the flow to 10 - 500 uWmin or as appropriate. 12.3.6.3 Observe droplets coming out of the tip of the probe. A fine m i s t should be expelled with no nitrogen leaking around the tip of the probe. Readjust the tip of the probe if no mist is observed. 12.3.6.4 Allow to equilibrate for approximately 10 minutes. 12.3.7 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.3.7.1 Drying gas 250-400 litershour 12.3.7.2 ESI nebulizing gas 10-15 litershour 12.3.7.3 HPLC constant flow mode, flow rate 10 - 500 pL/min 12.3.7.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.3.7.5 Source Block temperature 150" 12.3.7.6 Desolvation temperature 250" ETS-8-110.0 Analysis of Water Extract Using ES/I\.IS/MS Page 6 of 9 3M Environmental Laboratory Page 147 of 703 BACK TO MAIN 12.3.8 Print the tune page, with its parameters, and store it in the study binder with a COPY taped into the instrument log. 12.3.9 Using the cross-flow counter electrode in the ESMS source is recommended for a: the analysis of biological matrices. 12.3.10Click on start button in the Acquisition Control Panel (this may vary among MassLynx versions, see appropriate MassLynx USER'S GUIDE). Ensure start and end sample number includes all samples to be analyzed. 13.0 DATAANALYSIASND CALCULATIONS 13.1 Calculations: 13.1.4 Calculate matrix spike percent recoveries using the following equation: % Recovery = Observed Result - Backmound Result x 100 Expected Result 13.1.5 Calculate percent difference using the following equation: % Difference = Exuected Conc. - Calculated Conc. x 100 Expected Conc. 13.1.6 Calculate actual concentration of PFOS, or other fluorochemical, in matrix __ (C__l_d_m- L)-: - ~ I____ - - - ._. - __ [ng of PFOS calc. from std. Curve x 0.8 Dilution Factor) [Initial Volume of matrix (mL) + mL of Surrogate Standard) Final Volume (mL) x 1000 ng 14.0 METHODPERFORMANCE 14.1 Method Detection Limit (MDL) and Limit of Quantitation (LOQ) are method, analyte, and matrix specific. Please see applicable extraction method for a listing of current MDL and LOQ values. 14.2 Solvent Blanks, MetJhod Blanks, and Matrix Blanks 14.2.1 Solvent blanks, method blanks, and calibration blanks values must be below the lowest standard in the calibration curve 14.3 Calibration Curves 14.3.1 The i!value for the calibration curve must be 0.980 or better. 14.4 Matrix Spikes 14.4.1 Matrix spike percent recoveries must be within k 30% of the spiked concentration. 14.5 Continuing Calibration Verifications 14.5.1 Continuing calibration verification percent recoveries must be k 30% of the spiked concentration. ETS-8-110.0 Analysis of Water Extract Using ESMSIMS 3M Environmental Laboratory Page 7 of 9 Page 148 of 703 BACK TO MAIN 14.6 If criteria listed in this method performance section is 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 appropriate logbook. `. 14.7 If data are to be reported when performance criteria have not been met, the data must be footnoted on tables and discussed in the text of 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 RECORDS 16.1 Each 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 the tune page, sample list, and acquisition method from MassLynx to include in the appropriate study folder. Copy these pages and tape into the instrument runlog. 16.3 Plot the calibration curve by linear regression, weighted l/x, then print these graphs and store in the study folder. --______164- Printdataintegration summary,-htegratiormethod,mdchromatograms,from MassLyx, ----- -- and store in the study folder. 16.5 Summarize data using suitable software (Excel 7.0) and store in the study folder, 16.6 Back up electronic data to appropriate medium. Record in study notebook the file name and location of backup electronic data. 17.0 TABLESD,IAGRAMFS,LOWCHARATNSD, VALIDATIONDATA 17.1 None 18.0 REFERENCES 18.1 ETS-9-24.0,"Operation and Maintenance of the Micromass Atmospheric Pressure Ionizationbfass SpectrometerQuattro I1 Triple Quadrupole Systems" 19.0 AFFECTEDOCUMENTS None ETS-8-110.0 Analysis of Water Extract Using ESIMSIMS 3M Environmental Laboratory Page 8 of 9 Page 149 of 703 BACK TO MAIN 20.0 REVISIONS i Revision ' Number. Reason For Revision Revision - Date ETS-8-110.0 Analysis of Water Extract Using ES/MS/MS 3M EnvironmentalLaboratory Page 9 of 9 Page 150 of 703 BACK TO MAIN Appendix C: Sample Preparation Sheets This appendix includes log sheets from the sample preparation portion of the method. "Suitable Analytical" "Suitable Container" "Optimal Ratio" "Optimal RatioMass Balance" "Desorption Solvent" "Adsorption Kinetics" "Desorption Kinetics, Serial Method" "Adsorption Isotherms, Multiple Concentrations" "Desorption Isotherms, Multiple Concentrations" 3M Environmental Laboratory Page 151 of 703 Suitable Analytical ETS-8-159 Section 12.2 BACK TO MAIN Test Substance: PFOS i i 3M Environmental Laboratory Page 152 of 703 BACK TO MAIN Suitable Analytical 1 ETS-8-159 Section 12.2 Test Substance: PFOS I ' i I 1 E00-1311-0016 I E00-1311-0018 I E00-1311-0019 E00-1311-0020 I E00-1311-0022 E00-1311-0023 E00-1311-0025 II E00-1311-0027 E00-1311-0028 E00-1311-0029 II E00-1311-0031 E00-1311-0032 E00-1311-0033 E00-1311-0001 I E00-1311-0001 E00-1311-0001 I -00-1311-0002 I I E00-1311-0035 1 -00-1311-0002 E00-1311-0036 -00-131 1-0002 , -00-1311-0003 E00-1311-0038 I E00-1311-0041 I E00-1311-0042 E00-1311-0043 E00-1311-0044 E00-1311-0046 -00-1311-0003 I -00-1311-0003 1 100-1311-0004 1 I ZOO-1311-0004 I 100-1311-0004 I I -00-1311-0005 I -00-1311-0005 E00-1311-0005 ZOO-1311-0006 I 100-1311-0006 I EOO-1311-0006 I 1 - T I ! !I1 1 r'III 1 ,W lI l l Y 2 iv Y 1 X I I I It PI I I II PI I I II /rIIlII 1 1.11 I I I rIIIII V I I I II tIIIII I 5t=1 5t.1 5t=2 I1S T = l 5t=1 ST= 1 5t=1 5t.1 5t=1 IST=l 1 ST=l 5t=1 5t=2 5t=2 5t=2 5t=2 5t=2 5t=2 - d LPu x> 5t=3 3M Environmental Laboratory BACK TO MAIN 3M Environmental Laboratory Page 154 of 703 Suitable Container ETS-8-159 Section 12.3 BACK TO MAIN Test Substance: 3 2 3M Environmental Laboratory Page 155 of 703 Optimal Ratio ETS-8-159 Section 12.5 5 - BACK TO MAIN TFOS Test Substance Optimal Ratio ETS-8-158 Section 12.5 BACK TO MAIN Test Substance Optimal Ratio ETS-8-159 Section 12.5 BACK TO MAIN Test Substance Optimal Ratio BACK TO MAIN GLP Study Number: 3M Environmental Laboratory Page 159 of 703 Optimal Ratio BACK TO MAIN 3M Environmental Laboratory Page 160 of 703 Optimal Ratio ETS-8-156 Section 12.5 BACK TO MAIN If=s Test Substance GLP Study Number: E00-1311 3M Environmental Laboratory Page 161 of 703 BACK TO MAIN 3M Environmental Laboratory Page 162 of 703 Optimal RatidMass Balance ETS-8-159 Section 12.5 (ant.) BACK TO MAIN P F 0 . S Test Substance: GLP Study N u m b e r --'311 3M Environmental Laboratory Page 163 of 703 DesorDtion Solvent ETS-E-159 Section 12.4 BACK TO MAIN Test Substance GLP Study Number 3M Environmental Laboratory Page 164 of 703 TE ---------------------- BACK TO MAIN so, -_ =n aaincresEehmEineggLeLemseenre SmEmmast DDDnnn ooEzsREiEEmEReSoScSeaaAaEt UN TEETER ES Sim EaT a Tn eSEpS SEemEe mERm eEn, B . Ui e IIm NELa 44wm ee efioDom= m=mDmmm mEeEdboadaacr LoTLuITS miEmE eRSAdLasa | meromTeeitminepa3B aGILG oDNw eSeEl aaLaautcmee np3 Zerer mrme mlRmATlasleee. 3 PEs woCLVnan mooamalidlmmalgeasnce o| nonu zmoesaaameddssiunaeoddn 0 THERES Shs ee 0en 01tens HnE%iSfpl a1eDdr eetop esl gn o Ry nd Ct TSh oEamRt esRe 10%As nDiel Een i 1 | i FIm7 i t 50HN {51 & DO ail 4 SO BrW +i0RT 0 CT OT TTYiYMT WThr o|ls E fE EFT erestE B te elebT hee thtne TE YSR EEEE R e e e rae e teY dTefu0 N RE EHT E--)| f Pomo feo nree aet| o ST HErh e rE e o $Po [S om gm1 mannm Te m=[boiwe oeaaTlitee Toe[haE3SsEREeE nT H 1SI ne ssnf R SELo r poTeg AS1aH:la A2]T ee -- n C1a?5| {SemEEele en ge ty 3{MViemos lEoa ECEortsEfadEETETTGC fol ST4 5 13 fm domeemte teeea a R St EeEea T Rl RERC e Fig se -- EN-- -- t T I e pe a nn ne entAE rrsame F e Ge ) | 23p)3 i S e memnm m a t Ts eTTm a r T Iae a hRe mEr A ea e LT o rt eS n R Sb AYe EE RSEET | ALCSa --1131s 3H y<iy3i fEf anmeesncT e aelaenBm |e grioi E TSonm oeE meaHS R1e eR 11HTSE Rs GAT re iommea S LR orTIfE om 1 e E132 13E Ym a a e a or a -- ARAR Gotiepemee|l=oToaTewllaaTlrourleouLeanIlmieaoimoine t][o1y]|I HTEISSES NIS IASO (N3ToEf e aoo|Jdl | eea (TCE tele DESARNo loseour SSttaorrkk10:30m 0:00 Shsesnungme BraSut? Gotan lsh nC 34h0o0ur TIE EC Eoe Sd Ser Sertlome aM Environmental Laboratory Page 16501703 BACK TO MAIN w 1 Oh b 2h .E 4h d 8h 18h f 24h g 38k h 48h i BACK TO MAIN F 1 BACK TO MAIN Gzuz a b c d 0 I g h Gals Oh 2lw 4h 8h I8N 24h 3Bh 48N 3M Environmental Laboratory BACK TO MAIN Page 169 of 703 aLl2 b E d f # h ^. I mu3 a b E d e I g h PHW Oh 2h 4hr 8h Ish 24h 3Bh 48h BACK TO MAIN mlz a Oh b 2h .E 4 h d lh llh t 24h I 3Btw h 48hr C d 1 L 6 hours: BACK TO MAIN ETS-ElM) Col24: 48 hours: Test Substance:PFOS I I I 9 cn (D -l 0 0 GLP Study Number: Em-1311 1 of2 BACK TO MAIN Test Substance:PFOS -3. 2012 Adsorption Isotherms.Multiple Concentrations ETS-8-160 BACK TO MAIN Test Substance:PFOS *-.. cc) 0 GLP Study Number:EOO-1311 1 of 12 Adsorption Isotherms. Multiple Concentrations ETS-8-160 BACK TO MAIN Test Substance: PFOS c9 p-.. 0 b a, rn a m GLP Study Number: E00-1311 2of12 AdsorptionIsotherms, Multiple Concentrations ETS-5160 BACK TO MAIN Test Substance: PFOS *-.. 4/6 Col9 BalanceID C o l i 1 Inc ID A TimeIDatellnitials 1: Ib&,LlJ9/ O / C2n.C EquilStart !/OM' Qn &lQll3Lr;;pn C Col10 0.01 M CaC12 soh ID#e 4 4 4 2 EquilStop TlDil2'oo*n R IB lol mC p ~ ; ~ s ~ ; ; ~ a a~mo- i C o l l 2 Test Subst. ID #p/nnr - 0 3 -07 Test Substance conc.: 5OOuglmI T i m e i D a t e / l n i t i a l s ~ l / d ,0 I F)nc TimelDatellnitialsd:5 . m d /I'/ IO1 CmC Col13 Inc ID NR Equil Start TIDII Equil Stop TlDll )& __U__ Col14 BalanceID &- TimeiDate/lnitialsCU&- Co115 T l O n $ ~ ~ p r 2% I jq 101 mL Test Substance conc.: t o c l o m GLP Study Number: E00-1311 3 of 12 BACK TO MAIN a, u m l a 1- Col9 BalanceID - c Col10 0.01 M CaC12 soln ID #pool W - @ TimelDatellnitials~~Qh B I ki?;l&unc COI II Inc ID /& EquilStart TKIIIJ ! EquilStop TIDA w & 3 la 10 / g n c l&bu c //a1o/ pH ofTest Soh.,$--, .-,TirneiDatellnitials~:3~~ Co112 TestSubst.ID#DlCol-O_S_-_0_7___ ~~ Test Substanceconc.:-SOOug/rnl W C T i r n e l D a t e I l n i t i a l s ~ Y 5 ~la & , l a L GLP Study Number:00-131 1 4 of 12 AdsorptionIsotherms, MultipleConcentrations ETS-8-160 BACK TO MAIN Test Substance: PFOS *%. q/(O Col 9 BalanceID Time/Date/lnitials / O w I I20 141 (&., c Col 10 0.01 M CaC12 soln ID # o m ! -.7cr-/t -1- Col 11 Inc ID -/& 2 Equil Start TDII I f 01.. A//&I?D I Equil Stop T / D i l - l A l m u*l c t pH of Test Soh. Col12 Testsubst.I D I e J o O 1-0 3-7 Tirne/Date/lnitiald:3d,md / / 2 1 0 / ctnc Test Substanceconc.:-5Wug/ml Time/Date/lnitialsP:o>nma 114 / O l r m L a Col13 Inc IDJdA a . Equil Stalt TIWI N A EquiiStop T/D/IFJ4- - Col14 BalanceID G+3 TimeDate/lnitials@.--3--C--- - - 4 G d Col15 T/D@!C+W d / Iq lo\W c c 0 i i 6 T I D / I ~ ! ~ ~ ~ 1 0 1mc Col17 Tlona!o o p w 114 K>I CWICCollB SpikesolnID# -3- 141 Test Substanceconc.: J O w m TimeiDatehitialsJO!& 8 L30 IO I -c &nternalStandardID# \oo I n t a r n a l S T D c o n c . : ~ ~ p ?,;a~&: ! Time/Dateilnitials1I hd ow,& @iaI DI & c GLP Study Number: E00-1311 5 of 12 Adsorption Isotherms. Multiple Concentrations ETS-8-160 BACK TO MAIN Test Substance: PFOS &!; Col 9 Balance ID Time/Date/lnitials ~ Col 10 0.01 M CaC12 soh ID 1-.W-l . Ty/& a cc Col 11 Inc ID 1 EquilStart T i D 1~ I ~ a ; I L h I Q L c1m Equilstop T / D ~ I J # . W ~1~13 101 TimelDate/lnltialsd:/~ c*-I pH of Test Soh. SS' da TimelDate/lnitiald:3b!~a I o / c*tC Col12 Test Subst.ID #pinh I- b 3 - O 7 Test Substance conc.:-500ug/rnl T i m e l D a t e / l n i t i a l s S ! 4 ~ ~ r 3113-10- Co113 I n c I w Co116 T/Dlllo:3.47n d / i S / b I UJIC Equil S~tarl TlD/lg!'i5&n 2 ~/&I- Col 17 T/Dn -&/=UV\C %?? EquilStop TIDII & J d l w L Col18 Spike soh ID#- Col14 BalanceID Test Substance conc.:+w\ TirnelDate4nitials q:aSL& I ~ I T~imelDatCe/lnitials ' '3- 14 7 l&?d01 m c a n t e r n a t Standard-DI Col15 T/Dn q:as-Al/5-i 01 cm t lntemalSTDmnc.&'pa -01 13:SA Ad&&-- GLP Study Number: EM-1311 60f12 Adsorption Isotherms. Multiple Concentrations ETS-8-160 BACK TO MAIN Test Substance: PFOS +-... m 0 b a, cm n a GLP Study Number:00-1311 7of12 Adsorption Isotherms, Multiple Concentrations ETS4-160 BACK TO MAIN Test Substance: PFOS ,.-. c3 0 b Co19 BalancelD qlL( TimeIDatellnitials Il!%l Colll l n c I D 3 - / 2 /3t I O I t m c EquilStart T/D/l&!.'/L+ b I&lnLyr\ A/@ Col10 0.01 M CaC12 soh ID#pooOl -.My-/> EquilStop TID/17!cO& /&Iwc Tirne/Date/lnitial$ tDpm pH of Test Soh. 5; lo/ C bc CollZ TestSubst.ID#olOD1- 03-07 TirneIDatellnitiald: 33pd I (2101 clhc Test Substanceconc.:-500ug/ml TimeIDatellnitials~ ! ~ , S , & l & I O ) C GLP Study Number:E00-1311 80f12 Adsorption Isotherms, Multiple Concentrations 1 ETSS160 BACK TO MAIN Test Substance: PFOS +'- GLP Study N u m b e r : E00-1311 90f12 Adsorption Isotherms,Multiple Concentrations BACK TO MAIN ,- ETS-8-160 Test Substance: PFOS c-. m 0 a, a0m) GLP Study Number: E00-1311 10of 12 Adsorption Isotherms. MultipleConcentrations ', ETS-8-160 BACK TO MAIN Test Substance: PFOS m 0 h GLP Study Number: EOO-1311 1 1 of 12 Adsorption Isotherms, Multiple Concentrations ETS-8-160 BACK TO MAIN Test Substance: PFOS GLP Study Number: EW-1311 12 of 12 Desorption Isotherms. Multiple Concentrations ETS-8-160 BACK TO MAIN Test Substance: -5 1 of6 BACK TO MAIN ---- [e 7 ha Tr, EE ea i e pe a jo CRETE HI i [Sle = es i HHH gL ERT il e ERSe EE RA aH ie --ee) a ------ iB io Ei rasp e Hi mnie fe a i- Lif ok mor e h [aL ]fellsf i i i Hae E E mm EiE nhi n lFEET Ly = 3i Ei Fo Teees wringer. SET Tt. o) Shasta aris BB aurive on Tar" CEH Ea RE Bdom Desorption Isotherms. Multiple concentrations ETS4-160 BACK TO MAIN Test Substance: ?FO\ Col8T/D/l7!3oAm 2 I / ' ? 101 a*c Col14 InternalStan'dardl D # o i ~ lQ- s - O l Col 19 Centrifuge R Transfer a a3 Col23 Centrifuge 8 Transfer T/D/I~~.zo~~ IO\ M .I 3of6 Desorption Isotherms. Multiple Concentrations ETS-8-160 BACK TO MAIN Test >h> substance: Col8 l/O/I&z~em d / / 4 /Of&C Col13 l/!JllG Col 14 Internal Standard ID#pi001-a~-01 Col 19 Centrifuge 8 Transfer C o l 2 3 Centrifuge& Transfer T/DIlfi'.30* 2 /&luc DesorptionIsotherms. MultipleConcentrations ETS-8-160 BACK TO MAIN Test E Substance' 0 5 GLP StudyNumber: E o a- 1 31 / &-- e '1 ' Col23 Centrifuge& Transfer 50f6 Desorption Isotherms, Multiple Concentrations ETSB-160 BACK TO MAIN Test Substance:PfO5 +t------ - i 6of6 BACK TO MAIN Appendix D: Individual Sample Data This appendix includes processed individual sample data from the present study. Tier I: "Suitable Analytical Work" "Suitable Container" "Optimal Soil: Solution Ratios" "Adsorption Kinetics, One Concentration" "Mass Balance Calculations" "Suitable Desorb Solvent" Tier 11: "Tier 11: "Adsorption Kinetics, One Concentration" Tier 111: "Tier 111: "Desorption Kinetics, One Concentration" "Tier 111: "AdsorptionAlesorptionIsotherms" "Tier I11 "Mass Balance Calculations" 3M Environmental Laboratory Page 191 of 703 BACK TO MAIN Study E001311 Sunable Analylical PFOS AdsorbIDesorb 9s. Tier I "Suitable AnalvticalWork" 0'3 TheoretlcaiTest Measured Observed Solution % RSDof Recoveries Orlglnal Matrix Substance Dilution Concentratlon,uglL Concentratlon,uglL Average (Avergedover entire 2 3 Sample File Name Sample Description Solution Concentratlon,ugA Factor (frominstrument) [measuredx dilutlonfactor) Recovely,% Recovery, % soil type) mioizsowo 101: EW-13114016 EW-1311MxH 0 10 40.0 4w NIA ? 1010125-041 l o x EO0-131l-Wl7 EW-1311MxIz 0 10 40.0 -4w NIA 1010125-042 lox E00-1311-0018 EW-lJll-WO3 0 10 <40.0 ~400 NIA 1010125-043 lox EW-1311-0019 EW-l31lMI(U 0 10 <40.0 c4w WA 1010125-044 lox E00-1311CQ20 EW-1311MKIS 0 10 <40.0 4w NIA miom(y8 lox EW-131l-CQ21 EW-1311-WOS 0 10 e40.0 <400 NIA m10i2s-w9 lox EW-13114022 ECU1311MX17 0 10 40.0 c4w NIA Canlml Blanks H110125-OM mioizs_o5i . lox EW-13ll-W23 lOxE@C-l3lldM4 EW1311-0008 EW-1311Mx)o 0 10 0 10 c40.0 <40.0 <4m NIA 4W NIA lalO125-052 lox EW-1311-CQ25 EW-1311CQlO 0 10 c40.0 <4w NIA mioizs-056 lox EW-lJll-WZ8 EW-1311-Wll 0 10 40.0 <400 NIA mioizs-057 1Ox EW-1311-W27 EWlIll-0012 0 10 40.0 4400 NIA mio125-osa lox Em13110028 EW-1311-0013 0 10 c40.0 <400 NIA 1010125-059 i o x ~00-13ii-w29 EW-1311-Wl4 0 10 <40.0 c40a NIA mioi2s-OBO 101 EW-131l-W30 E00-1311-0015 0 10 <40.0 r400 NIA 10101250W4 lOIEW-131lMIJl EDI).lJll4001 5000 10 615.66 61566 123.1 mroins-ces lOlOl25-E4 lox EW-13114032 1Ox E00-1311Mn3 E00-1311-W01 EW-1311MIOl 5wo 10 swo 10 534.11 623.15 5341.1 8231.5 106 8 124.6 1010125-067 1Ox EW-l311-W34 E00-1311-W02 5WO 10 511.02 51102 102.2 mioizs-ffi8 lox EW-1311-W35 E00-13ll-W02 SOW 10 599.06 5990.8 119.8 115.2 Bsmes LoomSam Loam 1010125-072 lox EW-13114036 EW-1311MX12 5004 10 539.37 5393.7 107.9 1010125-073 lox EW-1311M137 EW-1311-0333 5000 10 602.7 6027.0 120.5 72 (010125-074 10xEW-Wl4038 EOO-lJll-WDJ 5000 10 543.28 5432 8 108.7 1010125_075 10xEW.13114039 EW-l311-W03 SOW 10 615.46 61548 123.1 lO10125-078 lox EW-1311-0040 ~oai~iid~w 5oM) 10 566.96 5669.8 1134 1010125-080 lox E00-1311-OLl41 EW-1311MX14 5000 10 561.3 56130 112.3 1010125-081 10xE00-1311-OW2 EW-13114CC4 5033 10 582.06 5820.6 116.4 010125-082 lox EW-1311-W43 EW-1311-W05 5000 10 560.81 5608.1 112.2 mioi25-083 10xEW-1311M144 EOQ1311-WOS SOW 10 629.91 8299.1 126 0 115.2 clay Loam(Carl Bmann) lolOl25-084 10xEW-l3ll-W45 EW-1311W05 5WO 10 548.47 5484.7 1W.7 m i 01zs-oss lox EMI-1311m46 EW-1311MMg Hx)O 10 570.84 5708.4 114.2 4.1 lOlO125-089 lox EW-13114047 EW-1311.WOB 5wo 10 814.54 8145.4 122 9 miom-ow lOxEW-13ll-CQ48 EW-13114006 5000 10 549.94 5499 4 1100 Page 1 of 2 BACK TO MAIN Study E001311 Suitable Analytical PFOS Adsorb/Desorb Sample FHe Name Sample Descrlptlon lOlOl25-091 1010125-092 miorzs-096 1010125~097 mioiz5-ose mioiz5-ow 1010125~lW 1010125-104 1010125-105 1010125-108 KHO17.5-107 1010125~108 1010125~112 mioi25-1i3 mioins-iir 1010125-115 ~10125~118 1010125~120 miaizs-izi 1010125-122 1010125~123 1010125-124 1010125~128 1010125-129 l010125~130 mt0125-131 miom-132 1OxEW-1311.0348 1oX EW-13114050 1oX EW-1311-W51 lox E00-1311-W52 10%EW-1311-W53 1oX EW-1311-0054 101:EW-13110055 lox E00-13ll-W53 IlOx EW-131lM158 lox EW-1311-W59 10%E00-1311-Mx10 lDxEW-13I1M)Gl 1OxEW-13114052 1Ox EW-1311-Mx13 lox E00-1311-0064 lox EW-1311-0065 10xEO~13114066 irn~ o a i ~ i i - 0 0 6 7 10xE00-1311-0068 lox EOC-1311-WS9 lox ~00-i3ii.w70 irn~oai31i-oo7i lox E00-131l-W72 lox ~oai3ii-0073 lox EW-1311-W74 lox EW-13ll-W75 Orlglnal Matrlx Solution EW-1311-WO7 EW13114007 EW-1311-WO7 EW.lIll-MM8 EODI~~I-WOI EW-1311-WO8 E001311M109 E00.1311MX)O EW-1311-MH19 EW-13114010 E0013114010 EW1311-WlO EW-1311-Wll EW-1311-W11 EW-1311-Wl1 EW-1311-Wl2 EW-1311-Wl2 EW-13114012 EW-1311-Wl3 EW-lJllM113 EW-1311-Wl3 E00-13114014 EW-13114014 EW-13114014 EW-1311-WI5 EW-13114015 EW1311-Wl5 Theoretical Test Substance Concentratlon, ugR 5030 MM) 5wO 5wo 5wil 5WO 5WO 5MM 5wo MW 5wa 5wo 5wo 5000 5wo swo 50W 5wa 5wo 5wo 5wo 5WO 5wo 5wo 5wo 5m 5MM Measured Observed Solution Dilution Concentration,ugR Concentration,ugn Average Factor (from instrument) (measuredx dilutionfactor) Recovery,% Recovery,% % RSD of Recoveries (Avergedover entire roll type) 10 635.II 10 539.81 10 402.35 10 417.47 10 359.31 10 360.97 10 609.1 10 603.9 10 540.32 10 680.88 10 543.97 10 617.2 10 549.02 10 605.04 10 529.29 10 613.74 10 535.27 io 547.43 10 326.1 10 457.52 10 586.47 10 412.39 10 473.07 10 399.6 10 428.08 10 471.39 10 418.75 6357.7 127.2 5388.1 108 0 4023.5 m15 4174.7 83.5 3593.1 71.9 99.8 Clay 3809.7 762 6091.0 121 8 21 6039.0 120.8 5403.2 108.1 BBo8.8 136.2 5439.7 108.8 6172.0 123.4 5490.2 109.8 6050.4 121 0 116.0 Sediment 5292.9 105.9 0137.4 122.7 8. 5352.7 107.1 5474.3 109.5 3261.0 65.2 4575.2 91.5 5864.7 117.3 4125.9 82.5 4730.7 94.6 88.3 Sludge 3996.0 79.9 4280.8 85 6 15' 4713.9 94.3 4187.5 83 8 2 W w Page 2 of2 BACK TO MAIN Study EW-1311 Suitable Container Tier I "SuitableContainer" Theoretical Test sOO120-036 EW-1311-1W2 Ohr none 0 2 sW120-037 EW-1311-1003 Ohr IlOI-lS 0 2 s00120-038 E00-131I d 0 0 4 Ohr none 100 2 ~00120-039 EW-1311-1W5 Ohr none 100 2 ~00120-043 EW-1311-1W6 Ohr none 100 2 cW120-044 E00-1311-1007Chi none IO00 2 sW120_045 EW-1311-1WB Ohr none 1WO 2 ~001201046 EW-1311-1W9 Ohr none loo0 2 ~ 0 0 1 2 0047 EW-1311-101024hour, OmglL. S I , C-1 POC~OPY~ne 0 2 ~00120~051 EW-1311-101124 hour, OmglL. SI. C-1 Polypropylene 0 2 ~00120-052 EW-1311-101224hr. OmglL. S I , C-1 Polypropylene 0 2 ~00120-054 EW-1311-101324hour,0 10mglL. SI. C-1 Polypropylene 100 2 ~00120-055 EOO-1311-101424 hwr. 0 10mglL. SI. C-I Polypropylene IW 2 sW120-059 EW-1311-101524hour,O.lOmglL, S I , C-1 Polypropylene 1w 2 sW120-061 EW-1311-101624hour. l.0mgA. S1, C-I Polypropylene 1WO 2 s00120_062 EW-1311-101724hour. l.0mglL. SI. C-I Polypropylene 1WO 2 sW120 063 EW-1311-101824hour, l.OmgR, S l . C-I Polypropylene 1WO 2 ~00120-068 EW-1311-101024hour, Om@, 52. C-I Polypropylene NIA 2 ~00120-069 EW-1311-1011 24 hour, OmglL. S2. C-I Polypropylene NIA 2 ~00120-070 EW-1311-101224 hour, Oman,S2. C-I Polypropylene NIA 2 ~00120-075 EW-1311-101324hour, O.lOmglL, S2. C-I Polypropylene NIA 2 ~00120~076 EOO-1311-101424 hour. O.lOmglL, S2.C-I Polypropylene NIA 2 ~00120-077 EW-1311-101524hour, O.lOmglL, S2, C-I Polypropylene NIA 2 ~00120-079 EW-1311-101624h w r , 1 Om@. 52, C-1 Polypropylene NIA 2 sW120-083 E00-1311-101724 hour, 1.OmglL. 52. C-I Polypropylene NIA 2 so0120 084 E00-1311-101824 hour, l.OmglL, S2. C-I Polypropylene NIA 2 ~00120-103 EW-1311-101924hour. 0mglL.SI. C-2 Polystyrene 0 2 ~00120-104 E00-1311-102024hour.OmgN, S1. C-2 Polystyrene 0 2 ~00120-105 EW-1311-102124hour. OmglL, S1, C-2 Polystyrene 0 2 ~00120~110 EW-1311-1022 24 hour, 0 IOmUL, S1. C-2 Polystyrene 100 2 sW120~111 EW-1311-102324hour. 0.lOmglL. S1. C-2 Polystyrene 100 2 ~00120~112 E00-1311-102424 hour, O.lOmg/L. S I , C-2 Polystyrene 100 2 ~00120-114 EM)-1311-102524hour. l.Omg/L. S I . C-2 Polystyrene low 2 ~ 0 0 1 2 0 ~ 1 1 8 E00-1311-102624 hour, 1 GmgR. S1, C-2 Polystyrene 1000 2 ~ 0 0 1 2 0119 EW-1311-102724hour. l.GmgR, S1, C-2 Polyst rene sOQl22a-035 EW-1311-101924hour, OmgIL, 52. C-2 Polystyrene NIA 2 sOO122a-036 EW-1311-1020 24 hour, OmglL. 52. C-2 Polystyrene NIA 2 sOO122a-037 EW-1311-1021 24 hour. OmglL. S2. C-2 Polystyrene NIA 2 sW122a-042 EW-1311-102224hour, O.lOmg/L. S2. C-2 Polystyrene NIA 2 soO122a-043 EW-1311-1023 24 hour, 0.lDmglL. SZ. C-2 Polystyrene NIA 2 sOO122a-044 EW-1311-1024 24 hour, 0 10mglL. S2. C-2 Polystyrene NIA 2 soO122a-046 EOO-1311-102524hour, I.OmgR, S2. C-2 Polystyrene NIA 2 sW122a-050 EW-1311-1026 24 hour, l.0mglL. S2. C-2 Polystyrene NIA 2 s00122a 051 EW-1311-102724hour, l.Omg/L. S2. C-2 Polystyrene NIA 2 <24 75 <24 75 <24 75 c24 75 s24 75 486 97 523 02 544 09 25 86 c24.75 C24.75 44.75 c24.75 424.75 462.08 475.12 505.67 r24.75 c24.75 <24.75 c24 75 c24.75 <24 75 11087 118.37 137.3 <24.75 c24.75 <24.75 <24.75 c24.75 c24.75 457.51 475 62 484.59 44.75 <24.75 c24.75 c24.75 ~24.75 g24.75 71.39 99.23 88.02 Observed Solution Concentration, ug/L (measured x dilution factor) <49 5 c49 5 4 95 496 c49 5 4 95 973 94 .. 10.4.6M1088 18 Point thrown out 4 95 <49 5 <49.5 49.5 c49.5 924.16 950 24 1011.34 4 95 <49.5 49.5 c49 5 49.5 <49 5 221.74 236.14 274.6 <49.5 <49.5 <49.5 49.5 <49.5 c49.5 915.02 951.24 969.18 <49.5 c49.5 4 95 4 95 49.5 49.5 142.78 198.46 176.04 ReCOVeN. % c49 5% <49 5% c49 5% 97 394 1MR M 108 818 49.5% <49.5% <49.5% 92.416 95.024 101.134- NIA NIA NIA NIA NIA NIA NIA NIA NIA 4 9 5% -=49.5% c49 5% 91.502 95.124 96.918 NIA NIA NIA WA NIA NIA NIA NIA NIA extractions. ua/L 96.19 244.: 94 51 172 1 Pagelof2 al BP) BACK TO MAIN Study EMF1311 Suilable Container PFOS AdsorbiDesorb *-.. m 0 b TheoreticalTest Measured Observed Solution Substance Concentration, Concentration, ugN Average Average Sample Data Centrifute Concentration, Dilution ug/L (from (measuredx dilution Recovery, Concentrationof a, I I I I 1 1 I 1 rn Sample Description TubeType UglL Factor Instrument) factor) Recovery. X W extractions, uglL am SW120-122 EW-1311102924how.Omgll. S1.C-3 glass glass 0 2 29 19 0 c24 75 58 38 <49 5 sw120-126 EW-1311-103024 hour, OmglL. S I . C-3 glass 0 c24 75 4 95 SW120-128 ECC-1311-1031 24 hour, 0.lOmglL. SI. C-3 glass 100 <24 75 c49 5 4 9 5% sW120-129 EW-1311-1032 24 hour, O.lOmg/L. SI, C-3 glass 1W <24 75 4 95 c49 5% 500120-130 E001311-103324hour, 0 1Omgil.. SI. C 3 glass 1W Q4 75 <49 5 4 9 5% ~00120~135 EW-1311103424hour, l.Om@L. S1. C 3 glass 1CCU 465 89 931 78 93 178 sw120-136 ~00120137 EW-1311-103524hour, l.Omgll, SI, C-3 EW-1311-103624hour. l.OmglL, Sl.C-3 glass glass IWO Im 490 88 494 39 981 76 308 78 98 176 98 878 96 74 03-1311-102824 hour, OmglL, S2,C-3 glass NIA <24 75 4 95 NIA EW-1311-1029 24 hour. OmglL, S2. C-3 glass NIA c24 75 c49 5 NIA sW122a-058 EW-1311-103024hour, Om&. S2. C 3 glass NIA c24 75 <49 5 NIA 001311-103124hour, O.lOm@L SZ.C-3 glass NIA 4 4 75 c49 5 NIA sOO122a-061 001311-1032 24 hour, 0.lOmglL. SZ,C-3 glass NIA e24 75 4 95 NIA sW122a-062 03-1311-103324 hour, 0.lOmgll. SZ, C 3 glass NIA C24 75 c49 5 NIA E00-1311-103424 hour, 1.OmglL. S2,C-3 glass NIA 261 99 523 90 NIA sLU3122a~068 EM)-1311-1035 24 hour. 1 OmgIL. S2,C-3 glass NIA 2 201 55 . - sW122a-069 EW-1311-103624hour 1 OmglL S2 C 3 glass NIA 2 133 08 sW120 142 00-1311-103724hour Omok S I C-4 Teflon 0 2 442 75 ~00120~143 00-1311-103824 hour, Omg/L. S I , C-4 Teflon 0 2 28.04 sW120-144 E001311-103924 hour, OmglL, S I . C-4 Teflon 0 2 c24.75 403 1 N/A 266 16 NIA 885 5 56.08 449 5 397 75 ~00120~148 EW-1311-104024hour, O.lOmglL, SI,C 4 Teflon 1W 2 c24.75 c49.5 49.5% sW120-150 EW-1311-104124hour, O.lOmg/L,S I . C 4 Teflon 1W 2 <24.75 019 5 e49 5% ~00120~151 ~00120-153 EW-1311104224hour, O.lOm&, S1, C-4 E00-1311-104324 hour, 1 OmglL. SI. C-4 Teflon Teflon 100 1000 2 C24.75 2 417.07 <49.5 835 74 C49.5% , 83 574 ~00120-154 s00120~158 EW-1311-104424 hour, I.OmglL, SI. C-4 EW-1311-104524 hour, 1 OmglL. SI. C-4 Teflon Teflon 1000 1000 2 455 03 2 469.4 910 06 938 6 91 w6 93 88 89.49 sOO122a-074 EW-1311-1037 24 hour, OmglL. 52.C-4 Teflon NIA 2 c24.75 <49.5 NIA sW122a-075 E00-1311-103824hour, Omg/L. 52. C 4 Teflon NIA 2 C24 75 c49 5 NIA sOO122a-076 EW-1311-103924hour, O m g L S2. C-4 T8flMl NIA 2 c24.75 c49.5 NIA sW122a-078 EOO-1311-104024hour, 0.lOmglL. S2. C 4 Teflon NIA 2 c24.75 e49.5 NIA sW122a-082 EW-1311-1041 24 hour. O.lOmg/L. 52, C-4 Teflon NIA 2 44.75 c49.5 NIA sOO122a-083 EW-1311-ID4224 hour, 0 IOmgn, SZ, C-4 Teflon NIA 2 c24.75 c49.5 NIA sOO122a-085 EW-1311-1043 24 hour, l.OmglL, S2. C-4 Teflon NIA 2 25.99 51.98 NIA sW122a-086 EW-1311-1044 24 hour, 1.OmglL. S2,C 4 Teflon NIA 2 84.89 169.78 NIA 94 sW122a-090 E001311-104524 hour, l.OmgiL. S2. C-4 Teflon NIA 2 30 68 61.36 NIA Note: Inall of the 0.lOmgiL test vessels lhe test substance was undetected. This IS due to the natureof the relationshipof the test subslance to the test vessel. some amount of adsorptionwas expected In this particular case the amount of test substance initiallypresent in the test vessels was relativelysmall. and the amlytical method was unable to delea the lest substam intha samples. For the remainder of the study the amount d test substanca administered to the test vessels was at least 5 times higher than the undetected0.lOmglL level. Page 2 of 2 BACK TO MAIN Study E00-1311 Optimal Ratios PFOS AdsorbIDesorb Tier I "Optimal Soil:Solution Ratios" Sample Data File Sample Description 5001207-037 ~001207-038 S001207-040 ~001207-044 5001207-045 1001215-037 l001215-0%8 twi2i5-039 1001215~041 1001215-045 1001215-046 1001207~047 ~001207-048 ~001207-052 ~001207-054 sM11207-055 ~001207-056 ~001207-061 ~001207-062 ~001207-063 1001211-038 ~001211-037 ~001211-038 S001211~040 ~001211-044 ~001211-045 soai21i-047 r001211-048 ~001211-052 ~w~zor-oae ~001207-089 ~w1207_070 ~oa1207-072 ~001207-076 ~001207-077 ~ooiza7-a79 SW 1207-080 ~001207-084 lox ECU1311-3002-Sl.O.orn@!L, Ohr. No soil, 12M71w lox EW-1311-3009S1,0.0mpll. Ohr, No soil, 1M7m0 lox E00-1311-3WkS15OmglL. Ohr, No soil, 121c71w lox E00-1311-3005SI. S.Om&. Ohr, No soil, 1M7m0 1Dx EM)-1311-3WgSl.5 am&. Ohr. No soil. 12M71w lox E051311-3W7-SI.O.OmgR, 48hr. No Soil. 12/071w lox EW-1311-300BS1.0.0mglL. 48hr. No Soil. IZR7m0 l o x E W - 1 3 1 1 - 3 ~ S I0..0m&. 48hr. NOSoil. 12/071w 10xEW-1311-3010S1,5.0m@, 48hr. No Soil. 12~97100 lox E00-1311.3011-S1.5 O W . 48hr. No Soil, 12/07100 l o x EW-13113012-S1.5 OmgA. 48hr. No S d . 121071M) lox E00-1311.3013.Sl. o.ompll. Ohr, 1.lday. 12/07/00 1Ox E00-1311-3014-S1,O.OmgR.Ohr. 1:lday. 12m71W 10xEW-1311-3015S1O, OmglL Ohr. 1.lday. 12107Mo lox E00-1311-3015S1, O.orn&. Ohr. 1:5clay. 12/07/00 1OxE00-1311-3017-S1.OOmglL Ohr. 1:Way. 12/071w lax E00-1311-3018-S1.o.omWl.,Ohr, 1:Sday. 121071w l o x E00-1311-3019-S1.O.Omg/L.Ohr. 1.25day. 12/071w l o x EO51311.302bS1,0 Om&. Ohr. 1'25clay.1M7RO lox E051311-3021S1,0 om&, Ohr. 1:Zblay. 1M7IW l o x EOD-1311-3022-S1,O.Ornp/L.48hr. 1:lClay. 12/07/00 ~ O X E C U ~ ~ ~ I J O ~ ~ SaI..mg&48hr. l:lC\ay. 12107100 lox E00-1311.3024S1, a.OmgR. 48hr. 1:lClay. 12/07100 lox E00-1311-3026S10OmSn.48hr. 1.5 Clay. 12D7100 lox E00-1311-3025S10.OmglL4. 8h, 1'5 Clay, 12107Mo lox E00-1311-3027-S1o.om&. 48hr 1:5 Clay, 12/07hX lox EOO-1311-302BS10mo@- 48hr. 1.25Clay. 12/07/W lox EM)-1311-302&S10.0mglL. 4% 1.25Clay. 12m71M) l o x E00-1311.3030-S1 o.omp/L. 48hr. 1:25 Clay. 12107lW ?OX EM)-i311-3MI-S1,5am@. Ohr. 1:lclay. 12m7100 lox E00-1311-3032-S1,5.0m~M, lr. l'ldey. 12/O7/M) lox ~~.1311.3033-~1,5.0mpO/h~r,,1:lday. 12/07/00 lox E00-1311-3o34-Sl,5.omglL.Ohr, l:5day, 12m7xx) 10%00-1311-3035S1.5om@!L.Ohr. 1Iday, 12m7mO lox E00-1311.303aS1.5.0mglL.Ohr.1.Way. lM7IO0 lox E~1-1311-303781,5[hnp/L.Ohr. 1.25day. 121071w lox EW-1311.303BS1,5.OmgIl.Ohr1. :tWay. 12/O7X)O 10%00-1311.3039-S1.5.0m~L,Ohr1. .25day. 12/O7/W Theoretical Test Time Substance SoilSoluti Point, Concentration, Soil Type on Ratio Hours u g l l Dilution Factor Measured Concentration, uglL (from Instrument) Observed Solution Concentration, ugR (measured x dilution factor) Amount o Substance Adsorbed % No soil none 0 No soil none 0 No soil none 0 No soil none 0 No soil none 0 No soil none 48 No soil none 48 No soil none 48 No soil none 48 No soil none 48 No soil none 48 Clay 1:1 0 Clay 1:l 0 Clay 1:1 0 Clay 1:5 0 Clay 1:5 0 Clay 1:5 0 Clay 1:25 0 Clay 1:25 0 Clay 1:25 0 Clay 1:1 48 Clay 1:1 48 Clay 1:1 48 Clay 1:5 48 Clay 15 48 Clay 1:5 48 Clay 1:25 48 Clay 1:25 48 Clay 1:25 48 Clay 1:1 0 Clay 1:1 0 Clay 1:1 0 Clay 1:5 0 Clay 1:5 0 Clay 1:5 0 Clay 1:25 0 Clay 1:25 0 Clay 1:25 0 0.0 10 0.0 10 5000.0 10 5000.0 10 5000.0 10 0.0 10 0.0 10 0.0 10 5000.0 10 5000.0 10 5000.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 0 0 0 a c25.0 -25 0 45.0 s25.0 <25.0 e5.a 0 50 c25.a C25.0 c25.0 <25.0 c25.0 398.29 449.17 <25.0 e250 <25 0 <25.0 e25.0 c25.0 s25.0 <25.0 <25.0 e25 a 26.41 47.72 74.95 386 389.48 390.3 427.38 401.2 450.84 0.00 0.00 0.00 0 00 0.00 <250 ~250 C250 <250 <250 e250 C250 <250 <250 <250 c250 c250 3982 90 4491.70 c250 c250 c250 ~250 C250 ~250 <250 ~250 c250 e250 284.10 477.20 749.50 3660.00 3894.80 3903.00 4273.80 4012.00 4508.40 1w.c 1w.c 1w.c >95' ,951 ,95' 947 90.4 85.0 26.8 22.1 21.9 14.5 19 7 98 Page 1of 5 2.G, L rn 5 2 5 5 ? 73 n, cn (D BACK TO MAIN Study 00-1311 Optimal R a t i s PFOS AdsorblDesorb Sample Data File Sample Description ~001207-105 SOOl207~106 ~001207-111 ~001207-112 ~001207-113 SOOl207-118 ~001207-119 S001207-120 ~001207-122 ~001207~126 ~001207-127 ~001207-129 ~001207-130 ~001207-134 s001207-13e ~001207-137 ~001207-138 rw1211-054 ~001211-055 swlzll-056 s001211-081 rwl211-062 ~001211-063 rCQ1211-068 soOl2ll-039 ~001211-070 sOol207-143 5001207-144 r001207-145 ~001207-I50 ~001207-151 s001?0?-15? ~001207-154 ~001207-158 sCQ1207-159 HBlO037.D HiIMO3B.D Hill0039 0 H~IIOO~I.D H1110045.D HtllOO46.0 HdIM)48.0 HillW49.0 H110053.D 1Ox E001311-3041-S1.5.0m~,2hr.1:lclay. 12/07/00 lox E001311-3042-Sl.5.6n~2hr.1.lday. 12/07/00 lox EoO1311-3043-S1.5.0rng5.2~I:,5day. 12/07/00 lox E001311-3044-S1,5 OmglL2hr. 1:Way. 12/07/M) l o x EoO1311-3~s-Sl.5.om~2hl.r5.day. 12/07/00 1Ox EW-1311-3045S1.5 omgR.2hr. 1:25day, 12/07/00 lox E001311-3047-S1.5OmgR.2hr. 1:25day, 12/07/00 lox 00-1311-304BS1.5.mglL,2hr,l.ZXlay, 12/07/00 lox E001311-3049S1.5.0mgR.4hr.1:lday. 12/07/00 lox E001311-3050-S1,5.omg/L.4hr. 1:1day. 12/07/00 lox E001311-3051-S1.5OmgR.4hr. l.lday. 12/07/00 1Ox EO0-1311-3052-Sl.5.0mg5.4hr. l:5day. 12/07/00 lox E0a1311-3053S1.5.6ng11.4hr.1.Sclay. 12107l00 l o x E00-1311-30WS1.5OmgL4hr. 1'5day. 12/07100 lox E001311-305SSl.5.OmgR.4hr.1:25day. 12/07/00 lox E001311-M56S1,5.0mgR.4hr.125day. 12/071w l o x E001311-3057-51.5OmgA.4hr. 1'25day. 12/07/00 lox EM)-1311-M5Ml. 5 m.8hr. IIClay, 12/07/00 l o x E001311-305kS1.5.OmglL. 6hr. l:lClay, 12/07/00 lox E o o - 1 3 1 1 - 3 0 6 o s 1 . 5 . ~8. hr. 1:lClay. 12/07/00 lox E00-1311-3081-S1, 5.omg5. 8hr. 1.5Clay.12/07/00 lox E001311-3062-Sl.5.6nglL. Bhr. 1:SClay. 12/07/00 lox EW-1311-3063-Sl.5.omgfL. 8hr. 1:SClay. 12/07/00 ~ o x ~ 1 3 1 1 - 3 0 8 4 -s~.o1m.gR. 8hr. 1:25Clay. 12m71w 1% E00-1311-3066S1, 5.omgR. Bhr. 1.25Clay, 12/07/00 101E00-1311-306&Sl, 5.Omg5. 8hr. 1:25Clay. 12/07/00 lox E001311-3ffi7-Sl.5.0m~5.18hr.1.lday. 12/07/00 lox E00-1311-306BS1.5OmgR,IBhr,1:lday. 12/07/00 l o x EW1311-3069-S1,5Omg5.16hr. 1:lday. 12/07/00 lox 001311-307aS1.5OmgR.16hr. 1.5day. 12/07/00 lox E00-1311-3071-S1.5Omg5.18hr.l:5day. 12/07mO :QiE"". ,3,1.11-"~- v ~ 2 - 3 l , ~ . O m g i l .i:i5~dhary.. 12/07/00 l o x E00-1311-3073-S1.5.omglC.16hr1.:25day. 12/07/00 1oX E00-1311-3074-S1.5.0mg~.l6hr.1:25day. 12/07/00 1Ox EoO1311-307iS1.5 Om@L.l6hr. 1:ZMay. 12/07/00 1Ox E00.1311-307BS1.5.0m~.Z4hr.1:lday. 12107/00 lox EW-1311-3077-S1.5OmgR.24hr. 1:lday. 12107100 102 EW-1311-307SS1.5 OmgR.24hr. 1:lday. 12/07/00 lox E(M1311.3079-S1.5.0mg/L.24hr.1:5day. 12/07/00 lox E001311-3080-Sl.5.0mgR.24hr.1:5day. 12/07/00 l o x E001311-3081-Sl.5.6ngR.24hr.1:5day. 12/07/00 lox E001311-3082-S1,5OmgR.24hr. 1.25day. 1M7/00 lox E001311-3083-sl.5.hgR.24hr. 1:25clay. 12/07/00 1OxE001311-308eS1.5OmgR.24hr.1.25day.12/07/00 TheoreticalTest Time Substance Soi1:Soluti Point, Concentration, Soil Type on Ratio Hours uglL Dilution Factor Measured Concentration, uglL (from Instrument) Observed Solution Concentration, ug/L (measuredx dilution factor) Amount of Substance Adsorbed, % Clay 1:1 2 Clay 1:1 2 Clay 1:5 2 Clay 1:5 2 Clay 1:5 2 Clay 1:25 2 Clay 1:25 2 Clay 1:25 2 Clay 1:1 4 Clay 1:1 4 Clay 1:1 4 Clay 1:5 4 Clay 1:5 4 Clay 1:5 4 Clay 1:25 4 Clay 1:25 4 Clay 1:25 4 Clay 1:1 8 Clay 1:1 8 Clay 1:1 8 Clay 1:5 8 Clay 1:5 8 Clay 15 8 Clay 1:25 8 Clay 1:25 8 Clay 1:25 8 Clay 1:1 16 Clay 1:1 16 Clay 1:1 16 Clay 15 16 Clay 15 18 Ciay 15 16 Clay 1:25 18 Clay 1:25 16 Clay 1:25 16 Clay 1:1 24 Clay 1:1 24 Clay 1:1 24 Clay 13 24 Clay 1:5 24 Clay 1.5 24 Clay 1:25 24 Clay 1:25 24 Clay 1:25 24 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 98.63 88.87 S25.0 155.7 140.92 317.1 318.56 326.3 113.88 86 39 92.13 126 4 113.16 136.92 326.15 328.21 319 46 1M.4 114.46 111.17 293.97 314.29 287.97 118.92 305.1 128.68 119.29 99.92 168.04 140.62 136 17 152.02 330.98 321.53 346.78 125.10 105.41 34 09 11870 11021 98 72 288 55 284.21 288.40 988.30 888.70 e250 1557.00 1409.20 3171.00 3185.60 3263.00 1138.80 883.90 921.30 1264.00 1131.60 1369.20 3281.50 3262.10 3 194.60 1304.00 1144.80 1 1 11.70 2939.70 3142.90 2879.70 1189.20 3051.00 1286.80 1192.90 999.20 1660.40 1406.20 ?36?.70 1520.20 3309.80 3215.30 3467.80 1251 .OO 1054.08 340.90 1166.96 1102.12 967.23 2885.54 2842.13 2884.61 80.27 88.23 .95% 68 86 71 82 35.58 38.29 34.74 77.22 82.32 81.57 74 72 77.37 72.62 34 77 34.76 36.11 73.92 77 10 77 77 41 21 37.14 42.41 76.22 38.98 74 26 76.14 80.02 66.79 -- -- 71.88 ,L I , 69.60 33.80 35.69 30.64 74.98 78.92 93.18 76.66 77.95 80.66 42 29 43.16 42 31 Page 2 of 5 BACK TO MAIN m-0 (D 0 s 4 0 0 Study E00-1311 Optimal Ratios PFOS AdsorbIDesorb Sample Data File Sample Description TheoreticalTest Time Substance SoikSoluti Point, Concentration, Soil Type on Ratio Hours uglL Dilution Factor ~wizir-07e lox E00-1311-308BS1,5.0mgll.36hr. 1:lClay. 12/07100 clay 1:t 36 ~001211-077 lox E00.1311-3087-S1. 5 OmplL, 36hr. 1:lClay. 12/07/00 Clay 1:l 36 sW1211-079 lox E001311-3088-Sl.5.OmglL.3ehr. 1:SClay. 12/07/00 Clay 15 36 SM)1211~080 lox ED01311-3089-S1.5 Omgll. 36hr. 1:SClay. 12/07/00 Clay 15 36 rw1211-084 lox EM).I~~I-~OWS~, 5.0mg/L 38hr. 1:SClay. 1m7mo Clay 1:5 36 mizii-oee 10xE00-1311-3091-S1,5.0mpn. 36hr. 1:25Clay. 12/07100 Clay 1:25 36 sW1211-087 101E00.1311-3092-Sl.5.Om~.36hr. 1:25Clay. 12107100 Clay 1:25 36 sw1211-088 lox E00-1311-3093-Sl.5.0mplL. 36hr. 1'2SClay. 12/07mO Clay 1:25 36 ~001211-093 lox EM1311-3096Sl. 5 OrngR,48hr. 1:lClay. 12/07/00 Clay 1:1 46 ~001211~094 1OxE00.1311-3w5S1.5.hdL 48hr. 1:lClay. 12/071W Clay 1:1 48 ~001211~095 lox E001311-309gSI. 5 OmglL 48hr. 1:lClay. 12/07/00 Clay 1:1 46 sM11211-1w lox EW-1311-309751. 5.OmgR. 48hr. I:5Clay, 12/07/w Clay 1:5 48 SW1211~101 lox E00-1311-309aSl.5.hplL. 48hr. 1:sClay. 12107/00 Clay 1:5 46 r001211-102 lox E00-1311-3099-S1. 5 OmgIL. 48hr. 1:SClay. 12/07/00 Clay 1:5 48 rW1211~1M lox E0Ll1311-3100-S1,5.0mglL. 48hr. 1.25Clay.12/071w Clay 1:25 48 SW1211~108 lox E00.1311-3101-S1.5.OmglL. 488. 1:25clay, 121071W Clay 1:25 46 SWlZll-IO9 lox E00-1311-3102-S1.5om& 48hr. l:25Clay. 12/07/00 Clay 1:25 46 H1W55.D lox EW1311-3105S1. 5.0mglL. Ohr. 1:lSedimenl. 12/07/00 Sediment 1:l 0 HrlKK158.D 10xEWl3173104S7, Somfl. Ohr. 1:ISedimsnt. I M 7 / 0 0 Sediment 1:l 0 H1110057.D lox E00.1311-3105-S1,5.0m(yL.Ohr. 1:lSediment.12/07/00 Sediment 1:l 0 HilK)062.D lox ELH3.1311-31OBSl. S.Dm(yL, Oh,. 1.5SedimenL 12/07/00 Sediment 1:5 0 HiliW63.D lox E001311-3107-S1.5.OmgR. Ohr. 1.5Sedlment.12/07/00 Sediment 1:5 0 Hill0064 D lox E001311.310BS1,5.OrnglL,Ohr. 1.5SedimenL 12107100 Sediment 1:5 0 H1i0069.D lox E001311-3109Sl. 5 Omsk. OW. 1.25Sedmm 12107iW Sediment 1:25 0 Hil10070.D lox E00.1311-3110-SI.5.OmglL. Oh, 1'25Sediment.12107/00 Sediment 1:25 0 Htli0071D lox E00.1311-3111-S1,5OmpR, Oh., 1'25Sedment. 12m7mO Sediment 1:25 0 H1110073.D lox EW1311-3112-S1.5.0mgiL,2hr. I'lSediment, 12/07100 Sediment 1:l 2 HdlM177.D lox E0~1311-3115S1.5 OmglL, 2hr. 1'1Sediment.1M7RO Sediment 1:l 2 H)llW78.D t0xE001311-3t14-S1, 5 0 W L . 2hr. 1:tSedimSnt. 12/07/00 Sediment 1 3 2 HilIM18O.D lox EW-1311-3115-S1,5 OmglL. 2hr. 1:5Sediment,121071W Sediment 1 5 2 HillOOBl 0 lox E00.1311-3116S1.5OmglL. Zhr, 1'5Sediment12x17X)O Sediment 1:5 2 HiiiaiOi .D lox EoO-1311-3117-S1,5OmVL,2hr. l:5Sedhent 12107100 Sediment 1:5 2 Hili0103 0 1Ox E00-1311-311&S1,5 OmglL, 2hr. 1:25 Sedtment. 12107/00 Sediment 1:25 2 H!110104.D lox E001311-3119.S1.5.OmglL. Zhr. 1:25 Sediment 12R7/M1 Sediment 1:25 2 HillOlO5.D lox E001311-3120-S1.5OrngiL. Zhr, 1-25Sediment. 12/07iW Sediment 1:25 2 Hi110110.D 1oxE001311-3121-S1,5.0mpn. 4hr. 1:l Sediment. 12107lW Sediment 1:l 4 Hill0111.D lox E00-1311-3122-Sl.5.OmgR.4hr. 1:l Sediment, 12/07/00 Sediment 1 : l 4 HIIIO112.D 10xE00.1311-3125S1,5Gmfl. 4hr. 1:l SedimeN 12x1703 Sediment 1:l 4 HXJll7.D lox E00.1311-3124-S1.5Om&. 4hr. 1 5 Sediment 12x17/00 Sediment 1:5 4 HiIIO118.D 10xE00-1311-312681.5h p n . 4hr. 1:5Sedlment 1M7lW Sediment 1 5 4 Hill0119.0 lox ED01311-312SSl.5 OmgIL, 4hr. 15Sediment. 12x1703 Sediment 1:5 4 H1ilO121.D lox E00.1311-3127-S1.5Omp/L. 4hr. 1.25 Sediment. 1z/o7xx) Sediment 1:25 4 ~111012D5 (OX ~ ~ ) - i 3 1 1 . 3 1 2 ~50~m1.,ai~.4hr. 1:25Ssdimenl.12107100 Sediment 1'25 4 HdIO12B.D lox ~00-1311-3129-s1,5OmUL,48.1'25 sediment. 121071~ Sediment 1:25 4 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000 0 10 5000.0 10 5000 0 10 5000.0 10 5000.0 10 5000 0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000 0 10 5000.0 10 Measured Concentration, uglL (from Instrument) Observed Solution Concentration, uglL (measured x dilution factor) Amount of Substance Adsorbed, % 138.13 44 59 103.26 119.9 129.42 299.09 313.39 289.84 59.14 62.48 69 48 92 9 IO7 09 95.8 301.58 331.37 381.05 118.32 121 89 87.39 451.55 442.99 447.e9 402.85 428.58 425 08 78 07 85.88 59.32 247 50 :em 331.41 365.63 e25.0 q25.0 c25.0 80.43 63.71 242.88 24e.91 245.14 380.34 374 21 38.9.7.3 1381.30 445.90 1032.60 1199.00 1294.20 2990.90 3133.90 2698.4 0 591.40 624.60 694.60 929.00 1070.90 956.00 3015 60 3313.70 3610.50 1163.16 1218.86 873.67 4515.51 4429.87 4476.92 4028.50 4265.82 4250.83 760.65 858.62 593.21 2475.02 2867.00 3314.09 3656.30 c250 <250 c250 804.32 637.06 2426.62 2469.09 2451.42 3803.38 3742.10 3687.56 73 61 72 37 91 08 79 35 78 02 74 12 40 18 37 32 42 03 88 17 87 51 88 10 81 42 78 58 80 88 39 e9 33 73 n 79 7e 34 75 e2 82 52 9 e9 11 40 10 46 1943 14 28 14 98 84 39 82 e3 88 14 50 50 46 26 33 72 26 87 >95% >95% >95% 83 91 87 26 51 43 50 e2 50 97 23 93 25 16 28 25 Page 3 of 5 -0 P) (P (D BACK TO MAIN Study E00-1311 Optimal Ratios PFOS Adsorb/Desorb Sample Data File Sample Description t001215-049 tOQl215-053 1001215~055 mo1215-oss 1001215-057 1001215-062 rnoizi5-oe3 1w1215-064 1001215-C89 1001215-070 1001215-073 100121 5-077 1001215-078 looinis-oso tOQ1215-081 rnoi215_085 tO01215-087 M01215-088 tWlZl5-009 Kx)1215-094 KH)1215-095 t00?215-0?0 1001215-116 LW1215-I17 1001215-118 1001215_120 1001215-124 tOO1215-125 ~01215_127 tWl215-I28 l00lZl5-132 1001215-134 rnoizi5-135 Kx)1215-136 1001215~141 M01215-142 KKJ1215-143 1001215-148 tW1215-149 KK)1215-1M 1001215-152 Kx)I215-1W 1001215-357 1(wEW-1311-3131-S1.5~fLB. hr. 1.1Sedimnt 121071w 10%EW-1311-3132-SI.5.OmpR. 8hr. 1:l Sediment 12/07/M) 10%E~1311.3130S1.5.Omg~8.hr. 1:s Sediment, 12/07/00 lox E00-1311-3134-S1,5 OmgiL. 8hr. 15 Sediment. 12/07/M) l o x EW-1311-3135-SI.5.OmgR. Bhr, 1.5Sediment 12/07/00 10%EW-1311-313i-S1,5 om& 8hr. 1.25Sediment 12/07/00 lox EX?-1311-313751.5.0mgR,Bhr, 1'25 Sediment 12/07/W lox EW-1311-313ES1.5ompn. 8hr. 1:25 Sediment 12/07100 10xEW-1311-3139-S1,5.omplL 18hr. 1:l Sediment. 12/07Mo lox EX?-1311-314BS1.5OmgIL. 18hr. 1:l Sediment. 12/07/00 lox EX?-1311-3142-S1,5omw. 16hr. 1 5 Sediment. 12/07/00 lox EX?-1311-3145S1.5om@. 18hr. 15 Sediment. l2/0i100 lox EW-I311-3144-S1.5.OmglL.16hr. 1:s Sediment 12/071w lox EW-1311-3145-S1, 5OmgA. 16hr. 1:25 Sediment, 12/07M) lox E ~ 1 3 1 1 - 3 i 4 E S 5I .ompR. 16hr. 1.25 Sediment 1M7M) lox EX?-1311-3147-S1.5.OmglL 16hr. 1:25 Sediment. 12/071w lox EW-1311-314ES1.5.OmgR. 24hr. 1.1 Sediment. 12/07/00 lox EM)-1311-314OSl,5.OmplL.24hr. 13 Sediment. 12/07/00 lox E~1311-3150-S1.5.0mglL.24hr. 1:1Sediment 12/07/00 lox EX?-1311-3151-S1,5.0mpll.24hr. 1:5 Sediment 12/07/00 lox EX?-1311-3152-S1,5Omglc. 24hr. 15 -ent IuO7100 lox EW-1311-3153-S1,5.0mgiL2. 4h. 1.5Sediment. 12107100 lox EW-1311-3154S1.5OmgR. 24hr. 1.25Sediment. 12/07/00 lox EX?-1311-3155S15. .0mgiL 24hr. 1% Sediment 121071w lox E00-1311-315&S1, 5.0mglL. 24hr. 125 Sediment 12/07/00 lox EW-1311-3157-S1.5.Omgll36hr. 1.1 Sediment. 12/07/00 10xE001311-315ES1.5.OmQlL.36hr. 1:1Sediment 12/07/00 lox EX?-1311-3159S1.5Om& 36hr. 1.1Sediment. 12/07/W lox EW-1311-316BS1.5.Omgll36hr. 1:5 Sediment 12/07/00 lox EW-1311-3161-S1.5.0mg~3,6hr. 1 5 Sediment 12/07/00 lox EW-1311-3162-SI.5.OmgR. 36hr. 1.5 Sediment. 1uO7IW i O x Cmi311-3163-Si. 5.OmglL. 38hr. 1.25 Sediment. 12107100 lox EW-1311-316451. 5.OmglL. 38hr. 1.25 Sediment. 12/07/00 lox EOC-1311-3165-Sl. 5.OmglL. 36hr. 1'25 Sediment 12/07iW lox EW-1311-3165S1,5.OmglL. 48hr. 1:l Sediment. 12/07/00 lox ECO-1311-3167-S1.5.0mpR. 48hr. 1'1 Sediment 12/07/W lox E00-1311-316ES1.5.OmgA. 48hr. 1:l Sediment, 12/07/W lox ECO-1311-3169-S1.5 OmglL. 48hr, 1.5 Sediment. 12/07RO lox E00-1311-3170-S1,5OmglL 48hr. 1:5 Sediment 12/07RO 1oxEW-1311-3171-Sl.50mgA. 48hr. 1.5 Sediment. 12/07RO 10xE00-1311-3172-S1,5.0m~. 48hr. 1:25SedimenL 12107/00 lox E001311-3173-S1,5 OmQIL.48hr. 1:25 SedimenL 12m7xM 1oxEDDl311-3176S1,5.Omgll 48hr. 1:25Sediment. 12/07/00 TheoreticalTest Time Substance SoikSoluti Point, Concentration, Soil Type on Ratio Hours uglL Dilution Factor 6 Sediment 1:1 8 Sediment 1:1 8 Sediment 1:5 8 Sediment 1:5 8 Sediment 1:5 6 Sediment 1:25 8 Sediment 1:25 8 Sediment 1:25 6 Sediment 1:1 16 Sediment 1:1 16 Sediment 1:5 16 Sediment 1:5 16 Sediment 1:5 16 Sediment 1:25 16 Sediment 1:25 16 Sediment 1:25 16 Sediment 1:1 24 Sediment 1:1 24 Sediment 1:1 24 Sediment 1:5 24 Sediment 1:5 24 Sediment 1:5 24 Sediment 1:25 24 Sediment 1:25 24 Sediment 1:25 24 Sediment 1:1 36 Sediment 1:1 36 Sediment 1:1 36 Sediment 1:5 36 Sediment 1:5 36 Sediment 1:5 36 Sediment 1:25 36 Sediment 1:25 36 Sediment 1:25 36 Sediment 1:1 48 Sediment 1:1 48 Sediment 1:1 48 Sediment 1:5 48 Sediment 13 48 Sediment 1:5 48 Sediment 1:25 48 Sediment 1:25 48 Sediment 1:25 48 5000 0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 5000.0 10 Measured Concentration, uglL (from Instrument) gees 92 97 87.04 396.95 233.83 271.00 322 07 341.64 340.94 65 07 80.84 248.78 247.05 268.5 355.44 338 22 355.34 71.71 57.44 38.51 229.84 237.34 220.8 355.21 320.83 304.11 83.87 00.37 50.58 208.79 212.87 253.48 319.84 318.04 371.72 68.84 60.37 30.48 198.79 237.42 196.59 304.44 368.92 346.68 Observed Solution Concentration,uglL (measured x dilution factor) Amount of Substance Adsorbed, % 986 60 929.70 870.40 3969.50 2338.30 2710.80 3220.70 3416.40 3409.40 650.70 808.40 2467.80 2470.50 2685.00 3554.40 3382.20 3 55 3.4 0 717.10 574.40 365.10 2298.40 2 373.4 0 2206.00 3552.10 3208.30 3041.10 838.70 803.70 505.80 2087.90 2128.70 2534.80 3198.40 3180.40 3717.20 686.40 603.70 304.80 1987.90 2374.20 1965.90 3044.40 3689.20 3466.80 80 27 81.41 82 59 2061 53.23 45.78 35.59 31.67 31.81 86.99 83.83 50.24 50.59 46.30 28.91 32 36 28 93 85 e5 88.51 92.70 54.03 52.53 55.88 28 96 35.83 39.18 83 23 83.93 89.88 58.24 57 43 49.30 38.03 36.39 25.66 86.27 87.93 93.90 60.24 52 52 80 68 39.11 28 22 30.66 ... 4 Page 4 of 5 BACK TO MAIN Study E00-1311 Optimal Ratios PFOS Adsorb/Desorb I 1 Sample Data File Isample Description Hi10129 0 Hill0133 D HilKH35.D Hi110138 D HIID137 D Hi110142 0 HWJ143 D Hi110144.D 1W1215-163 1001215-16E 001215-170 KM1215-171 1001215-173 lWl215-174 lox E00-1311-3175S1.0.OmgiL.Ohr. 1:l Sediment 17/07/00 10xECU1311-3177-SlO. .Om&. Ohr. 1:l Sediment. 17/07/00 lox EW-1311-317BSl.0.OmpR. Ohr. 1:s Sediment. 12/07Iw lox EW-1311-3179-W.0.0mgR. Ohr, 1:s Sediment. 12107/00 lox EM)-1311-318W4.O.C~YJA.Ohr. 1:s Sedinwnl. 17/07/00 l o x EM)-1311-3181-S1.0Om&. ohr. 1.25 Sediment. 12/07/00 10%EM)-1311-3182-S1.0.O~.hr. 1% Sediment 17JQ71w 1Ox ECQ-1311-3183-Sl,O.h&. Oh., 1'25 Sediment, 12/071w lox E~1311-31B4-SOi..Om&.48hr. 1:l Sediment 17/07/00 l o x EM)-1311-3185Sl.O.Om&. 48hr. 1'1 Sediment 17/07/00 lox EM1311-31sSSI. O.Om#L 48hr. 1.1 Sediment. 12/07/00 10%EW-1311-3187-S1.0Om&, 48hr. 1:s Sediment. 12/07EQ lox EM)-1311-3188-S1,O.~giL.48hr. 1 5 Sediment 12/07/00 lox EO0-1311-3189-Sl,O.OmgA.48hr. 1.5 Sediment 12/07/00 l o x E00-1311-319&Sl.0 OmplL, 48hr. 1'25 Sediment 12/07/00 1OxEW-1311-3191-S1.OOmgiL4.8hr. 1.25 Sediment 12/07nO l o x EW-1311-3192-S1.0Omst,48hr. 1'25Sediment. 12/07/00 I I lTheoreticaJ_t Time Substance Soil:Soluti Point, Concentration, ]SoilTypeIon Ratio IHours lugR I I I Measured Observed Solution Concentration, Concentration,uglL I Dilution IFactor u g l l (from Instrument) 1 (measured x dilution . factor) Amount ( Substanc Adsorbec % Sediment 1:1 0 Sediment 1:1 0 Sediment 1 5 0 Sediment 1:5 0 Sediment 1 5 0 Sediment 1:25 0 Sediment 1:25 0 Sediment 1:25 0 Sediment 1:1 48 Sediment 1:1 48 Sediment 1:1 48 Sediment 1:5 48 Sediment 1 5 48 Sediment 1:5 48 Sediment 1:25 48 Sediment 1:25 48 Sediment 1:25 48 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 0.0 10 _. . e250 e250 e250 e250 <250 e250 <250 <250 e250 e250 e250 <250 <250 e250 c250 C250 e250 Note: The control samples that did not w n t a i n soil (3004-3006,3010-3012)there was no recovery of the test substance. This was because the test vessels were mistakenly not dosed with the test substance. N 0 0 0, -4 0 w Page 5 of 5 BACK TO MAIN Study Em-1311 Adsorptlon % Cham PFOS Adsomesolb Adsorption Kinetics. One Concentration 4 - E EF. 0 0 2 2 2 4 4 4 8 8 8 16 16 16 24 24 24 36 36 35 48 48 48 Calcdabon of& (adsombon% at bine t) to be nloffedYS bine Calwlabon ofdlrtnbutlon Coeffluent & V. C. - H - E _s E "1 E 8 . f 2 i !i 5' 2 3 I 3 ; i 9 8 s *% 1 El I a: I $9 E I ,* f.; $ IB 50 i g g 3 -I a< E- 50 25 0.477 As - AverageAm, K. - 2. 7 r: i :, ! ?- 3 I 4E ;3 1 c 1" IT If : i !i %I I1' 6 :E I f e a Q-. o I7 rs ai 1;; it, 22.61 9 0 4 6 9006 1 B I; 5 E 1 I i 1 B E g 0 4 9875 9 502 12 5 5 0 62 5 3.895 13.82 22 10 23 61 2 4953 1421 25 0 50 125 4.012 24.70 1976 14 71 1 OW8 6 152 50 50 25 0.986 20.07 80 27 79 21 4 9841 4 082 12 5 5 0 62 5 1.557 43.04 68 86 70 34 2 4988 11 062 25 0 50 I25 3.186 45.36 36 29 35 a7 10012 14 222 50 50 25 0 884 20.58 82 32 80 37 5 W85 4 a 9 12 5 5 0 62 5 1.132 48.36 77 37 74 90 2 5105 17 021 25 0 50 125 3.262 43.45 34 76 3 5 2 1 10241 13005 50 50 25 1.145 19.28 77 10 76 26 4 9889 3 375 12 5 5 0 62 5 3 143 23.21 37 14 40 25 2 5122 2 940 25 0 50 125 3.051 48.73 38 98 63 15 1 0084 15837 50 50 25 0.999 2 0 . w 80 02 74 32 5 w35 4 001 12 5 5 0 62 5 1.362 45.48 72 77 71 41 2 4966 13377 25 0 50 125 3.215 44.62 35 69 33 38 0 9964 13 927 50 50 25 1.054 19.73 7 8 92 82 36 4 9953 3 746 12 5 5 0 62 5 1.102 48.72 77 96 78 42 2 5080 17627 25 0 50 125 2.842 53.95 43 16 42 58 1 w g g 18 795 50 50 25 1.381 18.09 72 37 79 02 4 9910 2 625 0 12 5 5 0 62 5 1.199 47.51 76 02 76 49 2 5308 15658 25 0 50 125 3.134 46.65 37 32 3 9 85 0 9940 14 976 50 50 25 0.625 21.88 87 51 87 26 4 9699 7 019 12 5 5 0 62 5 1.071 49.11 78 58 80 29 2 5174 18218 25 0 50 125 3.314 42.16 33 73 33 73 0 9859 12 934 Adsorption EquilibriumPlot -__ 10 20 30 40 50 4 Equi(lDr(urnT h e . h m Study E00-1311 Sample Data Flle n w mn HllWS3 D HlilWlO D H1K1077 0 HdI0081 D HIKIIM D HlllO111D n1011ll D HdlD12.5 D W17.15~049 l001213-CW moi2ts-o~~ 1001215_070 1001215-077 lCOl213-081 1001215-MM 1001215_095 1001215-117 1001215-124 lCO1215-128 1001215-135 1W1215-142 iC"J1215-149 I001215_1% h) 0 N 0 w Adsorption % Charts BACK TO MAIN 4 1 0 125 0 250 2 50 2 125 2 250 4 50 4 125 4 250 8 50 8 125 8 250 16 50 16 125 16 250 24 50 24 125 24 250 36 50 36 125 36 250 48 50 48 125 48 250 f f =i -r 1 :I i I X bj $3 i$ ;; -BvE rt 5- E rae;g; %E, ;$ 6 ; : iif 2;. 1219 0.. E$ ;E I_ P J i 51 IEP 18.91 50 62.5 4430 7 13 5.0 125 4286 1785 5.0 25 0 859 20 71 8283 8512 5.0 62.5 2 687 28 91 4626 4349 5.0 125 < 250 >59 30 ,95% 2687 5.0 25 0 804 20 98 8391 8559 5 0 625 2469 31 54 5062 51 01 5 0 125 3742 31 45 2516 2511 5 0 25 0 930 2035 8141 8142 5 0 625 2 338 3327 5323 3988 50 125 3416 39 59 3167 3302 50 25 0808 2096 8383 7369 50 625 2 685 2894 4630 4773 50 125 3382 4045 3236 5007 5 0 25 0574 22 13 8851 8896 50 625 2373 3283 5253 5415 5 0 125 3208 4479 3583 3466 50 25 0804 2098 8393 8568 50 62.5 2 129 35 89 5743 5499 5.0 125 3 180 45 49 3839 3269 50 25 0604 21 98 8793 8937 50 625 2374 3282 5252 5781 5.0 125 3 689 32 77 2622 3200 1.0199 4.9805 2.5095 1.0170 5.0081 2.5012 1.0434 4.9924 2.5067 1.0303 4.9916 2.5048 1.0168 4.9096 2.4987 1.0196 4.9766 2.4922 1.0315 5.W37 2.4954 1.032 4.085 4.842 4.288 m236 5.208 5.123 8.054 4385 5.676 11.247 5.194 4.303 11.761 7.721 5.536 13.693 5.246 6.765 13.866 7.277 5540 8.556 1w00 z 9000 g 8000 4000 3000 r' 20 00 tow t OW -low __ Adsorption Equilibrium Plot +1 5 Ratlo (sedtment) EqulllbriumTlme, h o u n Paw 2 Of 2 BACK TO MAIN Study E00-1311 Mass Balance Calculation PFOS AdsorblDesorb Tier I "Mass Balance Calculations" Sample Data Fi Sample Description ~001211-093 lox E00-1311-3094-S1.5.0mg/L.48hr. 1:lClay. 12/07/w sW~l2ll-094 l o x EW-13113095Sl. 5.OmgiL.48hr. 1:lClay. 12X71W ~001211-095 10xE00-13113096~1.5.0mgA48hr. 1:lClay. 12/07/w sW1211~100 lox E00-1311-3097S1,5Om~A..48hr,1'5Clay. 12/07Mo ~001211~101 l o x EW-13113098-S1,50mgll, 4&r, l:5Clay. 12/07/00 ~001211~102 sW1211-104 ~001211~108 lox E00-1311-3099S1.5.0mgA. 48hr, l:5Clay. 12/07/w 10xE00-1311-3100-S1,50mgiL.48hr. 1'25Clay. 12/07/00 lox E00-13113101-S1,5.0mgA4, &r, 1:ZSClay. 12107nO ~001211~109 t001215~141 1001215-142 1001215~143 001215-148 1001215-149 lox E00-1311-3102S1.5.Omgll.48hr.1:ZXlay. 12R7xx) l o x EW-13113168~1.5.0mgll.48hr1. : l Sediment. 12/07/00 lox E00-1311-3167S1.5.omgll.48hr. 1:l Sediment. 12/07/w 10xEW-13113168-S1,50mgll. 48hr. 1'1 Sedimenl, 12/07/00 lox EW-1311-3169Sl. 50mph. 48hr. 1:s Sediment 12/07/w l o x Em-13113170.S1.5 OmgA.48hr. 1'5 Sedimenl. 1ZD7/00 1001215-150 1001215~152 001215-156 lox E00-1311-3171S1,5.0mg5,46hr, 1:SSedimenl 12/07/w lox EW-13113172Sl. 5 Om@. 48hr. 125 Sediment 12/07100 lox E00-13113173Sl. 5.0mgR.48hr. 1:25Sediment.12/07/00 t001215-157 lox EW-1311-3174-Sl.5.0mgll.48hr. 1:25 Sediment. 12/07/00 Soil Type Clay clay Clay Clay Clay Clay Clay Clay Clay Sedimenl Sediment Sedimenl Sediment Sedlmenl Sediment Sed~ment Sediment Sediment SoikSolu tion Ratio I:< 1:1 1:l 15 13 1:s 1:25 1:25 1:25 1:l 1:l 1:l 1:s 1:5 1:s 1:25 125 1:25 Observed Solution Concentration, ug/L Final Volume of (measured x dilution Solvent added, factor) ml 591.40 9.0 624.60 9.0 694.80 9.0 929 M 6.0 1070.90 6.0 956.00 6.0 3015 60 6.0 3313.70 60 3610.50 6.0 686.40 9.0 603.70 9.0 304.80 9.0 1987.90 6.0 2374.20 6.0 1965.90 60 3044.40 6.0 3689.20 6.0 3468 80 6.0 Dilution Factor Measured Concentration, ug!L (from Instrument) 10 95 26 10 112.93 10 159.53 10 163.56 10 147.93 10 'Tube Bmke 10 476.98 10 520 09 10 501.18 10 83.19 10 100.14 10 51.56 10 166.19 10 324.9 10 21045 10 265.72 10 282 72 10 285.76 Solution Concentration, uglL (measured x dilution factor) Volume Of CaCI, Solution, L 953.6 1129.3 1595 3 16356 1479.3 O.W.50 0.0050 0.00% 0.01250 001250 4769.8 5200.9 5011.8 0.01250 0 0250 0 0250 0.0250 831.9 1001.4 515.6 1861.9 3249 2104.5 2657.2 2827.2 2857.6 0 0050 0.0050 0 0050 0.012% 0.01250 0.012% 0.0250 0.0250 0.0250 Volume of Total Test Substance Methanol Solution, L Recovery, % 0.m0 46.16 0.0090 0 ow0 53.15 71.33 o.offi0 O.Oo60 0o m O.Oo60 34.28 35.62 83 21 00530 0 offio 91 24 86.27 0.0090 43.68 0 0090 48.12 0.m 24.66 0 0060 0.0060 0.w60 0.0060 57.63 78 67 59.52 73.64 0.0060 0.0060 87.35 83.05 N w 0 Page 1 of 1 Study EW-1311 Desorb Soken! BACK TO MAIN Page 1 of 1 s3mI- b 0 .) BACK TO MAIN Study EM)-t311 Adxlrpbon Kfnebu Tier II: "AdsorptionKinetics,One Concentration" m e 1) to be ploned YI *me ltalculationof dbrtribulm CoemloentK, r(010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 HO10222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 H010222 do10222 H010222 n L L 0 0 4 7 1311.4007-51 HILLWE D 13114008-SI HILL0051 D 1311-4004s1 HILL0053 D 1311-401DS1 HILL0054 D 1311-4011-S1 HILL0055 D 1311-4012-SI HILLW57 D 13114013-S1 HILL0058 D 13114014-51 HILLW59 D 1311-4015S1 HlLLW65 D 1311-401641 HILL0088 D 1311-4017-S1 HILL0087 D 1311-4015S1 HILLW69D 13114019-Sl HILL0070 D 1311-402DS1 HILL0071D 1311-4021-51 HILL0073 D 1311-4022-Sl HI-74 D 1311-4023-S1 HILL0079 D 1311-4024-81 HILL0081D 13114025-51 HILL0082D 1311-402&SI HILL0083 D 1311-4027.Sl HILL0065 0 1311-4025Sl HILLWWD 1311-4D20Sl HILL0067 D 1311-4030-SI 0 00125 625 512 10 0 00125 625 552 10 551.79408 NIA NIA 0 0 0125 500.0 6.25 880 10 660.1895 NIA NIA 2 00125 M O O 6.25 52.8 10 527.68578 NIA NIA 2 0 0125 M O O 025 52.4 10 524 20804 NIA NIA 2 00125 5000 6 2 5 50.9 10 508.900oB NIA NIA 4 0 0125 5000 6 2 5 51.1 10 511.32918 NIA NIA 4 0 0125 5000 625 52.4 I O 523 53991 NIA NIA 4 0 0125 M O O 025 52.6 10 525.56529 NIA NIA 8 00125 5000 625 51.9 10 51862455 NIA NIA a 00125 5000 625 50.2 10 501 60536 NIA NIA 8 00125 5000 625 51.4 10 514.16988 NIA NIA 16 00125 M O O 625 49.0 10 490.01757 NIA NIA 16 00125 5.300 625 50.7 10 507 11023 NIA NIA 16 00125 M O O 625 50.2 10 502.12373 NIA NIA 24 00125 5000 625 55.8 10 557.78725 NIA NIA 24 00125 5000 625 49.3 10 492.73887 NIA NIA 24 00125 5000 625 52.2 10 521.8MM2 NIA NIA 36 00125 M O O 6 2 5 52.0 10 519 77988 NIA NIA 36 00125 5000 6 2 5 497 10 498.81929 NIA NIA 38 00125 M O O 625 522 10 522.22917 NIA NIA 48 00125 5000 625 505 10 505 05482 NIA NIA 40 00125 5000 625 53.4 10 53439476 NIA NIA 48 00125 5000 825 510 10 509.70915 NIA NIA NIA Nons NIA None NIA None NIA NIA None NIA None NIA None NIA NIA NMe NIA None NIA NMB NIA NIA NOM NIA None NIA Nons NIA NIA Nons NIA None NIA None NIA NIA None NIA None NIA None NIA NIA None NIA None NIA Nom MIA NIA None MIA None NIA PFOS AdroIbDexllb - K, : 2 /14 1 f-%e a i; NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA NIA Page 1 of 7 BACK TO MAIN Study 00-1311 Adrorpbon ffinetus PFOS AdSoMDerorb H010222 HILL0102 D 13114038-51 0 H010222 HILL0107D 1311403SS1 0 H010222 HILL0109 D 13114040-51 2 H010222 HILL0110D 13114041Sl 2 H010222 HILL0111 D 1311404241 2 H010222 HILL0113 D 13114043.51 4 H010222 HILL0114 D 13114046S1 4 H010222 HILLO115D 1311-4045-51 4 H010222 HILL0121D 13114045S1 8 H010222 HILL0122 D 13114047-Si 8 H010222 HILL0123 D 1311404&51 8 HO10222 HILL0125 D 13114049-Sl 16 H010222 HILL0126 D 13114050.S1 16 H010222 HILL0127 D 13114051-Sl 16 R010222 RUSH0037 D 13114052Sl 24 R010222 RUSH0038 D 1311405341 24 R010222 RUSHW39 D 1311454-51 24 R010222 RUSHOM1 D 1311-4055S1 36 R010222 RUSH0042D 1311405ES1 36 RO10222 RUSHOM3D 311-4057-S1(Pointlhmrm our 36 R010222 RUSH0045 D 1311-4055S1 48 R010222 RUSH0048 D 13114M9Si 40 R010222 RUSH0051 D 1311-406081 48 -V. - C. I 2 r P i ii f i i 1E E j i : 8 j t c 1 LIL. 00125 5000 6 2 5 0 0125 500 0 6 25 0 0125 SWO 6 25 00125 m o o 6 25 0 0125 M o o 6 25 0 0125 Moo 6 25 0 0125 M o o 6 25 0 0125 500 0 6 25 0.0125 500 0 6 25 0.0125 5WO 6 25 0.0125 5030 6 25 0 0125 5W 0 6 25 0 0125 MO 0 6 25 0 0125 5WO 6 25 0 0125 Moo 6 25 0 0125 5WO 6 25 0 0125 Moo 6 25 00125 500 0 6 25 0 0125 500 0 6 25 0 0125 500 0 6 25 0 0125 5000 6 25 0 0125 S W O 6 25 0 0125 5W 0 6 25 0 0125 500 0 8 25 ICalculation of dlstnbuUOn Coemoent. K. 366 33.0 28.9 11 7 10.4 11.3 11.5 9.9 10.2 13.6 11.2 12.9 9.5 87 10 4 11 3 10 1 1I 3 89 (18 o* 113 10.4 105 10 36577631 1677786125 2684474 10 33010608 2122924 33.96678 34.36 10 288.72178 2.64097775 42.25584 10 117.05089 4.766863875 76.58982 10 104.31161 4.948104875 79 13768 7772 10 112.87498 4.83406275 77.425 10 114.51078 4.81861525 77.09784 10 9828349 5.014206375 60.2273 79.W 10 101 64917 4.979385375 79.67017 10 135.62296 4.554713 72.87541 10 111.91357 4 851080375 ~1.61729 7486 10 129.49094 4.63136325 74.10181 10 9480544 5.064932 81.03891 10 86.89825 5.163771875 82.62035 8098 10 103 55901 4.955512375 79.2882 10 112.90206 4.83872425 77 41959 10 100.99263 4.987592125 79.80147 7817 10 113.48309 4.831461375 77 30338 10 89.29487 5.133814125 82.14103 10 87.70241 5.153719675 82.45952 8230 2Q a a 3 a 3 w a ~ o u D z D B 10 113.11806 483604925 77.37679 10 104 46575 4.944178125 79.10885 78.51 10 104.74724 4.9406595 79.05055 24919 24894 2.5035 2 4842 2.4873 2.5199 2 4914 2.4945 2.4971 2.4871 24893 2 4899 2 4967 24909 2 4868 2 4938 25087 2 4894 2 5097 25090 14914 24057 2 5228 24930 0 W2582898 0 00365374 0016462273 0 019063494 0017012975 0016890108 0020332124 0019617152 0013503133 0017413196 0 014364402 002139804 0023656115 0019243973 0017187085 0 019685775 0017102227 0 022908245 0 023421172 aJace%w 0017199516 0 018761883 0018919953 w e s t ounier 0 016293737 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2 60% 2.60% 2.60% 2.60% a.6~ 2 60% 2.60% 2.60% 9 9342243 14 052845 63 316435 73321131 65434519 64 961953 78 200479 75 450586 51 935128 66 97383 55 247701 82 300155 91 75429 74 015262 66 104172 7571452 65 777797 88 108635 90 08143 66 152214 72.769051( Page 2 of 7 BACK TO MAIN Sluudy Em1311 Adsorption Kinetics PFOS AdsorblDasmb 5WO 625 500 0 625 R010222 RUSH0069D 1311407C-S1 2 0 0125 5000 625 R010222 RUSH0070D 13114071-51 2 0 0125 500 0 6 2 5 R010222 RUSH0071D 1311-4072.51 2 0 0125 5000 825 RO10222 RUSH0073D 1311-407%51 4 0 0125 5000 625 R010222 RUSH0074 D 1311-4074-51 4 0 0125 5000 6 2 5 R010222 RUSH0079D 1311407651 4 0 0125 5000 6 2 5 R010222 RUSH0081D 1311407551 8 0 0125 5000 6 2 5 R010222 RUSH0082D 13114077-Sl 8 0 0125 5000 6 2 5 R010222 RUSH0063D 1311-407as1 8 0 0125 5WO 825 R010222 RUSH0065D 1311407851 16 0 0125 500 0 6 2 5 R010222 RUSH0086D 13114080S1 16 0 0125 5000 6 2 5 R010222 RUSH0087D 114061-51(Point T h M out. 16 0 0125 500 0 625 R010222 RUSH0093D 1311-4082-51 24 00125 500 0 625 R010222 RUSH0094D 13114085S1 24 0 0125 5 W O 625 R010222 RUSHW95 D 13114084-Sl 24 0 0125 MO 0 625 R010222 RUSH0097D 13114086S1 36 0 0125 5000 6 2 5 R010222 RUSn0098D 13114086Sl 36 00125 500 0 625 ROl0222 RJSH0099D 11-4087-S1(Pant Thmwn O W . 36 0 0125 500 0 625 R010222 RUShOlOl D 1311408851 48 00125 5W 0 625 R010222 RUSHO1M.D 13114WS-Sl 48 00125 5W0 625 R010222 RUSH0107D 13114090-S1 48 00125 5000 625 K, L_ f 2 i 1 P g !e 1 1E L L A;$ A 25058 10 0001351513 k 198126 408 10 408 06493 1 149186375 16 3870' 26 91 24904 0 0 0 1 1 ~ 1 8 2 60% 1349301 2-55 10 26488843 2938894625 470223 2 5288 0 00436774 2 60% 16 87592 103 10 19279449 3840068875 614411 2 4966 0 007978026 2 60% 30 68471. 222 10 22239068 34701165 5552188 58 05 2 5099 0 00621688 260% 2391W91 21 I 10 21399507 3 57M81625 5720099 25022 0006676637 260% 2567937 101 10 200 94518 373818525 59 81096 2 4999 0 007441502 260% 2862116 208 10 20636687 3670414125 58 72683 59 63 2 4878 0 007149238 260% 2749706 1s5 10 195 19751 3810031125 eom05 2 5214 0 007741275 260% 2977413' 21s 10 21944298 3 50696275 56 1114 2 4999 0 006392737 26096 2458744' 213 10 21305622 358879725 5738876 58 74 24952 0008746948 260% 2594979 218 10 216 3487 3 54564125 56 73028 24921 00065782 2 60% 25 293071 181 10 180 50238 3 99372025 63 89952 24932 0008874371 260% 3413219 161 10 160 62727 3 989659125 83 a3455 63 87 25087 om794743 260% 3382593 y1 S4 u d J x 4 ' u ~ l L 1 p o u aa36"""1O""I'c a.ew.aAaa4Sl 1SS 10 19945437 3 756820375 60 10913 2 5006 0 007532387 260% 2897072 178 10 177 74809 4 026148875 E4 45038 62 92 2 5269 0 CO6968%9 260% 3449365 170 10 17900609 4 012423675 64 19878 2 5061 0 008944161 260% 34400691 155 10 15509654 431126825 6898029 25242 0011012187 2 60% 42 35456! 163 10 152 77563 4 215304625 67 44487 08 21 24981 0010386443 260% 3967095 8a.a 19 336.u6u-126Uz3 w a . w u a % w -Q-tesIder 260% 3U6Z97Z13S4l! 171 10 171 14436 4 1106955 65 77113 2 4967 0 00961255 171 10 17050029 4 118748375 6589994 65 01 25038 OW9848DB7 0 009716499 2 60% 37 107941 188 10 16824527 4 146924125 6535095 2 4910 0 W989488 2 60% 38 05723; d 0 w Page 3 of 7 BACK TO MAIN Study EW-1311 PFOS AdSOlb/DBMrb R010222 R010222 R010222 R010222 R010222 R010222 H010309 H010309 H010309 H010309 H010309 H010309 H010309 H010309 H010309 H010309 H010309 no10309 H0103W H010309 Ho10309 H010309 H010309 H010309 RUSH0121 D RUSH0122 D RUSH0123 D RUSH0125 D RUSH0126 D RUSH0127 D HILL0038 D HILLW37 D HILL0038 D HILL0040 D HILL0041 D HILL0042 D HILLW44 D HlLLW45 D HILL0050 D HILL0052 D HILL0053 D HILL0054 D HILL0056 D HILL0057 D HILL0058 D HILL0064 D HILL0065 D HILL0066 D 1311 4097 S1 1311 4098 S1 13114099-S1 1311-4100.Sl 13114101 S1 1311 4102-51 E0013114101Sl E00.13114104S1 EO013114105-S1 E00.131141CSSl E00-1311-4107-Sl E0013114108-S1 EW-13114109-Sl E001311-4110S1 E0013114111-S1 E00.13114112-S1 E00-13114113-Sl E0013114114-S1 EO0-1311-4115-Sl Em13114116-S1 EW-1311-411741 EW-13114118S1 E00.1311411BSl EW-13114120S I a L. 0 00125 5W 0 0 00125 500 0 625 112 10 0 00125 5W 0 625 313 10 313.08584 2.338427 37.38283 2 00125 5000 625 1 4 ~ 10 14754934 440563325 7049013 2 00125 5000 625 155 10 155 3989 4 30751375 68 92022 2 00125 5000 8 25 14 0 10 14039852 449-185 719203 4 00125 500 0 6 25 8 012285 10 8012285 52484b4375 8397543 4 00125 500 0 6 25 8 1696 10 81 696 54780 876806 4 00125 500 0 6 25 8 375534 10 83 75534 5 20305825 83 24893 8 00125 500 0 6 25 11 534113 10 11534113 4808235875 7893177 8 00125 5W 0 6 25 11512441 10 11512441 4810944875 76 97512 8 00125 5000 8 25 10 789985 10 10769985 4901251875 7642003 16 00125 500 0 6 25 5 573715 10 5573715 5553285625 8885257 18 00125 M O O 8 25 5 956354 10 5956354 550545575 8808729 18 00125 M O O 6 25 5468121 10 54 88121 5 566484875 89 03376 24 00125 5W0 6 25 5 848499 10 5848499 5543937625 88703 24 00125 500 0 6 25 5 788465 10 5788465 5526441875 8842307 24 00125 BO 0 6 25 7 103971 10 71M971 5362003625 8579208 36 00125 500 0 6 25 5 890369 10 5890369 5513703875 8821926 36 00125 M O O 6 25 6 081278 10 8081276 54898405 8783745 36 00125 5W 0 6 25 5 518164 10 5516184 55604795 8896767 48 00125 M O O 625 6353969 10 8353969 5455753875 8729208 48 00125 5 W O 625 6139254 10 61 39234 548259575 6772153 48 00125 M O O 625 6088331 10 6068331 5491458625 8780334 51 25 7044 8496 7744 8867 87.54 88.34 8783 c P i 25x2 24849 2.4887 2 4927 24999 2 4857 24917 24963 2 5085 2 4875 24927 2 4906 2 5083 25139 2 4928 2 4966 2.5180 2.4911 2.5065 2.5096 2 4936 25084 25358 2 4820 0 007119182 0 os839883 0 0029985e-l 0011978482 0 011080073 001268013 0 026289368 0035573915 0 024784404 0 016758628 0 01678459 0018238209 0039721512 0 036787557 0 040840432 000339739163304151 0 030299451 0 037345068 0035971662 0 040424838 0034230472 003521738 0 036460001 - %cc - - Kr s d 5 I I i - i; eF jl 2 80% 2 80% 2 80% 280% 280% 280% 280% 2 80% 2 80% 2 80% 2 80% 2 80% 28wb 2 80% 2 80% 2 80% 2 80% 2 80% 2 80% 2 80% 2.80% 2 80% 0035302818 280% 260% : 2 ii! '5 42564! 4 428541 0 70922: 4278022 3S60026; 46WO4C 9304059: 127 0497 88 51572; 59 85224: 59 67353; 65 13646: 141 8623 131 3127 145 8586: 140 40361 135.4155; 108.2123: 133.37522 128.4702: 144 37442 122 2516s 1257763C 13021425 Page 4 of 7 Study EW-1311 LG, Adsorption Kineuw Icablauon of Aa (adrophon % at m e I)to be proned ys bme E. f3 BACK TO MAIN atculation of dishbution I =F== -Run R010314 13114127-S1 0 R010314 wsnc&wa 3ii-4128-Sl pantthmwnout"' 0 R010314 RUSH0045 D 1311-4129-51 0 R010314 RUSH0047.D 13114130-S1 2 R010314 RUSHW48.D 13114131-S1 2 R010314 RUSH0049.D 13114132-S1 2 R010314 RUSHW51.D 1311-4133-Sl 4 RO10314 RUSHW52.D 13114134-S1 4 R010314 RUSHW53.D 1311-4135-Sl 4 R010314 11-4138-51Pointthrownour" 8 R010314 RUSH0060D 13114137-51 8 R010314 RUSH0061 D 1311-4138-51 8 R010314 RUSHOW3 D 13114139-S1 16 R010314 R U S H W D 13114140-Sl 16 R010314 RUSH0065 D 13114141-51 18 R010314 RUSH0067 D 13114142-51 24 R010314 RUSH0068 D 1311-4143-51 24 R010314 RUSH0073 D 1311-4144-S1 24 R010314 RUSH0075 D 1311-4145.51 36 R010314 RUSHW76.D 1311-414681 36 R010314 RUSHW77.D 13114147-51 36 R010314 RUSH0079 D 1311-4148-51 48 R010314 RUSHW8O D 13114149-Sl 48 R010314 RUSH0081.D 13114150-Sl 48 00125 5000 825 00125 5 0 0 0 625 00125 5000 625 00125 5000 625 00125 M O O 625 00125 5000 6 2 5 00125 5W 0 625 00125 5000 625 00125 Moo 625 00125 500.0 6.25 0 0125 5 W . O 6.25 0 0125 500.0 6.25 0 0125 5w.o 6.25 0 0125 5wo 8.25 0 0125 5w.o 6 2 5 0 0125 500.0 8.25 0 0125 5w.o 6.25 0 0125 m.0 6 2 5 0 0125 5w.o 8.25 0 0125 5w.o 825 0 0125 500.0 6 2 5 0 0125 Mo.0 625 0.0125 5W.0 6.25 0.0125 Mo.0 6.25 370 4&a 273 243 21 9 250 225 233 237 4 22.8 23.2 20.7 20.4 21.0 204 21.3 20.7 195 192 190 201 20.0 20.2 10 10 -ZA80?4 10 27304294 283696325 4539141 10 243429 32071375 513142 10 21925888 3509264 5814822 10 24969091 3128863625 5006182 10 2248773 343903375 5502454 10 23320361 3334954875 5335928 10 23739043 3282519625 5252031 10 NIA NIA NIA 10 226.30806 3.39617425 54.33879 10 232.11374 3 34857825 53.57725 10 208.68992 3.668376 58.68202 10 203.85975 3.701753125 59.22805 10 209.76708 3 6279115 58.04858 10 204.22624 3.697172 59.15475 10 212.60589 3.592428875 57 47886 10 207.00305 3.682461875 58.59939 10 194.89952 3 813756 61 0201 10 19210652 38486685 61 5787 10 18995595 3875550625 8200681 10 201 23399 3 734575125 59 7532 10 2W.41683 3.744789325 5991663 10 201.72713 3.728410875 59.65457 3571 5251 5363 53.90 58.65 58.41 61.54 59.77 2526 25013 2 5058 25186 2 5W5 25058 25178 2 4991 2.5063 2.503 2.5161 2.5031 2.502 2.5051 2.5093 2.5228 2.4993 2.5021 25W7 2.5137 2.5048 2.5018 2.5064 0004153909 0 005258157 0006359818 0005011377 0006108378 000587958 0 W5532811 NIA 0.005943081 0.005733657 0.W7006628 0.007257527 O.OW903097 0 037214488 O.OW697774 0.007079099 0 007820553 0.00601137 0 008116468 0.W7409123 0.W7468825 0.W7374101 -No internalstandad 0.W7417263 1 30% 130% 130% 1 30% 130% 1 30% 1 30% 1 30% 1 30% 130% 13wb 130% 1 30% 130% 1 30% 130% 130% 1 30% 130% 1.30% 48 92167, 3854905 4698752 43 889071 42560081 NIA 45 71601 44 10505: 54 5125oj 55 82713' 53 106891 55 49606: 51 521333 54 454601 60 158101 81 62592t 62 434361 56 9932% 57.450961 56.723652 N 0 W Page 5 of 7 Study E001311 Adsorpbon ffinebcd t 7 - )CalculabonofA. (adrorptlon% a1bmeI) to be platfed vs f!m BACK TO MAIN ICaluJlabonof dislnbutlon Coement K. 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79.05055 Page 1 or6 00-1311 Tier 111: "DesorDtion Kinetics, One C BACK TO MAIN 9 ca H010309 HILL01ffi.D EOC-I~I-~OZCSJ NIA 10390455 2 HOlO309 HILLO136.D ~ ~ 1 3 1 1 4 0 2 a ~ 4 NIA 12302109 2 R010309 RUSHM57.D 1311-4028-S5 NIA 103 2 R010309 RUSH0093D 1311-402856 NIA 99 2 R010309 RUSH0135 D 1311402ES7 NIA 99 2 H010311 HILL0053.D EW-1311-4028-SB NIA 123 2 H010309 HILL0072.0 EOU131143C-S2 NIA ?07587S6 2 HOlO309 HILLOlO7.D EW-13114030.53 NIA 10082186 2 HOl03W HILL0137.0 EO0.131140M-S4 NIA 83CQM 2 R010309 RUSHW58.D 1311403O-S5 NIA 62 2 ROlO309 RUSH0094.D 1311-403as6 NIA 94 2 R010309 RUSH0136.D 1311-403CJ.87 NIA 104 2 no10311 H I L L W ~ ~ D EO@-1311.4030.S8 hlA 104 2 ~010309 H~LLWBOD ~ w n i i ~ 0 5 a s z 24157 9632074 2 rlOlM09 HIlLOllOD EW13114058-SJ 24857 3728289 2 R010309 RUShOO38D 1311-4058-S4 2487 96 2 R010309 RUSH006SD 1311405ES5 2.4857 27 1 2 R010309 RUSH0100 D 1311405ES6 2.4857 29 8 2 R010309 RUSH0140D 1311-4058S7 2 4857 27 7 2 H010311 HlLLWB9 D EO@-13114058.58 2 4857 29 8 2 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0 0125 < 2 m 2 20.0 0 0125 z. 2.08 2 < 20.0 00125 < 2.08 2 <zoo 0 0125 2.08 10.237 NIA c 0.237 NIA c 0.237 NIA c 0 237 NIA NIA NIA 2 z. 20.0 0 0125 `2.08 0.235 < 0.237 2 <zoo 00125 <206 c 0.235 0 237 2 c 20.0 D 0125 i2.08 c 0.235 < 0.237 3000 0 2000 1000 OW 0 20 40 60 Time. hours RO10404ed RUSHW61 D 13114179-15 2.4837 GI00 2 e 2 0 0 0 0125 5206 < 0.235 c0237 RO104MMax1 R U S W 8 D 13114179-56 2.4837 <loo 2 c 20.0 00125 < 2.08 ROlMMed RUSH0079D 13114179-57 2.4837 `100 2 <20.0 0 0125 < 2.08 R010404ed R0104048d RUSHWW D RUSH0037 D 13114179SB 1311418O-SZ 2 4m37 2.5205 `100 <loo 2 c 20.0 00125 C 2.08 2 <zoo 0 0125 C 2 0 8 ROlMMcxt RUSHOM7D 1311418D-S3 2 5205 ~100 2 < 20.0 00125 2.08 1311-4180-54 2.5205 tuhbblkm 2 NIA 0 0125 NIA R0104Mexl RUSH0052 D 131i 4 i 8 a s 5 2 5205 `100 2 < 20.0 00125 c 2.08 - I ROlMMsxt R010404sd RUSH0059 D RUSH0080 D 13114180-55 1311-4180-S7 2.5205 2.5205 `100 .=loo 2 c M.0 00125 c 2.08 2 < z o o 0 0125 C 2.08 RUSHW91 D 13114180.S8 2 5205 <loo 2 < 20.0 00125 c 2.08 ~0.237 NIA Page 6 of 8 Study EW-1311 Tier 111: "AdsorptionlDssorption Isotherms" I r- BACK TO MAIN =F H010311 H010311 H010311 H010311 H010311 H010311 H010311 H010311 HOl03ll HOlO3ll H010311 ROlMMa ROlMO2a R010402a H010311 H010311 ti010311 R010329s R010329a R010329a R010329s R010329a R010329a R010329a R010329a R010329a R010329a R010329a RO10329a HILL0105 D HILLOl07D HILL01090 HILL0110 D HILL0111 D HILL0113 D HILL0114 D HILLOll5D HILL0121 D HILL0122 D HILL0123 D RUSHW37 D RUSH0038 0 RUSHW39 D HILL0137D HILL0138 D HILL0139 D RUSHW37 D RUSH0038 D RUSHW39 D RUSHW41 D RUSH0042 D RUSHOM3 D RUSH0049 D RUSHOOM D RUSHW51 D RUSHWSJ D RUSHW54 D RUSH0055 D EW-1311-5W5 EW-1311 5wB 00-1311-5007 EM-1311 5008 EW-1311-5DW EW-1311 5410 E00-1311 5011 EOD.1311-5012 EO0 1311-5013 EO0-1311-5014 EOD.1311-5015 1311-5016 1311-5017 1311 5016 EW-13115022 00-1311-5023 EW-1311-5024 1311 5025 1311-5026 1311-5027 1311 5028 1311 5029 1311-5030 1311-5031 1311-5032 111 1-5033 1311 5034 1311-5035 1311-5036 Mo 5W 2wO 2wO 2wO 5w0 5wO 5w0 1wM) 1WW 1wW 5wW 5WW 50WO 5w 5W 5W 2wO 20% 2000 5000 5LW SOW lOW0 lOOW ww 50OW MWO 5woO 1975 1985 2532 1839 1695 4357 4035 4056 1027 1100 1029 69243301 63 879261 6431529 1868 1931 2003 15993 15292 14326 39137 23009 387 34 8281 8511 e~3s 4M55 41416 43398 2 2 10 10 10 10 10 10 100 1W 100 1WO 1000 1OW 2 2 2 IO 10 10 10 10 10 1W 1W iw 100 1W 1W 9505281 259665516 50 9862% 2 59877552 532 17072 340349298 339 44725 3 26468734 S95 33729 322925611 357 28356 3 63921582 133 37088 3 60566816 rn565759 3 6 ~ 1 3 0 8 12700043 401157053 19903071 4 MI24688 1288 8621 4 01236735 9243 301 4 84037776 3679261 4 80535988 X31529 480831423 7365555 2 57247144 386188014 258679879 400617808 260273025 15983353 320393952 152915715 318445212 143264531 3 15613868 391370145 359258769 230094744 33619067 3873 38636 3 58809082 82813209 391809961 85108829 392997359 80378359 ~905i3914 4045491 460697124 414163251 461717156 433978954 463746867 NIA NIA DO125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 0 0125 NIA NIA NIA 00125 NIA NIA NIA 0 0125 NIA NIA NIA 00125 NIA NIA NIA 0 0125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 00125 NIA NIA NIA 0 0125 NIA WA NIA 00125 NIA NIA --- NIA 00125 NIA NIA NIA o w 5 NIA NIA NIA 00125 NIA NIA Page 1 01 16 Adsorptbn Adsorption Isotherms BACK TO MAIN R010329a R010329s R010329a R010329s R010329a R010329. R010329a R010329a R010329a R010329a R010329a R010329a R010329a R010329a R010329a R010329b R010329b R010329b R010329b R010329b R010329b RO10329b R010329b R010329b R010329b RUSHW66 D RUSHW67.D RUSHW69.D RUSHOO7O.D RUSHW7l.D RUSHW77.D RUSHW78 D RUSH0079 D RUSHW8l.D RUSHW62.D RUSHW63.D RUSHW85.D RUSHOO9O.D RUSH0091 D RUSH0097 D RUSHW98 D RUSHW99 D RUSH0121 D RUSH0122 D RUSH0123 D RUSH0125 D RUSH0126 D RUSH0127 D RUSH0129 D RUSH0134 D RUSH0135 D RUSH0137 D RUSH0138 D RUSH0139 D 1311-5041 1311-5042 1311-5043 1311-5M4Sl 1311-5045 1311-5046 1311-5047 1311-5048 1311-5049 1311-5050-18 1311-5051 1311-5052 1311-5053 1311-5054 1311-5058 1311-5059 1311-5060 1311-5061 1311-5062 1311-5063 1311-5oM 1311-5065 1311-5056 1311-5067 1311-5066 1311-5069 1311-5070 1311-5071 1311-5072 5w 500 ZWO 2WO 2WO 5000 5WO MM) 10000 10000 1WW 50000 50030 5mo 5w 5w 500 2Ow 2m 2000 Mw sow 5000 low0 two0 10000 5wM) 5m 50000 96 20 58.15 460.98 305.78 > 501 183.73 166.25 156.55 359.52 > 501 351.68 211.71 253.43 207.41 31 83 34.15 32.79 135.13 141.11 142.97 83.18 77.82 77 95 179.53 187.10 171.68 101 23 103.30 109 27 2 192 408928 2 116.296416 2 921.958724 2 611.563282 2 NIA 10 1837.31918 10 1882.52521 10 1565.51161 10 3595.21967 10 NIA 10 35165502 100 21170.5882 1 w 25342.8747 20741.2664 63.66312 68 302058 2 65 5635 2 270.25587 2 262 215634 2 285.940358 10 831.7632 10 778.17175 10 779.50456 10 1795.32634 10 1871.04255 10 171879339 1W 10122.5113 - 1 w 10329.5wB 1 w 10926.5554 2 29%781( 2.28422522 2.06556833 2 96471148 2.7-14 NIA 3.2M18461 3.22076824 3.19465629 3.55572543 NIA 3.54611682 4.32573292 4.40385588 431683527 1.80388792 1.83443379 1.81679459 2.43177514 2.45058107 2.45627548 2.92W1014 2.89107546 2.89161866 3.2541434 3.27208366 3.23471803 4.00528827 4.01407933 4.03848327 1.8183721 2 44621055 2.9W%809 3.253&4837 4.01928362 2.492 0.0125 1.542893 0.186336 2.4698 0.0125 1.926378 0284741 2 . 5 W 0.0125 5.380307 0.730807 2.5154 0.0125 6699682 0.838828 25162 0.0125 NIA NIA 2.4949 0 0125 15.84573 1.199912 2.5008 0.0125 16.68204 1.222249 2 521 0.0125 17.0294 1231199 2.4853 0.0125 32.21332 1.508035 2.5132 0.0125 NIA NIA 2.4976 0.0125 32.4484 1.511193 2.5007 0.0125 144.1067 2.158684 ---- 2 5287 2.5065 2.4926 0.0125 ~~ 00125 0.0125 121.8864 2.065955 1459143 2.164098 2.187284 0.339905 2.4897 0.0125 2.184972 0.339446 0 338176 2.5098 0.0125 2.163801 0.335177 2517 0.0125 8.590307 0.934W9 2.5023 0.0125 8.581027 0 933539 0,934025 2.4912 0.0125 8.6W572 0.934527 2.462 0.0125 20.99223 1.322059 2.5173 0.0125 20.96407 1.321476 1.322114 2.5088 0.0125 21 02846 1.322807 2.5042 0.0125 40.95458 1,612302 2.4816 0.0125 40.94615 1612213 1.614521 2.4892 0.0125 41.59573 1.619049 2 4672 0.0125 2W.4126 2.301927 ---- 2.5011 0.0125 198.2653 2 297247 2.296913 2 4959 0.0125 lS1.6862 2.291585 Page 2 of 16 Study EOC-1311 N N 0 BACK TO MAIN 0.3015M 0.889584 1.248259 1.558925 2.211593 S l u gEm1311 tG, Adsorption Irolhemu BACK TO MAIN IROl0312 R010312 R010312 R010312 R010312 ROlO312 RD10312 R010312 H01M05mt HOlM051nl H010405ml ROlM12 R01M12 R010412 RO10412 ROlM12 R010412 R01M12 R01M12 ROlM12 R010412 ROlM12 ROlMl2 R010412 ROlM12 R010412 R010412 RUSH0075.D RUSHW78D RUSHW78 D RUSH0079 D RUSH0080D R U S H WD RUSHDOB7D RUSHWE8 D HILL0059 D HlLLDOMl D HlLLOOBl D RUSH0032 D RUSH0033 D RUSHO0U.D RUSHW4O.D RUSHOM1 D RUSHOo46.D RUSHOM8 D RUSHOC(9.D RUSHW5O.D RUSH0052 D RUSHOD53.D RUSH0054 D RUSHW6C.D RUSH0ffil.D RUSHOffi2.D RUSHOOB4.D RUSHOffi5.D RUSH006B.D 1311-5113 1311-5114 1311-5115 1311-5116 1311-5117 1311-5118 1311-5119 1311-5120 1311-5121 1311-5122 1311-5123 1311-5124 1311-5125 1311-5126 1311-5130 1311-5131 1311-5132 1311-5133 1311-5134 1311-5135 1311-5136 1311-5137 1311-5138 1311-5139 1311-5140 1311-5141 1311-5142 1311-5143 1311-5144 1 0 124 789652 2 OS310896 f 3 A 5W 61 1 2 122.284228 208737065 2522 00125 1872104 027233 5W 66.1 2 132.259912 2.12142823 2 5138 0.0125 1.828607 0.26212 2wo 324.3 2 648 68341 2.81203279 2 5025 00125 6 749633 0.829293 2wo 337.1 2 674 288876 2 828846 2 4887 0.0125 6.858653 0.823386 2wo 303.4 2 806.715152 2 782984M 2 4952 0.0125 6.919826 0.843WS 5wo 2N.5 10 2005 16531 3 30215018 2 4949 0.0125 1500478 1.17623 5wo 177.7 10 1777,00509 3.24968867 2 4973 0.0125 16.1324 1 207699 5ow 1woo 2046 437.953211 10 2M6.33186 3.31097802 10 4379.53237 3.64142774 2 4971 0 0125 14.78549 1.169836 2 5098 0.0125 27.99261 1.447043 1WW 503.530248 10 5035 30248 3 10202556 2 5067 0.0125 24.75714 1.3937 l o w 0 423.310937 10 4233.70937 3.62672104 2 4949 0.0125 28 89039 1.460753 5WW 235.149545 100 23514 9548 437131414 2 4978 0.0125 132.5419 2.122353 - 5WW 5wW 5w 235.642534 230 BMY8 2 1 842783 -1W 23564.2534 4.37225368 1W 23080.4348 4.363243% 2 49685526 1.89622989 2 4892 2507 2.4862 0.0125 0.0125 0.0125 132.7522 2.123242 ~~ 134222 2 127824 2.26407 0.35469 5w 18.05711 2 36114276 1.55187891 1,65237912 25069 0.0125 2.313045 0.3M184 0.35713 5w 25.248348 2 50.4926% 1.70322856 2.4965 0.0125 2.250687 0352315 2wo 112.2340% 2 224.468112 2.35115485 2 4891 0.0125 8.916536 0.950196 Mw 133.554484 2 267.108968 2 42668847 2.40381289 2.4995 0.0125 8.6SS188 0.937828 0.940441 2000 135.817446 2 271.634892 2.43398556 2.5191 0.0125 8.578303 0.9333 5003 85.165w2 10 851.85002 2.93038314 2 . 4 9 ~ 1 0.0125 20.75985 1.317224 5wo 76.528101 10 785.28101 2.88382094 2.89787562 2.5107 0.0125 21.08336 132394 1.322587 5wo 75.760492 10 757.60492 2.87944279 2.4999 0.0125 21.21282 1.328598 (WOO 157.011945 10 1570.41946 3.1oM11567 2.5018 0.0125 42.12095 1.624498 10033 155.224502 10 155224502 3.19096028 3.19196961 25128 0.0125 4202361 1.623493 1.824959 ' lOOW 1Y5015M 10 1545.01564 3.18693288 2.4954 0.0125 42.35285 1626883 SOW0 109 207528 1W 10920.7528 4.03625258 24892 0.0125 195.244 2.2927% sow0 99.477125 1W 9947.7125 3.99772323 4.w6738 2.4837 0.0125 2015757 23M438 2300469 MWD 86.43578 1W W3.578 3.9842382 2.5M1 00125 201 4517 2304171 N !2 Page 4 of 16 BACK TO MAIN Sludy EW-1311 R010412 R010412 R01M12 R010412 R010412 R010412 I7010412 RO10412 H010405ml H010405ml H010405ml H010329 H010329 H010329 HOIO329 H010329 H010329 H010329 H010329 H010329 H010329 H010329 H010329 H010329 H010329 H010329 H010329 RUSH0077 D RUSH0078D RUSHW84 D RUSH0085 D RUSH0088 D RUSH0086 D RUSH0089 D RUSH00900 HILLW63 D HILL0064 D HILLW65 D HILLOlMD HIL~~~ L01.0.5D~ HILLQI06.D HILLO116.D HILL0117.D HILLO118.D HILL0120.D HILLOl21.D HILL0122.D HILLO124.D HlU0129.D HILL0130.D HILL0132D HILL0133 D HILLO134.D HILLO136.D HILLO14I.D HlLL0142.D 1311-5149 1311-5150 1311-5151 1311-5152 1311-5153 1311.5154 1311-5155 1311-5156 1311-5157 1311-5158 1311-5159 1311-5160 1311-5161 1311.5162 1311-5166 13114167 1311-5168 13114169 1311-5170 1311-5171 1311-5172 1311-5173 1311-5174 1311-5175 1311-5176 1311-5177 1311-5176 13114179 1311-5180 '1I?dTnz 104604 500 500 2m 2000 20w 5w0 5000 50W 1o m lorn 1 om 50000 50w0 5ww 500 m 530 2w0 2000 2w0 50w 50W 5w0 10000 10w0 10w0 50000 50000 5w00 90.0833% 2 180.166796 152.507688 2 305.015776 470.275971 2 940.551942 481.768175 2 483.53635 461.55zms 2 923 10557 259.294489 10 2592.94489 273.244W 10 2732.44648 260.405148 10 2804.05118 58.237271 100 5623.7274 86 08401 1 w 8606.401 87 843583 1W 8784 3553 269.0021M 1W 28900.2164 - 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100 6272.7361 1W 64M.9464 1.847206W3 1.868763026 4 52E40225 l.MOM5678 4.74854221 2.405175476 16.9354277 2.401634428 2.4132936% 17.4863271 2.433071163 17.6696256 2 82566938 39.9532215 2.616095465 2.62561949 41 6449404 2.835W5625 41.8259395 3 0656M765 76.7442264 3.104M1W92 3 105435562 60.2732144 3.12590463 60.115345 3831301827 165 079747 3.797457017 3.651545057 373.362359 3 - 925676326 369 866401 0.65575315 0.6765w3 1.27729005 1.2426988 1.24722735 1.6015516 161956225 1.6214457 189621673 1.9M57065 190371571 2.5635757 2.57213053 2.566M488 0.66527269 1.25574133 1.61416658 1.8015017 2.56791704 Paps 11Of 16 S W EO01311 tG, h BACK TO MAIN 1311-5131 1311-5132 1311-5133 1311-5134 1311-5135 1311-5136 1311-5137 1311-5138 1311-5139 1311-5140 1311-5141 1311-5142 1311-5143 1311-5144 lubeb m b R010402s ROlMOZs R010402a R010402a R010402a R010402a R010402a R010402s R010402a R010402a ROlMOZa RO10402s ROlMZa RUSHW7O.D RUSH0076 D RUSHW77.D RUSHW78.D RUSH0080 D RUSHOO8l.D RUSHOO82.D RUSHOO64.D RUSHW8S.D RUSHW9O.D RUSH0092.D RUSH0093.D RUSHOW4.D 26.89W3 107.113316 111.287815 108.223884 289.673014 249.672867 276.014812 105377362 114.123143 103.239784 491 927102 509 061312 513 WlM5 0 NIA 1.727265272 NIA NIA 0.72885081 53.38wS 1727379058 5.35156682 0.72848095 214.226632 2 33087346 21 1183248 1.32465947 2 m i w 2.3474n6ii 2.3moicai 20.~80371iai27703( 1.31674988 212.447768 2.327252173 20.550379 1312819M 579 746028 2.76mn82 48.9%4753 1.68975691 2 499 345734 2.698401344 2.734533837 50.4478992 1.70284309 1 69796871 2 552 029624 2.741862364 50.26968 1.70130612 10 1053.77362 3.022741322 100.104259 2.WM5255 10 1141.23143 3057373724 3031322711 99.9198468 1.99965176 2.W077455 10 1032.39784 3.013847087 100 5158 2.00223433 10 4919.27102 3.69190075 463.787518 2.66831908 10 5090.61312 3.708T1W92 3.70293156 475.033485 2 67672422 2.87441332 10 5130.07645 3.710123837 478 846891 2.68019667 Page 12 of 16 StUdv EW-1311 LG, BACK TO MAIN 1311-5180 R010402b RUSH0142 D 1091215 100 7091 215 3850720653 254 718956 2 56195595 N 0 0 Page 13of 16 StWEW-1311 BACK TO MAIN PFOS Adosl.blOarorb c=- 1311-5203 1311-5204 1311-5205 1311-5206 1311-5207 1311-5208 1311-5209 1311-5210 1311-5211 1311-5212 1311-5213 1311-5214 1311-5215 1311-5216 ROlMOZb R010402b R010402b ROlMOZb H010402s HO10402s HOlMO2a HOlMOZa H010402a HOlMOZa H010402a H010402a H010402a H010402a RUSH0153 D RUSH0154.D RUSH0158.D RUSH0157.D HIlL0032.D HILL00340 HIlLOO35.D HIU00J6.D HILLW38.D HlLLW39D HlLLW4O D HILLOM8.0 HIlLMY7.D HlLLMHB D C 10.0 C10.0 G 10.0 elO.0 G 5.0 9070038 9.85038 7.3ggS84 16.467401 20.404358 19.025032 105 301943 92.717039 02.480199 2 NIA NJA NJA NIA NIA NJA 2 NIA NIA NIA NIA 2 NIA NIA NIA NIA 2 NIA NIA < 1.0 NIA NIA NIA 2 < 10 c 1.0 NIA NIA 2 18.140072 1.258639W 80 6437095 1 70278576 2 10.93W76 1 2771523511 1.235344845 60.9793446 1.78518275 1.703904Zl 2 14.799380 1.170243169 NIA NIA 2 32.934002 1.517855057 122.976586 2.08982244 2 40800712 1.610752008 1575556454 121807067 208567249 20869810 2 39651sM 1.596261417 121744813 2.08545011 2 210.603886 2.32340030 613 377164 2 7877276 2 185434070 2.26810954 2.269679595 614935101 2 78082934 2.7083718l 2 164.961598 2.217382055 614 552079 2.70855069 Page14of 16 Sludv EW-I311 tG, h BACK TO MAIN I Desorption1soth.m. Smdy Loam m73 (P (D PagslSoll6 Slue EW-1311 BACK TO MAIN ___ . Desorption Isotherms, Sludge li f' 0 0 0.5 1 15 2 2.5 LOOcaq rrndylom~ sedtmnl Log Kder -0.0811 -1 4088 14693 0.104447969 003901216 2946456271 1.012 1.01M 0.3272 0988142292 0.98386462 3056224719 Paw 16 of 16 Study EW-I311 Tier 111 "Mass Balance Calculations" BACK TO MAIN PFOS AdsorbiDesorb *-.. R"" HO10318 noio~i~ noi0~18 no10316 tlD10318 H010316 no10318 no10318 notom R010320 R010320 R010320 R010320 R01032O R010320 H010316 H010316 H010316 H010316 H010316 H010316 H010316 H010316 R010320 R010320 ROW320 R010320 ROlMM ROW405 R010405 15anpk Data F k HILL- D HILL0065 D HILL0066 D HILL0095 D HlLLW96 D HILL0101 D HILL0131 D HILL0132 D HILL0133 D RUSHOO55 D RUSHW56 D RUSHM)Gl D RUSH0083 D RUSH0084 D RUSH0389 D HILL0068 D HILLW73 D HILL0074 D HILL0103 D HILL0104 0 MlLLCIlO5 D HILL0135 D HILL0136 D RUSHW33 D RUSH0063 D RUSH0064 D RUSHW65 D RUSHW32 D RUSH0033 D RUSHW34 D -502233 -5023.53 -5024-S3 -502553 -5M6-S3 -502783 -5028.53 -502953 -503053 1311-5031-S3 1311-503283 1311-503343 1311-5O34-53 1311-5035-53 1311-5O3653 -505853 -5059-53 -5060.s3 -506153 -5062-S3 -5063-53 -5064-53 -506553 13113-506653 1311-506753 1311 - M 6 8 5 3 1311-5069-53 1311-507083 1311-507143 1311-5072-S3 00125 0 0125 00125 00125 0 0125 00125 0 0125 0 0125 00125 00125 0 0125 0 0125 00125 0 0125 00125 00125 00125 00125 00125 00125 00125 00125 ODlX oom 00125 00125 00125 00125 o 0125 50000 500 W 2OWW ?WOW 2WOW 5wo W 5wo W 5500 W lWOOW 1WWW IWOO w 50000 W 50000W SOW0 W Mo 5W Mo 2wo 2W0 Mw 5wD 5WO 5wD IWW lWW 1WW 54CW 5WW MOW 386188014 4W 811808 1589 3353 152915115 14264531 3913 70145 23W M144 3873 38636 6281 3209 85108m9 ea31 8359 IC454 01 41418 3251 133818854 6366312 68302054 655835 21025581 28221SE.4 285010358 8317832 71817115 11950450 1195328% 1871M255 171179338 101225113 103295oM 108265554 4 827350115 5 0011m 19 99189125 19 tl446438 17 W8oBB38 48szim813 28 761843 48 4113295 103 5165113 106 3851883 300 4 1 2 w En5 886315 517 7MoB34 5424136825 n ?%?as 0 853715125 0 81879315 3 378198375 3 527885425 3 574254475 I O 38129 9 7271d6815 8 743807 22 44151825 23 38en3188 21 45991134 ims3mi3 119 1181515 138 5810125 21 381228 23 912482 55 333452 57 811888 4n 6111568 111 971874 83458182 115 W 4 9 8 131 442794 133 111m 142 60345B 289 1 l W 8 410 188916 3781 1 m 21 87378 23 898% 5192214s 151 3611% 133 222922 to8 891334 229 32918 240 121M2 318 338512 811 e a r n 835 511088 658 12403 4 M 1 89701 3051 03229 3384 80983 omioisas 0 299856025 0 891C6815 0 12339ea o 58%8m15 1309848425 0 193238715 1448031225 1 843034825 1811471 17EW432 3 81770785 5 8113717 4 1301258 0 27342225 0 298131 o 724026825 1 88209895 1 8852B525 13361417 lee62225 3 COS210525 4 10(23215 10 013241 10444?2u, 8 334M315 E63481IXI3 38 21290363 42 43631288 00120 + 5 0 ooim c 5 0 00120 s 5 0 ooim 4 5 0 00120 ' 5 0 00120 56 ooim '50 00120 60 00120 6217634 ooim 5939702 00120 7871924 oofm 2265781 00120 1695932 ooim 4622885 ooim 426 ooim 489 ooim 570 ooim 1598 00120 2032 ooim 1808 O O ~ M 461 1 ooilo 2855 oo1m 3465266 o o ~ m 2981447 ooim 3605895 oo1m 337662 00120 4169038 oo1m 3516084 o oim 68.33123 zoo 2w 2w zw zw 2w 2w 2w 2w 2w zoo 2w 2m 2w 2w 2w 2w 2w 2w 2w 200 2 w 2w 2w 2w 2m lwoo 1ww too w <10 '012 <IO '012 <lo <012 10 < 10 11 182708 eo12 <012 0 1338525 <IO 12051E4 124352611 11 87- r012 0 1UBlW7 o 11muz 0 14255285 15143848 0 18882618 45 31%12 0 54318734 33 S l W 2 04070231 92 457108 85 10211 97 702138 113911118 1 E34825 102123242 1 1?2432@3 1387WBll 319525044 4oB 39942 38Y3Ms3 4 81878301 361644534 4 3 3 4 1 Y 1 oz? 14921 11 0851905 570908 em72 693 05sm 8 ~ I B B I U O 5 9 ~ 2 8 ~ p t l7 ISY~IO~ 12111w 8 65414848 615 323M 8 10388128 4189 0375 35180M 50 02845 42103&24 6833 1228 81 99741% z P I 1 t! ii I 193% 815% 84 ox 821% 794% 74ox 801% 47 3% 80 m 642% ea 6% 820% 81 6?& 83 8% 81 1% 33 4% 312% 4E 8% 36 4% 40 3% 31 0% 38 e% 31 3% 38 4% 325% 34m 30 3% 31 3% 33 5% 41 8% Page 1 of 3 BACK TO MAIN Study EOG13H 9s. a3?(D 5 I- M i i s 8.b- ~ 57tox I S m P k Data Fl!d HILL0076.D HILL0077 D nlLLWf8 u HILL0107 D HILL0108 D HILL0109 D RUSH0035 D RUSH0026 D RUSH0037 D RUSHW40 D RUSH0041 D RUSHW46 D RUSH0048 D RUSH0049 D RUSH0050 D HILL0080 D TuM broke HILL0081 D HILL0115 D HILL0116 D HILL0117D RUSH0052 D RUSH0053 D RUSHMI54 D RUSH0060 D RUSH0061 D RUSH0062 D RUSH0064 D RUSH0065 D RUSHW66 D 509453 -509553 -5096S3 sw7-s3 5098-S3 5099-53 i a iI-~IW-S~ 1311-5101S3 1311+10253 1311-510383 1311-5104-53 13114105-53 1311-5106S3 1311-510753 1311-5108-S3 -513053 Em-1311-5131 -5132.53 5133-53 -513463 -513553 1311-5136-53 1311-513 7 5 3 7311-5138-53 1311-513943 1311-514063 1311-5141-53 1311-514253 1311-5143-53 1311-514453 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 nom 00125 00125 00125 00125 00125 00125 00125 0015 00125 00125 00125 00125 00125 00125 5W 5W 2WU 2wO 2wO YKW 5w0 SWP lOwD 10000 lOwD MOW MOW Mwo 500 5W 5W 2wO ZWO 2OW 5WO YXiD 5x0 IWW IWW IWW 5woO XWU Mwo 1W888412 92307848 382488934 4oB850758 478255482 ,53757868 1400054(u llM)49807 320984698 3US792472 30544701 18011 5457 17Bm8055 17018 8OM 4955551 35114278 9492696 224488112 2671089BB 271834882 851 85002 76528101 75iBMPZ 151041W 1552245U2 1545075M 108207528 99117125 W1578 137110515 11~53 4 781228875 8 248134475 5 378103525 192197335 17 80068538 17 256?Zm 40 i 2 ~ 8 7 n 35 349059 38 1 8 ~ 2 5 2251443213 220 013188 212 758355 0621WW75 045142845 0 6311587 2 8058511 3 3388821 3 39543515 1064812525 9 566012625 i 4100815 19 83024325 19 40306275 19 3126956 135 50341 124 ME4063 120 5447% 70 YauY 89 2254 ,0986 252 13575 271 m3585 869 374834 654 78000 4e4 0531 l21844173 1272 33095 1335 M265 671111 B 2 6272 7381 8434 IWI 53 3SZORI 0 53 311ooB 214226652 2.w. 57553 212 447788 579 748028 499 345134 n 2 028624 1053n m 1141 23143 10?2397M 4819 27102 M9081312 5130 07U5 n *m127G2 n woi5775 3 1774% 3 151896875 3380Bb85 8357185425 8 184751125 855013875 15 23052183 15W1188 lS70378313 M 7~0~15 78 40920125 105m 3 06889012 0 066725015 2 677e329 2 782195375 28555871 7 24682535 8 241821875 8m 7 m 1317217025 14 ZB533288 12 9MW3 81 49W8775 63 83x64 84 12595563 0 orm o oim 0 0120 0 0120 0 0120 o oim 00120 0 0120 00120 00120 00120 0 0120 0 0120 0 0120 0 0120 0 0120 OOl20 0 0120 DO120 OOIW 0 0120 00120 0 0120 0 01m 0 0120 00120 o oim 00120 57.9 161.9 173.0 194.7 467.7061 371.418 485.0679 25 C 25 c 25 50.04657 61.22W1 65.68839 111.6 98.8 393.7 375.2 261.3 182.5579 190.9566 242.2879 < 25 < 25 < 25 < 25 c 25 c 25 2w 200 2w zw 2W 2w 2w 1WW 1W w IWW IW W 1ww IWM zw 2W 2W 2 00 2w 2w low low 10 w lwOW low w lwoW 1wO w 1wo w l0WW 115 756962 323 876812 345 931234 389 4 2 m 2 33541224 742818078 970 13-24 QYX) Q5W 52.24 6587 6122 W1 65BLI 83W 223 252154 0 1975801M 787 427278 754 306384 7225131k8 1625 87883 1- 58sLu 2422 87857 < 2MW 25000 <2Moo e 25000 mo 25000 1 38820378 38865197 4 15117481 41173142d2 11 n 4 w 9 891405544 11 8416288 e24 e24 <24 Bo OW8M 734e4012 78 W0728 2 87wz585 0 2 37wBf23 844912734 9 M367M1 8 67015778 21 W148 229147800 28 0745428 <Mo < 3W < 300 3M <Mo <Mo IJ Em 54 5% 47 4% 542% sa 2% 82 1% 55 5% 58 nu 44 3% 43 4m 43 ox 59 2% 59 5% 83 5% 63 5% NIA 58 7% 59 7% ea 5% 58 ox 83 1% 82 m 72 7% 1(1m %ox 25 8% 31 7% BO 1% 29 5% PFOS A d t o r b m s o r b *'. Page 2 of 3 Study EW-1311 BACK TO MAIN - Mmss &!am PFOS Adsarbmesorb ,.'- .... - HILL0088.D , ^--- I1,LL""III.Y HILL0119.D HILL0120 D HlLLOlZl D RUSHW47.D RUSH0046 D RUSH0049 D RUSHGO68 D RUSHW59 D RUSH0074 D RUSH0076 D RUSHOO77 D RUSH0078 D H1LL0091 D HILL0092 D HILL0093 D HILL0123 D HILL0124 D HILL0129 D RUSH0051 D RUSH0052 D RUSHW53 D RUSHW79 D RUSH0080 D RUSHW81 D RUSH0080 D RUSH0081 D RUSH0082 D -516753 -5,6&S3 -516953 -517053 -517153 1311517253 1311 5 1 7 3 5 3 1311-517453 1311-517553 1311-517653 1311-517753 1311-517853 13115179S3 1311-518053 -5202-53 -5203s3 -5204-53 -520553 -5206S3 -5207-S3 1311-520853 1311-5209-S3 1311-521Ds3 1311-521153 1311-521253 1311-521353 1311-521453 1311-521553 1311-5216-S3 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 00125 OM25 00125 00125 00125 00125 00125 00125 00125 01125 00125 00125 00125 00125 00125 00125 5m 500 2000 ZWO ZWO 50W 5,xQ SOW IWM 1wW IWM MMO 5mW 5wW 500 5W 500 zow ?wo 2OW YMI 5DM 5Mx) 1wW 1WW 1wW 5WW 5wW MMO iea 457972 lP920114 ea9 n534a 681 519332 730 094518 2037 97939 1871 00144 1915 10276 3713 23106 3711 74203 3897 08738 18328 86% 17828 1948 17980 O W WA WA WA NIA WA WA 141 28747 11420901 WA 1411 79531 23885w? 24481872 WE8139 730 -5 no 7908 1 9924oe2 2 33072-5 2 374W5175 862158685 8 51899185 9 126181475 25 47474238 23 -518 24 3137M5 a 4153005 4e 39877538 48 71359238 Pe 0833Z5 m ea481 224 W 3 3 8 WA WA WA WA NIA WA 1765M3375 1427812825 NI* 1 859941375 zgMB&55 3 057724 1058517375 9 13749375 9 6346rn5 88241506 85 243574 321 -78 298 140168 331 481791 761 3284 149 778958 758 575324 174s92474 163325491 1743 45547 7408 8281 7944 (u88 7091 215 WA WA WA WA WA < 10 18 1 4 W n 18 93w78 14 798W 32 934602 40 m i 1 2 39 8 5 1 W 210 503888 185 434078 184 PB1588 107331095 1 07801995 1 w55u675 4 01676085 3 7267521 4 1435n425 85188055 9 37223695 948219155 21 87419125 2041583638 21 79318338 02 60786375 99 M80825 88 401875 NIA WA WA WA WA WA 0 2Z7508 "0 23662595 1YY921 0 411885025 05101lW 0 49sM58 2 632548575 2 317925975 zoomism 0 0170 0 0120 0 0120 OOIZO 00120 00120 0 0120 00120 00120 00120 nom ooim 00120 00120 00120 ooim 0 0120 00120 001m ootm 00120 00120 00120 00120 0 0120 00120 0 0120 00120 0o m a9 1 65 7 298 3 267 4 327 9 .501 491 43 496 1706 c 25 < 25 < 25 < 25 < 25 < 25 363 25 2 301 97 6 127 8 98 9 332 321 244 5963 251 8495 490 2051 494 7347 ,501 47 25497 57 65922 66 77067 Irn 200 200 100 2W ZW 2W ZW low w lwoW 1WD W 1000 00 1000 W 1000 W 2W 200 2w zw ZW 2w ZW ZW ZW 200 ZW 200 IWW 1WW IW W *e* ?(2??? 131 385836 588 55581 534 1 2 m 655 794326 7 1032 983 2a5956 892 Y12d < 25oM <2 m <2 m < 2MW 25wo < 25WO 72 685522 50 441822 W 17112 195243738 255 648826 187 725208 WMlM as 192588 503 Bgew 98041Dm4 909 189372 WA 4725 4BB6 5765 s p 4 w n 067 I d I 3.' f31038% ii 8r 80 3m 79 zy 74 om M 6% 56Du 71 4% 73 1% YW 53 4m 56 4% s i 5m 51 5m 50 i m WA NIA NIA NIA WA WA 15w 12 1% WA 11 24 12 3% NIA 112% 12 Q n 14 7% Page 3 of 3 BACK TO MAIN Appendix E: Quality Control Sample Data This appendix includes processed matrix spike, control, and replicate sample data from the present study. The runs summarized are the following: so01 120a sOOl12Ob s001122a to10122 ~001211 to01215 so01207 H001214a&b to10123 to10124 to10125 R010320 H010405ext H010405int H010404ext R010404ext R010405 R010402a&b H010329 H010319a R010312 R010329aLkb H010402a&b H010222 R010222 H010309 R010309 H010315 H010313 R010314 H010311 H010316 H010412 R010412 Crossed out data was not used. 3M Environmental Laboratory Page 237 of 703 BACK TO MAIN Quality Control Sample Data I Sample Description IR U S H 0 0 3 3 . D RUSH0034.D RUSH0035.D RUSHO036.D RUSH0037.D RUSH0038.D RUSHO039.D RUSHO040.D R U S H 0 0 4 1. D RUSH0046.D RUSH0047.D RUSHO048.D RUSHO049.D RUSHO050.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.D RUSH0060.D RUSH0061.D RUSHO062.D RUSHO063.D IR U S H 0 0 6 4 . D RUSHO065.D RUSHOO66.D RUSHO067.D RUSH0068.D RUSHO069.D RUSH0074. D RUSH0075.D RUSHO076.D RUSH0077.D RUSH0078.D RUSHO079.D RUSH0080.D RUSH0081.D RUSHO082.D RUSHO083.D 1311-5071-S3 131 1-5072-S3 1311-5072MS-S3 131 1-5091-53 1311-5092-53 131 1-5093-53 1311-5093MS-S3 131 1-5103-S3 1 3 11-510 4 4 3 1311-5105-S3 131 1-5105MS-53 13 11-510 6 4 3 131 1-5107-S3 1311-5108-S3 1311-5108MS-S3 1311-5136-S3 1311-5137-53 1311-5138-S3 1311-5138MS-S3 1311-5139-S3 131 1-5140-S3 1311-5141-53 1311-5141MS-S3 1311-5142-S3 131 1-5143-S3 13 11-51 4 4 4 3 131 1-5144MS-S3 1311417543 1311-517643 1311-5 17 7 - 5 3 1311-5177MS-S3 1 3 1 1 - 5 17 8 - S 3 1311-5179-53 1311 - 5 1 8 0 4 3 1311-5180MS-S3 1311-521443 1311-521553 131 1-5216-S3 1311-5216MS-S3 Analytical Run Information*: Acceptable Quant Range: 25 ~ 1OOZnglml CalibrationCurve ?: 0.9880787 Target Analyte: PFOS InternalStandard: THPFOS Instrument: Rush - Run ID: R~ 010405 Measured Concentration, uglL 41.690375 35.16084 68.331228 268.971058 25 25.536054 c 25 226.293398 :2 5 .< 25 .< 25 2 2 1 . 0 7 5 6 17 50.046567 61.22001 65.688394 266.885789 182.567883 190.956582 242.287857 422.825169 *: 25 e: 25 *' 25 197.948699 25 e 25 < 25 199.992825 < 25 25 25 187.321981 < 25 < 25 < 25 191S 6 6 5 6 5 47.254966 57.659224 66.77067 243.807595 Theoretical Matrix Spike Concentration, uglL Replicate Sample % R S D 36 31 200 NIA 200 NIA -. 200 Ir .zoo . 2W 13.66 15.75 NIA 200 NIA ZOO NIA 200 NIA m 17.06 200 Matrix Spiki Recovery, 7 100.32 113.15 11054 100.60 90.27 98.97 100.00 93 66 95.78 88 52 Dilution Factor, Nx 10 1W 100 1W 2 2 2 2 100 100 100 100 100 1W 100 100 10 10 10 10 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 100 100 100 100 1 ? 3M Environmental Laboratory Page 238 of 703 BACK TO MAIN Qualitv Control Sample Data Instrument: Hillary -Run ID: H0~10319a - Sample Data File HILL0032.D HILL0033.D HILL0034.D HILL0035.D HILL0036.D HILL0037.D HILL0038.D H I L L 0 0 3 9 .D HILL0040.D H I L L 0 0 4 1.D HILL0046.D HILL0047.D HILL0048.D HILL0049.D HILL0050.D HILL0051.D t=iu HILL0053.D HILL0054.D HILL0059.D HILL0060.D HILL0061.D HILL0062.D I HILL0063.D HILL0064.D HILL0065.D HILL0066 D HILL0067.D HILL0068 D HILL0073 D HILL0074 D HILL0075 D HILL0076 D HILL0077 D I HILL0078 D HILL0079.D HILL0080.D HILL0085.D HILL0086.D HILL0087.D Sample Description 1311-4124-52 1311-4125-S2 1311-4 126-52 1311-4148-SZ 1311-4149-52 1 3 11 - 4 150-S2 1311-4124-53 1 3 11-412 5 4 3 1311-4126-S3 1311-4148-S3 1311-4149-S3 1311-4150-S3 1311-4124-S4 1311-4125-S4 1311-4148-S4 1311-4149-S4 asav 1311-412445 1 3 11-4125-S5 1311-4126-55 1 3 11 - 4 1 4 8 4 5 1311-4149-S5 1 3 11 - 4 150-55 1311-4124-S6 1311-4125-56 1311-4126-S6 1311-4126MS-56 1311-4148-S6 1311-4149-S6 1311-4150-S6 1311-4150MS-S6 1311-4124-S7 1311-4125-57 1311-4126-S7 1311-4148-57 1311-4149-S7 1311-4150-S7 1311-4124-S8 1 3 11 - 4 125-S8 1311-4126-S8 HILL0090.D HILL0091.D HILL0092.D 1311-4149-S8 1311-415QS8 1 3 11 - 4 150MS-S8 Measured Concentratlon, uglL < 2.5 < 2.5 < 2.5 30.5 32.4 30.4 < 2.5 < 2.5 < 2.5 39.1 38.5 43.7 < 2.5 4.9 131.4 78.0 zu.6 < 2.5 < 2.5 < 2.5 72.9 63.0 79.4 < 2.5 2.5 < 2.5 235 6 59 1 646 64 2 298 1 <25 <25 45 60 4 63.2 71.4 2.5 2.5 < 2.5 238.3 58.6 62.8 36.4 296.8 Matrix Spike Concentration, uglL Replicate Sample %RSD NIA 3 48 NIA 7.12 NIA 48 20 NIA 11.52 NIA 200 4 90 200 NIA 886 NIA ZM) 26 90 207 Matrix Spikl R e c o v e r y , OA 11778 11688 118 13 125.82 Dilution Factor, Nx 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 - Analvtical Run Information": Acceptable Quant Range: 2.5 1002nglml Calibration Curve 8:0.9999964 Target Analyte: PFOS Internal Standard: THPFOS 'Point thrown out. Compared to the values obtained from other fdiquots of the same sample during this run (30.4.43.7, 79.4, 64.2, 71.4. and 36.4) the value obtained for the -S4 sample (212.6) is about three time; higher. May be a bad injection. ?. 3M Environmental Laboratory Page 239 of 703 BACK TO MAIN Qualitv Control Sample Data Sample Data File Huw3a.D -Sample Description Instrument: Hillary - Run ID: - H010329 Measured Ccmcentratlon. uglL 3Waas66 Spike Concentration. UglL ReDliCate Sample %RSD Matrix SDlki Recovery, 7 100 &uw66s i4ucU6a HuoaSZa tduuwaa blNaw.D Hu4W4.D u4Luwa2 uuQW3.D h4uocua u4uWa.Q &ilusaQ 44uWw.Q &d&mwLD bluacwa &4uwa&D 4AuLcaW uuwWaD t.kuwoa buuQmaa b4uowaa l4uawaa b4uuoMa kNuowbD l4uwQ6a k!uw%D bluowa& l.luwaa HILL0104.D HILL0105.D HILLO106.D HILLO107.D HILL0108.D HILL0109.D HILLO1lO.D H I L L 0 115.D HILL0116.D HILLO117.D HILL0118.D HILL0119.D aaw&Maw - 4 w 4 4 4 a s s%l44aw -- 4 a M 4 M u 3 4w4&A6s .w44wGX -4 a 4 4 4 G a 4a44aaS -aua#w-w 43wAsLS s.Ua&-s -- 4 a 4 4 a - s -+%l&W%s - 4s%u6La %%uaasa --1311-516041 1311-516141 1311-5162-51 1311-5162MSS1 1311-5163-S1 1311-5164-S1 1311-5165-51 1311-5165MS-SI 1311-5166-S1 1311-5167-S1 1311-5168-S1 1311-5168MS-SI S?nfOC1'1 suU367. 3zao3cG -wu3awa aaaw.aa $i34iUa 2n3.sxa A35aaa 4,c Ls1 aJaus4a .4aawbw waaaQ3 a.aw4Qa a?.bsaw 46&auMs 4zwaazQ uZaua83 F6aaaaw aua43sw a6aSu26 sMQQ6a4 a4au43a .aaw666 - . - 4 .!89.002164 258.39539 266.033394 480.91678 36.247649 6.963474 C 5.0 :!13.508112 79.696368 93.228986 94.960207 321.371684 aca 100 cue 100 eye. 100 a6.w 100 2a9 200 Lzo 100 1oD 5.88 2w 95.84 200 9.38 200 -.ue4.i .laa&n S4a4 14Lso as0a-Q aE4.a 107.44 106.75 113.21 Dilution Factor, Nx 10 10 10 10 1w 100 100 100 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 10 10 10 10 100 100 100 100 2 2 2 2 2 2 3M Environmental Laboratory Page 240 of 703 BACK TO MAIN HILL0120.D 1311-516941 344.862674 2 HILL0121.D 1311 - 5 1 7 0 4 1 340.759666 3.71 2 HILL0122.D 1311-5171-51 365.047259 2 HILL0123.D 131 1-5171MS-S1 636.371356 200 135 66 2 H I LLO124. D 1311-5172-51 203.797939 10 HILL0129.D 1311-5173-51 187.700144 4.14 10 HILL0130.D 1311-517441 194.510276 10 HILLOl31.D 1311-5174MS-S1 422.244664 200 11387 10 HILL0132.D 1311-5175-51 371.3231 96 10 HILL0133.D 1311-5176-S1 371.174203 2.82 10 HILL0134.D 1311-5177-S1 389.708739 10 HILL0135.D 1311 - 5 1 7 7 M S S l 645.346514 200 127.82 10 HlLL0136.D 1311-5178-51 183.266658 100 HILL0141.D 1311-5179-51 178.291848 1.43 100 HILL0142.D ' HILL0143.D 1311-5180-51 1311-5180MSS1 179,600507 387.145146 200 100 103.77 100 Huau4.S suA.#s4 44a3a69 2 kluuk%a .Kw&ws4 60 (up. 2 kluW46s 4suHs%m 60 2 - blua4Ao wUal4m 4a4&a&& 60 40 aoo (up. 2 2 - kxuw4.m 60 (up. 2 l=&ws&D =M&w6-% &a 2 -- J.uux&D aa%uaa4 an0 63a1 2 J.uux&D 6.65ix4 2 kluc4ao .cW&aa% 4.4 14s1 2 l4LuUao Kw44aUx sa04644 2 - b l u a s & D hLLw6Qs aauuaGs -lQsaa6 a90 6Q.aa 2 za6ww 10 - i4uaa.Q 7-zu4a 10 - t 4 u a s a a a%Lua&S -3 10 klu&wao 46uaa4a aoo w 10 HILL0164.D 1311-5193-51 5a7.3m82 10 HILL0165.D 1311 - 5 1 9 4 4 1 375.628336 25 38 10 HILL0170.D 1311-5195-51 624.651539 10 HILL0171.D 1311-5195MS-S1 947.574722 2w 161 4 6 10 H I L L 0 172.D 1311-519651 25.400564 100 HILL0173.D 1311-519741 16.589279 21.21 100 HILL0174.D 1311-5198-51 20.475802 100 HILL0175.D 1311-5198MS-S1 236.975437 200 108 25 100 - kaLw?&D LAC 2 wua%ua -- nLLauaa niuoxKm -uu4ao& LAC (up. 2 LAE 2 83maW.s a90 4199 2 nkKU&Q w-MaGx% LFCO 2 uua%%#B %M44xe4 a (up. 2 44uwasa - Huula7a su4uu44 LAO a 2 aoo, (up. 2 buuUaQ 4au&uSw 44 2 huuwaaa %w4a&44 Gwa (up. 2 - buLuawa .su&wLS JdumaaD .sn - . 2 2 10 10 10 an0 ZOdD 10 kiU4axm %w&w-s wob66 10 b4uum.a J4uoxaB ylllnsn?n HILL0204.D xw4a#sa &u4va-S u44aa&& 1311-521441 -uaaz6% 3040 10 -.4636a6a 10 an0 ZaOK 10 8.468139 100 HILL0205 D 1311-5215-S1 7.309995 7 52 100 HILL0206.D HILL0207.D 1311-5216-S1 1311-5216MS-S1 7.707909 100 :!01 156105 200 98 72 100 Analvtical Run Information*: Acceptable Ouant Range: 5 - 1002nghl Calibration Cuwe 3:0.9925463 Target Analyte: PFOS Internal Standard: THPFOS 3M Environmental Laboratory Page 241 of 703 BACK TO MAIN Quality Control SamDle Data RUSHOMO.D RUSH0041.D RUSHOM2.D 1311-5018MS-S1 1311-507O-SZ 1311-5071-52 ausuw%o- 64Lwwaa- GusuoaD- RUSHW53.D 1311-5103-52 RUSH0054D 1311-51WS2 RUSHW55.D 1311-5105-S2 RUSH0056.D 1311-5105MS-SZ RUSH0057.D (":"":" RUSHW64.D :::;1311-510652 1311-5108MS-SZ RUSH0065.D 1311-5127-SZ RUSHOffi6.D 1311-512842 RUSHW67.D 1311-5129-62 RUSHOffi8.D 1311-5129MS-S2 RUSHW69.D RUSHO070.D 1311-5130-52 1311-5132-SZ RUSH0071.D 1311-5132MS-S2 RUSHW78.D 1311-513552 RUSH0077.D 1311-5134-52 RUSHW78.D 1311-513542 RUSHW79.D 1311-5135MS-52 RUSHW80.D 1311-513582 RUSHWE1.D 1311-513 7 4 2 RUSHW82.D 1311-5138-52 RUSHW63.D 1311-5138MS-SZ RUSH0084.D 1311-5139-52 RUSHOO65.D RUSHOOD0.D 1311-5140-S2 1311-5141-SZ RUSH0091.D 1311-5141MS-S2 RUSHOO92.D 1311-5142-52 RUSHOO93.D RUSHO094.D 1311-5143-52 1311-514442 RUSHW95.D 1311-5144MS-SZ RUSHOO96.D 1311-516342 RUSH0097.D 1311-51&cSZ RUSH0088.D RUSHO099.D 1311-5185-52 1311-5165MS-SZ A n a l v t i c a l Run Information': AcceptableQuanlRange: 5 . 1 W2nglml Calibration Curve 8:0.9997640 Target Analyte: PFOS Internal Standard: THPFOS _Ins_tru_me_nt:_Rush Run ID: R010402 (A) 23E.736167 45C.789701 305.703229 339 490983 528 022186 19ala- 121 844173 127 233095 133 630265 315491169 67.811262 62.727361 84,309464 273.509217 < 5.0 < 5.0 < 5.0. 21 1.lM9083 26.1376048 25.69003 246.!136174 107." 13316 111.:!87615 106.:!23884 361.d.46659 289.873014 249.f.72867 276.C14812 580.C20253 105.2 77362 114.123143 103,239784 293.385505 491.927102 509.061312 513.037645 715.922726 < 5.0 < 5.0 c 5.0 204.8.24182 204 20 78 86 21 '1 1 403 200 BO 93 2W , 81,80 I 2W 105 52 200 110.12 200 7.51 2w 5.38 m 2.22 m0 NIA zw 127.81 152.W 95.07 101.48 102.1 Dilution Factor, NX 1000 1000 1000 1w0 10 10 10 10 2 Contaminated 2 U)"lrnl 2 Manb 2 10 10 10 10 $03 100 100 1w 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 10 10 10 10 2 2 2 3M Environmental Laboratory Page 242 of 703 BACK TO MAIN Quality Control SamDle Data RUSH0141.D RUSHO142.D 1311-5179-S2 1311-5180-SZ - Analytical Run Information*: Acceptable Quant Range: 10 1002nglml CalibrationCurve ?: 0.9989973 Target Analyte: PFOS Internal Standard:THPFOS Instrument: Rush Run ID: R010402 (b) Measured 42.932438 Matrix Spike Concentration, uglL ,Replicate Sample %RSD 0.59 Matrix Spikc Recovery, % 276.700865 160.750438 149.070084 185.740897 443.490256 380.66422 374.889478 2w 5.40 2w 0.80 117.04 138.87 2w 171.28 3.84 2w 93.24 70.91215 5.77 2w 91.92 NIA 2w 85.50 *: 10.0 NIA 2w NIA 100.12 Dilution Factor, Nx 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 1w 1W 100 100 2 2 2 2 2 2 2 2 2 2' 3M Environmental Laboratory Page 243 of 703 BACK TO MAIN Quality Control Sample Data Instrument: HiJar~ Run ID: H010405, external standard auant I 1 Theoretical Matrix Measured Solke Concentration, Concentration, Replicate Matrix Spike Dilution Factor, ug/L ugll Sample %RSD Recovety, % Nx &u&uw4 10 55411107'1 aani 10 u345W.u a6zaaa5 100 4aAaaa5 10 a320 10 Quanted using 1w Ua4a33 d.ua internal 1M) ilas66U aQad&sa awsa30 aaa&W&u a22ouu 100 S-iS standard. mls 100 1M31 data not used 1W 10 10 10 100 4a4.bz 10 100 100 1w 1w I 2 A2.t.m 2 2 2 10 10 - l4LKUUa l=luUxm t4lww3m su&lsaa . - 10 10 1w aa75ia aL54 1CQ a&ua&iz 1w aM&sss4 am ULiO 100 HILLOO67.D 1311-5181-S1 27.424377 2 HILL0072.D 1311-518 2 4 1 < 10.0 tmvmi 2 HILL0073.D 1311-5183-51 c10.0 2 HILL0074.D 1311-5183MS-S1 144.847675 200 72.42 2 HILL0075.D 1311-5199-SI c10.0 2 HILL0076.D 1311-5200-Si <10.0 NIA 2 HILL0077.D 1311-5201-S1 40.0 2 HILL0078.D 1311-520lMS-SI 131.864428 200 65.93 2 - Analytical Run Information*: Acceptable Quant Range: 10 1002ng/ml CalibrationCurve ?: 0 . 8 9 7 9 3 3 5 Target Analyte: PFOS internal Standard:NONE 3M Environmental Laboratory Page 244 of 703 BACK TO MAIN Qualitv Control Sample Data I=----- Sample DataFile RUSH0032.D RUSH0033.D Sample Description 131 1-4154-S2 1311 - 4 1 5 5 4 2 RUSH0034.D 131 1-4156-SZ RUSH0035.D 1311-4178-S2 lRUSHOO36.D RUSH0037 D 131 1-4179-SZ 1311-4180-S2 RUSH0038 D 1311-4154-53 IRUSH0039.D 1311-4155-53 RUSH0040.D R U S H 0 0 4 1.D 131 1-4156-53 1 3 11-4178-S3 RUSH0046.D 131 1-4179-S3 RUSH0047.D 1311-4180-53 RUSH0048.D 13114154-54 1311-4155-54 RUSH0050.D R U S H 0 0 5 1.D 131 1-4156-54 1 3 11-417 8 4 4 (RUSH0052.D 1311-4179-S4 RUSH0053.D 1311-4154-S5 RUSH0054.D 131 1-415 5 4 5 IRUSH0055.D RUSH0060.D 1311-415645 131 1-4178-S5 RUSH0061.D RUSH0062 D RUSH0063 D 1311-4179-S5 1311-4180-S5 13114154-56 RUSH0064.D RUSH0065 D 1311-4155-56 1311-4156-S6 RUSHOW6.D 131 1-4156MS-S6 RUSHO067.D 1311-417846 RUSHO068.D 1311-4179-S6 IRUSH0069.D 131 1-4180-56 RUSH0074.D 1311-4180MS-S6 RUSH0075.D 1311 - 4 1 5 4 4 7 IRUSH0076.D 1311415547 RUSH0077.D 1311 - 4 1 5 6 4 7 RUSH0078.D 131 14178-57 lRUSHOO79.D 1311-4179-57 USHO080.D 1311-4180-S7 USHO081.D 1311-4154-S8 USHO082.D 1311-4155-58 1311 4 156MS-S8 RUSH0090.D RUSH0091.D RUSH0092.D 1311-4179-S8 131 1-418O-SB 13114180MS-SB - Analvtical Run Information*: Acceptable Quant Range: 10 1002nglrnl Calibration C u r v e ?: 0.9913280 Target Analyte: PFOS Internal Standard: NONE Instrument: Rush Run ID: R010404. external standard quant Measured Concentration, uglL c 10.0 10.0 < 10.0 < 10.0 c 10.0 < 100 e100 < 10.0 < 10.0 < 10.0 10.0 < 10.0 < 10.0 10.0 10.0 c 10.0 10.0 c 10.0 c 10.0 < 10.0 10.0 c 100 e100 < 100 e100 c 100 184.766805 10.0 10.0 I: 10.0 256.265166 c 10.0 :. 10.0 :10.0 .: 10.0 .: 10.0 .: 10.0 .: 10.0 ': 10.0 4 10.0 198.880502 .:.:10.0. 10.0 ': 10.0 155.579696 Matrix Spike Concentration, uglL Replicate Sample %RSD NIA NIA NIA NIA NIA NIA NIA NIA NIA 200 NIA 200 NIA NIA NIA ZW NIA 200 Matrix Spike Recovery, X 92.39 128 13 99.44 77.79 Dilution Factor, Nx 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 245 of 703 BACK TO MAIN Qualitv Control Sample Data Instrument: Hiilary -Ru_n _ ID:_H010404,external standard quant S a m p l e Data File Sample Description Measured Concentration, UglL Theoretical Matrix Spike Concentration, ugk Replicate Sample %RSD Matrix Spikc Recovely, % Dilution Factor, Nx IH I L L 0 0 3 1 . D 1311-4151-S1 c10.0 2 HILL0032.D 131 1-4152-S1 40.0 NIA 2 HILL0033.D 1311-4153-51 c10.0 2 HILL0034.D 131 1-4153MS-S1 168 305282 200 84 15 2 IH I L L 0 0 3 5 . D 1311-415 4 - 5 1 <10 0 2 HILL0036.D 1311-4155-51 <10.0 NIA 2 HILL0037.D 1311-4156-51 c10.0 2 HILL003B.D 131 1-4156MS-S1 157.148327 200 78.57 2 HILL0039.D 1311-4157-S1 c10.0 2 I HILL0040.D 1311-4158-51 40.0 NIA 2 HILL0045.D 1311-4159-S1 dO.0 2 H ILL0046. D 131 1-4159MS-S1 173.055241 200 86.53 2 I HILL0047.D 131 1-4160-S1 c10.0 2 HILL0048.D 1311-4161-S1 40.0 NIA 2 HILL0049.D 131 1-4162-S1 c10.0 2 HILL0050.D 131 1-4162MS-S1 165.193594 200 82.60 2 IH I L L 0 0 5 1.D 1311-4163-S1 dO.0 2 HILL0052.D 1311-4164-S1 :10.0 NIA 2 HILL0053.D 1311-4165-51 .:10.0 2 HILL0054.D 1311-4165MS-S1 166.210776 2w 83 11 2 HILL0059.D 131 1-4166-S1 .:10.0 2 HILL0060.D 1311-4167-S1 .:10.0 NIA 2 JHILLOWI.D 1311-4168-S1 .:10.0 2 HILL0062.D 1311-4168MS-S1 164.639012 2w 82.32 2 I HILL0063.D 1311-4169-S1 *:10.0 2 HILLOO64.D 1311-4170-S1 *:10.0 NIA 2 HILL0065.D 131 1-4171-S1 .:10.0 2 HILL0066.D 1311-4171-MS-S1 164.253095 200 82 13 2 HILL0067.D 1311-4172-S1 *'10.0 2 HILLO068.D 1311-4173-S1 10.0 NIA 2 HILL0073.D 131 1 - 4 1 7 4 4 1 10.0 2 HILL0074.D 1311-4174MS-S1 165.168607 200 82.58 2 HILL0075.D 131 1-417 5 4 1 c10.0 2 HILL0076.D HILL0077.D HILL0078.D HILL0079.D HILL0080.D HILL0081.D H I LLOO82. D 1311-4176-S1 131 1- 4 1 7 7 - S l 131 1-4177MS-Si 1 3 1 1 - 4 17 8 - S 1 1311-4179-S1 1311-4160-S1 1311-4180MS-Sl <10.0 e10.0 162.310247 <10.0 <10.0 e10 0 153 354131 NIA 200 NIA 200 81 16 76 68 2 i 2 2 2 2 2 2 - Analvtical Run Information*: Acceptable Quanl Range: 10 1002nglml Calibration Curve I+ 0.9979335 Target Analyte: PFOS Internal Standard: NONE 3M Environmental Laboratory Page 246 of 703 BACK TO MAIN -Sample Data File HILL0031.D HILL0032.D HILL0033.D HILL0034.D HILL0035.D HILL0036.D HILL0037.D HILL0038.D HlLL0039.D HILL0040.D HlLL0045.D HILL0046.D HILL0047.D HILL0048.D HILL0049.D HILL0050.D HILL0051.D HILL0052.D HILL0053.D HILLOO54.D HILL0059.D HILL0060.D HILL0061.D HILL0062.D HILL0063.D HILL0064.D HILL0065.D HILL0066.D k!uuwAB Y111nn71n &4luaw2 l.luwWa lduaaba 8duaw6a MuawZ,D 4=uuawa Sample Description 131 1-5043-S1 131 1 - 5 0 4 4 - 51 1311-5045-51 1311-5045MS-S1 1311-5049-51 1311 - 5 0 5 0 4 1 1311-5051-51 1311-5051MS-S1 13 11 - 5 0 7 9 4 1 1311-5080-S1 1311-5081-51 1311-5081MS-S1 1311-5085-S1 131 1-5086-51 1311-5087-51 1311-5087MSS1 13 11-5091-S1 1311-5092-51 13 11 - 5 0 9 3 - 5 1 1311-5093MSS1 1311-512141 1311-512241 1311-5123-51 1311-5123MS-51 1311-5157-S1 1311-5158-S1 -1311-515 9 4 1 1311-5159MS-S1 4aMA#GS 4%uaa&s %wsa3&a 4su&%Gs dauswxa 434&w-u sa&umss - Analytical Run Information*: Acceptable Quant Range: 5 1002ng/ml Calibration Curve +: 0.9998940 Target Analyte: PFOS Internal Standard: THPFOS Measured Concentration. uglL Theoretical Matrix Splke Concentratlon, UglL Replicate Sample %RSD 91.891635 56.765171 102.487507 326.622579 28.59 200 41.747357 51.741309 18.18 38.024002 234.690722 96.606457 121.213214 91.012507 305.185315 52.079333 51.355299 51.676981 256.670403 40.692073 12,250295 7.04131 228.112564 200 15.61 200 0.70 2w 90.58 200 437.953237 503.530248 423.370937 746.07087 56.237274 86.08401 9.39 200 23.15 87.843563 305.646245 a.%l&Sw 6aZ3.60 4 406Sw64 LAC 44 44 rFC0 2w Za.30 wa blA4 wa Matrix Splke Recovery, % 163 31 117.35 152 59 128.34 114.06 313.04 152.82 62.a blA4 sludge samples willbe quanted without the IS Dilution Factor, Nx 10 10 10 10 100 100 100 1w 10 10 10 10 100 1w i 00 1w 2 2 2 2 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 247 of 703 BACK TO MAIN QualityControlSample Data Sample Data File Sample Description k4ucaaD l4Wu3.D 44uwxaB MiWxe.0 kiuoB%D i4uLwsD &uucw6s HILL0067.D HILL0072.D HILL0073.D HILL0074.D HILL0075.D HILL0076.D HILL0077.D HILL0078.D --- a3u&aza m dauAsu4 43ua5as 131 1-5181-51 131I-5182-S1 1311-5183-51 1311-5183MS-S1 1311-519961 131 1-5200-S1 1311-5201-S1 1311-5201MS-S1 - Analvtical Run Information*: AcceptableQuanl Range: 10 1002ng/ml Calibration Curve ?: 0.9979335 Target Analyte: PFOS Internal Standard: NONE Instrument: Hillan/ Run ID: H010405, external standard quant Theoretical Matrix Measured Spike Concentratlon, Concentration, UglL ug/L aauuD34 55d44au awsCla8 Replicate Sample %RSD looI Matrix Spik Recoveiy, 01 1011.17Co 4oUw44a CIPIPlfi") C511nf?l cbwzzu asu4zsz asas364 27.424377 c 10.0 C'10.0 144.847675 e' 0.0 e' 0.0 e.o.0 131.884428 M6 ana 1554 2.w #DIVrni 2w NIA 2w .wu!a ULID 72.42 65 93 uanted using lernal andard. this ?tanot used Dilution Factor, Nx 10 10 10 10 1W 100 100 1w 10 10 10 IO 1w 1W 100 1W 2 2 2 2 10 10 10 10 100 1W 1W 1w 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 248 of 703 BACK TO MAIN Qualitv Control Sample Data Sample Data File RUSH0032.D RUSH0033.D RUSH0034.D RUSHOO35.D RUSHO036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0040.D RUSH0041.D RUSHO046.D RUSH0047.D IRUSH0048.D RUSHOO49.D RUSH0050.D RUSHOO5l.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.D RUSH0060.D RUSH0061.D RUSHOO62.D RUSHOO63.D RUSHO064.D RUSHOO65.D RUSH0066.D RUSH0067.D RUSHOO66.D RUSH0069.D RUSH0074.D RUSH0075.D IRUSH0076.D RUSH0077.D RUSH0078.D RUSHO079.D RUSH0084.D RUSH0085.D RUSHOO86.D RUSH0087.D RUSHOO88.D RUSH0089.D RUSH0090.D RUSH0091.D Sample Description 1311-5124-S1 1311-5125-3 1311-5126-S1 1311-5126MS-S1 1311-5127-S1 1311-512 8 - 3 1311-5129-S1 1311-5129MS-SI 1311-5130-S1 1311-5131-S1 1311-513241 1311-5132MS-S1 1311-5133-51 1311-513431 1311-5135-S1 1311-5135MS-S1 1311-5136-51 1311-513731 1311-5138-S1 1311-5138MS-S1 1311-513 9 41 1311-5140-81 1311-514141 1311-5141MS-S1 1311-5142-S1 1311-514 3 4 1 1311-514441 1311-5144MS-SI 1311-514541 1311-5146-Si 1311-514741 1311-5147MS-SI 1311-5148-S1 1311-5149-S1 131I-5150-SI 1311-5150MS-SI 1311-5151-SI 1311-515 2 4 1 1311-5153-S1 1311-5153MS-S1 1311-515441 1311-515SS1 1311-5156-S1 1311-5156MS-S1 R010412 Instrument: Rush -Run ID: _ R01_04_ 12 Measured Concentration, uglL 235.149546 235.642534 230.804348 493.847976 21,144501 40.0 -40.0 221.257013 24.842763 18.057138 25.246348 254.141 1 1 12.234056 133.554484 135.817446 386.683935 85.185002 76.528101 75.760492 321.006503 157.041946 155.224502 154.501564 424.195113 109.207528 99.477125 96.43578 343.24391 1 c10.0 40.0 <10.0 220.445044 123.282427 90.083398 152.507888 423.934455 470.275971 481.768175 461.552835 867.494012 259.294489 273.244648 260.405148 559.64233 IneoreIicai Matrix Spike Concentration, uglL Replicate Sample %RSD 1.14 200 N/A 200 17.78 200 10.23 200 6.61 200 0.84 200 6.56 200 NIA 200 25.61 200 2.15 200 2.93 200 Matrix Spike Recovery, % 131.52 110.63 114.45 125 43 122.62 134.85 123.40 110.22 135.71 202.97 149.62 Analytical Run Information': Acceptable Quant Range: 10 - 1002ng/ml Calibration Curve ?: 0.9999132 Target Analyte: PFOS InternalStandard: THPFOS 3M Environmental Laboratory Page 249 of 703 BACK TO MAIN Qualitv Control Sample Data Sample Data File IHILL0031.D HILL0032.D HILL0033.D HILL0034.D HILL0035.D HILL0036.D HiLL0037.D HILL0038.D HILL0039.D HILL0040.D HILL0045.D HILL0046.D HILL0047.D HILL0048.D HILL0049.D HILL0052.D HILL0053.D HILL0054.D HILL0059.D HILL0060.D HILL0061.D HILL0062.D IHILL0063.D HILL0064.D HILL0065.D HILL0066.D Sample Description 1311-518431 1311-5185-SI 1311-518641 1311-5186MS-S1 1311-5187-41 1311-5188-S1 1311-5189-S1 1311-5189MS-S1 1311-5190-S1 1311-5191-S1 1311-5192-S1 1311-5192MS-S1 1311-520241 1311-5203-S1 1311-52O4-Sl 1311-5204MS-S1 1311-5205-S1 1311-5206-S1 1311-520731 1311-5207MS-S1 1311-5208-S 1 1311-5209-S1 1311-5210 4 1 1311-521OMS-S1 1311-5211-S1 1311-5212-S1 1311-5213-SI 1311-5213MS-S1 Analytical Run Information*: Acceptable Quant Range: 10 - 400.8nglml Calibration Curve ?: 0.9913025 Target Analyte: PFOS Internal Standard: THPFOS H010412 Instrument: Hillary _ Ru_ n ID_: _ H0_ 10_ 412 Measured Concentration, uglL < 10.0 < 10.0 < 10.0 124.150116 < 10.0 < 10.0 < 10.0 125.816424 11.327739 14.704513 < 10.0 204.597109 < 10.0 < 10.0 10.0 110.900636 < 10.0 < 10.0 < 10.0 118.227093 14.126747 11.420901 10.0 194.375995 14.879531 23.895092 24.461872 215.92261 1 Matrix Spike Concentration, uglL Replicate Sample %RSD NIA 200 NIA 200 18.34 200 NIA 200 NIA 200 14.98 200 25.51 200 Matrix SDikf Recove&, ?4 62.08 62.91 102.30 55.45 59.11 97.19 95.73 3M Environmental Laboratory Page 250 of 703 BACK TO MAIN Qualltv Control Sample Data HlLLW33 D HILLW34.D HILLW35.D HILLOO36.D HILLW37.D HlLLW38.D HILLO039.D H1LLOMO.D HILLW45.D HILLW48.D HILLW47.D HILLOM8.D HILLW49.D HILLW50.D HILLW51.D HlLLW52.D HiLL0053.D HILLW54.D HlLLW59.D HILLO06O.D HILLW61.D tilLLW62.D HILLWB3.D HILLCOS4.D HILLW65.O H1LLWBB.D HILLW67.D HILLW68.D HILLW73.D HILLW74.D HILLW75.D HILLW76.D HILLO077.D HILLOO78.D HlLLW79.D HILLW8O.D HILLW8l.D HlLLW82 D HILL0087.D HILLW88.D HILLW89.D HlLL009O.D HILLW9l.D HILLW92.D HILLCW3.D HILLOCB4.D HlLLW95.D HILL0WS.D HILLO1Ol.D HILL0102.D HlLL0103.D HILLO1M.D HlLL0105.D HILLO1DS.D HILLOl07.D HILLD1OB.D WLLO(C+D HILLO1lO.D HlLLO115.D HILLOll6.D HILL0117.D HILLO118.D HILLO119.D HILLO~ZO.D HILL012l.D HILLO12Z.D HlLLOl23.D HILLO124.D HILLOIZB.D HILL0130.D HILLO~~I.D HILL0132 D HILL0133 D HILL0134 D HILL0135 D HlLLOlM D -5020-53 -5021-53 -5021MS-53 -5055-53 -5056S3 -5057.53 -5057MS-53 -5091-53 -5092-53 -5093-53 -5O93MS-53 -5127-53 -5128-53 -5129-S3 -5129M-3 -5163-53 -5164-53 -516553 -5165MSS3 -5189-55 -52-3 -5201-53 -5201MS-53 -5022-53 -5023-53 -502443 -5024MS-53 -5058-53 -505&53 -5060-53 -5ffiOMS-53 -5094.53 -509553 6-53 -5W6MS-53 -5130-53 -5132-53 -5132MS-53 -5166-53 -5167S3 -516553 -515BMSS3 -5202-53 -520553 -5204.55 -52MMS-53 -5025-53 -502653 -5027-53 -5027MS-53 -506143 -5062-53 -506553 -5063MS-53 -5097-53 -5008S3 509953 -5woMS53 6133-53 -5134-53 -5135-53 -5135MSS3 -5169-53 -5i70-s~ -5171-53 -5171MS-53 -520553 -52M.53 .uo7-sa -52071553 -5028-53 -5029.53 -5030-53 -5030MS-53 -5oBcS3 -506553 Analvtical Run Information': AmpUMe Quint R a w : 5.1WZndd CallbnWmC u m 8:0.9978856 Taw1 AnWe: PFOS InternalStsndaW THPFOS -- Instrument: Nilllry Run ID: H010316 C 5.0 c 5.0 193.2 XI) 5.0 c 5.0 NIA < 5.0 198.3 2m 10.9 27 8 81.5 r50 187.3 2m < 5.0 < 5.0 Nm < 5.0 207.2 am < 5.0 c 5.0 NIA < 5.0 199.1 W c5.0 < 5.0 MIA c 5.0 172.7 W <so c 5.0 Nm < 5.0 190.5 2m 42 0 48.9 4463 57.0 261 8 203 56.4 45 9 1221 57.9 268.0 W 111.6 8- 98.8 333.9 2m 142.0 99.1 37% 65.7 281.1 83 33.3 25.2 11124 30.1 205.7 205 ~50 < 5.0 NIA < 5.0 193.0 W 159.8 203.2 11W i7,4E180.8 4164 161.9 173.0 184 7 557.2 393 7 375.2 331.3 298.3 857.1 327.9 2m D1s m ,~ ~ 598.5 97.6 127.8 98.9 301.6 5.6. c50 5 42 60 2W 4 2m 461 1 285 5 86 11t gs 14 8367 ,ma 989 us% sn lm 44 1m5 ,4757 w.n 87W mu) 11763 181IJ 117 93 ,3532 101 55 87 47 Dllulion Level. Nx 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 L winternalstsndard n6pmse 2 2 2 2 l o w lnbrnal rlanderd n 6 p n 8 s 2 2 2 2 Low Internalslandard nsponse 2 2 2 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 251 of 703 BACK TO MAIN QualiW Control Sample Data Instrument: Hillary _ Run_ID:-H010311 Sample Dab File HILLW38.D HILLO037.D HILLW38 D HILLW39.D HILLOM0.D HlLLOMl D HILLOM2.D HILLOM3.D HILLOO44.D HILL0045.D HILLO050.D HiLLoai.~ HILLW52.D HILLW53.D HILL0054.D HILL0055.D HILLW58.D HILL0057.D HILLOO58.D HILL0059.D HILL0064.D HILLOffi5.D H1LLW.D HILLOffi7.D HILLW8.D HILL0069.D HILL0070.D HILL0071.D HILLOO72.D HILLW73.D HILLW78.D HlLLW79.D HILLWB0.D HILLOO81.D HILLW82.D HILLCO33.D HILLW84.D HILLW85.D HILLW86.D HILL0087.D HILLW92.D HILLOOB3.D HILL0094.D HlLLW95.D H1LLWSS.D HILLW97.D HILLW98.D HILLWg9.D HILL01W.D HILLOlO1.D HILLO1ffi.D HILLOlO7.D HILLO1DB.D HILLOlO9.D HILLO11O.D HILL0111.0 HILL0112.D HILLOf<J.D HILLOl34.D HILLOl15.D WLKuaUD HILL0121.D HILLO122.D HILL0123.D HILL01240 uuwl6.0 uuLca&o YlLLOuLD YlLLDIlPp HILLO133.D HILLOl34.D HILL0135.D HILLOl36.D HILL0137.D HILLOl38.D HILLO139.D HILL0140.D Sample h c l i p l l o n E00-1311-4059-S7 EW-l311-4060-S7 ~00-13i1.4064-s7 EW-1311-4ffi5S7 EW-1311.408gS7 EW-1311-4088-S7 EW-13114089S7 00-1311-4090-S7 EW-13114094-57 EW-13114085S7 EW-l3114O%S7 EW-1311-411E-S7 EW-13114118-S7 E00-1311-4120-S7 EW-13114004S8 EW-1311-4W5-SE EW-13114W6S8 EW-lJt140ffiMS-S8 EOC1311-4028-S8 EW-13114030-58 EO0-13114030MSSE EW-1311-4034-S8 EW-13114035S8 EW-13114036-SE E00-13134038MS-SB EW-1311-4058-S8 EW-1311-4059-S8 EW-13114060-S8 EOO-1311-4060MSS8 EW-131140MS8 00-1311406558 E00-1311-4066-S8 EW-1311-4068MS-SO E061311408E-S8 00-13114089-58 EW-1311-4090-S8 EW-1311.409OMS-SB EW-1311-4094-58 EW-13114085-S8 EDLL1371-4096.S8 EO0-1311-4098MSS6 E00-131441lE-SB EW-1311-4118-S8 E00-13114120-S8 E00-1311-4120MSSB EW-1311-5Wl-Sl EW-1311.5W2-Sl EW-1311-5W9-Sl EW-1311-5003MSSl E00-1311-50M-Sl EW-1311-5005S1 E00-1311-5wB-Sl EW-131l-S0ffiMSSl E00-1311-5W7-Sl E00-1311-5W8-Sl EW-1311-5009Sl EW-1311-5009MS-Sl EW-,JI,-SOIDSI EW-1311-5011-S1 ECC-1311-5012-S1 - E061311-501351 EW-1311-501CSl EW.1311.5015-Sl EW-1311-5015MS-Sl - - - EW-1311S019-Sl EW-1311-5020-Sl EW-1311.5021-SI E00-1311-5021MS-Sl EW-1311-5022-51 EW-1311-502381 EW.1311-5024-Sl EW-t31 1-5024MS-S1 I"C0rnnE.l Ma."* Maarund Spike COnoCnlnlion, Qmsenlnllon, 25 2 24.5 C 5.0 C 5.0 C 5.0 37.7 42.6 38 4 d50 c 5.0 C 5.0 29.5 28.8 28 9 C 5.0 c 5.0 r5O 205.4 100 12 3 10.4 214.9 W c50 < 5.0 < 5.0 205.9 W 29.8 11 5 25.7 241.8 80 < 5.0 c 5.0 C 5.0 213.8 W 40.2 41 4 37.5 256.5 W <50 < 5.0 5.0 1984 80 < 5.0 29.7 25.6 246.5 W 14.1 < 5.0 < 5.0 221.8 W 188.1 197.5 196.5 428.8 W 253.2 183.8 169.5 415.6 80 435.7 403.3 406.6 M nl 102.7 110.0 102.9 311.8 W 605.a OlLO 6s.s ml.6 W 15.6 5.0 < 5.0 207.9 W 188.8 193.1 203.3 437.0 W Repllcih NII 8 e7 WA ,e2 WA I 1 52 NIA 43m WA 5m Nm 10 s WA 0 e1 2212 4.33 IS4 463 WA 149 Malrlx Spike rm 69 ,m2* 1m 83 lWG2 106 m 417901071 10951 ISd30% DBW 41045 4,082 145 I. 3nm w > 501n#d 101 1 > 5oln#d >mlndd > 501n#d mu >5Oln#rd m3sl IIBS NI 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 10 10 10 10 1W 1w 1w 1w 100 100 1W 100 2 2 2 2 2 2 2 2 Analvtkal Run Information.: AcceptableOuanlRsnps 5 - 501n#mI t 3M Environmental Laboratory Page 252 of 703 BACK TO MAIN Qualitv Control Samale Data RUSHW33 D RUSH0034 D I RUSH0035 D RUSHOO36D RUSHW37 D RUSH0038 D RUSHWBD D nuwowaa RUSH0045 D RUSH0046 D RUSH0047 D RUSH0048 D RUSH0049 D RUSHWSO D RUSHW51 D RUSHW52 D RUSH0053 D RUSH0054 D luwo&aD RUSHOOM) D RUSH0061 D RUSH0062 D RUSH0063 D RUSHW64 D RUSH0065 D RUSH0066 D RUSH0067 D RUSHW68 D RUSHW73.D I RUSHW74.D RUSHW75.D RUSHW76D RUSH0077 D RUSHW78.D RUSH0079.D RUSHWBO D RUSH0081.D RUSHW82.D 13114123-S1 13114123MS-S1 13114124-S1 13114125-S1 13114126-S1 13114126MS-S1 13114127-Sl 13114129-Sl 13114129MS-SI 13114130 SI 13114131-S1 13114132-Sl 13114132MS-SI 13114133-Sl 13114134-SI 13114135 SI 13114135MS-SI xW44aua 13114137-S1 13114138-S1 13114138MS-Si 13114139-S1 13114140-S1 13114141-S1 13114141MS-S1 1311414281 13114143-S1 13114144-51 13114144MS-S1 13114145-SI 1311-4146-51 13114147-S1 131t4147MS-SI 13114148-S1 13114149-S1 13114150-51 1311 4 15OMS-SI Analvtical Run Information*: Acceptable Quanl Range: 2.5 -ZSO.Sn@!rnl Calibration Curve r? 0.9982281 Target Anawe:PFOS Internal Standard: THPFOS _ins_tru_me_nt:_Ru_sh _ Run_ID:-R010314 Mearurej Concentrat on, Theoretical Matrix Splke Concentration. Replicate Matrix Spike I e25 197 9 <25 <25 c25 1994 37 0 45Wl 27 3 231 6 24 3 21 9 25 0 232 9 225 23 3 23 7 225 7 GM 22 8 23 2 228 1 20 7 20 4 21 0 228 2 20 4 21 3 20.7 224.5 19.5 192 190 223.2 20.1 20.0 20.2 224.3 zw NIA 200 21 30 m 6 71 200 2 75 200 "NO Mernal StandardDelsded I17 200 143 2w 2 05 2W 200 0.29 2W 98 95 1 99 68 10217 10395 10096 10242 10362 101.88 102.09 IO204 Calculation (N 0.923233823 'Ptid neaviy 4128 ."mmrm out. 0 ".I". 0.M. andh e mabir IC abvlom Outlier was spike passed. Dilution Factor, NX 10 10 10 10 10 10 10 10 IO 10 IO 10 IO 10 IO 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 3M Environmental Laboratory Page 253 of 703 BACK TO MAIN Qualitv Control Sample Data i n s t r u m e n t Hillary - R u n ID: - HOT0313 HILLW32.D HILLW33.D HILLW34.D HILLW35.D HILLW36.D HILLW37.D HILLOO38.D HILLW39.D HILLW0.D MLLcaLD i4uow6a kbuuw&D &4uaMaD n&UMaD HILLW5O.D HILLW51.D HILL0052.D u4ucsaa HILLW54.D HILLW59.D H1LLWGO.D HILL0061.D HILL0062.D HILL0063.D HILLD064.D HlLL0065.D HILLW66.D HILL0067.D E00-1311-5063-S2 E00-1311-5063MS-S2 00-1311-50M-S2 . E00-1311-5065-S2 00-1311-5066-S2 EW-1311-5066MS-S2 E00-1311-5067-S2 E00-1311-5C68-S2 E00-1311-5069-S2 - - - ' - E00-1311-5091-S2 EW-1311-5092-S2 EW-1311-5093-S2 - 00-1311-5094-S2 EW-1311-5095-S2 EW-1311-5W6-SZ EM-1311-5096MS-S2 EW-1311-5097-S2 EW-1311-5098-S2 EW-I3115099-S2 EW-1311-5WSMS-S2 EW-1311-5100-S2 EW-1311-510l-S2 53.1 252 7 1147 120 2 188 2 415 8 438.9 417.8 333.4 ea lozls u67.6 44aJ2 11404 137 3 49.1. 33.t 13Lb 41.7 35.2 34.E 250.2 127 126.' 135.!i 353.c; 334 i' 327.6 200 29.03 200 14.08 100 16 17 100 75.71 100 1012 2w 4.01 2QQ 2.19 99.62 Calculation (N= 3) 113.82 +LZ10 laCUn ,501 nUmL ,501 ngmL ,501 nglrnL ,501 WmL ,501 "gmL 30WQ I S T k 7 W Q.844821802 107 79 laem - A n a l V t i c a l R u n Information': AcceptablePuanl Range 5 501nglml Calibrationcurve rZ: 0.9961319 Target Analyte: PFOS Internal Standard: THPFOS Dilution Factor, Nx 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 254 of 703 BACK TO MAIN Quality Control Sample Data -- Instrument: Rush Run I D R010309 I hsontied Melrlx Measured Spike Concenldion. Concentration. Rwilisate M m x Spike RUSH0470 D RUSH0071D RUSH0472 D RUSH0073 D RUSH0476 D RUSHW79D RUSHWB0.D RUSHW81.0 RUSHWB2.D RUSHW83.D RUSHWBI D RUSHOO65.D F4USHOOBB.D RUSH0067.D RUSH0W.D RUSH0093.D RUSHWO4.D RUSHWg5.D RUSHW98.D RUSHOOg7.D RUSHW98.D RUSH0DgB.D RUSHO1OO.D RUSHO1Ol.D RUSH0106.D RUSHO107.D RUSHOlO6.D RUSHOlO9.D RUSHO1lO.D RUSHO1Il.D RUSH0112.D RUSH0113 D RUSHO114.D RUSHO11S.D RUSHOl2O.D RUSH0121.D RUSH0122.D RUSH0123D RUSH0124.D RUSH0125.D RUSHO126.D RUSH0127.D RUSH0128.D RUSH0129.D RUSHO134.D RUSHO135.D RUSHO1JS.D RUSH0137.D RUSHOl38.D RUSHOl39.D RUSHOl4O.D 1311406555 1311-406855 13114066-55 1311-4069-S5 13i1-409as5 1311409CSS 1311-409555 13114096-55 1311-4115S5 1311-4llsS5 i311-412as5 1311-4004S6 1311-400556 13114wB-% 13114006MS-56 13114025% 1311-403a56 13114OMMSSB 1311-403CS6 1311-4036S6 1311403656 1311-4026MSSB 1311-405as6 13114059.56 1311-406056 13114ffiOMS-56 1311~oBcS6 1311-4065sB 1311-406646 1311-4066MS% 1311-408a~6 13,140L)B-SB 13114CSUS6 1311409OMSSB 13114OgcS6 1311-4095SB 1311-4w6-S6 1311-409sMS-SB 13114iia~g 1311-4119-S6 1311-4120-sB 1311412OMSS6 13114WCS7 1311-4W5S7 1311-4006-S7 13114025S7 1311-4030-S7 1311-403cS7 1311403587 1311-4036-57 13114OSBS7 - Analvtical Run Infonnatlon': AccepUMs Quanl R a w : 5 250.5n!dml Calibbsn CUM ?. 09926833 Targelhalfla: PFOS lnlernd Standard:THPFOS 40 3 43 6 45 4 <5 0 4.0 L5.0 16.9 24 1 26.3 4.0 c5.0 -50 217.8 9.9 9.4 241.4 <5.0 <5.0 4.0 226.5 29 6 26.0 27.2 208.2 rs.0 c5.0 4.0 220.6 36.5 40.5 36.7 260.5 s5.0 <S.O 4.0 211.0 29.6 28.5 2b 9 262.6 <5 0 ~5.0 4 0 9.9 10.1 e.0 6.9 -5.0 27.7 WA ((I 31 WA 2m 3.W Nm 2m 4W 2m WA 2m I a2 zm WA m 6 IB 205 HIA Ifa WA ICs 8 ,160 ll3.3 900 (@a3 1102 103 4 (155 Dilution Factor. NK 2 2 2 1 2 2 2 2 2 2 2 2 2 2 2 2 2 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 a 2 2 2 2 2 2 2 2 2 2 1 2 2 2 2 2 2 2 1 2 2 1 2 2 2 2 2 2 2 7 2 7 1 2 2 2 3M Environmental Laboratory Page 255 of 703 BACK TO MAIN Qualitv Control Sample Data Instrument: Hillaly Run ID: H010309 HILL0125.D EW-1311-4085-S3 HILLll126.D E00-1311-41i8S3 8.254569 HILL0127.D EW-1311-4118-S3 < 5.0 HILL0128.D EW-1311-4120-S3 45.097179 HiLL0133.D EW-1311-40W&4 < 5.0 HiLL0134.D EW-1311-4W544 5.0 HILLO135.D EW-1311-4006-S4 5.0 HILL0136.D EW-131I-4028S4 12.302809 HILL0137.D EW-13i1-4030-S4 8.300846 n 47 HILLO1JB.D EW-1311-4024-S4 < 5.0 HILL0139.D EW-131I-4035S4 5.0 WA HILLOi4O.D EOO-13I1-4OMS4 <50 Analvtlcal Run Information': Auepmbla QwnlRings: 5.400.8nglrnl CaliLrabonCurva ?: 0.9924853 T a w 1Analytc: PFOS internalStmd.rd. THPFOS Dllution Factor, NX 10 10 IO 0 10 10 IO 10 10 10 10 10 90 10 IO 10 10 10 10 10 10 10 10 IO 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 i 2 2 1 2 2 2 2 2 2 2 1 3M Environmental Laboratory Page 256 of 703 BACK TO MAIN Qualltv Control SarnDle Data -- _ Instr_ume_nt:-Rush Run ID: mi0222 131140M-S 1I 0 13114WBsl 31.3 Analvtical Run Information': Acceptable Quant Range: 5.0ppb-500.lppb Calibration Curve ?: 0.9999393 Target Analyie: PFOS Internal Standard: THPFOS 'For mom run info. See the Data Review Form includedin lhe Raw Data e 46 127 4.57 NIA NIA ?2 18 7 27 2 78 1.48 0.13 e 57 3 42 1w 89 101 24 24 rn 504 1w35 1w.w 90 38 00883 0.9976 0.9577 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 IO 10 10 10 10 10 10 10 10 10 10 10 10 10 IO 10 10 10 10 10 10 10 High internalstandard response 10 10 10 10 IO 10 10 10 10 10 10 IO 10 IO 10 IO 10 10 10 10 10 10 10 10 10 10 10 10 3M Environmental Laboratory Page 257 of 703 BACK TO MAIN Qualitv Control Samole Data -;ample Data File HILL0037.D HILLW38.D HILLW39.D HILLW40.D HILLW41.D HlLL0042.D HILLW43.D HILLOW4.D HILLW45.D HILL0046.D HILLO051.D HILLW52.D HILL0053.D H1LLWM.D HILL0055 D HILLW56.D HILLW57.D HILLW5B.D HILLW59.D HILLW6O.D HILLOC65.D HILLW66.D HILL0067.D HILLW68.D HILL0069 D HILLW70.D HILL0071 D HILLW72.D HlLLW73.D HILLW74.D HILLW79.D HILL0080 D HILLW8f.D HlLLOOd2.D HILL0083.D HILL0084 D HlLL0085.D HILLW86.D HILLW87.D HILLW88.D HILLW93.D HILLW94.D HILLW95.D HILLW96.D HILLW97.D HILLW98.D HILLW99.D HILL0100.D HILLOIOI.D HILL0102.D HILL0107.D HILLO1W.D HILL0109.D HILLO1lO.D HILL01l l . D HILLO11Z.D HILLO113.D HILL0114.D HILLOI15.D HILL0116.D HILLOl21.D HILL0122.D HILL0123.D HILL0124.D HILL0125.D HILL0126.D HILL0127.D HILL0128.D Sample Description 13114001-S1 13114002-SI 1311 4 W 3 - S l 13114003MS-S1 1311 4 W 4 - S l 13114W5-Sl 13114006-Sl 13114W6MS-Sl 13114W791 13114WB-SI 13114009-Sl 13114W9MS-SI 13114010-S1 13114011-S1 13114012-SI 13114012MS-S1 13114013-S1 13114014-S1 1311 4 0 15-S1 13114015MS-S1 13114016Sl 13114017-SI 13114018-S1 1311 4 0 18MSS1 13114019-S1 1311402oS1 1311-4021-SI 13114021MS-SI f311-4022-S1 13114023-S1 13114024-Sl 13114024MS-S1 131f-4025-Sl f31f-4026-Sl 13114027-S1 13114027MS-51 fJfi-4028-Sf 13114029-S1 13114030-SI 13114030MS-S1 13114031-S1 13114032-S1 13114033-SI 13114033MS-S1 1311403491 1311 4 0 3 S S 1 13114036-S1 13114036MS-S1 13114037-51 13114038-SI 13114039-S1 1311-4039MS-S1 13114040-S1 1311-4041-51 13114042-Sl 13114042MS-S1 13114043-S1 1311-4044-SI 13114O45-Sl 13114045MS-SI 13114046-S1 13114047-SI 13114048-Sl 13114048MS-S1 13114049-SI 131l-lO50-Sl 1311405151 13114051MS-SI 5.0 <50 204.7 5.0 c 5.0 5.0 204.3 51 2 55.2 86.0 256.1 52.8 52.4 50.9 247.2 51.1 52.4 52.6 251.1 51.9 50.2 51.4 245.8 49.0 50.7 50.2 247.5 55.8 49.3 52.2 247.3 52.0 49.7 52.2 249.1 50.5 53 4 51.0 248.3 c 5.0 < 5.0 < 5.0 200.9 c50 c 5.0 36.6 33 0 224.8 10.4 1.1. 3. 210 8 11.5 9.9 10.2 209.8 13.6 11.2 12.9 211 8 9.5 8.7 10.4 209.5 Analytical Run Information': Acceptable auant Range 5 Oppb-250 5ppb Calibralion Curve? 0 9983566 Target Analyts PFOS Internal Standard THPFOS T o r more run info See the Data ReviewForm includedin the Raw Data Instrument: _ Run_ID:-H010222 ThForeticdl- NIA 2w NIA 2w 29.70 2w 1.92 2w 1.411 2w 1.71 2w 1.76 ZOO 622 200 2.71 200 199 2w NlA m NIA 11.75 2w 7.95 200 9 79 204 11.76 200 102.15 102.15 115.05 98.17 99.29 87.19 98.67 97.54 9812 98.65 100.45 99.75 99.81 99 41 98.59 Dilution 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 IO 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 3M Environmental Laboratory Page 258 of 703 BACK TO MAIN Quality Control Sample Data 1311-4153-51 - Analvtical Run Information': Acceptable Quant Range: 2.5 1002nglrnl CalibrationCurve r! 0.9987251 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Hillary Run ID: H010402 fA) .:2.5 IS> 130% IS, 130% IS> 130% IS> 130% IS, 130% IS> 130% IS> 130% IS, 130% IS> 130% IS> 130% Dilution Factor, Nx 2 2 10 10 10 10 10 10 10 10 100 100 100 1CQ 2 2 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 259 of 703 BACK TO MAIN Quality Control Sample Data I RUSHO038.D RUSHO039.D RUSH0040.D RUSH0041.D RUSH0042.D IRUSH0043.D RUSHO048.D RUSH0049.D RUSHOO5O.D RUSH0051.D 131 1-5026-S1 1311-5027-51 1311-5027MS-SI 131 1-5028-S1 131 1-5029-S1 1311-5030-S1 1311-5030MS-S1 1311-5031-51 1311-5032-51 1311-5033-51 RUSHO054.D RUSHOO55.D RUSHO056.D RUSH0057.D RUSH0062.D RUSHO063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSHO068.D RUSHO069.D RUSH0070.D RUSH0071.D RUSH0076.D RUSH0077.D RUSH0078.D RUSHO079.D RUSHO080.D R U S H 0 0 8 1.D RUSHO082.D RUSH0083.D RUSHO084.D RUSHO085.D RUSH0090.D RUSH0091.D RUSH0092.D RUSHOO93.D RUSH0094.D RUSHO095.D RUSHO096.D RUSHO097.D RUSHOOS8.D RUSHO099.D 1311-5035-51 1311-5036-SI 131 1-5036MS-S1 1311 - 5 0 3 7 6 1 1311-5038-1s 1311 - 5 0 3 9 4 1 131 1-5039MS-S1 1311-5040-51 131 1 - 5 0 4 14 1 131 1-5042-S1 1311-5042MS-St 1311-5043-81 131 1-5044S1 1311-5045-S1 1311-5045MS-S1 1311-5046-51 1311 - 5 0 4 7 4 1 1311-5048-51 131 1-5048MS-S1 1311 - 5 0 4 9 4 1 131I-5050-1s 1311-5051-SI 1311-5051MS-S1 1311-5052-S1 1311-5053-S1 1311-5054-51 1 3 11- 5 0 5 4 M S - S 1 1311-5055-SI 131 1 - 5 0 5 6 4 1 1311-5057-SI 1311-5057MS-S1 1311-5058-Si 1311 - 5 0 5 9 4 1 1311-5060-Si Analvtical Run Information": Acceptable Cluant Range: 5 - 5Olng/ml Calibration C u r v e ?: 0.9997025 Target Analyle: PFOS Internal Standard: THPFOS Instrument: Rush -Ru_n ID_: R_010329a Measured Concentration, ugn 159.93 152.92 143.26 415.70 391.37 230.09 387.34 > 501 82.81 85.11 80.38 329.29 404.55 414.16 433.98 > 501 13.57 5.0 5.0 205.86 99.69 96.20 58.15 306.23 460.98 305.78 > 501 > 501 183.73 166.25 156.55 423.27 359.52 > 501 351.66 > 501 211.71 253.43 207.41 499.47 41.77 10.29 5.71 227.32 31.83 34.15 32.79 Matrix Spike Concentration, wn- Replicate Sample %RSD Matrix Spike Recovery, X 5.50 200 136.22 27.35 201 286 . NIA 202 123 2 2 3 59 203 NIA NIA 204 NIA 27.21 205 121.02 28.62 206 NIA 8 16 207 128 85 1.56 208 NIA 11.34 209 138 74 101.93 210 105.53 3.54 Dilution Factor, NX 10 10 10 10 10 10 10 10 1w 1w 100 100 100 100 100 100 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 3M Environmental Laboratory Page 260 of 703 BACK TO MAIN Qualitv Control Sample Data Sample Data File RUSHO120.D RUSH0121.D RUSH0122.D RUSH0123.D RUSH0124.D RUSH0125.D RUSH0126.D RUSH0127.D RUSH0128.D RUSH0129.D RUSH0134.D RUSH0135.D RUSH0136.D IRUSH0137.D RUSH0138.D RUSH0139.D RUSH0140.D RUSH0141.D RUSH0142.D IRUSH0143.D RUSH0148.D RUSH0149.D RUSH0150.D R U S H 0 151.D RUSH0152.D RUSH0153.D RUSH0154.D RUSH0155.D RUSH0156.D RUSH0157.D RUSH0162.D RUSH0163.D RUSH0164.D RUSH0165.D RUSH0166.D RUSH0167.D RUSH0168.D RUSH0169.D RUSH0170.D RUSH0171.D RUSH0176.D RUSH0177.D RUSH0178.D RUSH0179.D Sample Description 1311-5060MS-S1 131 1-5061-S1 1311-5062-51 1311-5063-S1 131 1-5063MS-S1 131 1-5064-S1 1311 - 5 0 6 5 4 1 1311-5066-51 1311-5066MS-S1 1311 - 5 0 6 7 4 1 1311-506841 131 1-5069-S1 1311-5069MS-S1 131I-5070-SI 1311-507141 131 1 - 5 0 7 2 4 1 1311-5072MS-S1 1311-5073-51 1311-507441 1311-507541 1311-5075MS-S1 1311-5076-S1 1311-507761 1 3 11- 5 0 7 8 - S 1 131 1-5078MS-S1 131 1-5079-S1 131 1-5080-S1 1311-5081-S1 1311-5081MS-S1 131 1-5082-S1 1311-5083-S1 131 1 - 5 0 8 4 4 1 1311-5084MS-S1 131 1-5085-S1 1311-5086-51 1311 - 5 0 8 7 4 1 1311-5087MS-SI 1311-5088-51 1311-5089-Si 1311-5090-S1 1311-5091-S1 131 1-5092-S1 1311-5093-SI 1311-5093MS-SI - Analytical Run Information*: Acceptable Quant Range: 5.0 5Olnglml CalibrationCurve ?: 0,9998900 Target Analyte: PFOS Internal Standard: THPFOS Instrument: &&I Run ID: R010329b Measured Concentration, ug/L .:5.0 g. 5.0 5.0 > 501 > 501 > 501 > 501 5 501 > 501 > 501 > 501 c 5.0 254.22 135.13 141.11 142.97 427.65 83.18 77.82 77.95 329.52 179.53 187.10 171.68 465.00 101.23 103.30 109.27 359.43 207.59 75.82 75.66 95.65 324.00 486.79 238.27 236.36 226.44 303.36 279.64 283.95 29.08 5.29 221.42 Matrix Spike Concentration, UglL Replicate Sample %RSD 2.93 2w 3.84 200 4.30 200 200 NIA 2w 13.95 200 NIA 2w 2.72 2w NIA 2w 4.37 97.90 2w Matrix Spike Recovety, % 142.34 125.78 146.66 125.08 I 103 80 114 18 NIA NIA NIA 110.71 Dilution Factor, Nx 2 2 2 2 2 10 10 10 10 10 10 10 10 1w 100 1W 100 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 10 10 10 10 100 100 100 2 2 2 2 3M Environmental Laboratory Page 261 of 703 BACK TO MAIN Qualltv Control Sample Data -- Instrument: Rush Run ID: R010312 Dllution Factor, NI tm Im im tm 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 IO 10 10 10 10 im IW tm tm 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 1 2 2 2 2 2 2 3M Environmental Laboratory Page 262 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup _ Run ID: s0011_ 20a ~ 500120-078 SOI120-079 00-1311-1533 ohr E00-1311-10W h r EW-1311-1w 5 h r 00-1311-1006 h r 00-1311-1007 h r E00-1311-101524hour, O.lOrngll, SI. C-I 00-1311-101524 hour 0 l0mgh. S2.C.1. MS EW.1311-101624 hwr. 1Omm. S2 Gl EW-1311-101724 hwr, i.Om&. 52. C-I EOD1311-101824hwr. l.Orng/L.S2. GI ECO-1311-101824hwr, 1 Orngh. 52. GI. MS Measured Concentration, Splke Concentration, UgL c24.75 g24.75 44.75 g24.75 <24.75 c24.75 488.97 523.02 544.09 25.86 **~omnmt mwn out 64.75 <24.75 217.61 2w ~24.75 <24.75 <24 75 253.23 200 462 08 475.12 505 67 71903 2W <24.75 c24.75 <24.75 248.01 200 84.75 c24.75 44.75 254 5 2w 11087 118.37 137.3 344 75 200 Replicate Sample XRSD NIA NIA 5.58 NIA NIA 4.65 NIA NIA 11.15 Matrlx Splk, Recovery, ? 108.81 126.62 106.68 124.01 127 25 103 73 Q-Test Calculation (N = 3) Analvtical Run Information*: Acceptable Ouant Range: 24.75ppb-991.78ppb Calibration Curve ?:0.996939 Target Analyte: PFOS , Internal Standard:THPFOS 'For more run info. See the Data Review Form included in the Raw Data 3M Environmental Laboratory Page 263 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run ID: so01120b Sample Data File ~00120-103 ~00120-104 so01 20-105 so0120-1 06 s00120~110 so0120-1 11 l S 0 O 1 2-0 ~ 1 1 2 ~00120-113 ~00120-114 soolzo-118 S00120~119 s00120~120 so01 20-121 so0120-1 22 sOO120-126 ~00120-127 S00120~128 so0120-1 29 ~00120~130 so0120-1 34 ~00120-135 sOO120-136 ~00120-137 so01 20-138 so0120-1 42 so0120-143 so0120-1 44 so01 20-145 so0120-1 46 SOOl20-150 SOO120~151 ~00120-152 SOO120~153 S00120~154 so01 20-158 SOOlZO 159 Sample Description E00-1311-101924 hour, Omg/L. S1, C-2 E00-1311-102024 hour, OmglL. S1, C-2 E00-1311-1021 24 hour, Omg/L. S1. C-2 E00-1311-102124 hour, Om@, S1. C-2. MS E00-1311-102224 hour, O.lOmglL, S1. '2.2 E00-1311-102324hour.O.lOmgR. Sl.C.2 EM)-1311-102424 hour, O.lOm@L. S1. C.2 E00-1311-1024 24 hour, 0.lOmgR. S1, C.2. MS E00-1311-102524 hour, l.Omgll. S1, C-2 EW-1311-102624 hour, l.OmgR. S1. C-2 E00-1311-102724 hour, 1.OmgiL. S1, C-2 EW-1311-102724 h w r , l.Omg/L. S1, C-2. MS E00-1311-1028 24 hour, O m g l l , S1, C 3 EW-1311-102924 hour, Omg/L. S1. C-3 E00-1311-103024 hour, Om@, S1. C 3 E00-1311-103024 h w r , OmgR, S1. C-3klS E00-1311-1031 24 hour, O.lOmg/L. S1, C-3 EM)-1311-103224h w r , O.lOmglL, S1. C-3 E00-1311-103324 hour, 0.lOmgR. S1, C-3 EW-1311-103324 hour, O.lOmgR, S1. C-:3 MS E00-1311-1034 24 h w r , l.Omg/L. S1. C-3 E00-1311-103524 hour, 1.0mgiL. S1.C-3 E00-1311-103624 hour. l.OmgR. S1. C-3 E00-1311-103824 hour, l.Omg/L. S1. C-3 MS 00-1311-103724 hour, Omg/L. S1. C-4 E00-1311-1038 24 hour, OmgR. S1. C4 EW-1311-103924hour,Omg/L.S1. C-4 E00-1311-1039 24 hour, OmgR. S1. C-4 MS EW-1311-104024hour, 0.lOmgR. S1. C-d. E00-1311-1041 24 hour, O.lOmg/L. S1. C-r E00-1311-104224 hour, 0.lOmgL. S1, C-r E00-1311-1042 24 hour, O.lCmg/L. S1. C-4 MS EW-1311-104324 hour, l.Omg/L. S1. C-4 E00-1311-104424 hour, l.OmgR, S1, C-4 EW-1311-104524 hour, l.0mgA. S1, C4 E00-1311-1045 24 hour. l.Omo/L. S1. C-4 Ids Measured Concentration, uglL c24.75 c24.75 c24.75 340.34 -24.75 c24.75 ~24.75 374.07 457.51 475.62 484.59 790.19 29.19 ~24.75 c24.75 366.46 c24.75 c24.75 c24.75 391.81 465.89 490.86 494.39 824.37 442.75 28.04 <24.75 376.04 c24.75 c24.75 c24.75 389 417.87 455.03 469.4 466.25 Spike Concentration, uglL 200 200 200 200 200 200 200 200 200 Replicate Sample %RSD N/A NIA 2.92 N/A NIA 3.21 124.58 NIA 5.94 Matrix Spikt Recovery, ?4 170.17 187.04 152.80 183.23 195.91 164.99 188.02 194.50 -1.57 Analytical Run Information*: Acceptable Quant Range: 24.75ppb-991.78ppb Calibration Curve ?:0.982880 Target Analyte: PFOS Internal Standard: THPFOS 'For more run info. See the Data Review Form incli ded in the Raw' Data 3 3M EnvironmentalLaboratory Page 264 of 703 Quality Control Samde Data BACK TO MAIN Instrument: Soup _ Run_ID_ : s0_ 011_22a Q-Test 1 IsW122a-059 sOOl22a~060 sW122a 061 lsoo122a&sz sWi22a-068 sm122a 067 sOOi22a-ffi8 soo122a-ffi9 sW122a 070 ~001228-074 sW122a-075 sOO122a-078 ~001228077 s00122a-078 soO122a-082 smi2 2 a ~ ~ s4LIl22a-084 s00122a_o85 rOO122a-086 soO122a_090 sm122a-Wl 00-1311-103024 hour. OmWL, S2. C-3 E00-1311-103024 hour, om,; 52. c-3 MS EW-1311-io31 24 hour, o.iomen. sz.c-3 EW-1311-103224 hour. O.IOm@L. S2. C 3 EW.1311-103324 hour, 0.IOmgA. S2. C-3 EW-1311-103324 hour, O.lOmg/L. S2. C-3 MS EW-1311-103424hour. 1.Omoll. 52. C-3 Em-1311103524 hour, l.omgA. 52. C-3 - EW-1311-103624hour, l.Omg/L.S2.C-3 E00-1311-103624 hour, l.omg/L. 52. c-3 MS EW-1311-103724 hour, om@. S2. C 4 Em-1311-103824 hour. Om& 52. C 4 EW-1311-103924hour. om@, 52. c 4 EM)-1311-103924 hour, O m . S2. C-4 MS EW-1311-104024hour. O.lOmg/L. S2. C 4 E00-1311-104124 hour, o.lOmwL. 52. C4 EW-1311-104224hour.O.lOmg/L. ~ 2 . ~ 4 Em-1311-104224 hour. o.lOmg/L. 52. C 4 MS EW-1311-i04324 hour, l.omg/L. s2. c 4 EW-1311-104424 hour, I.Omg/L. 52. C 4 EW-1311104524 hour, l.Omgh, S2. C4 EW-1311-104524hour. I.OmgfL,S2.C4MS -24.75 439 66 ~24.75 <24 75 q24.75 459 97 261.99 `ii<24.75 g24.75 <24.75 449.6 c24.75 c24.75 44.75 439.78 25.99 84.89 30.68 496.84 3i 1 200 NIA 2M) 2W 21983 1 229.99 246.21 200 224.80 200 69.38 2W 219.89 233.08 0 531145761 0.920373514 I 3M Environmental Laboratory ? Page 265 of 703 BACK TO MAIN Quality Control Sample Data - Instrum- ent: - Tucker -Ru-n_ ID:_ to1_ 0122 Sample Data File 1010122-040 m i01zz-041 to10122-042 1010122-043 1010122-044 1010122-048 1010122-049 1010122-050 1010122-051 to10122-052 m i0122-056 m i0122-057 1010122-058 mioi2z-059 1010122-060 to1 01 22-064 1010122-085 1010122-066 1010122-067 rnioizz-o68 1010122-072 1010122-073 1010122-074 1010122-075 0 10122-076 1010122-080 m io i22-081 to10122-082 1010122-083 1010122-084 lolOl22-088 to10122-089 m i o i22-090 1010122~091 1010122-092 1010122-096 Sample Description EOO-1311-2001. Oug PFOS. conlro1.1122101 CMC 00-1311-2002, Oug PFOS.wntrol,lR2/01 CMC E00-1311-2003. Oug PFOS. wnlro1.1/22/01 CMC EOO-1311-2003ms.Oug PFOS.contml.112Zhl1 CMC E00-1311-2004.0.75ug PFOS.conlro1.1122111 CMC E001311-2005.0.75ug PFOS.mntro1.1/22/11CMC E00-1311-2006.0.75ug PFOS.conlrol.1122/1)1 CMC E00.1311-2W8ms. 0.75ug PFOS. contml.lmm1 CMC E00-1311-2007.7.5ug PFOS. control.1122X)I CMC E00-1311-2008.7.5ug PFOS. control.lRZM I CMC E m 1 3 11-2009.7.5~9PFOS, mnlrol.112Z~CI MC E00-1311-2009ms. 7.5ug PFOS. wnlrol,li2:'/01 CMC E00.1311-2010, Oug PFOS. Clay.lnZM1 ChlC E00.1311-2011. Oug PFOS.Clay,lR2/01 CLlC E001311-2012. Oug PFOS. Clay,1/2ZM1 CklC E00.1311-2012mt. Oug PFOS.Clay.l/ZZMl CMC E00.1311-2013.0.75ug PFOS.Clay.l/2Z/01 CMC EW-1311-2014.0.75ug PFOS,Clay,l/Z2/01 CMC ~ 0 0 - i 3 i i - ~ o i 5 , 0 . 7 5P~F0OS. ciay.inziui CMC E00-1311-2015ms. 0.75ug PFOS,Clay.1122111 CMC E00-1311-2016.7.5ug PFOS. Clay.l/22/01 CMC E00-1311-2017.7.5ugPFOS. Clay.lR2nl CMC EOC-1311-2018.7.5ug PFOS. Clay.lR2C4 CMC E00-1311-2018ms. 7.5ug PFOS. Clay.l/22/0 I CMC EW-1311-2019. Oug PFOS. Sediment.112ZO1 CMC E00.1311-2020. Dug PFOS. Sedimen1,lRZX)I CMC E00-1311-2021. Oug PFOS,Sedimenl,li22/01 CMC E00-1311-2021ms. Oug PFOS. Sedimen1.112:!1 CMC EM)-1311-2022.0.75ug PFOS.Sedimen1,lR:YOl CMC E00-1311-2023.0.75ug PFOS.Sediment.lR:'/Ol CMC EOC-1311-2024.0.75ug PFOS. Sediment.lR:/Ol CMC E00-1311-2024ms. 0.75ug PFOS, Sediment,l122/01CMC EGG1311-2025.7.5ug PFOS. Sedimen1.11221~I1CMC E00-1311-2026.7.5ug PFOS. Sediment,l/Z2/111 CMC E00-1311-2027.7.5ug PFOS. Sediment,l/ZZAM CMC E00131t2027ms. 7.5ug PFOS, Sediment,lL!2/01 CMC Measured Concentration, uglL <25.0 <25.0 c25.0 194.28 95.92 96.85 95.39 331.94 802.01 567.71 671.3 757.91 C25.0 e25.0 g25.0 174.47 63.71 75.13 74.74 275.64 627.98 682.43 461.56 897.56 C25.0 <25.0 -25.0 192.1 109.78 89.72 88.54 250.93 568.24 608.75 625.2 930.32 Matrix Spike Concentration, uglL Replicate Sample %RSD N/A 200 0.77 200 15.72 200 N/A 200 9.11 200 19.48 200 N/A 200 12.43 2w 4.68 200 Matrix Spike Recovery, % 97.14 118.26 43.31 87.24 100.45 218.00 96.05 81.20 152.56 3M Environmental Laboratory Page 266 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run ID: sOOlZll 1001211-037 ~001211-038 a01211 x44 roo1211-M5 r001211-046 I -~001211M 7 s001211-M8 rw1211-052 ~001211~053 rw1211-0% 5001211~055 so0121l b s s *w1211_m rw1211-061 raOl21l-ffi2 s001211_ffi3 sWl2ll-069 ~001211-070 sw1211-071 ~001211072 rwl211-076 1~001211477 sWl2ll-078 ~001211-079 r001211~080 sw1211-084 ~001211-085 Iroo121l_OW ~001211-087 sw1211-088 r001211-082 rW1211-093 ~001211~095 rW1211-103 rOO1211-1M s001211~108 r001211-108 s001211_110 lox EW-1311-3023-S1,O.Om+L. 48hr. 1:lClay. lM7/W lox EO0-1311-3024S1.0Om@-, 48hr. 1:lClay. 1 M 7 W lox E00-1311-3026S1O.OmwL. 48hr. 1 3Clay. l M 7 m 1OxEm1311-3027-Sl o OmWL,48w. 1:6 Clay. 12x17100 lox EW-1311-3027ms-SIO.Omgll, 48hr. 1:s Clay. 1M7fi10 fox ~ ~ 1 3 i i - 3 0o.2om~gl~l. a1hr. I:~~CI.Y. i 2 m m (Ox EW-1311-3029-S1O.Om&. 48hr. 1.25Clay. lM7XK lox EW-1311-3030-SI O.Chn@-, 48hr. 1:25 Clay. 12m7AX 1Ox EW-1311-3030mr-Sl 0.0mgll. 48hr. 125CI9.12107rW lox EW-1311-305841,O.Sm#L. 48hr. 1:lCIay. 12m7Xx) 101 E0&1311-3058-S1.0.5m#L. 48hr, l:lClay, 121071w 10xEW-131lJffi~Sl.0.5mpn.48nr. 1:lClsy. 12m71w 10%EW-1311-3ffiOmcS1,0.5nWL. 48hr, 1:lClay. 12x17ilx) lox EW-1311-3ffil-Sl. 0.5m#L. 48hr. 1:SCI.y. 1M71W i o x ~ m i 3 i i - m z ~ i . o . ~ m4g.ml.l ,I:~CIPY. i m 7 m lox EW-13113063.Sl. OSm+L,48hr, 1:Xlay. 1 M 7 m 1OxE00-1311-3063m-Sl.O.Smg(L.48hr. 1:5CIay, 1M7KO lox E00-1311-30&CSl,O.Smp(L. 48hr. 1:25Clay. 12107/w lox EW-1311i)ffi5-S1,0.5m#L, 48hr. 1:25Clay. 1 M 7 m lOxEW-1311-3056S1.0.5m#L. 48hr. 1:25Ciay. 12107100 lox E00-1311-3086msSlo. .smwL,48hr. 1:2Xlay. 12iU71W 1 0 x ~ ~ - 1 3 i i - 3 0 8 9 - ~.1 . 0 . 5-n nJlBLh. r. i:icIav izm7mo ~ O EXW-1311-3086Sl. O.Sm#L. Mhr. 1:lClay. 1M7/IXI lox EW-1311-3087-S1, 0 5mg(LRM. hr. 1:lCIay. lM71W lox EW-1311-3087ms-SI.osmgll. am,i:ici.y, 1~17101 lox EW-1311-3088Sl. 0.5wL. Whr, 1:5Cl.y. 1207MO lOxEW-1311-3M18-S1,0.5~M.hr. 1 : X l s ~l.m 7 m lox E00-1311-3090Sl.0.5m& 36hr. 1:5CI9. 1M71W (Ox EW-1311-3090ms-S10. .5m+L. Whr. 1:SCI.y. 12x171011 lox E00-1311-3091-Sl.Odmgrl. 36hr. 1:25Clay. 12107/M) lOxEW-13ll-3092-S1.O.5mpllL,Mhr. 1:25U.y. 12x17100 1OXEW-1311-3093-S1. o.5m* Whr. 1:25CIay. 1 m 7 m lox EW-1311-3093mr-Sl. 0 . 5 ~~ .h r1.:25~1ayiz.m711m lOxEW-1311-30'34.S1,O.5mprL.48hr. l:lCl.y, 12x17m lox EW-1311.3095-Sl. 0.5mgll. k8hr. 1:lCI.y. l M 7 m lox EW-1311.3096Sl. 0.5mpll. 18hr.1:lcI.y. i ~ 7 r n o lox EW-1311-309&S1. 0 . 5 m 48hr. 1:5Clay, 1M71w lOxEW-1311-309BSl.O.5mgll. 48hr. 1:K)I.y. 1 M 7 m 101EW-13113099m-S1,0.5m9L. 48hr. 1:5Clay, 121071w 1Ox EW-1311-3100-SI. 0.5mpll. 48hr. 1:25CIpy. 1M7XIO lOxEW-1311i)101-S1.0.5m+L,48hr, 1:ZSClay. 12/07Ro lox E00-1311-3102-SI.0.5m#L. 48hr. 1:25CI.y, 1M71W 1Ox EW-1311-3102msSl.O.h#L. 48hr. 1:25CIay. 12x17101 Measured Concentration, uglL eoreticai Matrix Splke Concentralon, uglL <40.0 ~40.0 e40.0 lgS.55 2w c40.0 <40.0 <40.0 185.82 2w 440.0 ~40.0 c40.0 399.71 2w 130.4 114.48 111.17 306.74 200 293.97 314.29 287.97 655.18 118.92 305.1 'PoinlThmwn 200 0141 128.68 2w 131.97 138.13 44.59 433.65 200 103.26 119.9 129.42 3Y.95 zw 298.09 313.39 288.84 497.01 200 59.14 82.46 69.48 M5.73 2w 92.9 107.W 95.6 286.04 200 301.56 331.37 361.05 555.88 2w Replicate Sample %RSD NIA NIA NIA 8.56 4 62 5.57 49.88 11.27 3.94 8.29 7 85 8.98 Matrlx Splki Recovery, 'I 98.28 92.91 199.86 97.79 183.80 80.61 194.53 102.77 103.69 138.13 95.22 97 42 Analvtical Run Information': Acceptable Quant Range:40.0ppb1001.7ppb Calibration Curve 8:0.992493 TargetAnalyte: PFOS internalStandard:THPFOS 'For more tun info.See the Data ReviewFormIncluded inthe Rau Data Q-Test Calculation (N = 3) 0.947577613 -0.93414582 3M Environmental Laboratory Page 267 of 703 Qualitv Control Sample Data _ Inst_ rum_ ent:-Tucker _ Run_I D _ 1001_215 BACK TO MAIN Analvtlcal Run Information.: AccepIaMeOuant Ranga: 25 0wb.l~l.lwb haw: Calibn(ronCurve ?0.9%117 Target PFOS Internal Slandard: THPFOS *For mom mn info. See lhe Dall Rsnw Form includedin lhe Rsw Dall 3M Environmental Laboratory 0405391721 4 78328092 Page 268 of 703 BACK TO MAIN Qualitv Control Sample Data I n s t r u m e n t : soul, -- Run ID: ~001207 ~001207-071 s001207_072 sw1207-078 ~001207-077 ~001207~078 ~001207-079 ~001207-080 ~001207-OM ~001207-085 rW1207-lM ~001207-105 rM11207-108 ~001207-110 r001207-111 ~001207-112 rW1207-113 ~001207-114 ~091207-118 sGUl207-119 ~001207-120 swlm7-121 1001207-122 tW1207-1X sWl207-127 ~001207-128 awirn7-12~ rW1207-1M ~001207-134 ~001207-135 smirn7-i~ ~001207-137 sWl207-lZd W01207-142 ~001207-143 r001207-144 sWl207-145 ~001207-148 sWlZO7-1M sWl207-151 ~001207~153 SWl207-158 ~001207-159 1W1207-1MI 10xEW-1311-3033msS1.0.5mslL. Mlr. 1:lday. 1M71O0 OXI E O ~ - ~ ~ ~ ~ - ~ O Y S I .i:O5u.ay~, ~i m~ ~7 m, O ~ ~ , lox EW-1311.M35S1.0.5mglL,Ohr. 1:5dsy, 1 ~ 7 1 ~ lox EW1311-30MS1.O.VnplL.Ohr. 1:Way. lM7100 lox E00-1311-30JBmrS1,0.5mpll,0hr.1:5day,12107m lox ~~-i3ti-3037-si.0.5mgl~.oh1r:z. sd.y. 12107100 lox E W - ~ ~ H J O S L I S I . O . S ~ ~ ~ ,i:O25~d~a, y. 121071~ lox E~l311-3038~1.0.5mglL.Ohr1.:25d.y. 12107100 lox E~1311-3039mrSl.O.5mpR.Ohr1. :25diy. l M 7 m 1OxEW-1311-3MDSl.O5mglL.21w.1:lday. l M 7 m lox EW-1311-3Ml-S1,0.5mslL,2nr. 1:l-y. lW7100 101 EW-1311JM2Sl.O.SmglL.2hr. 1:ld.y. 1M71W lox EM1311-30(2~1.(1.5mpR.2hr. 1:lday. lM7100 10xEW-1311-3M3S1.05mph.Zhr. 1:W.y. l M 7 m lox E~1311-301CS1.0.5mglL.2hr1. :5d.y. l M 7 m 10xEW-1311-3MW1.0 5mpA.Zhr. 1:5day. 1 M 7 m lox ~ ~ - i 3 i i - ~ ~ ~ m s ~ i . o . ~ mi:wg sl y~..12~h7r1. 0 0 lOxEW-1111-304&Sl.O5mph.2hr. 1:25dsy. 1M7100 101EW-1311-3M7~Sl.0.5mpll2hr.1'25d.y. 12107100 lOxEW-1311-3M&Sl.0.5mpn.2hr.1:25day,1 M 7 m lox E00~1311-3M8m-S1,0.5mglL.2h1r:.25dey. lM7RO lox EW-1311-3M8S1.0.5mglL.4hr.t'lday. 1u07m lox EW-1311-3050-Sl.0.5mglL.4hrl.:ld.y, IM71W lox EW-1311-3051-S1.0.5~.4hr,l'ldey. 1M7100 1OxEW-1311-3051mr-S1.0.5nwL,4hr., 1:lday. 12107100 lox EW-1311-9052-Sl.0.5mglL.4hr. 1:W.y. lM71W 10%EW-1311-305~S1.0.5mplL4hr.15d.y~12107mO lOxEW-l311-3W-S1.0 5mglL.4hr. 1:Sohy. lM7100 lox EW-1311.M54n~-Sl.O.5mph4hr, 1:Wy. 12107100 lDxE~'13,,-9055-51.0*-..nL ,:2W.y. ,M,Pm lox EW-1311-305bS1.0.5mglL,4hr,1:ZSd.y. lM7100 1OXE~l311-505?S1.0.5~.4h1:r2.5&y. 1u17Mo l o r EW-13lI-3OS7mr-Sl.0.5mglL.4hr 1:25day, 1M7mo l o x EW-1311.3067.S1.0.~.18hr. l:lday, im?mo 1 0 x E ~ 1 3 1 1 J 0 8 8 S 1 . 0 . 5 ~ 1 8 n1r :.lday. l M 7 m lox EW-1311-3068S1.0.5rrmL.18hr.1:ld.r. 1M7)00 lox EW-1311-308BmsSl.0.5nwL.18hr.1:lday. 1M7100 lox EW-1311~307O-Sl.O.VnplL,18h1r:5,day. 1 M 7 m 1OxE0D1311~3071-51.O.~.15h1r:5.clsy. 1 M 7 m lox EW-1311-3072~51.O.5mglL.18h1r.:W.y. lM71W lox EW-1311-3072nu-SI.OSmphlOhr,1:Sd.y. lZID7Ew lox EW-13ll~M71-51.0.5mph.lMr.1:25day. 12107mo lox EWl3ll-M7CSl.O.5mglL,l8h~1:,25d.y. 12m71C-I lox ~ ~ - i ~ i i . 5 0 7 5 - s i . o . ~ m p ~i :.zi ~~ler .y1, ~ 7 1 0 0 lox EW-1311-M75mss1.0.5~.18hr.l:2~aimy.7100 Theoretical Matrix Measured Spike ConcentraUon. ConcentnUon. ug/L ug/L ~ 2 05 <25.0 c25.0 243.94 2w <25.0 U5.0 <25.0 341.05 200 <25.0 <25.0 -25.0 483.23 2w ~ 2 05 -25.0 U5.0 151.28 2w 398.29 449.17 ~25.0 287.37 200 26.41 47 72 74 95 547.85 200 366 389.48 390.3 554.07 2w 427.38 401.2 450.84 447.03 2w 144.29 98.83 88.87 2M.89 2w <25.0 155.7 140.B2 351.48 200 317.1 318.S 328.3 515.02 2w 113.M 88.39 92.13 431.57 200 126.4 113.18 138.92 333 48 20 1 326.1s 3X.21 319.4E 525.54 202 118.29 99.92 1W.M 438 97 203 140.82 138.17 Repllcate Sample %RSD NIA NIA NIA NIA 8.49 48.86 3.81 582 38.55 7.05 1.54 14.03 9.49 1.20 26.47 5.72 Matrix Splke Recovery. K 121.97 170.53 231.62 75.84 133.89 238.45 81.89 .I45 91.01 105.28 94.3 18B.R 07.70 102.02 13445 346.78 518.38 Analvtical Run Information.: Acceptable Quant Rnnge: 25.0ppb1001.7ppb CalibrationCurve ?:0.996026 Target Analyte: PFOS Internal Standard: THPFOS *For mwB run info. See the Data Review Form included in UW Raw Data Q-Test Calculation (N 0.560980835 3M Environmental Laboratory Page 269 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Run ID: H001214a Bb Hi110109.D Hi110110.0 Hill0111.D I Hi110112.D Hi110113.D HillOll7.D I HiIIO118.D HillOl19.D I Hilh3120.D Hi110121.D Hi110125.D Hi110128.D I H1110127D H~110128D HillOl29.D Hi110133 D Hi110134.D I Hi110135.D Hilh3138.D HllD137.D Hi110141.D Hi110142.D Hi110143.D HiiI0144.D Hi110145.D E1311-3120MSS1 El311-3121-S1 E1311-3122-S1 E1311-3123.51 E1311-3125MSSl E1311-3124-51 1311-3125-51 11311-312551 E1311-3128-MSS1 E1311-312761 E1311-312BS1 El311-31ZSSl E1311-3129-MS-S1 E1311-317551 E1311-317~Sl E1311-3177-Sl E1311-3177-MSS1 E1311-317851 E1311-3179-SI E1311-3180-S1 E1311-3180-MSSl E1311-3181-S1 E1311-3182.S1 E1311-3183.S1 E1311-3183.M.S-S1 Measured Concentration, ug/L 125.100 105.408 34.090 275.722 118.696 110.212 98.723 280.717 288.554 284.213 288.461 471.683 118.318 121.886 87.387 284.087 451.551 442.987 447.892 847.955 402.850 428.582 425.083 811.G97 78.085 85.862 59.321 289.180 247.502 288.700 331.41 448 22 385.83 65.0 e25.0 183 42 C25.0 80.43 83.71 2w.01 242.88 248 91 245.14 424 19 380.34 374 21 988 76 541 70 <25 0 Q5.0 -25.0 241.98 C25.0 45.0 65.0 184.71 c25.0 e25.0 e25.0 188.81 Theoretical Matrix Spike Concentration, uglL Replicate Sample %RSD 54.29 200 9.45 2w 0 86 2w 17.37 2w 0.98 200 3.33 2w 18.33 2w 15.44 2w NIA 2w 2w 200 2w 201 202 WA 203 Matrix Spike Recovery, % 120.82 8z.w 91.60 98.34 1CU.13 93.01 104.82 58.40 91.71 72.85 89.53 e5 47 120.38 01.44 93.01 Analvtical Run Information'': Acceptable Puant Range: 25.0ppb-1001.7ppb(aand b) Calibration Curve ?:0.9998(a), 0.9998(b) Target Analyte: PFOS Internal Standard: THPFOS 'For more run info. See the Data Review Form includedin the Raw Data 3M Environmental Laboratory Page 270 of 703 BACK TO MAIN Qualitv Control Sample Data Sample Data File 1010123_W2 Sample Descrfptlon lox ~ ~ - 11-30017.s2. OWL P F O S . ~SO~II. 48h.irn3m1I lox EW-l311-3WB-S2.O n W PF0S.m soil. 48h.1103101M:I C lox EW-1311-3009-S2,Om#L PF0S.mmI,48h.llOM1 4M: C 1010123~010 1010123-01 1 lox EW-1311-3011-S2,5mpll PF0S.m soil. 48h,11031011M: C 10x EW-1311-3012-S2,O mPFOS.no soil,48h.llOM1 1M: C 1010123-018 miotz3-019 1010123_020 1010123~021 11010123I022 Ml0123-026 1010123-027 mi0123-028 1010123-029 mror23_o30 miom-0% 1010123-035 miom-03s 1010123-037 1010123-038 m10123-w~ mioi23-~3 1010123-044 Imioi~3_ws 1010123-046 mioiz3-050 lO10123_051 mi01231052 m1ni23-0~3 mioi23-OY 1Ox EW-13113025S2. Om& PFOS.1:l dsv. 48h.1103101 CMC 10x E00-1311-3024-S2,0&L PFOS.1:'I day, 48h.110M1 CMC ?OxEW-1311-3024ms-S2.OmpnPFOS.1:l day. 48h.1103,01 CMC lox EW-1311-J025-S2,O W L PFOS.1:I day. 48h.llOYOl CMC 10aEMl311-302BS2 OmphPFOS.1 5d.y 48h 1103101 CYC lox EW-I~~~-~OZ~.OSWZ,L PFOS 1 5 day. 4 ~ h . i m m iCHC IOxEW-131l-Jo27rnsS2,~P~FOS,1:5day. 4Bh.lm3131 CMC lox EW-1311-3028-S2,O W L PFOS,1:25 day. 48h.1103iW CMC 1Ox EW-1311-3029-S. O M PFOS.!:25 day. 48h.1103m CMC 10%EW-1311-3030-sz.Om#L PFOS,1:25 day. 48h.1103/0' cMC 1Ox EOC1311JOMms-52.0mpll PFOS.1:25 day,48h,110:101 CMC lox EW-1311-3094-S2.5 W L PFOS.1:l day. 48h.llOM1 :MC lox EW-1311-~85S2W. L PFOS.1:I day, 48h.1IOm1M:, C 10xEW-1311-30QS-S2.5m&PFOS,4:1 day.48h.llOM1 M:I C lox EW-131130ffim-S2,5~ PFOS.1:l day,48h.11031111CMC 1oX E00-1311-M97-S2, 5m#L PFOS.15 day. 48h.llOM1 CMC lox EW-l311-3098-S2,6mpll PFOS.1:5 day, 48h.1103101 1M: C 11% EW-1311-3098mrS2.5rn~PFoS,1.5 day, 48h.im3n11CMC 10xE00-1311-31W-S2,5WL PFOS.1:25day.~8h.110~1cMC lox EW-1311-310142.5nX.lR PFOS.1:25 daw 48h.lXIMl CMC 1Ox E00.13113102-S2,5nW PFOS.1:25 day. 48h.llOM1 CMC 101EW-1311-3102rnsS2,5 n W PFoS.125 day. 48h.110~01CMC 101EW-1311-3166S2..5 W. L PFOS.1:l Sed. 48h.1103101 (:MC 1Ox EW-1311-31658-S2,5nW PFOS.1:l Sed. 4Bn.110M1CMC 1Ox EW-1311-3168-Y,Irn#L PFOS.1:I Sed. 48h.1103101c MC 10xEW-1311-3168ms-S2,5m&PFOS.1:1 Sed.48h.lDM1 CMC Analytical Run Information.: Acceptable Quant Range: 25.Oppb-IMHlppb Calibration Curve f:0.997776 Target Analfl8: PFOS internalStandard:WPFOS 'For InareN n info. Seethe Data ReviewForm includedinthe R m Data -- Instrument:Tucker Run ID: t010123 Theoretlcai Matrlx Measured Spike Concentratlon, Concentntlon, Repilcate Q5.0 45.0 174.31 c25.0 c25.0 45.0 194.29 c25.0 e~~ 5 0~ C25.0 170.06 Q5.0 <25.0 45.0 129.49 c25.0 C25.0 <25.0 154.79 95.36 112.83 159.53 377.94 163.56 174.93 408.33 476.98 520 L)8 501.18 886.63 8~3~1..9 1W.14 51.56 242.84 2w NIA 2w N...IA. 2w 2w NIA 2w 27.05 200 4.75 200 1 I, 2w 31.49 2w 1 Matrlx Spike 87.16 97.15 85.03 64.75 77.40 109.21 116.70 1 197.73 95.64 P-Test Calculation (N = 3) -0.651090964 3M Environmental Laboratory Page 271 of 703 BACK TO MAIN Qualitv Control Sample Data _- Instrument: Tucker Run ID: to10124 I__ I SampleData File 1010124~003 1010124-W4 1010124-W5 tO10124-006 1010124-007 1010124-011 t010124~012 1010124-013 1010124-014 1010124~015 1010124-019 1010124~020 1010124-021 tO10124-022 1010124-023 t010124_027 1010124-028 toioiz4-029 1010124-030 1010124-031 Sample Description 1Dx EW-1311-3169-S2.0.5rngILPFOS.1:5 Sed. 48h 1/03/01 CMC l o x EW-1311-3170-S2,0 5mgL PFOS,1:5 Sed, 48h 1/03/01CMC 1Ox EW-1311-3171-S2,0.5mgR PFOS,1:5 Sed. 48h 1/03/01CMC l o x EW-1311-3171ms-S2,0.5mslL PFOS.1:5 Sed, 48h.1/03/01 CMC l o x EW-13113172-S2.0.5mgR PFOS.1:25 Sed, 4811.1/03/01 CMC l o x EW-1311-3173-S2.OSmgIL PFOS.1:25 Sed, 481i.1103/01 CMC 1Ox EW-1311-3174-S2,0 5mgL PFOS,1:25 Sed, 4811,1/03101 CMC l o x EW-1311-3174ms-S2,0.5m&il. PFOS.l:25 Sed. 48h.1/03/01 CMC l o x EW-1311-3184-S2,0m&il. PFOS.1:l Sea, 48h.1/33/01 CMC l o x EW-1311-3185-S2,OmUL PFOS.1:I Sed, 48h,l/J3/01 CMC 1Ox EW-1311-3186-S2.DmgR PFOS.1:l Sed. 48h.l113/01 CMC l o x EW-l311-3186ms-S2,Omg/L PFOS.I:~ Sed. 48k.im3m1 CMC l o x EW-1311-3187-S2,Omg/LPFOS.1:S Sed, 48h,lbl3/01 CMC IOx EW-1311-3188S2.0m& PFOS,l:5 Sed. 48h.lflWUl CMC 1Ox EW-1311-3189-SZ.OmslL PFOS.1:5 Sed. 48h,l/l13/01CMC l o x EW-1311-3189ms-S2,Omg/LPFOS.l 5 Sed, 48h,1/03101 CMC l o x EW-1311-319o-S2,Oman. PFOS.l 25 Sed. 48h.1103101 CMC i ~ ~ x~ - 1 3 1 i - 3 1 9 1 - ~o2m@. PFOS.I 25 sed. 48h.irnmi CMC 1Ox EW-1311-3192-S2,0m& PFOS.125 Sed, 48h.1!03/01 CMC l o x EW-13113192ms-S2. Omgk PFOS.125 Sed. 48i,1/03/01 CMC Measured Concentration, uglL Spike Concentration, UglL 186.19 324.9 210 45 469.73 200 265.72 282.72 285.76 407.27 200 `40 0 e40.0 e40.0 161.33 200 ~40.0 ~40.0 ~40.0 186 26 ZW c40 0 <40 0 440 0 188 01 200 ReDliCate Sample KRSD 30.80 3.88 N/A NIA NIA Matrix SDlkt Recovery, .A 129'.64 60.76 80.67 93 13 94 01 Analvtical Run Information*: Acceptable Quant Range: 40.0ppb-1000ppb Calibration Curve ?:0.997388 Target Analyte: PFOS Internal Standard: THPFOS `For more run info. See the Data Review Form included in the Raw Data 3M Environmental Laboratory Page 272 of 703 BACK TO MAIN Qualitv Control Sample Data Instrument: Tucker - Run ID: - tOlOlZ5 Sample Data File 1010125-040 miom-041 1010125-042 1010125-043 mioi~s-w mioi2s-048 mioizs-049 1010125-050 miom-osi 1010125-052 mior2s-oss 1010125-057 toioi2s-058 mio12s-os9 mioi2s-oso mioi25-OM 1010125-065 mioins-osa 1010125-067 1010125-068 mioi2s-072 miom-073 mioi2s-074 lOlOl25-075 mioiz5-076 mioi2s-oso Sample Description l o x EW-1311-0016 lox E00.1311-0017 lox E00-1311-0018 1Ox E00.1311-0019 lox E00.1311-W20 1OX E00-1311.0021 lox E00.1311-0022 <OX EO0.1311M)Z3 1OX EW13114Q24 1OX E00-1311-0025 lox EM)-1311-0026 iOx EW-1311-0327 1OX EW-1311-0028 1Ox E00.1311-0029 lox EW-1311-0030 lox E00.1311-0031 1OX EW-1311-0032 lox E00.1311-0033 l o x E00.1311-W34 1OX EW-13114035 lox EW-l311M)36 1OX EW-13114037 lox EW-1311-0038 1OX EW-1311-0039 1OX E00-1311.0040 1OX EW-1311-0041 1Ox E00-13114042 Measured Concentration, Theoretical Matrix Spike Concentration, Replicate Matrix Spike UglL UglL Sample%RSD Recovery,% 2 <40 0 NIA -0 0 <40.0 <40 0 NIA <40 0 n Cd" --.1 e40.0 NIA c40.0 c40.0 e40 0 NIA c40.0 <40.0 <40 0 NIA c40.0 815.66 534.11 623.15 511.02 8.36 599.06 8.17 539.37 002.7 543.28 615.48 m86 8.58 1010125-084 mioi2s-oss l010125~wO mioi25-wi 1010125-~2 1010125~oeS mioizs-w7 mioi25-oa8 mioizs-wg mioi2s-ioo mioizs-io4 miom-io5 mioizs-ioa 11010125-107 mioizs-10s mioizs-ii2 010125-113 mioizs-114 lOlOl25-115 lOlOl25-116 rnioi25-i20 1010125-121 1010125-122 miom-123 mioins-i24 mioizs-i2s mioi2~-129 1010125-130 1010125-131 mioizs-i32 1OX EW-1311-0044 lox EW-1311-0045 l O x E00-1311-0047 1OX EW-1311-0048 1OX EM13110049 lox EW-1311-0050 lox EW-1311-0351 lox EW-1311-0052 1Ox EM1311-0053 lox EDa1311-0054 1OX EW-1311-0055 1OXEW-1311-0058 1OX EW-1311-MW7 lox EW-1311.0058 10x EW-1311-0058 1OX EW-13114080 lox EW-1311-0081 1OXECC-1311-w82 1OX E001311-w83 1oX E M 1 3 1 1 - ~ 1Ox EW-l311MY)5 1OX EW-1311-WgB lox EW-1311-CC67 1OX E00.13114088 1OX EW-1311-WB9 1OX EW-13114070 1OX EW-1311-0071 1OX EM)-1311-0072 1OX E00.1311-0073 101: E00.1311-0074 101 EW-1311-M75 629.91 ". 614.54 549.94 035.77 539.81 402.35 417.47 359 31 380.97 609.1 603.9 540.32 6Bo.88 543.97 ~~ 817.2 y5.02 805.04 529.29 613.74 535.27 547.43 326.1 457.52 588.47 412.39 473.07 399.6 428.08 471.39 418.75 Analytical Run Information": Acceptable Quant Range 40ppb1000ppb Calibrabon Curve ? 0 998087 Target Analyte PFOS internal Standard THPFOS 'For more run info See the Data Revlew Form included in the F aw Data 7.57 5.70 22.31 7 62 6.55 .- 1.'1..,e 1 7.00 7.47 28.51 9.18 6.38 3M Environmental Laboratory Page 273 of 703 BACK TO MAIN Appendix F: Notes to File aind Deviation forms This appendix includes all notes to file and deviation forms generated in this study. 3M Environmental Laboratory Page 274 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File - P.r_o_ject or Study.Nu-mber: PFOS Ads-orb/Deso-rb- I _ _ -EOO- 13 1 1 Associated Study Number: - _--_ In the "Suitable Container" section of this study the spiking concentration differs fkom the method but is stated correctly in the protocol. In this case the protocol takes precedence over the method. 3M Environmental Laboratory Page 275 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File P-ro-ject__or- S-tudy Num-b-er: PFOS AdsorbDesorb I I E00-13 11 In method ETS-8-159.0 the specified shelf life for the test solutions was different from that recorded in the standard logbook when the solutions were actually made. The shelf life of the solutions in the method were chosen arbitrarily and do not reflect accepted lab practices, namely that solutions have a 6-month shelf life (except in rare cases of highly unstable compounds). The method will be revised to reflect actual practices prior to the start of the next study. 1 Recorded By: 3M Environmental Laboratory Page 276 of 703 BACK TO MAIN Record of Deviation I, Identification Study / Project No. t PFOS Adsorbmesorb/ E00-1311 .- (Check one) 0 Protocol 0 Other: Docknent Number: ETS-8-110.0 -_ . i Date(s)of occurrence: 11 Dec 00 to12 Mar 01 I I II. Description: Required Procedure/process: ETS-8-110.0 section11.lstates, "the average of two standard C_u-rves will bep_ l_ot_te_d- b- y~ l~in_e-ar- r- e-g-r-ession (y = mx+b), weighted I/x, not forced throughzero-"__I .... ... ............... . ... .......... .................. .... .^._ ................ ._............ .- .................................... . Actual Procedure/process: Run s001;!17 was quantified using three curves. In addition, none of the runs in thissiudy were quantified using a linear or a weighted curve. A quadratic. unweinhted curve wasused instead. ....... . . . . . . . . . ..................................... .. .................................................................................................... Jll. Actions Taken: (such as amendment issued, SOP revision, etc.) __I___- No additional action will be needed. ................ ............................................... ............................ ........................................................ - ._ - - __. -_____- ~_________ -- - Recorded By: PwkJ IV. Impact on Study/ Project Date: f/q/o / This deviation does not adversely affect the quality of the da-t-a_. - --________I_~____~_______ I _________I I 3M EnvironmentaILaboratory 3M Environmental Laborafory Deviation No. (assigned by Study Director or Prqject Lead at the end of study or project) Page 277 of 703 BACK TO MAIN Rocord of Deviation 1. Identification Study f Project No. E - - -PF-OS Adsorb/Desorb/ E00-1311 Deviation Type: PSOP U Method dEquipment %%edure----- (Check one) 0 Protocol 0 Other: .__ Document Number: ETS-8-110.0 - ._ _ -_ -- - Date(s) of occurrence: -11 Dec 00 to12 Mar 01 i 11. Description: Required Procedurelprocess: ETS-8-110.0 section10.2.1 states, " Matrix spikes are prepared for each sample set and analyzed todeterhine%e matrix effect on t-h-e-re-covery efficiency." - -- ~ Section 10.2.3 states, "analyze the matrix spike &d the matrix spike duplicate ( ifprepared) in the same run as the original samule." Actual Procedure/process: Matrix spjkes were not prepared for some sample sections, therefore, they were not analyzed. These matriK spikes were not required by method ETS-8-159 or ETS8-160. .- 1VI. Actions Taken: (such as amendment issued, SOP revision, etc.) -. A protocol amendmentwas drafied to address thi-s iss-ue. - - _- - Recorded By: -. - -- Date: s'/?/d / IV. lnrpact on Study/ Project _ _ .. Thisdeviatio-n do~es n~ot a_dver_sely-affe-ct t-he quality of the data. Sufficient matrix spikes - Were prepared to gauge the quality of the data. 3M Environmental Laboratoty Date: 1 ofj*$h, / / Deviation No. (assigned by Study Director or Prplect Lead at the end of study or project) 3M Environmental Laboratory Page 278 of 703 BACK TO MAIN Record of Deviation 1. Identification _. b d y / Project No. . _. .- PFOS Adsorb/Desorb/ E00-1311 - - - _ _ I _ _ _ _ - _ _ _ - ---- -- -- -- . - - - leviation Type: ljq SOP 0 Method 0 Equipment Procedure (Check one) 0 Protocol 0 Other: locument Number: ETS%155.0 Date(s) of occurrence: 11 Dec 00 to12 Mar 01 I II. Description: lequired Procedure/proc-ess:- -E.T.-S--8-155.0 se-ct-ion. l0._ 2.1 states, " Matrix spikes are prepared 'or each s%npie s&and analyzed to determine the matrix effect on the recovery efficiency." ;ection 10.2TstatesY"analyze the matrix spike and the matrix spike duplicate ( if prepared) in he same run& the original samule." Ictual Procedure/process: Matrix spikes were not prepared for some sample sections, therefore, hey were not analyzed. These matrix spikes were not required by method ETS-8-159 or ETSi-160. fll. Actions Taken: (such as amendment issued, SOP revision, etc.) ZTS-8-155 mefiod has beenrevised !iothat matrix spikes may be preuared atthe discretion Recorded Bv: - _.-. .- - 4+/ __ Date: IV. Impact on Study/ Project This deviation does not adversely affcct the quality of the dat~ a: -Sufficient matrix spikes _ _ _ _ - _ - - . - _ ~ _ ~ _ _ _ _ I ~ _ _ _ _ - - _ _ I _ _ _ _ ~ Were prepared to gauge the quality of`the data. 3M Environmental Laboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) Page 279 of 703 BACK TO MAIN Record of Deviation 1. Identification - Study / Project No. __ - - __ P-FOS Ad-s_o_ r-b-me-so--rb__/ E_0_0--~1311 -I -__I _ - I ~ Deviation Type: fit SOP 0 Method 0 Equipment Procedure (Check one) 0 Protocol 0 Other: Document Number: ETS-8-155.0 Date(s) of occurrence: 11 Dec 00 to12 Mar 01 11. Description: Required Procedure/process: ETS-8-155.0 section11.Mates, "the average of two standard Curves will be plotted by linearregression (y= mx+b)~, w-eighted l/x, not forced through zero" __I_-- Actual Procedure/process: Run t001215 was quantified using three.cu-rves. 111. Actions Taken: (s_u_c_h as am-en_d-m- .en_t_i-ss~u-e-dI, SOP revision, etc.) - . - - .-._.-_-___I__- ~ ~ No additional action will be needed. I-I.-- - Recorded By: _. - - . IV. Impact on Study/ Project _T_his_ de_ via.tion does not a_d_v_e_rs_el~y -affcct the_ _q_u-al-i_ty of the data. _l____l__ Date: qh/O/ - - _I -- 3M EnvironmentalLaboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) Page 280 of 703 BACK TO MAIN Record of Deviation 1. Identification Study / Project No. i t PFOS Adsorb/Desorb/ E00-1311 Deviation Type: &-SOP Method 0 Equipment Procedure (Check one) 0 Protocol 0 Other: Document Number: ETS-8-155.0 Daie(s) of occurrence: 11 Dec 00 to12 Mar 01 11. Description: Required Procedure/process: ETS-!I- 155.0 section11.2states, "If the calibration curve does Not meet acceptance criteria perform routine maintenance or prepare a new standard curve (if necessarv) and reanalvze" ..... . . .. ...... ,,..... .. ... .. .. . ..... . - ..... ..., .. ... . . ~ ... Actual Procedure/process: Some analytical runs contained one low curve point that failed acceptance criteria but was intentiondly left in the calibration curve. The elimination of this Point would have .-__ r_e_ sulted in-successive failure-s o- f e-ac-h n-e_xt highest point - in the curve. These - -I-__ I- ___-__I_ Low points serve to anchor the quadratic curve and are needed to achieve an acceptable ._ Calibration of the instrument. Ill. Actions Taken: (such as amendment issued, SOP revision, etc.) b+&w Recorded By: IV. Impact on Study/ Project Th-is deviation does not-adversely aff :ct ._ the quality of the - data. __ Date: 5/Y/d - -- -~ __ - - - --- 3M Environmental Laboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) Page 281 of 703 BACK TO MAIN Record of Deviation 1. Identification Study / Project No. i. i --- __ --- -~ PF__O__S Adsorb/Desorb/ E00-1311 Deviation Type: 0 SOP- -KMethod 0 Equipment Procedure (Check one) 0 Protocol 0 Other: Document Number: ETS-8-155.0 Date(s) of occurrence: 11Dec 00 to12 Mar 01 11. Description: Required Procedure/process: ETS-8-155.0 section16.4 states, "Print the integration summary, -In-tegration me- thod,- and- - c_ h;I o- m- - ato--grams..rand store in th-e - sIt- u_ dI_ y fo_l-de.r-.- - - I I Actual Procedure/process: Each acquisition sequence is set up similarly in that they begin with - Solvent bla&s). and one set of standards Drior to &e samdes bracketed bv calibration curves. \ ,I - -.- I -T~ hese samples - serve to condition the c__o_l-wk-a-nd- warh up' the ins_tr_u_ment-._' These - samples were __l__ I_ _ I _ - _ _ I - _ - - l _ _ I -____ Not orocesied along; with the study samoles and no chromatograms were printed out. This was Because they do not relate to the study in any way. 111. Actions Taken: (such. as amtwdment_ -i_ss-u- e-d,-SOP revision-_, et_c_ .) - __ _ I _-_I_ No additional action will be needed. ....... .. Recorded By: ... ^... - .. . . ...... .. ,. . . .. . Date: xknt on Study/ Project T-h-i-s de_v_iation_ d-o- _es_n-ot_a_d_v_e_r_se_ly__a__f_-f_x__t th_e_quality of th-e data. 3M Environmental Laboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) Page 282 of 703 BACK TO MAIN Record of Deviation ~ 1. Identification Study / Project No. i ___PFOS Adsorb/Desorb/ E00-1311 Deviation-Type: OSOP - KMehod d EquipmentPGcedure (Check one) 0 Protocol 0 Other: Document Number! ETS-8-155.0 Date(s) of occurrence: 4/4jO1,4/2/01, 4112/001 11. Description: _-Requ-ir_ ed Pro_ cedure_ /pr_o--cl- e-_ sl_ s_:^-l_E--T- _ ~S-l--- 8l-l_ 1-5_ --5I-.0 seI ctio- n 1_ 4.4 sta_ tes, "C- onti- nuin- g__C_a_l_ib--- r-ation Verification (CCV) percent recoverilx must be f30% of t_he_ -standard concentration" .- - Actual Procedure/Drocess: In runs R010404. R010402(b). R010405. H010404. and R010412 The 5ndml CCV was outside the acceDtable calibration rang-e and was outside the +30% Criteria. Since these points were outside the calibration range they were not accurately Quantifiable, and the 250.5ng/ml points were used as the acceptable CCV's. These points __ _W__e_re used to demonstratethe continued acceptability_o_f_t_he calibration and the 5ng/-m-l - __-_. _._^__I_-__-__-____ _ I _ _ _ ^ ___-lllll_ -__I_Ic Points ~~ ~ were iga nored. Ill. Actions Taken: (such as amendment issued, SOP revision, etc.) No action is needed. Recorded B y // IV. Impact on Study/ Project W This deviation does not adversely affxt the quality of the data. Date: J I 3M EnvironmentalLaboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) Page 283 of 703 BACK TO MAIN Record of Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 0SOP fl Method Equipment Procedure 0 Protocol 0 Other: Document Number: ETS-8-155.0 , Date(s) of occurrence: 11 Dec 00 to12 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 section 14.2 states, "Solvent and method blanks must-be~l-ess than one half -. of the_lo_w_es_t s_ta_n_d._a_rd_used in the calibration_ cu.r_ v.e_ _ ." _ _ --- __ I_ Actual Procedure/process: Run rO10329b the area counts of the solvent blanks averaged 56% Of the area count of the lowest standind used in the curve. This amount of contamination is Not expecte-d-to h-a_ve_a__s_ignifican_t- ef_fe--c_t_o_n-_ the - s- a. m-p-le-qu-an-t-ita-t~io--n- . - __ .-- I --I_- -__I_ (SIL Actions Taken: - (such as amendment issued, SOP revisio-n,_et_c._)- _ _--_I_-_ _I I _ ~ _ __ No additional action will be needed. Recorded By: b L c k Cccr; IV. Impact on Study/ Project Date: 51 / C / O / This d- e-v-ia- ti.on does not-a-d. v_ ersely__a_ffcct th- e qu-ality__of the -d-ata.- - - - _I 3M Environmental Laboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Pro.ject Lead at the end of study or project) Page 284 of 703 BACK TO MAIN Record of Deviation = 1. Identification Study / Project No. i PFOS Adsorb/Desorb/ E00-1311 Deviation Type: -0SOP YMethod 0 Equipment Procedure (Check one) 0 Protocol 0 Other: Document Number: ETS-8-155.0 Date(s) of occurrence: 11 Dec 00 to12 Mar 01 II. Description: Reauired Procedure/r>rocess: ETS-$1-155.0section 11.2 states. "If the calibration curve does Not meet acceptance cri-teria-perform routine maintenance or p-rIe_p_are a new stan~ dard-cur_v_ e- I (if necessary) and reanalyze." Actual Procedure/mocess: High/low level standards were eliminated from curves to better fit Y The ranges appropriate to the data. Additionally calibration points that did not meet acceptance Criteria were thrown out of the curve. ,111. Actions Taken: - _ _ ___ - _____(_such a_s__ame-n-dm~ent issued, SOP rev-i-sion, e-tc-.)- _- - - ___^ I____ _I I _ I The SOP will be revised to reflect these changes in the method. Recorded By- IV. Impact on Study / Project Thi_s_d_e-v_ia_ti_o_ n does n_o_t_ adversely affc ct t-he- qua.l_ i-t-y of . the d-at_a_._ _I. Date: .-- I 6! 3M EnvironmentalLaboratory 3M Environmental Laboratory Deviation No. (assigned by Study Director or Prqject Lead at the end of study or project) Page 285 of 703 BACK TO MAIN Rctcord of Deviation I. Identification Study / Project No. Deviation Type: (Check one) Document Number: I! PFOS Adsorb/Desorb/ E00-1311 b SOP Method 0 Equipment Procedure 0 Protocol Other: ETS-8-155.0 ._ - Date(s) of occurrence:-11 Dec 00 to12 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 section 10.1.2 states, ''Analvze a method blank and A matrix blank Drior to each calibrat.on curve'' . __~ ....... ................ ...................... ........................ Actual Procedure/process: There were several runs that did not analyze these blanks prior to the Calibration curve. These blanks wen: run alongside the samples being analyzed instead. Since The matrix &d method blanks are to measure the co-ntamination in--the sample prep procedure_s_ ~ l__l_ -----I_-- __--I --_-l_l__.__ &d in the matrix solutions this is not expected to affect the results of the studv. ............................................... ............................. .... (Ill. Actions Taken: . .... (such as amendment issued, SOP revision, etc.) ...~.._-I^_.___l.l_~__ No additional action will be needed. ____l._ "__I________. ..................................................... .............................................................................................. _______I ......................... Rec0rded.By : -. . . . . . . . . . . - ~ : ............ ."............................ Date: bck W L W (. i 5l IS 101 IV. Impact on Study/ Project 5-1IS/c\ I This .. deviation . does .n..o.. t adversely affect the q-ualit-y of the data._. .. _ - .. 3M Environmental Laboratov 3M Environmental Laboratory Deviation No. (assigned by Study Director or Prqject Lead at the end of study or project) Page 286 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File 'i E00-1311 Instances where a sample needed a different dilution factor than what was originally made: The analyst went back to the original sample aliquot and started over. The latest date of dilution on each of the spreadsheets corresponds to the dilution factor that was acceptable. Date I 3M Environmental Laboratory Page 287 of 703 BACK TO MAIN 3M ENVIRONMENTLA,ALBORATORY Note to File I __P_r_o_j_e_c_t-o-r Stu-d-y-N-u-_m_ ber: -PFOS Adsorbmesorb -- - __-- - - Some of the standards prepared in this study did not record a balance number in the logbook. In all cases this balance ID was #914. I Recorded By: 3M Environmental Laboratory Page 288 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File Each acquisition sequence is set up similarly in that they begin with.solvent blank(s), 2 high standards, solvent blank@),and one set of standards prior to the samples bracketed by calibration curves. The purpose of injecting the initial series of blanks and standards in each sequence is solely to ensure the column is sufficiently conditioned, the mass spec. is "warmed up," and the instrument is suitable prior to analysis of samples. Therefore, the appropriate standards are labeled "system suitability" on the data summary sheets. These injections are for qualitative purposes only, and are not to be used to quantify the data or be scrutinized for meeting quality control standards. 3M Environmental Laboratory Page 289 of 703 BACK TO MAIN 3M ENVIRONMENTALALBORATORY ~~ Note to File i Project or Study Number: PFOS Adsorbmesorb Some acquisition sequences in this study were run with two CCV concentrations. This was done so that if the need arose the calibration range could be extremely narrow. In some cases the lowest, Sng/mL, was outside of the calibration range. This does not mean that the samples are bracketed by failing CCV's, rather that one CCV concentration was outside the calibration range. In these cases the higher concentration CCV was able to demonstrate the continued acceptability of the calibration. The data is in compliance with the method and does not need to be flagged. 3M Environmental Laboratory Page 290 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File - Pr-o-ject o-r S_tu_dy-N-u-mb- er: PFOS Adsorbmesorb - Eoo-i 3 i 1 Associated Studv Numlber: - _- I - - - Many of the samples analyzed in this study were diluted prior to analysis. The prep sheets note the samples that were diluted with a mechanical diluter. In these cases an appropriate amount of the original study sample was withdrawn from its vessel, and the diluted sample was dispensed into a new pre-labeled vial. This allowed for the retention of an und luted sample and provided a consistent final sample volume of 1.OO mL. The diluters were calibrated to dispense a final volume of 1.OOmL for every dilution level used in this study. In the case of the Desorption Kinetics samples there was insufficient sample volume to use a mechanical diluter, In this case the dilution was 1: 1 accomplished by hand with a syringe, and the final sample volume was 200uL. In the cases of Sam Aes that were not diluted the fmal sample volume was 1.OmL in all cases. 3M EnvironmentalLaborafory Page 291 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File Project or S_t_udy-Nu-mber: PFOS AdsorbDesorb - _- - ___ E00-13 11 There were a number of steps in the preparation of study samples that were described in the analytical method but not specifically recorded on the prep sheets. The method was followed in all cases, these steps were just not recorded. These implied but unrecorded steps were: ETS-8-160.1: Section 12.2.12 - "centrihge until the aqueous layer appears clear" ETS-8-160.1: Section 12.3.7 -"add an (:qual amount of fresh CaC12solution to the tubes after the withdrawal of the sample aliquots" ETS-8-160.1: Section 12.4.9.2 -"Centrifuge until the aqueous layer appears clear" 3M Environmental Laboratory Page 292 of 703 BACK TO MAIN 3M ENVIRONMENTIAlALBORATORY Note to File Project or Study Number: PFOS AdsorbDesorb E00-1311 There was no documentation of the pH strips used in this study. In all cases they were the EM Science product called "colorpHast", pH 5- 10, Lot number 60179026. 3M Environmental Laboratory Page 293 of 703 BACK TO MAIN 3M ENVIRONMENTALLABORATORY Note to File _ _ - -P_r_oject or Study Number: PFOS AdsorbDesorb E00-1311 There was no documentation of the specific centrifuge listed in the prep sheets for this study. The centrifuge in all cases was #415835, which was located in the prep lab. 3M Environmental Laboratory Page 294 of 703 BACK TO MAIN 3M ENVIRONMENT]AJALBORATORY Note to File i t Project or Study Number: PFOS AdsorbDesorb I ~-_^-I_______._____. E00-1311 Associated Study ~--. _- The 00002-104 calibration standards used in this study had a recorded THPFOS concentration of 250ppb, but the actual concentration was 249.3 Ippb. Since the internal standard THPFOS is used to monitor instrument performance this is not a significant difference. Additionally this small difference in concentration is not independently distinguishable given the resolution capabilities of the instrument. No additional documentation or requantitation is needed. 3M Environmental Laboratory Page 295 of 703 BACK TO MAIN 3M ENVIRONMENTA]JLABORATORY Note to File Project or Study Number: Associated Study Number: PFOS Ads-or-bDesorb _I__-_ E00-13i - - I- - -~- Two analytical methods were used in the analysis of samples in this study. The LC/MS/MS instrument (Soup) was run according to method E1'S-8-110.0 and all others were run according to method ETS-8- 155.0. Recorded By: Date I 3M Environmental Laboratory Page 296 of 703 BACK TO MAIN 3M ENVIRONMENTLAALBORATORY Note to File i - Project or Study: - PFOS A--dsorblDesorb I__.- _-__ _ _ __ I --_--__I ~ -__ I ition regarding significant figures: _ As a result of using two different software programs (HP ChemStation and Excel) to acquire, process and report analyical data, data containing three different amounts of 1the data packets. The.ch-rom. atograms, batch report, -an~d d-at~a im- p-or-ted- in-to Excel are cach unique. The imported data (i.e. area counts a~nd- concentrations) in .Excel a.lw_a_ ys-ha_s_the.highes.t number - _ of .significant figures. The electronic da~ta s_yst_em_sca_rry_mo_re s_ignificant figures than- a~re-di_sp_lay_ed-. U_n_for~tun_at_ely-, _ mot be adjusted to display a consistent number of nificant figures. However, by reporting all final concentrations - with three-s- ig-n-ifi-c_ant ~ I ~ _ ~ I I _ `s of significant figures displayed in any of the raw data - p-rintout-s is negated. __. I_ ___-I_ ___ __ .I_- I - -- -- - -I_--___ U Recorded By: Date 3M Environmental Laboratory Page 297 of 703 BACK TO MAIN 3M ENVIRONMENTALALBORATORY Note to File ~ o o - t .. -Pro-ject-or _S_t_u-d-y-N-u-m-b--e-r:- -P-F-OS Adsor-b-De_s_ or-b - - i7i i - - I Associated Study Number: The Q-test is a simple statistical test to determine if a data point that appears to be very different from the rest of the data points in a set may be discarded. Only one data point in a set may be rejected using the Qtest. The test uses the following formula: Q = J suspected outlier - closest value I 1 maximum value -minimum value 1 The value of Q is compared to a critical value, Q,. Table of Q Critical values (80% confidence) N Qc 3 .781 4 .560 5 .451 6 .386 7 .344 If Q is larger than Q, the outlier can be c iscarded with an 80% confidence. ' Date I 3M Environmental Laboratory Page 298 of 703 BACK TO MAIN 3M Environmental Laboratory Page 299 of 703 BACK TO MAIN 3M Environmental Laboratory Page 300 of 703 BACK TO MAIN 3M Environmental Laboratory Page 301 of 703 BACK TO MAIN Appendix G : Chromatograins A representative set of chromatograms from the present study is included in this appendix. The complete set of chromatograms is archived in the 3M Environmental Laboratory database and may be reviewed upon request. 3M Environmental Laboratory Page 302 of 703 Data File: D:\chem\Hillary.i\EIOlO222.b\HILLOO93.D Report Date: 20-Mar-200116:l'r BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i\,H010222.b\HILL0093.D Lab Smp Id: Inj Date : 23-'FEB-200110:02 Operator : KLT Inst ID: hil1ary.i Smp Info : 1311-4031-S1 Misc Info : Comment : Method : D:\chem\Hillary.i~~HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-200122:42 Cal File: HILL0032.D Als bottle: 54 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * LIF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS 427 499 3M Environmental Laboratory Page 303 of 703 BACK TO MAIN -. Data File: D:\chem\Hillary.i\HOlO222.b\HILLOO93.~ Page 2 D:\chem\Hillary.i\HOlO222,b\HILLOO93,D 2.77 (D 2,6; 0 LL a 2.5; 1 I- 2.4: ;2,3j '2.2: 2.1; 2.0:: 1.9; 1.8; 1.7; 1.6; 1.5; 1,4{ 1.3; 5 1.2; - l*lj Lo; 0.9: 0.8; 0,7; 0.6: 0,s: 0,4; 0.3; 0.2: 0.1; . . .w . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1,0 1.5 2.0 2,5 3,O 3:5 4.0 I d. . . . . . . . . . . . . . . . .1. .1 . . . . . . . . . . . . . . 4.5 ! 5+5 6+0 6+5 7+0 7.5 8.0 Min I . . . . I . . . . , . . . 1. 8,5 9.0 9,s r!1THPFOS I on 2,41 24 1.81 @ 1.5- 4 1.2- Y ~ 0.9- I \ 0.6: 0.3: , . . . , . . I. ,I. \. . , . 1. . , . . . 4.0 4.4 4.8 5.2 5.6 Min 2 PFOS (Undetected) I on 2.8: 2.6.3: 2.4: 2.2: 2.0j ,-. 1.8: <m 1.6; '0 ;1 1.4; " 1.23: 1.0: 0+8j 0.6: 0.44 . . , . . . , . . . , . . . , . . . , . 4 4 4.8 5.2 3M En\lHlmrnenta?~~bo&& Page 304 of 703 Data File: D:\chem\Hillary.i\:HOlO222.b\HILLOO94.D Report Date: 20-Mar-200116:17 BACK TO MAIN Page 1 3M Knvironmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i'\HOlO222.b\HILL0094.D Lab Smp Id: Inj Date : 23-FEB-200110:13 Operator : KLT Smp Info : 1311-4032-S1 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-200122:42 Als bottle: 55 Cal File: HILL0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 305 of 703 BACK TO MAIN Data File: D:\chem\Hillary.i\HO10222,b\HILL0094.D Page 2 D:\ch~?m\Hillaryri\HOlO222.b\HILL0O94~D 2.97 2.8: 2.7; 2,6: : 2.5: '12.4; 2,3! 2.2: 2.1: 2,o; 1.9: 1.8: 1+7: 1.6; i 1.5: i 1+4< i 1.3; . 1.2; 1.1: 1.6-i 0.9: 0.8; 0.7; 0,6: 0.5: 0.4; 0.3; 0.2: .el. 0.1: :. . . . . , . . . . , . . . . , . . . . , . . . . , . . . . , .- . 0.5 1.0 1.5 2,O 2.5 3.0 3.5 4.0 4.5 Mir J. .I . . . . . . . . . . . . . . .I. I. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0 5+5 6.0 6.5 7.0 7,5 8,0 8.5 9.0 9,5 )t 1 THPFOS 2.71 2.4; 2.11 CI 1,8{ 1,5{ xr( 1.21 V > 0.9; 0.61 0.3; h N d II I 1 2 PFOS (Undetected) Ion 1 Page 306 of 703 Data File: D:\chem\Hillary.i\HOlO222.b\HILLOO95.D Report Date: 20-Mar-200116:17 BACK TO MAIN Page 1 3M 3nvironmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chern\Hillary.i1\HO1022.2b\HILL0095. D Lab Smp Id: In] Date : 23-FEB-2001 10:24 Operator : KLT Inst ID: hil1ary.i Smp Info : 1311-4033-S1 Misc Info : Comment : Method : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 56 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * ~ J F* CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -_---_- _ 427 499 RT BXP RT REL RT RESPONSE ==== ======== ======== ======== 4.929 4.902 (1.000) 1055100 Compound Not Detected, CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= 249.300 ( ug/L) ---_---_-- 3M Environmental Laboratory Page 307 of 703 BACK TO MAIN Data File: D:\chern\Hillary,i\HO10222.b\HILLO~~95.D Page 2 D:\ch~?m\Hillary.i\HOlO222~b\HILLOO95.D 2.6r 2,s: 2.4j 2.3; F2.24 i. 2.1; 2.0; 1.9; 1.8; 1+7; 1.6; 1.5; I 1.4; , 1.3; !: 1.2; . 1,1; 1.0; 0,s; 0.8; 0.7; 0.6; 0.5; 0.4: 0.3; 0.2; 0.1; . . .w . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1,0 1 + 5 2.0 2.5 3.0 3.5 4,O 4,5 Min L.\.I . . , . . . . , . . . . . . . I. .I . . . . . . . . . . . . . . . . . . . . . . . . . 0 5.5 6.0 6 + 5 7.0 7.5 8,O 8.5 9.0 9:5..' % 1 THPFOS 2 PFOS (Undetected) I on 2.6; 2.4; 2.2; 2.0. ~ 1+8; p 1.6; 0 rl 1+4; .? 1.2; Lo; 0.8; 0.6; 0.4; . . , . . . , . . . ' . . . , . . . , . % Erl?Q&wr%~ntalsL'abbot%8n Page 308 of 703 Data File: D:\chem\Hillary.i\HOlO222.b\HILLOlOl.D Report Date: 20-Mar-2001 16:17 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\chem\Hillary.i'jH010222.b\HILLO101.D Lab Smp Id: Inj Date : 23-FEB-2001 11:31 Operator : KLT Smp Info : 1311-4037-S1 Inst ID: hi1lary.i Misc Info : Comment : Met hod : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-2001 16:Ol Cal Date : 22-FEB-200122:42 Als bottle: 62 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Processing Host: W19401 terrell Quant Type: ISTD Cal File: HILL0032.D Compound Sublist: all sub Concentration Formula: Amt * LIF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ___-_ __ _ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) ---_-----_-----__--------_ ----_-_---___ _-___-_ -_ _____ ----___ 4.922 4.902 (1.000) 995964 249.300 5.153 5.126 (1.047) 876072 36.5776 36.6 3M Environmental Laboratory Page 309 of 703 BACK TO MAIN 2,4{ 24 (u (u t ?d. 1.8- 1.5- 6d 1.2{ W ~ 0*9; 0.6; 0,3- . , . . . , . . .1 ~ .. .r . , . 1. . , . . . 2 PFOS 2.21 2,o;: Ion m Ti m 1.8; .-. 1+6; 1+4; &Lo 1.2; "2 1.0; > 0.8; 0.6; 0.4; 0,2{ . . , . . . , .1 . . , . .1 . , . . . , . 3h E?&,,t%&ta~t%bot%&fBory Page 310 of 703 Data File: D:\chem\Hillary.i\:3OlO222.b\HILLOlO2.D Report Date: 20-Mar-200116:1'7 BACK TO MAIN Page 1 3M 13nvironmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\chem\Hillary.i',HOlO222 .b\HILL0102.D Lab Smp Id: Inj Date : 23-FEB-2001 11:42 Operator : KLT Inst ID: hil1ary.i Smp Info : 1311-4038-S1 Misc Info : Comment : Method : D:\chem\Hillary.i\,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-2001 16:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 6 3 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * ClF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _--_-_-_ 427 499 RT EXP RT REL RT RESPONSE ==== ======== ======== ======== 4.922 4.902 (1.000) 992751 5.153 5.126 (1.047) 788043 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= ( ug/L) ======= 249.300 33.0166 33.0 3M Environmental Laboratory Page 31 1 of 703 BACK TO MAIN Data File: D:\chem\Hillary.i\HOlO222.b\HILLOlO2.D Page 2 2,4! 2.3; 2.2: r,. 2*1.; D:\ch~?m\Hillary,i\HOlO222.b\HILLOlO2.D LV) 0 LaL i I- t2.0; 1.9j 1.8: 1.7: 1.6; 1+5! 1.4: 1.3: i 1.2; I 1.1; ' Lo: 0.9; 0.8; 0.71 0.6; 0.5: 0.4: 0.3; 0.2; 0.1; . . .I.N . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 , . . . . , . . . . )t 1 THPFOS 2.42.24 2.0; 1.8: 1.6; C; 1.4: b 1.2r r"xl 1.0; =- 0.8; 0.6:' 0.4: 0.2: CIU JQ: d I I\ 1 2 PFOS Page 312 of 703 BACK TO MAIN 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dita file : D:\chem\Hillary.i\HOlO222 .b\HILL0107.D Lab Smp Id: In] Date : 23-FEB-2001 12:38 Operator : KLT Smp Info : 1311-4039-S1 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\chem\Hillary.i\HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Als bottle: 64 (la1 File: HILL0032 .D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _---____ 427 499 CONCENTRATIONS ON-COLUMN RT BXP RT REL RT RESPONSE (ng/mL) ---- ---_------- -_-------------- -__--_-_____======= 4.917 4.902 (1.000) 985052 249.300 FINAL ( ug/L) ======= 5.141 5.126 (1.046) 683545 28.8722 28.9 BACK TO MAIN M 1 THPFOS 2.41 2.1: 1.8: h Ln 1.51 0 rl 1.2: Y >- 0,9{ 0,61 0.3; 2 PFOS *? + - A I I BACK TO MAIN 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\chem\Hillary.i\HOlO222 .b\HILL0108.D Lab Smp Id: Inj Date : 23-FEB-200112:49 Operator : KLT Inst ID: hi1lary.i Smp Info : 1311-4039MS-S1 Misc Info : Comment : Method : D:\chem\Hillary.i\HOlO222.b\HOlO222t~m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-200122:42 Als bottle: 65 Cal File: HILL0032 .D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ----_ 427 499 RT EXP RT IlEL RT ---- --_----_ 4.914 4.902 (1 000) 5.138 5.126 (1,046) CONCENTRATIONS ON-COLUMN RESPONSE (ng/mL) - -_--_________-======= FINAL ( ug/L) ======= 844071 249.300 4577937 224.827 225 BACK TO MAIN 9.3:' 9,OL 8.7; 8+41 'i8.1: 7.8{ 7.5; 7.2; 6.9: 6.6: 6.3f 6.0; 5.7; 5,4{ 5.1:' & 4.8; "dx 4.5; 2. 4.21 3.91 3.61 e 3.3: (D 3.01 a 2.71 1 2,4{ I- 2.1; 1.8; 1,5: 1.2:' 0.9; 0+6{ 0.3: . . .I-. I I. . . . , . . . . , . . . . , . . . . , . . . . I . . . . . . . . . . . . . . . . . . .1. . . . .%. .L. . . .I . . . . 11 I % I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1,8; 1,6+ c. 1.4; 2? 1.2; 1.0: " 0,8: 2. 0.6; 0.4; 0,2; 1 1 2 PFOS BACK TO MAIN 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daka file : D:\chem\Hillary.i\HOlO222.b\HILLOlO9.D Lab Smp Id: In] Date : 23-FEB-2001 13:OO Operator : KLT Inst ID: hil1ary.i Smp Info : 1311-4040-S1 Misc Info : Comment : Method D:\chem\Hillary.i\HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-200122:42 A l s bottle: 6 6 (la1 File: HILL0032 D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _-_____ - 427 499 RT EXP RT F.EL RT RESPONSE ==== ---_-_----_- ---------- -------_-_ 4.909 4.902 (1.000) 990932 5.140 5.126 (1.047) 277725 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ( ug/L) __ ___ ___ _-__ _ __-_ _ _ _ _ _ 249.300 11.7051 11.7 BACK TO MAIN Data File: D:\chem\Hillary,i\HO10222.b\HILLO109.D Page 2 2.6; 2.5: 2,4: ,: 2.3: t2,2; 2,1; 2.0; 1.9; 1.8; 1.7; 1.6; 1.5; , 1.4; 1Jj -I 1.2; 1.1; 1.0: 0.9; 0.8; 0.7; 0.6; 0.5; 0.4; 0.3; 0.2j 0.1: . . . v. u. . . . . . . . . . . . . . . . . . . . . . . . Ea - 0 ) 0 ll. . , . . . . ( . . . . . . . . . . . .1. . . . .1 . . . . . . . . . . . . . . .I. I. . . . . . . . . . . . . . . . . . . . . . .1. . . . . . . L 2,4{ 2.1; 1.81 Ec. 1,5{ d 1.21 " X > 0.9{ 0.6; 0.3: 2 PFOS ?rl 0 1 n d " 0 d > -. -_ . _ . . bo&ry Page 318 of 703 Data File: D:\chem\Hillary.i\HOlO222.b\HILLOllO.D Report Date: 20-Mar-2001 16:18 BACK TO MAIN Page 1 3M .Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i'\H010222.b\HILLO110.D Lab Smp Id: Inj Date : 23-FEB-2001 13:12 Operator : KLT Smp Info : 1311-4041-S1 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\chem\Hillary.i',HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 67 Dil Factor: 1,00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * TIF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 319 of 703 BACK TO MAIN Data File: D:\chen\Hillary,i\HOlO222+b\HILLOllO.D Page 2 D:\cham\Hillary.i\HOlO222.b\HILLOllO,D 2.6; a0) 2,5: 1 LnL I- 2.4: ,2.3; 't2.2; 2.1: 2,o; 1.9: 1.8: 1+7; 1.6; 1+5; , 1.4; 1+3: 1.2; 1.5; 1.0; 0.9: 0,8; 1 0.7; 0.6; 0.5; 0.4; 0,3; 0.2: 0J.j . . . . . . . . . . . .I'. .c.l . . . . . . . . . . , . .I .t. , . ' . . , . . . . , . . . . , . . . . , . . . . , . . . . 0.5 1.0 1.5 2.0 2+5 3.0 3.5 4.0 4.5 5+0 5.5 6,O 6.5 7.0 7.5 8.0 8.5 9.0 9.5 2.42.11.81 1.51 1.2: 0.9: 0.6; 0.3: 2 PFOS d + ?* I. 1 Page 320 of 703 Data File: D:\chem\Hillary.i\l3OlO222.b\HILLOlll.D Report Date: 20-Mar-2001 16:1;3 BACK TO MAIN Page 1 3M 13nvironmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i',HOlO222 .b\HILLOlll.D Lab Smp Id: Inj Date : 23-FEB-2001 13:23 Operator : KLT Inst ID: hi1lary.i Smp Info : 1311-4042-S1 Misc Info : Comment : Method : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 68 D i l Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * CF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---- 427 499 _ _ _ _RT EXP RT REL RT RESPONSE --_- ======== ======== =====E== 4.908 4.902 (1.000) 982392 5.139 5.126 (1.047) 265448 CONCE"R?iTIONS ON-COLUMN FINAL (ng/mL) --------- ( ug/L) - - - - - - - 249.300 11.2875 11.3 3M Environmental Laboratory Page 321 of 703 BACK TO MAIN 2.3; *: . t2.2; 2.1: 2.0j 1.9: 1.8; 1.7; 1.6; 1.5; 2c; i.4; 1.3: 5 1.2: >. 1.1; Lo; 0.9; 0.8; 0.7; 0.6; 0.5; 0.41 0.3; 0.2: 0.1; . . . v. .u. . . . . . . . . . . . . . . . . . . . . . . . I . . . . ( . . . . . . . . . . . . .ll. . . . .1 . . . . . . . . . . II ................................... 2.4: 2.11 1.8: 2 1.51 <0 r( 1.2: X V 0.9>. 0,6: 0.3- 2 PFOS ? - 0 d 1 1 ;I! 2,0{ 1.0: . . , . . . , . . . , . . . , . . , , . 4lh En%7hd&tal ??$bborabf&y Page 322 of 703 Data File: D:\chem\Hillary.i\110lO222.b\HILLO112.D Report Date: 20-Mar-2001 16:113 BACK TO MAIN Page 1 3M Znvironmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i\,HOlO222.b\HILL0112.D Lab Smp Id: Inj Date : 23-FEB-2001 13:34 Operator : KLT Smp Info : 1311-4042MS-S1 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\chem\Hillary.i\HOlO222.b\HOlO222t.m Meth Date : 13-Mar-2001 16:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-200122:42 Als bottle: 69 Cal File: HILL0032.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 323 of 703 Data File: D:\chem\Hillary,i\HO10222+b\HILLOL12.D D:\chem\Hillary,i\HO10222,b\HILL0112.D 9,0{ BACK TO MAIN Page 2 2.11 1.81 1.5: 1.2{ 0.9: M 1 THPFOS 2.0:' 1.8: h 1.4; Y0-j i.2; " 1.0; > 0.8; 0,6; 0.4; 0.2; 2 PFOS n; I I* 1 Page 324 of 703 Data File: D:\chem\Hillary.i\:3OlO222.b\HILLOll3.D Report Date: 20-Mar-2001 16:1'3 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i'~HOlO222.b\HILL0113.D Lab Smp Id: In? Date : 23-FEB-2001 13:45 Operator : KLT Smp Info : 1311-4043-S1 Inst ID: hil1ary.i Mikc Info : Comment : Method : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-2001 16:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Als bottle: 70 Cal File: HILL0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * IIF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -_--____ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) ____- _---_-_--------_----_-____------__ ___________ __-_______ 4.914 4.902 (1.000) 984852 249.300 5.145 5.126 (1.047) 269994 11.4511 11.4 3M Environmental Laboratory Page 325 of 703 BACK TO MAIN Data File: D:\chem\Hillary,i\HOlO222,b\HILLOtl3+D Page 2 0) 2.6; 0 LL 2.5; I1 1 - 2.4; ,2*3: '12.2: 24 2.0: 1.9; 1.8; 1.7; 1.6; 1.5: ; 1.4; ; 1+3; I 1*2; - 1.1; 1.0; 0.9; 0.8; 1 0.7; 0.6; 0,s: 0,4: 0.3; 0.2: 0*1; . . .v.u, . . . . , . . . . , . . . . , . . . . , . . . . . . . . . . . . . . . . . . . . . . . . I.. . u./. ..I. . . . 0.5 1.0 1.5 2,O 2.5 3.0 3.5 4,O 4.5 5,O 5.5 . , . . . . , . .I. I. . . . . . . . . . . . . . . . . . . . . . . . 1. . I...' 6.0 6.5 7.0 7.5 8,O 8.5 9.0 9.5 H 1 THPFOS rl 2.4: t ?0 2.1: 1.8i 1,s: 1.21 0.9: 0.6- 0.3- , . . . , . . . I,. . . . , . .1 . , . . . 2 PFOS 7.01 6.0; ,-. 5.0: p 4.0: A 0. : "x 3,Oi 2.0; 1.0; t-s ? LD 1 1 Page 326 of 703 Data File: D:\chem\Hillary.i\l3OlO222.b\HILLOll4.D Report Date: 20-Mar-2001 16:1;3 BACK TO MAIN Page 1 3M 13nvironmental Laboratory E00-1311 PFOS Adsorb/Desorb D&X file : D:\chem\Hillary.i',HOlO222.b\HILLOll4.D Lab Smp Id: Inj Date : 23-FEB-2001 13:56 Operator : KLT Inst ID: hillary.i Smp Info : 1311-4044-S1 Misc Info : Comment : Method D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-2001 16:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 71 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * EF * CpndVariable Cpnd Variable Local Compound Variable compounds - -. . . . . . . . . . . . . . . . . . . . . . . . . . * 1 THPFOS 2 PFOS QUANT SIG MASS ____ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) __ ___ _-___--______---_- ---___---_----_--_-- _---_____-- =E===== 4.925 4.902 (1.000) 999207 249.300 5.149 5.126 (1.046) 236262 9.88635 9.89 3M Environmental Laboratory Page 327 of 703 BACK TO MAIN Data File: D:\chem\Hillary,i\HOlO222~b\HILLOll4.D Page 2 D:\ch~?m\Hillary,i\H010222.b\HILLO114+D 2.6; 2.5; 2.4j ,2+3; 5.2; 2.1: 2.0: 1.9; 1.8; 1,7; 1+6! 1.5; ; 1.4; 2 1.3; 5 - i.2; 1.1; 1.0; 0.9; 0.8; 0.7; 0.6; 0.5; 0.4; 0.3; 0.2; 0.1; :...?I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . -/ - . . . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1.0 1.5 2.0 2.5 3.0 3+5 4+0 4.5 5.0 5.5 6+0 6 + 5 7.0 7.5 8 + 0 8.5 9.0 9.5 Y 1 THPFOS 2.41 24 1.81 CI yj i.5; :: 1.21 V 3 0.9: 0.6; 0,3{ L-cu ? d I\ 1 2 PFOS Page 328 of 703 Data File: D:\chem\Hillary.i\l~010222.b\HILL0115.D Report Date: 20-Mar-2001 16:113 BACK TO MAIN Page 1 3M Hnvironmental Laboratory E00--1311PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i~,HOlO222.b\HILLOll5.D Lab Smp Id: Inj Date : 23-FEB-2001 14:07 Operator : KLT Inst ID: hil1ary.i Smp Info : 1311-4045-Si Misc Info : Comment : Method : D:\chem\Hillary.i\,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-2001 16:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Als bottle: 72 Cal File: H1LL0032.~ Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ____ 427 499 RT EXP RT REL RT RESPONSE __-_-----_--------_------- -------_-- 4.922 4.902 (1.000) 997394 5.146 5.126 (1.046) 242527 CONCENTRATIONS ON-COLUMN FINAL _(n_g/_mL-)-_____-_( __u__g_/__L_)__ _ _ 249.300 10.1649 10.2 3M Environmental Laboratory Page 329 of 703 BACK TO MAIN Data File: D:\chern\Hillary,i\HO10222.b\HILLOL15,D Page 2 D:\ch~~m\Hillary.i\H010222.b\HILLO115.D 2.6; 0 LL a 2.5; c 1 2.41 ,! 2.3: 12.2: 2.1; 2.0; 1.9; 1.8; 1.7; 1+6{ 1.5; i; 1.4; 1.3; : 1.2; . 1.1: 1.0, 0,9! 0.8:: 0.7; 0.6: 0.5; 0.4; 0.3; 0,2; 0.1: . . . . . . . .v.u, . . . . , . . . . , . . . . , . . . . , . . , . . . , . . . 1 . . I J II .............................. . I . . . . , . . .. , . . . . , . . . . , . . . . 1 THPFOS 2.4: 2.11 1,8{ 1.51 1.21 0.9: 0.6; 0.3; a: L T u d 1 t 1 2 PFOS 6+5? 6.0; 5.5:: 5.0: 4.5: p~ 4.0; 3,5; $; 3.0: 2 2.5; > 2.0: 1.5; 1.0; 0.5: [ $ Ion Page 330 of 703 Data File: D:\chem\Hillary.i\:HOlO222.b\HILLOll6.D Report Date: 20-Mar-2001 16:19 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i'iH010222.b\HILLO116.D Lab Smp Id: Inj Date : 23-FEB-2001 14:18 Operator : KLT Inst ID: hil1ary.i Smp Info : 1311-4045MS-S1 Misc Info : Comment : Method : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-200122:42 Cal File: HILL0032.D Als bottle: 73 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * CF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _-_____ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RBSPONSE (ng/mL) ( ug/L) _ _ _ _ _-_____-----__-_--_-------_-_--___--____-__--_______-_______ 4.923 4.902 (1.000) 861434 249.300 5.154 5.126 (1.047) 4358791 209.780 210 3M Environmental Laboratory Page 331 of 703 BACK TO MAIN Data File: D:\chem\Hillary.i\HQlQ222.b\HILLQll6.D Page 2 '. D:\ch~sm\Hillary.i\HQlQZ b\HILLQ116+D 9,Q: 8.7: 8,4: 8.11 ,7,8{ `17.51 7.2: 6,91 6.6: 6.3: 6.0; 5,7: 5.41 5.1: ; , 4.8; 43: - 4+2{ 3.9: 3.61 3.3; 3.0: 2.71 2.41 2,Lf 1,8{ 1.5; 1.2; Q.9; 0.6; Q,31 II 0,5 1.0 1+5 2.0 2.5 3,O 3.5 4.0 4.5 5.0 5+5 6.0 6+5 7.0 7.5 8.0 8.5 9.0 9.5 Min H 1 THPFOS I\ 1.4; r 1.2; 3" 10..08;; 4,Q 2 PFOS ... ,. .. 4.4 4+8 5.2 Min ., .. . 5,6 Page 332 of 703 Data File: D:\chem\Hillary.i\HOlO222.b\HILLOl2l.D Report Date: 20-Mar-2001 16:18 BACK TO MAIN Page 1 3M 3nvironmental Laboratory E00-1311 PFOS Adsorb/Desorb Daka file : D:\chem\Hi11ary.i1~H010222.b\H1LL0121.D Lab Smp Id: Inj Date : 23-FEB-2001 15:14 Operator : KLT Smp Info : 1311-4046-S1 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\chem\Hillary.i~,HOlO222.b\HOlO222t.m Meth Date : 13-Mar-200116:Ol terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Als bottle: 74 Cal File: HILL0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * CIF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -_-_-- 427 499 RT BXP RT RBL RT RESPONSE --_____-_____-_---__=-=_==-==== ======== 4.923 4.902 (1.000) 1017804 5.147 5.126 (1.046) 330798 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= 249.300 ( ug/L) --__-__---__ 13.5623 13.6 3M Environmental Laboratory Page 333 of 703 Data File: D:\chem\Hillary.i\HOlO222+b\HILLOl2l.D BACK TO MAIN Page 2 % 1 THPFOS Ion 2+2: 2.0; 1.8; 1.61 * 1.4{ y 1.2r 3 Lo; X 0.8: > 0,s; 0.4; 0.2; , . . . , . I. . , . . . I I .. . I .. . 4.0 4.4 4.8 5.2 5,6 2 PFOS 7.0; * I on h -! m >2.0; Page 334 of 703 Data File: D:\chem\Rush.i\R013222.b\RUSHOO53.D Report Date: 09-Mar-20011 O : O l BACK TO MAIN Page 1 3M Environmental Laboratory DAta file : D:\chem\Rush.i\RO:L0222.b\RUSH0053.D Lab Smp Id: Inj Date : 23-FEB-2001 02:39 Operator : KLT/MLA Smp Info : 1311-4061-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Als bottle: 26 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * 1)F * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---___ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ---- -------- _--_------_-- -_--_____ ___ ___ _ _ _======= ( ug/L) ======= 5.555 5.512 (1.000) 713961 249.300 Compound Not Detected. 3M Environmental Laboratory Page 335 of 703 Data File: D:\chem\Rush.i\RO10222,b\RUSHOO53.D BACK TO MAIN Page 2 1 THPFOS 1.8; 1.61 1.4i ~ 1.2: 6Ln 1.0; rxl 0.8; v >- 0.6; 0.4; 2 PFOS tundetected) 2.8; 1 2.6j 2.4: 2.2; 2.0; 2 1.8; Page 336 of 703 Data File: D:\chem\Rush.i\R013222.b\RUSHOO54.D Report Date: 09-Mar-20011 O : O l BACK TO MAIN Page 1 3M jznvironmental Laboratory Data file : D:\chem\Rush.i\R010222.b\RUSH0054.D Lab Smp Id: Inj Date : 23-FEB-2001 02:50 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4062-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R0:-0222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSH0032.D Als bottle: 27 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---_-_ 427 499 RT EXP RT REL RT RESPONSE ==== ======== ======== _-_-_-== 5.559 5.512 (1.000) 722949 5.783 5.722 (1.040) 52969 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= 249.300 ( ug/L) -__-_---__- _- 2.96660 2.97 3M Environmental Laboratory Page 337 of 703 Data F i l e : D:\chen\Rush,i\RO10222,b\RUSHOO54.D BACK TO MAIN Page 2 H 1 THPFOS 2.0: 1.8; 1.6: Y eb-i b-i 1.4: A 1+2{ bIs) i.0; d ,X 0.8: >. 0,6{ 0,4: 0.2: . . , . . . , 1. . . ,\ . . . , 1. . . , . 2 PFOS 8.0; 7.0: 6,O:' ' 6 5.0; < 4 4.0; " > J+O{ 2.0; r ? Ion CD b-i 1 Page 338 of 703 Data File: D:\chem\Rush.i\R013222.b\RUSHOO55.D Report Date: 09-Mar-20011 O : O L BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\RO:L0222.b\RUSH0055.D Lab Smp Id: Inj Date : 23-FEB-2001 03:Ol Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4063-S1 Misc Info : Comment : Method : D:\chem\Rush.i\ROL0222.b\ROlO222t.m Meth Date : 09-Mar-200109:15 terrell Quant Type: ISTD Cal Date : 22-FEB-200122:45 Cal File: RUSH0032.D Als bottle: 28 D i l Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Locial Compound Variable 3M Environmental Laboratory Page 339 of 703 Data File: D:\chem\Rush,i\R010222,b\RUSH0055,D D:\chem\Rush.i\R010222,b\RUSHOO55.D "22 1.9; LL 1 1 I- 1.8; ,:1+7: i: 1.6: 1.5; 1+4; 1,3; 1.21 1.1; 1.0: I i 0,s; 0.8; 0.7; 0.64 0+5{ 0,4{ 0.3: 0,2{ 0.1; . . .1J.-d, . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1 . L .l 1 THPFOS tu, 1,8{ L? UJ 1.61 1.4; h 1*2{ Lio, i.0; Ti YX 0,8{ >- 0.6: 0,4; 0,2{ . . , . . . , .1. .. ,1 . . . ,1 . . . , . 2 PFOS (Undetected) I Ion BACK TO MAIN Page 2 Page 340 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO65.D Report Date: 09-Mar-2001 1 O : O : L BACK TO MAIN Page 1 3M Environmental Laboratory Ddta file : D:\chem\Rush.i\ROI-0222.b\RUSH0065.D Lab Smp Id: Inj Date : 23-FEB-2001 04:53 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4067-S1 Misc Info : Comment : Method : D:\chem\Rush.i\ROI.0222.b\RO10222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSH0032.D Als bottle: 34 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * CF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS 2 PFOS QUANT SIG MASS -_ _-____ 427 499 _ R_ T_ _ EXP RT REL RT _ _ _ _ _ _=_=--=-_===== RESPONSE ======== 5.532 5.512 (1.000) 715149 5.750 5.722 (1.039) 708991 CONCENTRhTIONS ON-COLUMN FINAL (ng/mL) ( ug/L) =5===== =====E= 249.300 39.3413 39.3 3M Environmental Laboratory Page 341 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010222,b\RUSHOO65,D Page 2 D:\chem\Rush.i\R010222,b\RUSHOO65.D 2.0: 1.9; 1.8: !; 1.71 i. 1.6; 1.5: 1.4: 1+31 1.21 1.1: , > 1.0{ + : 5 0.9; 0.81 0.7: 0,61 0.5: 0.44 0,3{ 0.24 0.1: :..!+ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .....,..... . . ,. . . . . .,.........,. . . . . ., . . . . , . . . . , . . . . 0.5 1,0 1,5 2.0 2.5 3,O 3.5 4.0 4,5 5.0 5 6.0 6+5 7.0 7,5 8.0 8.5 9,O 9,5 Min 1 THPFOS 2,o: 1,s: 1,6{ 1.4: r\ 1.2: P 3 1.0: ' vx 0.8' > 0.6: 0.4: 0,21 PU J 1 \ 1 2 PFOS h Lo 0 4 " >- Page 342 of 703 Data File: D:\chem\Rush.i\R013222.b\RUSHOO66.D Report Date: 09-Mar-2001 1 O : O L BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\RO:LO222.b\RUSH0066.D Lab Smp Id: Inj Date : 23-FEB-2001 05:04 Operator : KLT/MLA Smp Info : 1311-4068-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\R010222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Als bottle: 35 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * LIF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --__ 427 499 CONCENTRATIONS ON-COLUMN RT BXP RT RBL RT RBSPONSE (ng/mL) --_-_- --_-_--___-_----__-__--_-_--_--_--__________- _ _ _======= 5.525 5.512 (1.000) 718563 249.300 FINAL ( ug/~) -----___ 5.749 5.722 (1.041) 738565 40.8065 40.8 3M Environmental Laboratory Page 343 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010222,b\RUSHOO66.D Page E D:\chem\Rush.i\R010222.b\RUSHO066.D 2.0; 1,9! ... 1.8; . '1.7; 1,6; 1.5: 1.4: 1.3: 1.21 ; 1,1: : 1.0: 0.9; 0.81 0.7: 0.61 0.5; 0.4: 0.3; 0.2; 0.1; . . .IN . I . . . . , . . . , , . . . . , . . . . , . . . . , . . . . , . 0.5 1,O i.5 2.0 2,5 3.0 3.5 4.0 4,5 5.0 5 J. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6.0 6.5 7.0 7.5 8.0 8,5 .,....,.. ., 9.0 9.5 W 1 THPFOS 2.0: 1,8; 1.6{ 1.41 6c. 1,2: Lo t.0; d Y 0,8{ >- 0.61 0.4; 0,2; I-? N Iz) I )l 1 2 PFOS 2.0; 1.8; 1,6: 1,4; 90 1.0; d 5 0.8; 0+6: 0.4: 0.2: Ion r $ 1 \I Page 344 of 703 Data File: D:\chem\Rush.i\R011~222.b\RUSHOO67.D Report Date: 09-Mar-2001 1 O : O : L BACK TO MAIN Page 1 3M Environmental Laboratory Daka file : D:\chem\Rush.i\RO:t0222 .b\RUSH0067.D Lab Smp Id: Inj Date : 23-FEB-2001 05:16 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4069-S1 Misc Info : Comment : Method : D:\chem\Rush.i\ROI.0222.b\RO10222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSHO032.D Als bottle: 36 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target: Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * ClF * CpndVariable Cpnd Variable Local Compound Variable Compounds QUANT SIG MASS CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL R T RBSPONSE (ng/mL) ( ug/~) 3M Environmental Laboratory Page 345 of 703 BACK TO MAIN Data F i l e : 1.9; 1.8; D:\chem\Rush,i\R010222.b\RUSHOO67..D p D:\chem\Rush.i\R010222,b\RUSHOO67.D i1.7: t. 1+6: 1.5; 1.4: 1.31 1.2; 1.1; ; 1.0{ -4: 5 0,s: - 0.8; 0.7; 0.61 0.5; 0.4; 0.3: 0.21 o,1; . . .Id . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1,0 1,5 2,O 2.5 3.0 ,....,..,............................................. 3.5 4.0 4,5 5,O 5.5 6.0 6 + 5 7.0 7,5 8.0 8,5 Min 1 THPFOS Page 2 .,. . . .,. . . . 9,O 9.5 Er. 1+2; 1.0; d vX 0 , 8 { + 0.6; 0.4{ 0.21 . . , . . . , I. . !. , . . . , 1. . . , . 4.8 5.2 5.6 6,O 6,4 Min 2 PFOS Page 346 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO68.D Report Date: 09-Mar-2001 1O:O:- BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\R010222.b\RUSH0068.D Lab Smp Id: Inj Date : 23-FEB-2001 05:27 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4069MS-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Als bottle: 37 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---- 427 499 RT BXP RT RBL RT RBSPONSB _--- ----_-_--_- ----------_- --------- 5.539 5.512 (1.000) 626695 5.763 5.722 (1.040) 3383101 CONCBNTRATIONS ON-COLUMN FINAL (ng/mL) ( ug/L) - -_-_--__-__ _======= 249.300 228.263 228 3M Environmental Laboratory Page 347 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010222+b\RUSH0068.,D 6.91 6.6: 6.31 6c 6,0{ 5,7{ 5,4{ 5.1- 4.81 4.51 4.21 3.91 3.61 2 3.3; - 3.01 2.71 2.41 2.1; 1,81 1.5: 1.2: 0.91 0.61 0.31 . . .I-. .I. . . . . . . . . . . . . . . . . . . . . . . . 0,5 1-0 1.5 2,O 2.5 D:\chem\Rush.i\R010222.b\RUf ,....,....,.... , . ... ,.... 3.0 3,5 4.0 4.5 5,O 5:; Hin 1 THPFOS 068. D Page 2 6.0 6.5 7.0 7.5 8.0 8,5 9.0 9,5 2 PFOS Page 348 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO69.D Report Date: 09-Mar-2001 10:0:! BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\RO:.0222 .b\RUSH0069.D Lab Smp Id: Inj Date : 23-FEB-2001 05:38 Operator : KLT/MLA Smp Info : 1311-4070-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\ROI.0222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Als bottle: 38 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds ____ _ _ _ _ _ _ _______-____ _ _ _ _ _ _ ____ * 1 THPFOS 2 PFOS QUANT SIG MASS - _ _ __ 42 7 499 CONCENTRATIONS ON-COLUMN RT BXP RT RBL RT RESPONSE (ng/mL) _ _ _ _ -----______---__--_____-----___-_____=5===== 5.541 5.512 (1.000) 723074 249.300 FINAL ( ug/L) -- -___-_______ 5.758 5.722 (1.039) 353028 19.2794 19.3 3M Environmenfal Laboratory Page 349 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010222,b\RUSH0069,D Page 2 2.0; 1.91 1.81 ,. .;1,7{ D:\chem\Rush.i\R010222.b\RUSH0069.D LCD e9I- 1.61 1.51 1.41 1.31 1.21 , 1.11 1 > 1.01 !' : 0.91 0.81 0,7+ 0.61 0,5< 0.4; 0.3; 0.2: 0.11 . . .I . N, . . . . , . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1 . . . . .1 . . . . . . . . 0.5 1.0 1.5 2,O 2.5 3+0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 , . , . . . . . . . . . . . . . . . . . . . . . . . . . . . 7+0 7.5 8,O 8.5 9,O 9,5 1 THPFOS 2 PFOS IIIjl9+0i 8.0; Ion a, -Lo '5 Lo 7.0; r\ 6.0; 60 5.0; txi 4.0: Y >. 3.0; 2.0:: - L o ; I . . . , . . .I.1. .C. L. .-. . . . . . Page 350 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO7O.D Report Date: 09-Mar-200110:0:! BACK TO MAIN Page 1 3M IZnvironmental Laboratory Daka file : D:\chem\Rush.i\R0:!0222.b\RUSH0070 .D Lab Smp Id: Inj Date : 23-FEB-2001 05:49 Operator : KLT/MLA Smp Info : 1311-4071-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\R010222t.m Meth Date : 09-Mar-200109:15 terrell Quant Type: ISTD Cal Date : 22-FEB-200122:45 Als bottle: 39 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all sub Processing Host: W19401 Concentration Formula: Amt * CF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS __ __ -___ 427 49 9 RT EXP RT REL RT RESPONSE _____- __------_-____---------_------------ 5.541 5.512 (1.000) 713569 5.758 5.722 (1.039) 401704 CONCENTRATIONS ON-COLUMN FINAL _-(n--g-/--m-_L_)____ __(__u_g_-/_L__)____ 249.300 22.2391 22.2 3M Environmental Laboratory Page 351 of 703 Data File: D:\chem\Rush,i\R010222,b\RUSHO07O,D D:\ciem\Rush.i\R010222.b\ 1.9; 1,8{ iH, 0070,D to D t E BACK TO MAIN Page 2 1.21 1.11 ' LO{ i: 5 0.9; 0,3{ 0,2{ 0.1; :. . !?. . . . , . . . . , . . . . , . . . . , . . . . , . . . . , -. . 0,5 1.0 1,5 2.0 2,s 3.0 3.5 4.0 4.5 5.0 5 Min Y 1 THPFOS 1.8; 1+6; - * Ion t r*l Y Lo 1,4{ 5 i.2; Lo 1.0; x 0.81 W > 0+6{ 0.41 0t2ja 0,2{ . . , . . . , . 1 . . , . . . 1, . . . I . 1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . , . . . . 6.0 6.5 7.0 7.5 8,O 8.5 9.0 9,5 2 PFOS Page 352 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO7l.D Report Date: 09-Mar-200110:0;! BACK TO MAIN Page 1 3M Ehvironmental Laboratory Data file : D:\chem\Rush.i\R01.0222.b\RUSH0071.D Lab Smp Id: In] Date : 23-FEB-200106:OO Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4072-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSH0032.D Als bottle: 40 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -_-_-__ - 42 7 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ny/mL) ( ug/L) ==== =E====== ======== ==== === ==== == I= = - - - - _ _ 5.539 5.512 (1.000) 710887 249.300 5.756 5.722 (1.039) 385139 21.3995 21.4 3M Environmental Laboratory Page 353 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010222,b\RUSHOO7l,D Page 2 D:\c?em\Rush,i\R010222.b\RUSHOO7l.D 1.9: 1.8; 1,7{ *:1.6{ 1.5; 1.41 1,3; 1.21 1,1{ ; 1.0; I 0.9: ' 0.81 0.71 0.61 0.5: 0.4: 0.3; 0.21 .d O , l { . . .I . N, . . . . , . . . . , . . . . , . . . . , . . . . , . . . . , . 0.5 1.0 1.5 2+0 2.5 3.0 3.5 4.0 .,.... 4.5 5+0 5 Min .,....,.... I . . . . , . . . . , . . . 6+0 6.5 7+0 7.5 8.0 1 THPFOS . ( . . . ., . . . . , . . . . 8,5 9.0 9.5 2 PFOS I on Page 354 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO72.D Report Date: 09-Mar-2001 10:0;! BACK TO MAIN Page 1 3M E:nvironmenta1 Laboratory Data file : D:\chem\Rush.i\R01.0222.b\RUSH0072.D Lab Smp Id: Inj Date : 23-FEB-2001 06:11 Operator : KLT/MLA Smp Info : 1311-4072MS-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Als bottle: 41 Cal File: RuSH0032.~ Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS ---- 42 7 499 RT EXP RT RBL RT RESPONSE --_-_- --------- -------- -------- 5.539 5.512 (1.000) 626987 5.756 5.722 (1.039) 3324237 CONCENTRATIONS ON-COLUMN (ng/mL) --====== FINAL ( ug/L) ======= 249.300 223.877 224 3M Environmental Laboratory Page 355 of 703 Data File: D:\ohem\Rush,i\R010222.b\RUSHOO72.,D 6.91 6.6: 6.31 16.01 1 5.71 5.41 5.11 4.81 4.51 4,2{ . 3.91 ' 3.61 g 3.3: e 3.01 2.71 2.41 24 1.81 1.5: 1.21 0,9{ 0.61 0.3: . . .I.- .I. . . . . . . . . . . . . . . . . . . . . . . . D:\chem\Rush,i\R010222.b\RUSHOO72+D I '. " I ' ' Y 1 THPFOS 1.2: 4c; 1.0; 0.8; X 0.61 > 0,4{ 0.2{ 2 PFOS BACK TO MAIN Page 2 Page 356 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO73.D Report Date: 09-Mar-200110:0:1 BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\R0:!0222 .b\RUSH0073.D Lab Smp Id: In] Date : 23-FEB-2001 06:23 Operator : KLT/MLA Smp Info : 1311-4073-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-200109:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Als bottle: 42 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * I3F * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS __-- 427 499 RT EXP RT RBL RT RESPONSE _ _ _ _ ________-_-_-___-__-___ ___-_ _ _ _ 3======= 5.546 5.512 (1.000) 719422 5.770 5.722 (1.040) 366061 CONCENTRATIONS ON-COLUMN (ng/mL) ======= 249.300 FINAL ( ug/L) ======= 20.0945 20.1 3M Environmental Laboratory Page 357 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010222.b\RUSH0073,D Page 2 1.9: 1.81 1.71 ,. 'i1.6; 1.5: 1,4! D:\cl1em\Rush.i\RO10222+b\RUSHOO73.D Ev ) 0 LL [L 1.34 1.2; 1.11 ; 1.Of > 0.9; 2 + 0.8: 0,71 0,6; 0.5; 0,41 0.3{ 0.24 0.1; 1 . . !?. . , . , . . . . , . , . . , . . . . I . . . . , . . . .,, -. . 0.5 1.0 1,5 2,O 2.5 3.0 3.5 4.0 4.5 5,O Min .i.. , . . . . , . . .-., . . . . , . . . . ;. . . : , ::. . I " . ' , " " 5.5 6,O 6.5 7.0 7,5 8.0 8.5 9.0 9.5 H 1 THPFOS 1 -: 4.8 5.2 5.6 6.0 6.4 2 PFOS Ion 9.0; 8.0; 7.0; Page 358 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO74.D Report Date: 09-Mar-200110:0;! BACK TO MAIN Page 1 3M Etnvironmental Laboratory Data file : D:\chem\Rush.i\R01.0222.b\RUSH0074.D Lab Smp Id: Inj Date : 23-FEB-200106:34 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4074-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-200122:45 Cal File: RUSH0032.D Als bottle: 43 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _- _-_ _ 427 499 CONCENTRATIONS ON-COLUMN FINAL R T EXP R T RBL RT RESPONSE (ng/mL) ( ug/L) ____ ________ --__________-____---__--__-_ _ _ _ _ _ _ _ 5.546 5,512 (1.000) 721925 249.300 5.770 5.722 (1.040) 377219 20.6367 20.6 3M Environmental Laboratory Page 359 of 703 Data File: D:\chem\Rush,i\R010222.b\RUSHOO74..D 1.9; 1.8; I,1*7.: i. 1.6: 1.51 1.41 1.3; 1.2r 5H0074.D 'v) 0 LL Q 1 I- BACK TO MAIN Page 2 0.6: 0.5; 0,4{ 0.3; 0.2; 0.1; :+ . . . . , . . . , , . . . . , . . . . , . . . . , . . . . , -. . 0.5 1,0 1,5 2,O 2.5 3.0 3,5 4.0 4+5 5.0 5 X 1 THPFOS t. , . . . . , . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6,O 6.5 7,O 7 + 5 8+0 8.5 9.0 9.5 1.61 1.41 c. 1*2L " . UJ ( Lo: 4 X 0,8{ >- 0.64 0.41 0.2: 2 PFOS 1.0: 0.9: 0.8; 0.7; ;; 0.6; 6 0.5; 5d 0.4; 0.3; 0.2j 0.1; 11. 1 er. '5 Lo 1 L I._ Page 360 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO79.D Report Date: 09-Mar-200110:0;! BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\R010222.b\RUSHOO79.D Lab Smp Id: Inj Date : 23-FEB-2001 07:30 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4075-S1 Misc Info : Comment : Method D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Cal Date : 22-FEB-2001 22:45 Quant Type: ISTD Cal File: RUSH0032 .D Als bottle: 44 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _-_____ _ 427 499 RT EXP RT REL RT RESPONSE -_____---------- -------- -_------ 5.547 5.512 (1.000) 721016 5.779 5.722 (1.042) 356402 CONCENTRATIONS ON-COLUMN FINAL __(_n__g_/__m_L-_)_ _ _=( =u=g=/=L=)= 249.300 19.5198 19.5 3M Environmental Laboratory Page 361 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO79..D BACK TO MAIN Page 2 Y 1 THPFOS 1.8; 1.6; 1.4: A 1.2; 6Lo i.0; " . rl X 0.8; > 0,6{ 0.4; 0,2; 2 PFOS Y L b m lli I Page 362 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO8O.D Report Date: 09-Mar-20011 0 : 0 : 1 BACK TO MAIN Page 1 3M IZnvironmental Laboratory Data file : D:\chem\Rush.i\RO:L0222.b\RUSH0080.D Lab Smp Id: Inj Date : 23-FEB-200107:41 Operator : KLT/MLA Smp Info : 1311-4075MS-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\R010222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-200122:45 Als bottle: 45 Cal File: RUSH0032.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * I I F * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---_ 427 499 RT BXP RT REL RT RESPONSE ==== = = = = e = = = ======== ======== 5.541 5.512 (1.000) 630748 5.772 5.722 (1.042) 3329105 CONCENTRATIONS ON-COLUMN (ng/mL) ======= 249.300 FINAL ( ug/L) __----___ -_- _- 222.791 223 3M Environmental Laboratory Page 363 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO8O,D I6.01 t 5.71 5.41 5.11 4.81 4.51 4.21 3,9{ A L<n 3.61 0 4 "x 3.31 > 3.0: 2.71 2.41 2.11 1.81 l.5{ 1.21 0.9{ W 1 THPFOS m 0 aLL I/ I- BACK TO MAIN Page 2 2 PFOS Page 364 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOO8l.D Report Date: 09-Mar-200110:02 BACK TO MAIN Page 1 3M Etnvironmental Laboratory Data file : D:\chem\Rush.i\R01.0222.b\RUSH0081.D Lab Smp Id: In] Date : 23-FEB-2001 07:52 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4076-S1 Misc Info : Comment Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-200122:45 Cal File: RUSH0032.D Als bottle: 46 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ____ 427 499 CONCENTRATIONS ON-COLUMN RT EXP RT REL RT RBSPONSE (ng/mL) _____ ___--_______- -_- _-_ _ _ - -_-__-______- _____- E====== FINAL ( ug/L) =====I= 5.553 5.512 (1.000) 721345 249.300 5.777 5.722 (1.040) 400719. 21.9443 21.9 3M Environmental Laboratory Page 365 of 703 Data F i l e : D:\chem\Rush,i\R010222,b\RUSHO0814.D D:\c-1em\Rush,i\R010222,b\RUSHOO8l~D *:. 1,7; . `1.6; 1.5: 1.4; 1.3: 1.2: . 1.1; 1.0: ''5 . : 0.9: 0.8; 0,4{ 0.3: 0.2; 0.1{ .. .., ................................................ 0+5 1.0 1.5 2.0 2.5 3.0 3.5 4,O 4,5 5,0 Min W 1 THPFOS BACK TO MAIN Page 2 2 PFOS 0.7; 3$ 0.6: 0.5: v 0.4; 0.3; 0.2: 0.1; , . . . , . . . 1 I . . . ,1. . . , . . . `83M%virio5dhenfd La6d;atory Page 366 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOlO7.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Da%a file : D:\chem\Rush.i\R010222.b\RUSH0107.D Lab Smp Id: I n j Date : 23-FEB-2001 12:43 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4090-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSH0032.D Als bottle: 64 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 367 of 703 BACK TO MAIN Data File: D:\chem\Rush.i\R010222.b\RUSH0107.D Page 2 D:\chem\Rush,i\RO10222,b\RUSHQIQ7.D 1,8{ 1.7; d 1.6 t: 1.5{ 1.4; 1.31 1.21 1.11 ' 1.0; i 0.9; 0.81 0,7{ 0.6; 0.5; 0.41 0,3{ 0.2; 0.1: . . .I. .d. . . . . . . . . . . . . . . . . . . . . . . . 0,5 1.0 1.5 2 + 0 2.5 - , . . . . , . . . . , . . . . , . . . . , . . . .1 , - ................................ 3.0 3.5 4.0 4.5 5.0 5, 6.0 6.5 7.0 7+5 8,O 8,5 Min W 1 THPFOS 9. ,IQ. . . 9. :5"' 2 PFOS Page 368 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOlO8.D Report Date: 09-Mar-200110:03 BACK TO MAIN Page 1 3M Environmental Laboratory Data file : D:\chem\Rush.i\R010222.b\RUSH0108.D Lab Smp Id: Inj Date : 23-FEB-2001 12:54 Operator : KLT/MLA Smp Info : 1311-4090MS-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-200109:15 terrell Cal Date : 22-FEB-2001 22:45 Als bottle: 65 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Processing Host: W19401 Quant Type: ISTD Cal File: RUSH0032.D Compound Sublist: all.sub Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---- 427 499 RT BXP RT RBL RT RBSPONSB ==== ======== ======== ======== 5.521 5.512 (1.000) 594782 5.745 5.722 (1.041) 3043722 CONCENTRATIONS ON-COLUMN (ng/mL) ------- 249.300 FINAL ( ug/L) -_------_--__ 215.511 216 3M Environmental Laboratory Page 369 of 703 Data File: D:\chem\Rushri\R010222.b\RUSHO108.D BACK TO MAIN Page 2 M 1 THPFOS 2 PFOS 5.0; ' 6 4.0: ' 6I S ) : ,-I 3.0; \ " > 2.0; fl 1.0; , . . . , . 1. . 1 , . .,. , . .r .A, . . . *3M%6vi&henklPLa bbhtory Page 370 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOlO9.D Report Date: 09-Mar-200110:03 BACK TO MAIN Page 1 3M Environmental Laboratory DGta file : D:\chem\Rush.i\R010222.b\RUSH0109.D Lab Smp Id: Inj Date : 23-FEB-200113:05 Operator : KLT/MLA Inst ID: Rush.i Smp Info : 1311-4091-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\R010222t.m Meth Date : 09-Mar-200109:15 terrell Quant Type: ISTD Cal Date : 22-FEB-200122:45 Cal File: RUSH0032.D Als bottle: 66 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUpSSr SIG MASS _--_- 427 499 CONCENTRATIONS ON-COLUMN FINAL RT BXP RT RBL RT RESPONSE (ng/mL) _--_--- __- -_- -_____- -_---_---_--_--_ -_-___-_--_--_- - _ _======= ( ug/L) ======= 5.520 5.512 (1.000) 696138 249.300 Compound Not Detected. 3M Environmental Laboratory Page 371 of 703 Data File: D:\chem\Rush,i\R010222,b\RUSHOlO9.D 1.9; 1.8; ,?,1,7{. '1.6; 1.5: 1.4: 1.3{ 1.2: 1.1; ;' 1.0; 0.9,: 0.81 0.7; 0.6; 0.5; 0,4; 0.31 0.24 0.q IM M 1 THPFOS 1,8< 1.6; 1.4; ~ 1.2; 1.0; d x 0.8: w >- 0.6L 0.4; 0.2; . . . . . , . ,. . I ' " 1 1 ..'I. 4,8 5.2 5.6 6.0 6.4 Min 2 PFOS (Undetected) I Ion 1 2,4; 2.21 2.0; 8 1.8; 1.6; 1+4i -4 1.2; 1.0; 0.8: 0.61: 0.4: , . . . , . . . , . . . , . . . , . . . 4*83M%fi~i&henfaf'La60?atory BACK TO MAIN Page 2 au) 0 LL 1 t 1. Page 372 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOllO.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Datta file : D:\chem\Rush.i\R010222.b\RUSHO110.D Lab Smp Id: Inj Date : 23-FEB-2001 13:16 Operator : KLT/MLA Smp Info : 1311-4092-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSH0032.D Als bottle: 67 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --_-_ _ 427 499 RT EXP RT RBL RT RESPONSE __ ___ ___-_ _ _ _ _ _ _ ------_--- ----_-_-_-_-_= 5.502 5.512 (1.000) 702240 Compound Not Detected. CONCENTRATIONS ON-COLUMN (ng/mL) ======= FINAL ( ug/~) ======= 249.300 3M Environmental Laboratory Page 373 of 703 Data File: D:\chem\Rush.i\R010222~b\RUSHOllO~D D:\chem\Rush,i\R010222. 1.81 1,7{ 1,6; ISHO11O.D -cn 0 LL Q I I- BACK TO MAIN Page 2 1.31 1.2{ 1.1; rr 1.0; bLo 0,s; " > 0.81 0.7: 0.6; 0.51 0.41 0.31 0.2{ 0,1; . . .I.N . . . . . . . . . . . . . . . . . . . 0.5 1,O 1.5 2.0 1 THPFOS . , . . . . , . . .. , . . . . , . . . . ,.. .. ,. .. 2.5 3,O 3.5 4.0 4.5 5.0 Min - .I.d. . , . . . . , . . . . , . . . . , . . . . , . . . . , . . . . , . . . . , . . . . 5 6*O 6*5 7+0 7.5 8+0 8.5 9,0 9,5 4.8 5.2 5.6 Min 2 PFOS <Undetected> I on 1,s; l,6: 1.41 h p 1.2; 0 v rxl 1.0: l 6.0 6.4 O*4- , . . . , . . . , . . . , . . . , . . . 4+83M?5?wi&henktpLab$yf%tory Page 374 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSHOlll.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Ddta file : D:\chem\Rush.i\R010222.b\RUSHOlll.D Lab Smp Id: Inj Date : 23-FEB-2001 13:27 Operator : KLT/MLA Smp Info : 1311-4093-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010222.b\ROlO222t.m Meth Date : 09-Mar-2001 09:15 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:45 Cal File: RUSH0032.D Als bottle: 68 D i l Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---_-_ 427 499 RT EXP RT RBL RT RESPONSE ==_= _-_-__---_--_-_--_-=-== ======== 5 . 5 0 4 5.512 (1.000) 713216 Compound Not Detected. CONCENTRATIONS ON-COLUMN FINAL (ng/mL) =E===== ( ug/L) ======= 249.300 3M Environmental Laboratory Page 375 of 703 Data File: D:\chem\Rush,i\R010222~b\RUSHOl11.D BACK TO MAIN Page 2 1.9; 1.81 ~ F 1.71 . '1+6; 1*5{ 1.4; 1,3; 1.2: 1.1; ' 1,o; ' 0.91 0,8{ 0.7; 0.6{ 0.5i 0.4; 0.31 0.2: 0.1; . . .I.N. . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1.0 1.5 2.0 2.5 ,....,....,.... ,....,... 3.0 3.5 4,0 4.5 5,O Hin Y 1 THPFOS f . . . , . . . . , . . . , . . . . , . . . . , . I . . , . . . . , . . . .,....a 6.0 6.5 7.0 7.5 8.0 8,5 9,O 9.5 1.41 Err 1.2; 1.0; .x-I 0.8; v . > 0+6{ 0.41 0.21 I 1.81 1.6: 1.4: 1*21 0 1,0{ I,x I 0.8: II 1 Ion b Page 376 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILLOO36.D Report Date: 28-Mar-200109:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Diita file : D:\Chem\Hillary\HO10309.b\HILL0036.D Lab Smp Id: 1311-4103-S1 In] Date : 09-MAR-2001 22:29 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-200121:32 Cal File: HILL0031.D A1s bottle: 14 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 377 of 703 BACK TO MAIN Data File: D:\Chern\Hillary\HO10309.b\HILLOO36.D Page 2 D:\Chem\Hillary\HO10309.b\HILL0036.D v) ? i 2,2; n. i 2.14 c 2.0: 'il.9; 1.81 1.7; 1+6; 1.5; 1.4; 1.3: ;G 1.2; 1.1: " 1.0; > 0.9; 0.8; 0.7; 0.6: 0.51 0,4; 0.3:' 0.22 0,1{ c . . .I . N, . . . . , . . . . , . . . . , . . . . , . . . . , . . . . . . . . . . . . . . . . . . . .1. . . . . . . . . . . . . . ,. . . . ,. . . . 0,s 1.0 1 3 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5,s 6.0 6.5 7,O 7,5 8,O 8.5 9,o 9.5 2.21 2.0< 1.8: 1.6; c. 1.42 y 5 1.2; id?; V 0.8: 2- 0.61 0.4; 0.2; ? I - m Is) I,\ 1 Page 378 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0037.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\Chem\Hillary\HO10309.b\HILL0037.D Lab Smp Id: 1311-4104-S1 Inj Date : 09-MAR-200122:40 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment Met hod : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:lO anderson Quant Type: ISTD Cal Date : 09-MAR-200121:32 Cal File: HILL0031.D Als bottle: 15 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: a l l sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --_- 427 499 RT EXP RT REL RT RESPONSE ==== ======== ======== ======Ei= 5.037 5.009 (1.000) 1221819 5.268 5.233 (1.046) 215844 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) =E===== (ug/mL) ======= 254.000 6.16960 6.17 3M Environmental Laboratory Page 379 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0037~D BACK TO MAIN Page 2 w 1 THPFOS 2.2: 2.0; 1.81 1.6; 1.4j 1.2: 1,o; 0.8; 0.61 4 c1.3 Lo 2 PFOS Page 380 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0038.D Report Date: 28-Mar-200109:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data f i l e : D:\Chem\Hillary\HO10309.b\HILL0038.D Lab Smp Id: 1311-4105-S1 Inj Date : 09-MAR-200122:51 Operator : KLT Smp Info : Study Number E00-1311 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:lO anderson Quant Type: ISTD Cal Date : 09-MAR-200121:32 Als bottle: 16 Cal File: HILL0031.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds .......................... * 1 THPFOS 2 PPOS QUANT SIG MASS ---- 427 499 RT EXP RT ==== E======= REL RT RESPONSE ======== ======== 5.042 5.009 (1.000) 1028599 5.266 5.233 (1.044) 237536 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ug/mL) =------ 254.000 8.37553 8.38 3M Environmental Laboratory Page 381 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10309~b\HILLO038,D Page 2 2.2f 2.1; .2.0; . il.9:' D:\Chem\Hillary\HO10309.b\HILLOO38~D LV) 0 LL LL i I- 1.8: 1.7; 1.6; 1.5; 1.4; . 1.3: 1.2; ; ' : 1.1: 1.0; 0.9: 0,s: 0.7: 0,6; 0.5:' 0.41 0.3: 0.2: 0.1: . . .l/.L.l . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . I,. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . M 1 THPFOS 2 PFOS c. . . . . . Page 382 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILLOO39.D Report Date: 28-Mar-200109:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dkta file : D:\Chem\Hillary\HO10309.b\HILL0039.D Lab Smp Id: 1311-4105MS-S1 Inj Date : 09-MAR-200123:03 Operator : KLT Smp Info : Study Number E00-1311 Inst ID: hi1lary.i Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-200121:32 Als bottle: 17 Cal File: HILL0031.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS -_-___ 427 499 _R_T --__-E__X_P---R__T-_--__R-_E_L-_-R_T _-_R____B____S_P__O_- _N___SB__ 5.029 5.009 (1.000) 874849 5.260 5.233 (1.046) 3963142 CONCENTR?iTIONS ON-COLUMN FINAL (ng/mL) ======= (ug/mL) ======= 254.000 190.967 191 3M Environmental Laboratory Page 383 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10309.b\HILL0039.D Page 2 D:\Chem\Hillary\HO10309 \HILLOO39,D 6.9: , 6.6; 6.3: 6.01 5.71 5.41 5.11 4,81 4.5: 4.21 3.9: 3.61 3.3- 3.0- 2.7; 2.41 2.11 1.81 1.5; 1.21 0.91 0+6: 0.3: . . .I-. .I. . . . . . . . . . . . . . . . . . . . . . . . . . . . . tfn P 1 k- 1 . . . . . . . . . . . . . . . .1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . ,1 . . .1 . , -. 1 THPFOS 11.8; 1.6: 1,4{ 1.21 1.0: 0.8: 0.61 0.4: 0.2; I on1 cn N ? Lo . . . , . . . ,I . J. .\ , . . .1 , . . . , 4.4 4.8 5.2 5.6 6.0 2 PFOS Page 384 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILLO04O.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\Chem\Hillary\HO10309.b\HILL0040.D Lab Smp Id: 1311-4106-S1 Inj Date : 09-MAR-2001 23:14 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 18 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable * 1 THPFOS 2 PFOS 427 5.036 5.009 (1.000) 1468017 254.000 499 5.260 5.233 (1.045) 452939 11.5341 11.5 3M Environmental Laboratory Page 385 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10309.b\HILLO04O+D D:\Chem\Hillary\HO10: 3,b\HILL0040,D 3.2: (D 0 LL 0 1 I- Page 2 `i2.7; 2.6; 2.5; 2.4: 2.3: 2.2; 2.1: 2.0; 1.9: 1.8: A 1.7; b 1+6{ `";1 1.5; > 1.4: 1.3; 1.2; 1,li 1.0: 0,sj 0.8{ 0.7: 0.6: 0.5: 0.4; 0.3: 0.2j 0.1; . . .IF.. ,I . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1.0 1.5 2.0 1 , . . . . , . . . . , . . . . , . . . .1, . . . . . . . . . . . . . . . . .I .I . . . . . . . . . . . . . . . . . . . . 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7+5 8,O 8.5 , . . .. ,.... 9.0 9.5 1 THPFOS 3.0{ 2.7: 2.4: 2.1: 1.8: : 1.51 1.2; > 0,sj 0.6: 0.35 4r9 tr-7 Lo . . . , . . . , 1. . . , . . 1 . ( . . ` I 1.0- 0.9; 0,s; 0.7r A 0.6; Lo 0 0.5: Ti " 0.4; > 0,3; 0.2; I on - m0 N. Lo Page 386 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILLO04l.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory Dits E00-1311 PFOS Adsorb/Desorb file : D:\Chem\Hillary\HO10309.b\HILL0041.D Lab Smp Id: 1311-4107-S1 Inj Date : 09-MAR-200123:25 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:lO anderson Quant Type: ISTD C a l Date : 09-MAR-200121:32 Cal File: HILL0031.D Als bottle: 19 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds .......................... * 1 THPFOS 2 PFOS QUANT SIG MASS _-_--- 427 499 RT EXP RT REL RT RESPONSE ==== ======== =====_== si======= 5.034 5.009 (1.000) 1055707 5.265 5.233 (1.046) 325164 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) (ug/rnL) ===E=== 254.000 11.5124 11.5 3M Environmental Laboratory Page 387 of 703 Data File: D:\Chem\Hillary\H414349.b\HILLOO4l.D BACK TO MAIN Page 2 2.1; F $2.4;. t1,9; 1.8; 1.71. 1+6; 1.5; 1.4; 1.3; ; 1,2; 1.11: 1 1,o; 0.9; 4.8; 0.7; 0.6; 4.5; 0.41 4,3; 0.21 0*1; . . .I.A,l. . . . , . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1 . . . .1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1.4 1.5 2+4 2.5 3.0 3.5 4.0 4.5 5.0 5 + 5 6.4 6.5 7 , O 7 + 5 8.4 8.5 9 + 0 , . . .I . - 9.5 H 1 THPFOS 2.21 2.0; 1.8; 1.6; gcI 1+4j i.2: g 1.4; V 0.8; >. 0.6; 0+4; 4.23: m f-? Lo II 1 2 PFOS 7,O; 6.0{ Ion u u 'u. m 5.4: 4,4: 4 : x 3.0f V Jl 2.0; 1.4; . , . . . , . .I ./ .L. . I, . . . , . . 44 M P&h~n&nf8*EabMoty Page 388 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0042.D Report Date: 28-Mar-200109:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\Chem\Hillary\HO10309.b\HILL0042 .D Lab Smp Id: 1311-4108-S1 In] Date : 09-MAR-2001 23:37 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 20 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds .......................... * 1 THPFOS 2 PFOS QUANT SIG MASS --___-- 427 499 RT EXP RT RBL RT RESPONSE ==== ======E= ======== = = = = = = a = 5.026 5.009 (1.000) 1050237 5.250 5.233 (1.045) 304848 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ug/mL) 254.000 10.7900 10.8 3M Environmental Laboratory Page 389 of 703 Data File: D:\Chem\Hillary\HO10309+b\HILL0042.D D:\Chem\Hillary\HO10309.b\HILL0042.D 2.2; 2.1; c,2.0;. t1.9; 1.8; 1.7; 1.6; 1.52 1,4; 1,3{ ; 1.2; i 1.1; ; 1.0; 0,s; 0.8; 0.7; 0.6: 0,s; 0.4; 0.3; 0.2; 0.1; ............................................ 0.5 1.0 1.5 2,O 2,5 3.0 3.5 4,O 4:5" Mir 1 THPFOS 2.21 2.0; 1.8; 1.6; :CI 1.41 L.2; rl L o ; X V 0.8: >- 0.6: 0.4; 0.23: Liu ? Lo . . . , . . . , I.. . . , . . 1. 6.01 5,Of ; 4.04 < 0$ 3,OC k qLo BACK TO MAIN Page 2 Page 390 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0043.D Report Date: 28-Mar-200109:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\H010309,b\HILL0043 .D Lab Smp Id: 1311-4108MS-S1 In] Date : 09-MAR-200123:48 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\HO10309.b\HOlO3l2.m Meth Date : 12-Mar-2001 11:lO anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 21 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds --_--- _ _ _ _ _ _ _ = =___-_--_-_==------= * 1 THPFOS 2 PFOS QUANT SIG MASS --_____ 42 7 499 , RT EXP RT RBL RT RESPONSB ==== ==------ ======== -------- 5.028 5.009 (1.000) 865040 5.259 5.233 (1.046) 4001498 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= 254.000 (ug/rnL) _--_----_--_ - _ 195.209 195 3M Environmental Laboratory Page 391 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10309.b\HILL0043.D Page 2 1 6.9: 6.6: 6.31 ; 6.0: `5.7: 5.41 5.11 4.8; 4.51 4.21 3.9: i 3.61 :i 3.3; 3.0{ 2 2.71 v) 2.4: a 2.11 1 I- 1 1.8: 1.5- 1.21 0.9: 0.6: 0.3: . . .I-. .I. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . t.l . . . . . . . . ( . . . . , . . . . , . . . . , . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1,O 1.5 2.0 2.5 3,O 3.5 4.0 4+5 5.0 5.5 6.0 6.5 7.0 7.5 8 , O 8.5 9.0 9.5 W 1 THPFOS i,6{ L4{ 1.21 yP-J. 1.0; 2 0 " 0.8; 0.6: 0,41 0.2: I. 1 2 PFOS ;L + 2.0; 1.0; .,. .. ,. .. ,..., .. .,. . 43h4E%d$q$r&nt&fabc%a?oty Page 392 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0044.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\Chem\Hillary\HO10309.b\HILL0044.D Lab Smp Id: 1311-4109-S1 In] Date : 09-MAR-200123:59 Operator : KLT Smp Info : Study Number E00-1311 Inst ID: hil1ary.i Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:lO anderson Quant Type: ISTD Cal Date : 09-MAR-200121:32 Als bottle: 22 Cal File: HILL0031.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -___ 427 499 RT BXP RT REL RT RBSPONSE ==ii= ======== ======== ======== 5.027 5.009 (1.000) 1073533 5.258 5.233 (1.046) 173898 CONCENTRATIONS ON-COLUMN (ng/mL) ======= 254.000 FINAL (ug/mL) ======= 5.57372 5.57 3M Environmental Laboratory Page 393 of 703 BACK TO MAIN c 2.1; *! 2,o: t: 1.9: 1.8; 1.7; 1.6: 1.5: 1.4; 1.3; 1.2: 1.1: 1.0; 0.9; 0.8: 0.7; 0.6; 0,51 0.4: 1 0.3; 0.2: 0.1: . . .I . N , . . . . , . . . . I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .I, . . . .U ......................... .,... .(....,....,.... 2.2:: 2.0; 1.8; 1+6: E.-. 1.4: 1.2: 2 1,o: V > 0.8; 0.6: 0.4; 0.21: - : 4.4 2 PFOS fi I n? - ( u -4.8 5.2 5.6 6.0 Page 394 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0045.D Report Date: 28-Mar-200109:OO BACK TO MAIN Page 1 3M Environmental Laboratory Dits file : E00-1311 PFOS Adsorb/Desorb D:\Chem\Hillary\HO10309.b\HILL0045.D Lab Smp Id: 1311-4110-S1 Inj Date : 10-MAR-20010O:ll Operator : KLT Smp Info : Study Number E00-1311 Inst ID: hil1ary.i Misc Info : Comment : Method D:\Chem\Hillary\HO10309.b\HO10312.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Als bottle: 23 Cal File: HILL0031.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS ---_-- 427 499 CONCENTRATIONS ON-COLUMN FINAL _ _ _ _ _ _ _ _ RT EXP RT REL RT RBSPONSB (ng/mL) (ug/m~) -_-_-_ _-__--__--_-__ ___-----_--_ _ _ - _ _=I==== ==== ==== 5.031 5.009 (1.000) 1045079 254.000 5.262 5.233 (1.046) 179135 5.95635 5.96 3M Environmental Laboratory Page 395 of 703 Data File: D:\Chem\Hillary\HO10309+b\HILL0045.D BACK TO MAIN Page 2 Y 1 THPFOS 2.2:' 2.0; 1+8r 1.6; 1.4: 1,2; 1.0; 0.8; 0.6; 0.41 0.2; 2 PFOS 3.6; 3.2; 2.8; QLn I> I I on Page 396 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILLO05O.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DAta file : D:\Chem\Hillary\HO10309.b\HILL0050.D Lab Smp Id: 1311-4111-S1 In) Date : 10-MAR-200101:08 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010309.b\H010312.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 24 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MMS __-_-- 427 499 RT BXP RT RBL RT RBSPONSB ==== ======== ======== ======== 5.027 5.009 (1.000) 1036444 5.258 5.233 (1.046) 165195 CONCENTRATIONS ON-COLUMN PIN- (ng/mL) ======= (ug/mL) ======= 254.000 5.46812 5.47 3M Environmental Laboratory Page 397 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10309+b\HILLO05O~D Page 2 D:\Chem\Hillary\HO10309.b\HILLO05O.I1 2.2; 2.1; 2.0; I ,? . . i1.F 1.8j 1.7; 1.64 1.5; 1.4; 1.3: ; 1.2; : 1.1; ? 1.0; 0.9; 0,8r 0.7; 0.6; 0.51 0,4< 0.3; 0.2j 0+1; . . .I. .N. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0,5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1. . . . . . . 0 5.5 6.0 6.5 7.0 7+5 8.0 8.5 9.0 9.5 w 1 THPFOS 2 PFOS 3.6; 3.31 3.0; 2.71 2.4; 2,11 1.8; 1.51 1.2: 0.9: 0.6; Page 398 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILLOO5l.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\H010309 .b\HILL0051.D Lab Smp Id: 1311-4111MS-S1 Inj Date : 10-MAR-2001 01:19 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\HO10309.b\HOlO3l2.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD Cal Date : 09-MAR-200121:32 Cal File: HILL0031.D Als bottle: 25 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS __--_ RT BXP RT RBL RT RBSPONSB s = = = = = = ========= ======== 5.028 5.009 (1.000) 869342 5.259 5.233 (1.046) 3920789 CONCBNTRATIONS ON-COLUMN FINAL (ng/mL) =====E= (ug/m~) ======= 254.000 190.081 190 3M Environmental Laboratory Page 399 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10309.b\HILLOO51.D Page 2 D:\Chem\Hillary\HO1030 b\HILL0051,D 6.61 6.3: 6.01 'i5.71 5.41 5,1{ 4,s: 4.51 4.21 3.91 ; 3.61 1 3,31 ' 3.0: 2.71 2,41 24 1.8: 1.51 1,2{ 0.9: 0.6: 0.31 . . .I-. ,I . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5:O Hin 1 THPFOS 1. .1. . . . . .I. . .I.I. . . . . . . . . . . . . . . . . . . . . . . . . . .I. . . -.1 . . . 5,5 6.0 6+5 7.0 7.5 8,O 8.5 9.0 9.5 1+81 1,61 1.41 1.2: CI b 1.0: "$ 0,s: >- 0.6: 0,4{ 0.2; rcu 3 LD I. 1 2 PFOS Page 400 of 703 Data File: D:\Chem\Hillary\HOlO309.b\HILLOO52.D Report Date: 28-Mar-2001 09:OO BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dsta file : D:\Chem\Hillary\HO10309.b\HILL0052.D Lab Smp Id: 1311-4112-S1 Inj Date : 10-MAR-2001 01:30 Operator : KLT Inst ID: hil1ary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\HO10309.b\HOlO3l2.m Meth Date : 12-Mar-200111:lO anderson Quant Type: ISTD C a l Date : 09-MAR-200121:32 Als bottle: 26 Cal File: HILL0031.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---- 427 499 RT EXP RT RBL RT RESPONSE ==== = = = = = e = = ==E===== ======== 5.034 5.009 (1.000) 1043258 5.265 5.233 (1.046) 170915 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ug/mL) ---_---_-___ 254.000 5.64850 5.65 3M Environmental Laboratory Page 401 of 703 Data File: D:\Chem\Hillary\HO10309.b\HILL0052.D 2.2; 2.11 2.0; BACK TO MAIN Page 2 0.4; 0.3; 0.2; 0.1; IN 2.2: 2.0; 1,s; 1.6; cI 1.4; !? 1.2; '0 ;1 1.0: W > 0.8i 0.6,' 0,4; 0.2: 2 PFOS *+ Lmo ? ln It 1 1 1 1 Page 402 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHOO29.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dkta file : D:\chem\Rush.i\R010314.b\RUSHOO29 .D Lab Smp Id: Inj Date : 14-MAR-2001 2 3 : 5 7 Operator : KLT Inst ID: Rush.i Smp Info : TN-A 4802 MeOH Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 92 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable ........................ Compounds ---------------_--------I= * 1 THPFOS 3M Environmental Laboratory Page 403 of 703 BACK TO MAIN Data File: D:\chem\Rush+i\R010314,b\RUSH0029~D Page 2 D:\chem\Rush.i\R010314.b\RUSH0029.D 6.41 6.2; 6.0; 5.8; ;5+6; t5.4; 5.2; 5,O; 4.81 4.6; 4.4; 4,2; 4.0; 3.8; E 3.6; 5 3.41 2 3.2; >- 3.0; 2,s; 2.6; 2.4; 2.2: 2.04 1.8; 1.6; 1.4; i 1+2; 1.0; 0.8; 0.61 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i i 2 i 6 t, i Min M 1 THPFOS (Undetected) I on 900- 850; 8001: 750: 700: 650: 600; >- 550; 500; 450: 4001 350,) 300:. .. ,. .. ,.. .,.. ., .,', 4+8 5.2 5.6 6.0 6.4 Min 2 PFOS .... .... .... .... ,,., i io il i2 Page 404 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHO03O.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daka file : D:\chem\Rush.i\R010314.b\RUSHO03O.D Lab Smp Id: Inj Date : 15-MAR-20010O:ll Operator : KLT Inst ID: Rush.i Smp Info : TN-A 4802 MeOH Misc Info : Comment Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-2001 23:28 Cal File: RUSH0027.D A l s bottle: 92 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds QUANT SIG MASS CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 3M Environmental Laboratory Page 405 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010314.b\RUSHOO30.D 6.4: 6.2; 6-0; 5,8; ;% 5.6; 15.4; 5.2: 5.0: 4.8; 4.6; 4.4:' 4.2; 4.4:: 3.8; ; 3.6; 3,4; 5 3.21 . 3.0: 2,s; 2.6; 2.4; 2.2; 2,or 1.81 1.6; i+4; 1.2; D:\chern\Rush.i\R414314.b\RUSH443O.D Page 2 0.6: 1 2 3 4 n 1 THPFOS (Undetected) Ion 680; 644L 600; 564; 520; >. 480; 4442 E 400; 360 320; . . . , . . . , . . . , . . . , . . . , 4.8 5.2 5.6 6.0 6+4 Hin 2 PFOS .. .... .... .... .... .... .... .... 5 t, i i i io il i2 Hin 4,8+ Lo 4.4; 4.4: 3+6{ 3.2< 4 2.8; Y X 2.4; >- 2.01 1,6: 1.2: 4+8; .,..., ... ,. .. ,..., .. . 4+4M,!?&it&$rhent& tabbrdtory Page 406 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHOO3l.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\chem\Rush.i\R010314.b\RUSHO03l.D Lab Smp Id: In] Date : 15-MAR-2001 00:26 Operator : KLT Smp Info : 1311-4121-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-2001 23:28 Als bottle: 14 Cal File: RUSH0027 . D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ==== 427 499 RT BXP RT RBL RT RESPONSE ==== ===== ===I === == = ==== ===== 5.467 5.462 (1.000) 1425324 Compound Not Detected. CONCENTRATIONS ON-COLUMN (ng/mL) ======= 254.000 FINAL ( ug/L) ======= 3M Environmental Laboratory Page 407 of 703 Data File: D:\chem\Rush,i\R010314~b\RUSHOO31.D 3.81 3.61 ,: 3.41. '3,21 3.01 2.81 2.61 2.41 2.2: 2.0; 0 rxl 1.81 Y 1.6; 1,41 1.21 1.0; 0,81 0.6; D:\chem\Ri BACK TO MAIN Page 2 1 1 H 1 THPFOS - J. . . . . I.I . . . . . . . . . . . . . . . . . . . . . I. -.1 1 tu, i 1 6 1 io il 12 Ill,, 3.3: 3,0{ 2.7: rr 2,4{ 7 2.1; $; L a ; 5 1.5: > 1.21 0.91 0.6: 0.31 Is) I Jx 1 2 PFOS 5,5r 5,O; 4.5; 4.0; CI 3,5< &m 3,Oj "rXl 2.5; >. 2.0; 1.5, 1.0; (Undetected) Ion Page 408 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0032.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daka file : D:\chem\Rush.i\R010314.b\RUSH0032.D Lab Smp Id: In] Date : 15-MAR-200100:40 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4122-S1 Misc Info : Comment : Method D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 15 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS --____- 427 499 CONCENTRATIONS ON-COLUMN FINAL RT BXP RT REL RT RESPONSE (ng/mL) ( ug/L) -_____--_----_---_--------_---_-_--_= _ -=I== ==== ==== = = ======= 5.466 5.462 (1.000) 1078944 254.000 Compound N o t Detected. 3M Environmental Laboratory Page 409 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010314.b\RUSH0032~D Page 2 2.9: 2.8; 2.7; 2.6; 2.5; '2.4; 2.3i 2.2: 2.1; 2.0; 1.9; 1.8; 1.7; 1.6; I 1.5; 1.4; 1.3; 1.2; 1.1; 1.0; 0.9; 0+8; 0.7; 0.6; 0.54 0.4; 0.3; 0.2: 0.1; . 1.. 4. . . . . . . . . . 1 1 . . .. D:\chem\Rush,i\R010314.b\RUSH0032.D Lrn 0 LL r 1 I- . . . . . . y.\I. . . . . J.I . . . . . . . . . . . .. . . . .. . , . l.J - , 2.7; 2.4: 2.11 CI 1.8: l,S{ r"xl 1.21 >- 0.9; 0.61 0,3{ t uu 4 Lo I .\ 1 I on 5.2; 4,8+ Page 410 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0033.D Report Date: 20-Mar-20011 5 : 4 7 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dkta file : D:\chem\Rush.i\R010314.b\RUSH0033 .D Lab Smp Id: Inj Date : 15-MAR-20010 0 : 5 4 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4123-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 16 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS - _- ____ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) = _ = = ======= ====I === ==5= == = == =I====* =5===== 5.466 5.462 (1.000) 1090803 254.000 Compound Not Detected. 3M Environmental Laboratoty Page 411 of 703 BACK TO MAIN Page 2 D:\chern\Rush,i\R010314+b\RUSHOO33.D 2.9; 2.8: 2.7; 2.6; i2.5: 2.4: 2.3: 2.2: 2.1; 24 1.9: 1.8: 1.7: &,-. 1.6: Lo 1.5; "1;: 1.4: > 1.3: 1.2; 1.1; 1.0: 0.9; 0.8: 0.7: 0,65 0.5: 0.4: 0.3; 0.2: 0.1: . l.A.l . . . . . . . . . . . . . . . . . . 1 5 5 4 6 1. . . . . . . . . . . . . . . . -. . . . . . . . . . . I. . L t, 1 6 Hin i io il i2 Y 1 THPFOS 2.7: 2.4: 2.11 ,-. 1,8{ Ls) 6 1.51 d V 1.21 > 0.9: 0.6: 0.3: 4 L a Ls) l,L 1 2 PFOS (Undetected) I I on ,-. m 0 rl " > Page 412 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHO06O.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dkta file : D:\chem\Rush.i\R010314.b\RUSH0060 .D Lab Smp Id: Inj Date : 15-MAR-200107:22 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4137-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 35 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SI0 MASS --_____ 427 499 RT BXP RT RBL RT RESPONSB ==== ======== e = = = = = = ========= 5.477 5.462 (1.000) 1099389 5.687 5.679 (1.038) 757619 CONCBNTRATIONS ON-COLUMN FINAL (ng/mL) ( ug/L) ii====== ======= 254.000 22.8306 22.8 3 M Environmental Laboratory Page 413 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010314.b\RUSH0060.D Page 2 D:\chem\Rush,i\R010314.b\RUSHO06O.D cn 0 2.9; aLL 2.8; c 1 2.7; 2.6: si2.5: 2,41 2.3: 24 2.1; 2.0: 1.9; 1.8: 1.7; .-. 1.6; 6D 1.5; dx 1.4: v > 1.3; 1+2; 1.1; 1.0: 0.9; 0.8; 0.7; 0.6; 0,s: 0.4: 0.3; 0.2; 0.1: . I. d. . . . . . 1_1 . . . . . . . . . . .. 1 . . . . . . . . . . . . . . . . ... . . . . . .. . . . . . . 111 16 t, 1 1 i io il i2 Min 1 THPFOS 2.71 2,4{ 24 fn 1.8; 1.5: 2d 1.2: > 0.9; 0.6; 0.31 b -b 0, D 1 1. 1 2 PFOS Page 414 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHOO6l.D Report Date: 20-Mar-200115:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dkta file : D:\chem\Rush.i\R010314.b\RUSHO06l.D Lab Smp Id: Inj Date : 15-MAR-200107:36 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4138-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-200115:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 36 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all I sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd,Variable Local Compound Variable 3M Environmental Laboratory Page 415 of 703 BACK TO MAIN 2+9< 2.8; 2.7; 2.6; D:\chem\Rush,i\R010314+b\RUSH0061~D (D 0 nL.L 1 t ,: 2.5; `2,4: 2,3< 2.2; 2.1: 2.0; 1.9: 1,s; 1.7; CI 1+6: 1,5{ 3 1.4; 5 1.3; i.2: 1,lj 1.0: 0.9; 0,s; 0.7; 0.6; 0.5; 0.4: 0.3: 0,2; 0.1, rs . I. d. . . . . . . . . . i 1 . . . . . . . . . I. . JI. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 6 iM, in j 6 1 io il 12 H 1 THPFOS 2 PFOS 1,s; 1.6; 1,4{ 1.2: 1.0; 0.8{ 0.6; Y Ion a co Lo Page 416 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHOO62.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\chem\Rush.i\R010314.b\RUSH0062.D Lab Smp Id: Inj Date : 15-MAR-2001 07:50 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4138MS-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 37 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _- _- _ _ 427 499 RT EXP RT REL RT RESPONSE ==== ======== =====E== e = = = = = = = 5.470 5.462 (1.000) 947454 5.687 5.679 (1.040) 4939810 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= ( ug/L) =-----_ 254.000 228.058 228 3M Environmental Laboratory Page 417 of 703 Data File: D:\chem\Rush,i\R010314.b\RUSH0062~D BACK TO MAIN Page 2 1 THPFOS 0 2.4; b 4 2.2: Ki 2.0: 1.8: 1.6; 1.4; 1.2; 5 1.0; > 0.8; 0.6: 0+4j 0.23: . . . , . . . ,I . .. . , . . . ,1 . . . 2 PFOS Page 418 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0063.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\chem\Rush.i\R010314.b\RUSH0063 .D Lab Smp Id: Inj Date : 15-MAR-20010 8 : 0 5 Operator : KLT Smp Info : 1311-4139-S1 Inst ID: Rush,i Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-200115:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Als bottle: 3 8 Cal File: RUSH0027.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -__- 427 499 RT EXP RT REL RT RESPONSE --_--- --_-_-----_- _-_-_----------- -------- 5.469 5.462 (1.000) 1086262 5.687 5.679 (1.040) 684895 CONCENTRATIONS ON-COLUMN (ng/mL) ------___ FINAL ( ug/L) _______ 254.000 20.6690 20.7 3M Environmental Laboratory Page 419 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010314.b\RUSH0063.D Page 2 D:\chem\Rush,i\R010314+b\RUSH0063.D 2.9; 2.8; 2.7: 2.6; i2.5: 2.4; 2.3: 2.2; 2.1; 2.0; 1.9; 1+8: 1.7; I& 1+5; 1.4; ' 1.3: - 1.2: 1.1: 1.0; 0.9; 0.8: :L 0.7: 0.6: 0.5; 0.4: 0.3; 0.2; 0.1: .... .. .. . . .. .. . . .... . . 1 1 1 1 6 . .... .... .... .... .... .... .... tM, in 1 1 1 io il i2 i3 w 1 THPFOS 2.41 4 I on 0 I.Lo ,6 6.0 6+4 1.61 4 1.41 1.21 1.0; 0.8: 0.6: Page 420 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0064.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\chem\Rush.i\R010314.b\RUSH0064 . D Lab Smp Id: Inj Date : 15-MAR-2001 08:19 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4140-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 39 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 421 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0064.D 2.9j 2.8; 2,7{ 2+6+ i2.5: 2.4: 2+3j 2.2: 2.1; 2.0: 1.9; D:\chem\Rush.i\R010314+b\RUSH0064.D (0 0 LL E[L BACK TO MAIN Page 2 2.4: 2.1: 1.81 gU J 1.51 "rxl 1,21 > 0.9i 0.61 0,31 2 PFOS 1.61 1,4{ 1.2{ LD 11. I I on 0.2: JI Page 422 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0065.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DAta file : D:\chem\Rush.i\R010314.b\RUSH0065.D Lab Smp Id: Inj Date : 15-MAR-2001 08:34 Operator : KLT Smp Info : 1311-4141-S1 Inst ID: Rush.i Misc Info : Comment : Met hod D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-2001 23:28 Cal File: RUSH0027.D Als bottle: 40 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS _---__-_ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT BXP RT REL RT RESPONSE (ng/mL) ----_ -_-__--__--__-_-_-__--_--_-_- __-_____-___=_====== ( ug/L) ======= 5.481 5.462 (1.000) 1075484 254.000 5.691 5.679 (1.038) 687097 20.9767 21.0 3M Environmental Laboratory Page 423 of 703 BACK TO MAIN Data File: D:\chem\Rush.i\R010314~b\RUSH0065.D D:\chem\Rc 2.9: 2.8: 2.7; 2.6: qi2.5: 2.4: 2.3; 2.2: 24 2.0: 1.9, 1.8: 1+7; cI 1.6: 5 1.5; 1.4; " 1.3: > 1.2: 1.1: 1.0: 0,Yi 0.8i 0.7: 0.6: 0.5; 0,4: 0,3! 0.2: 0,lj . l.h l. . . . . . . . . . . . . . . . . . . 1. 1 5 1 16 1 THPFOS *rl 0) 2.71 Lo 2.41 2.11 cI 1 3 1 Lbo 1.5: "rxl 1.21 >. 0.91 0.61 0,31 . . . , . . . ,I . .I. , . . .1 , . . . ' Page 2 ! . . . . . . . . . . . . . . . . . . . . . . . . . . L.J-. t, 1 6 1 io il 12 Min 2 PFOS I on 1.6{ Page 424 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0066.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory i E00-1311 PFOS Adsorb/Desorb Ddta file : D:\chem\Rush.i\R010314.b\RUSH0066.D Lab Smp Id: Inj Date : 15-MAR-200108:48 Operator : KLT Smp Info : 1311-4141MS-S1 Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mas-200115:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Als bottle: 41 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Processing Host: W19401 C a l File: RUSH0027.D Compound Sublist: all.sub Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ==== 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) _--__-----___---_--__--__--------_- ----___-______======= ( u~/L) =------ 5.473 5.462 (1.000) 915669 254.000 5 . 6 8 4 5 . 6 7 9 (1.038) 4776931 228.225 22 8 3M Environmental Laboratory Page 425 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0066.D BACK TO MAIN Page 2 8.7; B 8,4; i8*1; 7.8; 7,5: 7.2; 6.9; 6.61 6.3; 6.0; 5.7; 5.41 6 5.11 4.81 "rxl 4.5: > 4.2: 3,s: $ 3.61 (D 3.3: 0 LL 3.01 2.7: 2.41 2.1: 1.81 1.5: 1.21 0.9: 0.6: 0,3{ . I, I . . 1. . . . 1. . . . 1. . . . 1. . . . ii . I. . '. 1 . 2. . . . 1. . . . A . . . . . i . . . . io . . . . il . . . . i2 . It , , H 1 THPFOS 4.8 5.2 5,6 6.0 6.4 Min 2 PFOS Page 426 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSHOO67.D Report Date: 20-Mar-200115:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\chem\Rush.i\R010314.b\RUSH0067.D Lab Smp Id: Inj Date : 15-MAR-2001 0 9 : 0 2 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4142-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-2001 23:28 Cal File: RUSH0027.D Als bottle: 42 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds . . . . . . . . . . . . . . . . . . . . . . . . . . * 1 THPFOS 2 PFOS QUANT SIG MASS ==== 42 7 499 CONCENTRATIONS ON-COLUMN FINAL RT U P RT REL RT RESPONSE (ng/mL) __--_-_-_-_-__________--_-____-______-___-__ ___======= 5.478 5.462 (1.000) 1079679 254.000 ( ug/L) -- ----_-_-_-s 5.695 5.679 (1.040) 673507 20.4226 20.4 3M Environmental Laboratory Page 427 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010314.b\RUSH0067.D Page 2 D:\chem\RL +i\R010314.b\RUSH0067,D 2.9: '07 2.8; 0 IA a 2.7; 1 I- 2.6; i.2.5: t 2,4{ 2.3: 2.2; 2.1; 2.0; 1.9; 1.8; 1.7; P. 1+6{ '7 1+5: 4 1.4; 1+3; 1.2; 1.1; 1,oj 0.9; 0.8: 0.7; 0.6; :I 0.5; 0.4; 0.3: 0.2; 0.1; .... .... .... .... .... .. 1 ;1 4 6 . . . . l. l . . . . . . . . . . . . . . . . . . . . . L. L. dM i I 1 6 1 10 il 12 11&11 M 1 THPFOS 2,7{ 2.41 2.11 1,sr 1.5; 1.21 0.9i 0.61 0,3{ . .. t Ll-. Lo I ,\ 1 2 PFOS Page 428 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0068.D Report Date: 20-Mar-2001 15:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DJta file : D:\chem\Rush.i\R010314.b\RUSHOO68.D Lab Smp Id: In] Date : 15-MAR-2001 09:17 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4143-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-20011 5 : 0 2 terrell Quant Type: ISTD Cal Date : 14-MAR-2001 23:28 Cal File: RUSH0027.D Als bottle: 43 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --_____ 42 7 499 RT EXP RT RBL RT RESPONSE -_-----____----_------_ -_-_------------ 5.470 5.462 (1.000) 1108514 5.687 5.679 (1.040) 716747 CONCBNTRATIONS ON-COLUMN FINAL (ng/mL) ( ug/L) _- _-______======= 254.000 21.2606 21.3 3M Environmental Laboratory Page 429 of 703 BACK TO MAIN Data File: D:\chem\Rush.i\R010314~b\RUSH0068.D Page 2 D:\chem\Rush.i\R010314~b\RUSH0068.D 3.0; 2.9; 2.8; 'v) 0 LL LL 1 I- 2.7; .; 2+6; t 2.5; 2.4: 2.3: 2.2; 2.1; 2.0; 1,s: 1,8: 1+7; 1.6; > 1.5; 1.4; - 1*3; 1.2: 1.1: 1.0: 0,s: 0.8; 0.7; 0.6j 0.5: 0.4: 0.3; 0,2; 0.1; . 1. 4. . . . . . . . . . . . . . . . . . . . 111 16 i.L . . . . . . . . . . . . . . . . . . . . . . . . . . . . i, i .A i io il i2 Min 1 THPFOS I on 3+0: 2.71 2.4; 2.11 Fn 1.8; 1.51 ,rxl 1,2; >. 0.9: 0.61 0.3; . . . , . . . , . . . , . . . ,1 . . . , 4.8 5.2 5.6 6.0 6.4 Min 2 PFOS Page 430 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0072.D Report Date: 20-Mar-2001 15:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D$ta file : D:\chem\Rush.i\R010314.b\RUSH0072.D Lab Smp Id: Inj Date : 15-MAR-2001 10:14 Operator : KLT Smp Info : TN-A 4802 MeOH Inst ID: Rush.i Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-200115:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Als bottle: 93 Cal File: RUSH0027 D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 431 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0072.D 9.3: 9.Of 8.71 8.4; 8.11 7,81 7.5: 7.2{ 6.91 6.61 6.31 6.0; 5*7{ , ' 5.41 5.i: 4.81 4.5: 4,2{ 3*9f 3.61 3,3: 3.01 2.7: D: \chem\Rush \R010314,b\RUSH0072,D y 1 THPFOS (Undetected) 680{ 640; 600r Ion n ...,. .. ,..., .. .,... 4,s 5.2 5,6 6.0 6.4 Min 2 PFOS BACK TO MAIN Page 2 Page 432 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0073.D Report Date: 20-Mar-200115:49 BACK TO MAIN Page 1 3M Environmental Laboratory Dits file : E00-1311 PFOS Adsorb/Desorb D:\chem\Rush.i\R010314.b\RUSH0073 .D Lab Smp Id: Inj Date : 15-MAR-200110:29 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4144-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D A l s bottle: 44 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds QUANT SIG MASS CONCENTRATIONS ON-COLUMN RT EXP RT RBL RT RESPONSB (ng/mL) FINAL ( ug/L) 3M Environmental Laboratory Page 433 of 703 BACK TO MAIN Data File: D:\chem\Rush,i\R010314+b\RUSH0073+D Page 2 D:\chem\Rush.i\R010314.b\RUSH0073.D 2.9: 2.8; 2.7; 2.6; `i2.5; 2.4; 2.3; 2.2: 2.1: 2.0; 1.9; 1+8: 1,7+ , ' 1.6; 1.5; 1.4; -` 1.3; 1.2: i.1; LO! 0.9: 0.8; 0,7; 0.6; 0.5; 0.4; 0,3; 0.2: 0.1: . .. . . ... ,.. . . .. . .. .. . 1 h 2 4 6 1 k . . . . 1. . . . A . . . . 6 . . . . i o . . . . il . . . . i2. . . , Hin M 1 THPFOS 2.71 2.41 2.11 CI 1.8; Lo b 1.5; rl 1.2: U > 0.9: 0.6: 0.31 LCO b, Lo It` I 2 PFOS 1.8: 1.61 1.4; 1.21 ;; 1.0; 0 rl 0,8{ "x . >- 0.6; 0.4: 0.2; b 0 Lo 1 \ Page 434 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0074.D Report Date: 20-Mar-2001 15:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DJta file : D:\chem\Rush.i\R010314.b\RUSHOO74.D Lab Smp Id: In] Date : 15-MAR-2001 10:43 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4144MS-S1 Misc Info : Comment : Method : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-2001 15:02 terrell Quant Type: ISTD Cal Date : 14-MAR-2001 23:28 Cal File: RUSH0027.D Als bottle: 45 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --_-_ 427 499 RT EXP RT REL RT ==== ======== =====E== 5.462 5.462 (1.000) 5.686 5.679 (1.041) RESPONSE ====e=== 895662 4609795 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ( ug/L) ==I==== 254.000 224.468 224 3M Environmental Laboratory Page 435 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0074+D \R010314,b\RUSH0074.D BACK TO MAIN Page 2 2,7{ 2,41 2.1; 1,8{ 1.5; 1,2{ 0.9; 0,6{ 0,3{ . I.. .I . .. .. 1 THPFOS 2.2; 3 Lo 2.0; 1+8; 1+6; 1.4; s?! 1.2; x 1.0: v >- 0.8; 0.6; 0.4; 0.2:: . . . , . . . ,I . I. .C, . . I . , . . ` 1 2 PFOS c 1 1 ... 1 . . . . . . . . . . . . . . . . . . . . . . . . . . 1. 1 . iM, i n 1 1 1 io il 12 I, Page 436 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0075.D Report Date: 20-Mar-200115:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Rush.i\R010314.b\RUSH0075.D Lab Smp Id: Inj Date : 15-MAR-2001 10:57 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4145-S1 Misc Info : Comment : Method D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-20011 5 : 0 2 terrell Quant Type: ISTD Cal D a t e : 14-MAR-200123:28 Cal F i l e : RUSH0027 D Als bottle: 4 6 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds . . . . . . . . . . . . . . . . . . . . . . . . . . * 1 THPFOS 2 PFOS QUANT SIG MASS ==== 427 499 RT BXP RT RBL RT RBSPONSB ==== ======== ======== ======== 5 . 4 6 7 5 . 4 6 2 (1.000) 1070260 5.684 5.679 (1.040) 640428 CONCENTRATIONS ON-COLUMN (ng/mL) FINAL ( ug/L) ======= 254.000 19.4900 19.5 3M Environmental Laboratory Page 437 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0075.D D:\chem\Rush.i\R010314.b\RUSH0075.D 2.9: 2.8; 2.7; 2.6: : 2.5: (2.4; 2.3-j 2.2; 2.1: 2.0: 1.9, 1.8; 1.7: 1,6{ 1,s; 2 1.4; 1.3: + 1.2: 1.1; LO{ 0.9; 0.8: 0.7; 0.6; 0.5; 0.4; 0,3: 0,2; 0.1; . 1.a.1. . 1. . . . 1 . . . . 2 . . . . 1. . . . 6 . H 1 THPFOS 2,4{ 2.1{ 1.81 1.5; 1.2- 0.9r 0.6: 0,3{ 2 PFOS 11% 1 BACK TO MAIN Page 2 Page 438 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0076,D Report Date: 20-Mar-2001 15:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\chem\Rush.i\R010314.b\RUSH0076.D Lab Smp Id: Inj Date : 15-MAR-200111:12 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4146-S1 Misc Info : Comment : Met hod : D:\chem\Rush.i\R010314.b\R010314t.m Meth Date : 20-Mar-200115:02 terrell Quant Type: ISTD Cal Date : 14-MAR-200123:28 Cal File: RUSH0027.D Als bottle: 47 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds ........................... * 1 THPFOS 2 PFOS QUANT SIG MASS ---- 427 499 RT BXP RT RBL RT RBSPONSB -_--__--__ _-_-_-_-_-___ --_----_-__-_--_-===E==== 5.459 5.462 (1.000) 1090781 5.676 5.679 (1.040) 644391 CONCENTRATIONS ON-COLUMN (ng/mL) ======= FINAL ( ug/L) ======= 254.000 19.2107 19.2 3M Environmental Laboratory Page 439 of 703 BACK TO MAIN Data File: D:\chem\Rush.i\R010314.b\RUSH0076.D Page 2 D:\chem\Rush,i\R010314+b\RUSH0076.D I 2.9; 2.8; 2.7; 2,6: 'i2+5f 2.4; 2.3: 2.2; 2.1; 2.0; 1.9: 1.8; 1.7; \ 1.6: 1.5; 2 1.4; ' 1.3; 1.2: 1.1; 1.0; 0.9: 0,8i 0.7; 0,6+ 0.5; 0.4; 0.3; 0.2; 0.i: . I. d. . .. .. .. . . . . . . .. ., . I , 1 .i 1 i 6 . . . . . I.I ._ . . .... .... .... .... IL .... d i 6 4 io il i2 Min M 1 THPFOS 2.7; 2.4; 2.11 1.8: 6m l.5{ rl ux 1.2: d. L L o Lo 2 PFOS Ion 1.6; 0.2; . , . . . , . .I . f, .L. . I, . . . 4'??Ml!&i~f/hent& Pab8htory Page 440 of 703 Data File: D:\Chem\Hillary\HOlO404.b\HILLO03l.D Report Date: 09-Apr-200113:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DAta file : D:\Chem\Hillary\HO10404.b\HILLO03l.D Lab Smp Id: 1311-4151-S1 Inj Date : 04-APR-2001 21:52 Operator : CMC Inst ID: hi1lary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc Info : Comment : Method D:\Chem\Hillary\HO10404.b\HO10404.m Meth Date : 09-Apr-2001 13 :02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 41 Dil Factor: 1.00000 Intesrator: Falcon Compound Sublist: all.sub Targgt Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ----_ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT BXP RT DLT RT RBSPONSB (ng/mL) -_--__----_-_-----____-_------ --_-_-________ _=s===== (ng/mL) ======= 5.108 5.092 0.016 1562301 254.000 254 compound Not Detected. 3M Environmental Laboratory Page 441 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO31~D I D:\Chem\Hillary\HO10404.b\HILLOO31.D BACK TO MAIN Page 2 1 THPFOS I 2.74 2,4{ n 2.11 < 7 0 1.8; 1.5: V > 1.21 0.91 0.6: 0.31 I. 2 PFOS (Undetected) ~ I on Page 442 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0032.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daka file : D:\Chem\Hillary\H010404.b\HILLOO32 . D Lab Smp Id: 1311-4152-S1 Inj Date : 04-APR-200122:07 Operator : CMC Inst ID: hil1ary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026 .D Als bottle: 42 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds .......................... 1 THPFOS 2 PFOS QUANT SIG MASS _------_ 427 499 CONCENTRATIONS ON-COLUMN FINAL _ _ _ _ _ _ _ _ _ _ _ _RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) -__-__---_----_-_--_--_--_--_--_--_- _--=ii=====E====== 5.111 5.092 0.019 1575594 254.000 254 Compound Not Detected. 3M Environmental Laboratory Page 443 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO32.D 3.41 3.21 i3,Oi 2.81 2.61 2.41 2.2; -. 2.01 1.8; '5 : 1.6: 1.41 131 1.0; 0.81 0.61 D:\Chew\Hillary\HO10404.b\HILLOO32~D .IJ.Q. I. .I_lJ-.-. . . . . . . . . . . . . . . . 11 1 16 Min Ion rl 1 rl 3.3: i Lto 3.01 - 2.7{ 2.4: m 2,1{ & 1.81 4x 1.5: W 1.21 >- 0.9; 0.61 0,3{ - . . . . . . . . , , 1 . 1 I...I..'I 4.4 4.8 5.2 5.6 6.0 Min 2 PFOS (Undetected) I on 3.3: 3,O; BACK TO MAIN Page 2 Page 444 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0033.D Report Date: 09-Apr-200113:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&a file : D:\Chem\Hillary\HO10404.b\HILL0033.D Lab Smp Id: 1311-4153-S1 Inj Date : 04-APR-200122:21 Operator : CMC Inst ID: hil1ary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc Info : Comment : Method D:\Chem\Hillary\HO10404.b\HO10404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Als bottle: 43 Cal File: HILL0026.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --__ 427 499 RT BXP RT DLT RT RESPONSE ==== ======== ======== ======== 5.106 5.092 0.014 . 1560062 Compound Not Detected. CONCENTRATIONS ON-COLUMN (ng/mL) FINAL (ng/mL) ===E=== =_===== 254.000 254 3M Environmental Laboratory Page 445 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0033.D 3.4: 3.21 ,; 3.0- i: 2,81 2.61 2.41 2.2: 2.0: 1.81 1.6: 1.4: 1.21 1.0: 0.81 0.6: 0.41 0.21 . . . . i ' . . . 1. . . . 1 1 THPFOS D:\Chem\Hillary\HO10404.b\HILL0033.D 1 6 Hin BACK TO MAIN Page 2 2 PFOS (Undetected) I I on 1 mCI 0 d " > Page 446 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0034.D Report Date: 09-Apr-200113:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\H010404.b\HILL0034.D Lab Smp Id: 1311-4153MS-S1 Inj Date : 04-APR-2001 22:36 Operator : CMC Inst ID: hil1ary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Cal File: HILL0026.D Als bottle: 44 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -_- _ _ _ E 42 7 499 RT EXP RT DLT RT RESPONSE ==== ======== ======== s = = = = = = = 5.105 5.092 0.013 1537278 5.315 5.309 0.006 3170996 CONCENTRATIONS ON-COLUMN FINAL (ng/rnL) ======= (ng/mL) ======= 254.000 2 54 168.305 168 3M Environmental Laboratory Page 447 of 703 BACK TO MAIN Data File: D:\Chern\Hillary\HO10404.b\HILL0034.D Page 2 D:\Chem\Hillary\HO10404.b\HILL0034,D 7.2: 6.51 6.61 6.3: 'i6.01 5.7; 5.41 5.1{ 4.81 4,5{ 4,2{ , 3,531 ; 3.61 3.31 - 3.01 2.71 2.41 2.11 1.81 1.51 1.21 0.9r 0.6; 0.3; . . . . 1. . . . 1. . . . 1.1 . . . 1. . . . t . [.I . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 5 1 b io il i2 1 THPFOS Ion 2 PFOS Page 448 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0035.D Report Date: 09-Apr-200113:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daka file : D:\Chem\Hillary\H010404.b\HILL0035.D Lab Smp Id: 1311-4154-S1 Inj Date : 04-APR-200122:50 Operator : CMC Inst ID: hil1ary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 45 Dil Factor: 1,00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -_-- 427 499 RT EXP RT DLT RT RESPONSE ==== ======== ======== ====E=== 5.098 5.092 0.006 1599896 Compound Not Detected. CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ng/mL) ======= 254.000 254 3M Environmental Laboratory Page 449 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO35.D I D:\Chem\Hillary\HO10404.b\HILL0035,I) BACK TO MAIN Page 2 1 THPFOS I 3.6: 3.31 3,Oi 2.71 2.4: ;; 2.1: 6 1.81 dx 1,5{ V ~ i*2: 0,Sf 0.6: 0.3; Cfn 9 Lo If 1 2 PFOS (Undetected) I on Page 450 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0036.D Report Date: 09-Apr-200113:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\H010404.b\HILL0036.D Lab Smp Id: 1311-4155-S1 In] Date : 04-APR-200123:04 Operator : CMC Inst ID: hil1ary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc I n f o : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Cal File: HILL0026.D Als bottle: 46 Dil Factor: 1,00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 451 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10404.b\HILLOO36.D Page 2 D:\Chem\Hillary\HO10404.b\HILLOO36.D 3.61 3.41 ,: 3.2; t' 3.0; 2.81 2.61 2.41 2.2; 7n 2.01 . 3 1.81 # x . 1.61 1.4- 1.2; 1.0; 0,81 0.6: 0.4: 0.2; . . . . . . . . . . . . . . . . . . . . . . .1 . . . . . . . . . . . , . . . . . . . . , , . . , . , . . 1 1116 tM, in 1 6 1 1'0 il 1'2 1 THPFOS 2 PFOS 3.6: 3.3r (Undetected) I on Page 452 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0037.D Report Date: 09-Apr-200113:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\HO10404.b\HILL0037.D Lab Smp Id: 1311-4156-S1 Inj Date : 04-APR-200123:19 Operator : CMC Inst ID: hil1ary.i Smp Info : Omg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 47 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --- ---E 427 499 CONCENTRATIONS ON-COLUMN PINAL RT ---- EXP RT DLT RT _----_--_----_-________=-== = RESPONSE -----_-_-____-_ _-(_ng_/m_-L_)___-_-_(-_-n-_g-_-/=_m_L) 5.093 5.092 0.001 1644662 254.000 254 Compound Not Detected. 3M Environmental Laboratory Page 453 of 703 Data File: D:\Chem\Hillsry\HO10404~b\HILL0037.D 3+83.6: 3.41 *;3,21 3,O; 2.81 2.61 2.4; 2,21 ; 2.01 2 1.8; * 1.61 1.41 1.21 1.0; 0.81 0,61 0.4: 0.21 D:\Chem\Hillary\HO10404.b\HILL0037~D n 1 1. I 1 THPFOS Ion 3.6: 3,3: 3.0< 2.71 4 2,4; c; 2.1: 1.8{ 5 1.5: > 1.21 0.94 0.6: 0,3{ . . . , . . . , . 1. . , . . . , . . .1 I 4.4 4.8 5.2 5.6 6.0 Hin 2 PFOS 5.2; 4.8; 4.4; 4.0: (Undetected) Ion BACK TO MAIN Page 2 1.2; 0.8; Page 454 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0039.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D&ta file : D:\Chem\Hillary\HO10404.b\HILL0039.D Lab Smp Id: 1311-4157-S1 Inj Date : 04-APR-200123:48 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Cal File: HILL0026.D A l s bottle: 49 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --_-_ 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSE (ng/mL) ==== ======== === === ===== == i= = == = = = = E (ng/mL) ======= 5.098 5.092 0.006 1587389 254.000 254 Compound Not Detected. I 3M Environmental Laboratory Page 455 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO39~D 3.64 3.4; ,3,2; i: 3*0: 2.8; 2.6; 2.4; 2.2: , 2.0; - 1,s: I 1+6: 1.4; 1.2; 1.0; 0.8; 0,6; 0,4; 0,2; . ... . . .. ... . D:\Chem\Hillary\HO10404.b\HILL0039~D n . . h- . . . . . . . 1 THPFOS BACK TO MAIN Page 2 2 PFOS (Undetected) ~ 1.31.2; l,l{ 1.0: 0,9{ 6n 0,8+ d 0.7: ~ I on 0.2: 0.1; Page 456 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO4O.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\HO10404.b\HILL0040.D Lab Smp Id: 1311-4158-S1 In] Date : 05-APR-20010 0 : 0 2 Operator : CMC Inst ID: hi1lary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 50 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SI0 MASS --_- 427 499 RT --__== EXP RT =E====== DLT RT ====E=== RESPONSE ===t==== 5.098 5.092 0.006 1567309 Compound Not Detected. CONCENTRATIONS ON-COLUMN FINAL (ng/mL) (ng/mL) =r-===== 5====== 254.000 254 3M Environmental Laboratory Page 457 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLO04O~D D:\Chem\Hillary\HO10404.b\HILLO04O.D 3.61 3.4- 3.21 9 . (3.0: 2.8: 2.61 2,4{ 2.2; c, 2.01 Ki 62 1.8: . V 1.6; >. 1,4{ 1,2{ l,O{ 0.81 0.61 0.41 0.2: .m. . . . . . . . . . . . . . . . . . . 1 . . . . . . . . . . . . 1 1 1 1 1 d 1 Min 1 THPFOS 3.6: 3,3; 3.0: 2.7: 2.4: 4cj 2.1; 1,s; x 1.5: V >- 1 * 2 { 0.9: 0.61 0.31 +m 9 Ki 2 PFOS 1.21 1.0- (Undetected) I on 1 > , 4. M. .,.. ., .. .,. .. /!`n8v,.sn5&n2en&%Lab%itow BACK TO MAIN Page 2 Page 458 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLO04l.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\H010404.b\HILL0041.D Lab Smp Id: 01003-07-03 Inj Date : 05-APR-200100:16 Operator : CMC Smp Info : 5 ng/mL PFOS in MeOH Inst ID: hi1lary.i Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Als bottle: 3 Cal File: HILL0026.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds .......................... 1 THPFOS 2 PFOS QUANT SIG MASS ---- 427 499 CONCENTRATIONS ON-COLUMN RT ==== 5.105 EXP RT E======= 5.092 DLT RT RESPONSE (ng/mL) ======= === == === ==i == I.== 0.013 1307817 254.000 5.315 5.309 0.006 101216 2.67325 FINAL (ng/mL) ======= 254 2.67 3M Environmental Laboratory Page 459 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO41.D 2.01 1.91 1.81 ,. i1.71 1.61 1,51 1,41 1+31 1.21 ,'; 11.*011L: 0.9; 0.81 0.7: 0.61 0.5; 0.41 0.31 0,2: 0.11 D:\Chem\Hillary\HO10404.b\HILLOO41.D r 1 THPFOS BACK TO MAIN Page 2 2 PFOS Page 460 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0045.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\H010404.b\HILL0045.D Lab Smp Id: 1311-4159-S1 I n j Date : 05-APR-2001 01:14 Operator : CMC Inst ID: hi1lary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Als bottle: 51 Cal File: HILL0026.D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG _ - _ MASS --_a 427 499 CONCENTRATIONS ON-COLUMN --___-- RT EXP RT DLT RT RESPONSE (ng/rnL) = E = = = = = = ==I= ==== ==== == == ======= FINAL (ng/rnL) ======= 5.098 5.092 0.006 1569488 254.000 254 5.315 5.309 0.006 202756 7.96638 7.97 3M Environmental Laboratory Page 461 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0045.D 3.6: 3.41 3.21 I . i3.01 2.8: 2.6: 2.41 2.21 2.0: ' > , 1.81 !. 1.6- 1.4: 1.2: 1.0: 0,s: 0,6{ D:\Chem\Hillary\HO10404.b\HILL0045.D BACK TO MAIN Page 2 1 THPFOS 3.6: 3.3{ 3.0{ 2.7: 2.41 2.1: $, i.8: d x 1.5; W ~ 1.2; 0.9; 0.6; 0.3: 2 PFOS 4.8: 4.4; 4.0; 3.6; 3.2; 2 2.81 &, 2.4; dW x 2.0; 1.6; 1*2; 0.8; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A- 3 16-1 Is) IJ 1 ,+ d Is) Page 462 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0046.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DJta file : D:\Chem\Hillary\HO10404.b\HILL0046.D Lab Smp Id: 1311-4159MS-S1Inj Date : 05-APR-200101:28 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method D:\Chem\Hillary\HO10404.b\HO10404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 52 Dil Factor: 1.00000 Intesrator: Falcon Compound Sublist: all.sub TargGt Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS =E== 427 499 RT EXP RT DLT RT RBSPONSE ==== ==e===== ======== ======== 5.098 5.092 0.006 1521100 5.315 5.309 0.006 3255972 CONCBNTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ng/mL) ======= 254.000 2 54 173.055 173 3M Environmental Laboratory Page 463 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10404.b\HILL0046.D D:\Chem\Hillary\HO10404~b\HILL0046.D 7.21 6.9: 6.61 36.3{ 6.0: 5.7: 5.41 5.11 4,8{ 4,5; 4,21 ; 3.9: 3 3.6: 5 3.31 .. 3.0- 2.7: 2,4{ 2.1; 1.8; l,5{ 1.2: 0.9: 0,6- 0.32 >". I . . . , .' .1 . . , . . . . , .I . . . I . . . . 1 2 3 4 6 7 8 1 THPFOS 3.3; 3.01 2.71 2.44 .P 2.11 n& 1.81 rxl 1.5; Y > 1.2; 0,9{ 0.61 0.34 8"Ion IJ I 2 PFOS 7.0; 6,Of 5.0; CI 4,0{ I\ 0 d"x 3,oj' 2,o; 1.0- Page 2 9 10 11 12 Page 464 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO47.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\Chem\Hillary\H010404.b\HILL0047.D Lab Smp Id: 1311-4160-Sl Inj Date : 05-APR-2001 01:43 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 53 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds QUANT SIG MASS CONCENTRATIONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) 3M Environmental Laboratory Page 465 of 703 Data File: D:\Chem\Hillary\HO10404+b\HILL0047+D BACK TO MAIN Page 2 1 THPFOS 3.0: 2,7{ 2.41 g 2.11 1.8: d x 1.51 V > 1.21 0.9; 0.61 0.31 2 PFOS Lo I. 1 1.2; pCI 1.0: 0 rxl 0 + 8 { V > 0.61 Page 466 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO48.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dita file : D:\Chem\Hillary\H010404.b\HILL0048.D Lab Sny? Id: 1311-4161-S1 Inj Date : 05-APR-200101:57 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\HO10404.b\HOlO4O4.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Cal File: HILL0026.D Als bottle: 5 4 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT S I G MASS ---- 427 499 CONCENTRATIONS ON-COLUMN FINAL RT BXP RT DLT RT RESPONSE (ng/mL) ==E= ======== =I== === ==== ===== (ng/mL) ---------- 5.098 5.092 0.006 1535494 254.000 254 Compound Not Detected. 3M Environmental Laboratory Page 467 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0048.D 3.4; 3.21 ; 9 3.01 2.8: 2.61 2,41 2.2: 2.0: t 1.8: ! : 1.61 1.41 1.21 1.0: 0.81 0.61 0.4: o D:\Cher 1 *1 2 2 3 i 4 i5 1 THPFOS d + Hin BACK TO MAIN Page 2 Q..'. . . . . . . . . . . . . . . . . 1 io 11 12 2 PFOS (Undetected) Page 468 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0049.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dita file : D:\Chem\Hillary\H010404.b\HILL0049.D Lab Smp Id: 1311-4162-S1 Inj Date : 05-APR-200102:11 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\HO10404.b\HOlO4O4.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 55 Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS --_- 427 499 RT BXP RT DLT RT RBSPONSB ==== ======== ==== = ii== === === = I 5.093 5.092 0.001 1528194 Compound Not Detected. CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ng/mL) ======= 254.000 254 3M Environmental Laboratory Page 469 of 703 Data File: D:\Chen\Hillary\HO10404.b\HILL0049.D BACK TO MAIN Page 2 1 THPFOS 3.3: 3.0: 2,7{ 2.41 CI 2.1: 6Ui 1.8; $ 1.5: V 1.2; pm 9 Lo 2 PFOS (Undetected) I Ion Page 470 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO5O.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta file : D:\Chem\Hillary\HO10404.b\HILLO05O.D Lab Smp Id: 1311-4162MS-S1 Inj Date : 05-APR-200102:26 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method D:\Chem\Hillary\HO10404.b\HO10404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Cal File: HILL0026.D Als bottle: 56 Dil Factor: 1.00000 Intemator: Falcon Compound Sublist: all.sub Targgt Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS -__-_- 42 7 499 CONCENTRATIONS ON-COLUMN RT EXP RT DLT RT RESPONSE (ny/mL) ==== ======== ===---_-----__------__------ ======= 5.097 5.092 0.005 1514404 254.000 FINAL (ng/mL) -_-_---_____ 254 5.315 5.309 0.006 3115242 165.194 165 3M Environmental Laboratory Page 471 of 703 BACK TO MAIN Data File: D:\Chem\Hillary\HO10404.b\HILLO05O.D Page 2 D:\Chem\Hillary\HO10404.b\HILLO05O.D 6.91 6.6- 6.3; `i 6.01 5.7: 5.41 5.11 4.81 4.51 4-21 ~ 3.9: D , 3.6: ; 3.3; - 3.01 2.71 . 2.41 24 1.81 1.51 1.21 0,9{ 0.61 0,3{ i . b. l . 1. 1 1 I . . J . . 5 . . . . 2 . . . . 4 . . . . 6 . . \.I . t . . . . . .j . . . 6 . . . . . 1 . . . . io . . . . il . . . . 12 . . . Hin 1 THPFOS 3.3; 3.0{ 2.71 2.4: A 2.1: 6Lo 1.8; 2 1,5: W >- 1.21 0.9; F ?ar Ln Page 472 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLO05l.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DAta file : D:\Chem\Hillary\H010404.b\HILL0051.D Lab Smp Id: 1311-4163-S1 Inj Date : 05-APR-200102:40 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Als bottle: 57 Cal File: HILL0026.D Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 473 of 703 Data File: D:\Chem\Hillary\HO10404+b\HILLOO51.D 3.4{ 3.21 "( 3.01 2.81 2.61 2.4{ 2.21 2.01 ' 1,8{ I 1.61 1.41 1.21 1.01 0.8: 0.61 0.4- D:\Chem n 1 THPFOS 4.4 4.8 5.2 5.6 6.0 Hin 2 PFOS 0.41 II BACK TO MAIN Page 2 Page 474 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO52.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dkta file : D:\Chem\Hillary\H010404.b\HILL0052.D Lab Smp Id: 1311-4164-S1 In] Date : 05-APR-2001 02:55 Operator : CMC Inst ID: hi1lary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\HO10404.b\HOlO4O4.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date . : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 58 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable 3M Environmental Laboratory Page 475 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0052,D BACK TO MAIN Page 2 1 THPFOS 2 PFOS 2.2: 2.01 1.8; 1.6; ; 1.4; 6 1.2; ;v1 1.0; ~ 0.8; 8 I on M, Lo - 0.4; 0.2:- I . . . , . .-J. . . . . . 1. . . . . . . Page 476 of 703 BACK TO MAIN Appendix H: Raw Data Summaries This appendix includes the raw data summary information from all the analyses conducted in the course.of this study. 3M Environmental Laboratoty Page 483 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILLOO53.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb DAta file : D:\Chem\Hillary\H010404.b\HILL0053.D Lab Smp Id: 1311-4165-S1 I n j Date : 05-APR-200103:09 Operator : CMC Inst ID: hi1lary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Met hod : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date .: 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Cal File: HILL0026.D Als bottle: 59 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: al1,sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ---- 42 7 499 \ 3M Environmental Laboratory Page 477 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0053.D I D:\Chem\Hillary\HO10404.b\HILL0053.D I BACK TO MAIN Page 2 1 THPFOS 3,3: 3.0; 2.71 2.4: 2.11 6Lo 1.81 TxI l + 5 { W > 1.21 0.91 0,6{ 0.3{ p ? Lo I I 2 PFOS Page 478 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0054.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dita file : D:\Chem\Hillary\H010404 .b\HILL0054.D Lab Smp Id: 1311-4165MS-S1 Inj Date : 05-APR-2001 03:23 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method . : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date : 04-APR-2001 20:41 Cal File: HILL0026.D Als bottle: 60 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable QUANT SIG MASS ===F 427 499 RT BXP RT DLT RT ==== ======== =====E== 5.098 5.092 0.006 5.308 5.309 -0.001 RBSPONSE ======== 1500713 3133475 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ======= (ny/mL) ======= 254.000 254 166.211 166 3M Environmental Laboratory Page 479 of 703 BACK TO MAIN Page 2 D:\Chem\Hillary\HO10404.b\HILL0054.D 7.26.91 6.6; 6.3: d t 6.01 5.71 5.41 5.1; 4.81 4.5: 4.21 6n 3+9{ Lo 3.61 r,xl 3,31 >- 3.0; 2.71 2.4: 2.1; 1.8: 1.5; 1.2; 0.9: 0.61 0.3; . . . I I. . . . . . . . . . . . . . . . . . . . . 1..1 .I I . . . . .-.. i i i i 6 i, i Hin .................... 6 i io il i2 1 THPFOS 3.3: I-rn 4 3.01 Lo 2.7: 2.41 cn 2.1: 1.81 4 x 1.5{ V 1.2; >- 0.91 0.6; 0.31 . . . . . . . . . I.I . . . . . I 2 PFOS 7.0: 6.0; 5.01 4.0t 3,O: F ? 0 Lo Page 480 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0059.D Report Date: 09-Apr-200113:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\Chem\Hillary\H010404.b\HILL0059.D Lab Smp Id: 1311-4166-S1 Inj Date : 05-APR-2001 04:35 Operator : CMC Inst ID: hil1ary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment . : Method : D:\Chem\Hi11ary\H010404.b\H010404.m Meth Date : 09-Apr-200113:02 carlson Quant Type: ESTD Cal Date : 04-APR-200120:41 Als bottle: 61 Cal File: HILL0026 D Dil Factor: 1.00000 Integrator: Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host: WW19376 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds ............................ 1 THPPOS 2 PFOS QUANT SIG MASS -__- 427 499 RT ==E= EXP RT ======== DLT RT ==E===== RBSPONSB ======== 5.098 5.308 5.092 5.309 0.006 -0.001 1687410 183857 CONCBNTRATIONS ON-COLUMN (ng/mL) ======= FINAL (ng/mL) ======= 254.000 6.98024 254 6.98 3M Environmental Laboratory Page 481 of 703 Data File: D:\Chem\Hillary\HO10404.b\HILL0059.D 3.8: 3.61 3.41 i 3.21 3,OL 2.81 2.61 2.41 2,21 3 2.0; j 1,s; 1.6; 1.41 1,21 1,or 0.81 0.61 1 THPFOS 3.6; 3.3; 3.01 2.,72: 5 2,4! Gn L;: 2,1: 2s"t 1.81 1.5; >. 1.2; 0,9{ I 00.66:1 0.3: IS bQ, Lo * IJ3 i1 4 4-4 4.8 5.2 5.6 6.0 2 PFOS 4.0; 3.6:' 3.2; 2.8; 2,4; 4 2.0; .? 1.6: 1.2; 0.81 x Ion Q, -0 I\ BACK TO MAIN Page 2 Page 482 of 703 BACK TO MAIN ~ ~~~~ Appendix H: Raw Data Summaries This appendix includes the raw data summary information from all the analyses conducted in the course of this study. 3M Environmental Laboratory Page 483 of 703 BACK TO MAIN Guantrfy Co-und summary Report PFOS Adsorb/D..rorb Study, LCAk9 Instrumsat: Tucker ( I M W Sample list: Last m d z f i d : blethod: Last aodifid: Job Cod.: c:~sLYNx\II~atur.m\s.npleDB\to1o123 Wed Jan 24 07:48:32 2001 C:\aMssLm\~atur.PROU&thDB\PFOS Wed an 24 06:43:49 2001 - RIPFOS Printed: Wed Jan 24 07:54:16 2001 M Nara 1 to10122 098 /2 t010122-099 3 t010122~100 f 4 to10122 101 5 t010122~102 6 t010122-103 7 t010122-104 I 8 t010122 105 9 t0101221106 \ 10 t010122-107 11 to10122 108 12 tOiOl22IlO9 13 tO10122-1x0 14 t010122-111 15 t010122-112 16 t010122-113 17 t010122-114 - 18 t010122 115 19 t010123IOOl 20 t010123-002 21 t010123-003 22 t010123-004 23 t010123-005 24 t010123-006 25 t010123-007 26 t010123-008 27 t010123-009 28 to10123 010 34 t010123-016 35 t010123I017 36 t010123-018 37 t010123-019 38 t010123-020 39 t010123-021 40 to10123 022 41 t010123I023 42 t010123-024 43 t010123-025 44 t010123 026 45 t010123I027 46 t010123-028 47 t010123-029 48 to10123 030 49 t010123I031 50 to10123 032 56 t0101231038 57 t010123-039 58 t010123-040 59 t010123-041 60 t010123-042 61 t010123-043 62 t010123-044 63 t010123-045 64 t010123-046 6 5 t010123-047 66 t010123-048 67 t010123-049 68 t010123-050 69 t010123-051 70 t010123-052 71 t010123-053 72 t010123-054 73 t010123-055 74 t010123-056 75 t010123 057 81 t010123I063 E2 t010123-064 Samplelist T u t MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 oob FC Nix 00002-104-01 2.5`ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 25 bib FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank. TN-A-4740. Alia. 12/04/00 lox 800-1311-3007-52, O m g / i PFO5,no soil.. lox 600-1311-3008-52, Omg/L PFOS,no soil.. 10% E00-1311-3009-S2, Omg/L PFOS,no soil.. 10% E00-1311-3009m-S2, Omg/L PFO5,no SO.. lox E00-1311-3010-S2, 5mg/L PFOS,no soil.. 250 ppb FC Hix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox EOO-1311-3011-52, 5 m g / L PFO5,no soil.. lox E00-1311-3012-S2, Omg/L PFO5,no soil.. lox E00-1311-30121~-52, Omg/L PFOS,no so.. lox E00-1311-3022-52. O m g l L PFOS.1:l cla.. lox 800-1311-3023-52, Omg/L PFO5,l:l cla.. 250 ppb FC f i x 00002-104-10 MeOH Blank, TN-A-4140. Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 lox E00-1311-3024-s2, Omg/L PFOS.1:l cla.. lox 600-1311-3024m-S2, Omg/L PFOS, 1:l c.. lox 600-1311-3025-52, Omg/L PFOS,1:5 cla.. lox E00-1311-3026-S2, OrnglL PFOS,1:5 cla.. lox E00-1311-3027-52, OmglL PFOS,1:5 cla.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-3027m-52, Omg/L PFOs,l:5 c . . lox E00-1311-3028-s2, Omg/L PFOS,1:25 cl.. lox E00-1311-3029-52, Omg/L PFOS,1:25 cl.. lox lox .. E00-1311-3030-52, OmglL PFOS,1:25 cl.. E00-1311-3030m-S2, Omg/L PFOS,1:25 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-3094-S2, 5 m g / L PFOS.1:l cla.. lox E00-1311-3095-S2, S m g / L PFOS.1:l cla.. 1 O x E00-1311-3096-SZ, 5mg/l. PFOS.1:l cla.. lox E00-1311-3096~-S2, 5mg/L PFO5,I:I c.. 10x 600-1311-3097-S2, 5mglL PFOS,1:s c l a . . 250 ppb FC K i x 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 lox E00-1311-3098-S2, 5 m g / L PFOS,1:5 cla.. lox 600-1311-3098m-52. 5mg/L PFOS,1:5 c.. lox E00-1311-3100-S2, 5 m g l L PFOS,1:25 cl.. lox E00-1311-3101-s2, 5 m g / L PFOS,1:25 cl.. lox E00-1311-3102-52, 5 m g / L PFOS,1:25 cl.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-31021~-SZ, Smg/L PFOS,1:25 .. lox E00-1311-3166-S2, 5 m g / L PFOS.1:l Sed.. lox E00-1311-31668-S2, 5 m g / L PFOS,l:l Sa.. lox E00-1311-3168-S2, 5 m g l L PFOS.1:l Sed.. lox E00-1311-3168ms-S2, Smg/L PFOS.1:l S.. 2 5 0 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 ppb FC Mix 00002-104-01 2 . 5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix OOOOZL104-04 25 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 RT 6.290 6.443 6.241 6.546 6.278 6.309 6.452 6.486 6.460 6.326 6.313 6.376 6.314 6.229 6.472 6.469 6.529 6.436 6.578 6.406 6.310 6.431 6.468 6.458 6.386 6.254 6.568 6.157 6.097 6.117 6.121 6.119 6.098 6.108 6.119 6.362 6.502 6.106 6.119 6.106 6.109 6.131 6.124 6.420 6.455 6.392 6.230 6.529 6.155 6.403 6.514 6.256 6.531 6.423 6.350 6.375 6.218 6.432 6.299 6.253 6.251 6.322 6.253 6.410 6.302 6.411 6.447 6.190 6.182 6.203 6.120 6.074 6.349 6.384 6.382 6.156 6.159 6.457 6.431 6.408 6.396 6.355 149480 155378 144563 164749 166221 181623 212615 292832 353867 139196 583060 690084 1303673 2036643 3108558 3415199 185076 151445 167484 153481 152060 157526 1093934 161601 1278160 144604 162354 147959 123999 1142929 167082 120568 1461557 120451 130250 158587 1212317 127365 139236 125310 1458323 95010 96165 967775 166690 166376 148831 1212415 1329455 154776 165352 919833 1105460 1302358 2227419 1351396 1295576 163488 155335 1338917 2190122 3728466 3779124 3814147 1341100 166983 166594 4547300 873810 1003813 582014 1618471 1337470 171733 174436 154736 107657 179721 196874 231081 314548 396613 -me 0.000 0.000 0.000 346.252 399.780 436.052 499.891 689.623 84 1.868 1162.333 1595.061 1977.399 451 9.670 8986.881 12406.422 17167.793 0.000 0.000 0.000 350.116 366.988 378.684 3271.735 382.904 4385.279 0.000 0.000 341.086 273.510 3615.037 311.722 255.127 4623.544 0.000 0.000 347.233 3198.718 260.600 292.171 251.422 4339.379 0.000 0.000 2502.035 376.511 382.084 335.207 2936.432 4518.724 0.000 0..000. 1916.324 2217.788 3017.893 6771.423 3087.088 4505.026 0.000 n...o.o..n 3282.293 7297.900 8481,570 9225.336 8899.134 4483.275 0.000 0.000 15741.143 1707.559 1998.291 1165.110 4449.399 3739.611 0.000 0.000 0.000 218.235 380.367 456.559 546.187 754.134 988.034 ppb 0.00 0.00 0.00 3.79 6.92 9.03 12.76 23.83 32.71 51.10 76.63 98.92 246.93 506.27 704.16 978.81 0.00 0.00 0.00 4.02 5.00 5.69 174.31 5.93 239.11 0.00 0.00 3.49 0.00 194.29 3.53 0.00 252.97 0.00 0.00 3.85 170.06 0.00 0.64 0.00 236.44 0.00 0.00 129.49 5.56 5.88 3.15 154.79 246.87 0.00 0.00 95.36 112.93 159.53 377.94 163.56 246.08 0.00 0.00 174.93 408.33 476.98 520.09 501.18 244.81 0.00 0.00 896.63 83.19 100.14 51.56 242.84 201.55 0.00 0.00 0.00 0..0.0 5.78 10.23 15.46 27.63 41.24 Flags bb bb bb bb bbX bbX bbX bb MM bb bb bb bb bb MM bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb' bb bb bb bb HH bb bb bb bb bb bb bb bb bb bb MM bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb ~ bbX bbX bbX bb bb UDw 177 81 28 -5 -18 3 2 -1 -1 1 -6 -2 -4 1 -5 -1 -2 -2 -19 131 105 55 11 3 od Comment 3M Environmental Laboratory Page 484 of 703 BACK TO MAIN Quantify conpotmd summary &port PFOS Msorb/Dmsorb Study, L C M Instrutcant: Tuck- (IA052) . s.rple l i s t : c : \ M A S S L Y N X \ ~ ~ a t u r . P a O \ S ~ l ~ ~ \ t 0 1 0 1 2 3 Iart mdified: Wed Jan 24 07:48:32 2001 - mthod: c : ~ s L Y N X \ o s ~ ~ t ~ . ~ ~ T~W\POPS P o s Last rodifid: Wed Jan 2 1 06:53:49 2001 Job Code: Printd: Wed Jan 24 07:54:16 2001 c..p&...l 1: PFoS(499) I N83 t010123-065 84 t010123-066 85 t010123-067 86 t010123-068 87 t010123-069 88 tO10123-070 89 t010123-071 90 t010123-072 91 t010123-073 S-lelirt T e x t 50 ppb FC Mix 00002-104-07 75 ppb FC Hix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Hix 00002-104-11 750 ppb FC Mia 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740. Aliq, 12/04/00 12/04/00 RT 6.303 6.374 6.300 6.340 6.150 6.163 6.156 6.164 6.141 rue. 463216 623373 740153 1392032 2222555 3363541 4161343 131404 141494 RmspoTue 1186.763 1561.132 1995.565 4451.828 9308.893 13449.481 18086.088 0.000 0.000 Dpb P1.91 52.83 bb 74.65 bb 99.98 bb 242.98 bb 524.93 bb 764.42 bb 1031.66 bb 0.00 bb 0.00 bb whv 6 -0 -0 -3 5 2 3 od ComEnnt Page 2 puantitated and Printad by QdC on 24 Jan 01 Study .I E00-1311 3M Environmental Laboratory (jmc , (94' Page 485 of 703 BACK TO MAIN Gumtify C m p a u n d Surmrary w o r t PFOS Adrorb/Desorb Study, LC/biS Inst-t: Tuoker (IJLo52) Sample List: Last H f i e d : lkthod: Last mdified: Job Code: C:MssLmx~ulatur.P\S~le~~\tOlOi23 - Wad Jan 24 07:48:32 2001 C : \ M R s S L ~ \ D s ~ ~ t u r . p R o ~ u l o B \ P F OTSHPFOS Wed Jan 24 06:53:49 2001 Printad: Wed Jan 24 07:54:16 2001 C& 2: 1 . S . (TH-PMS) (427) I N- Samplelist Text 1 t010122-098 MeOH Blank, TN-A-4740, Aliq. 12/04/00 2 t010122-099 MeOH Blank, TN-A-4740, Aliq. 12/04/00 3 to10122 100 MeOH Blank, TN-A-4740. Aliq. 12/04/00 4 t010122~101 0 ppb FC Mix 00002-104-01 5 t010122~102 2.5 ppb FC Mix 00002-104-02 6 t~ 01~ 01~ 22 1. 03 _5 ppb FC Mix 00002-104-03 7 t010122~104 10 ppb FC Mix 00002-104-04 8 t010122-105 25 ppb FC Mix 00002-104-05 9 t010122-106 40 ppb FC Mix 00002-104-06 10 t010122-107 50 ppb FC Mix 00002-104-07 11 to10122 108 75 ppb PC Mix 00002-104-08 12 t0101221109 100 ppb FC Mix 00002-104-09 13 t010122-110 250 ppb FC Mix 00002-104-10 14 t010122 111 ~~~ 500 ppb FC Mix 00002-104-11 15 t010122I112 750 ppb FC Mix 00002-104-12 16 t010122-113 1000 ppb FC Mix 00002-104-13 17 t010122-114 MeOH Blank, TN-A-4740, Aliq. 12/04/00 18 to10122 115 MeOH Blank, TN-A-4740. Aliq. 12/04/00 19 t010123I001 MeOH Blank, TN-A-4740, Aliq. 12/04/00 20 tOlOl23_002 lox E00-1311-3007-S2, O m g l L PFOS,no soil.. 21 t010123-003 lox H00-1311-3008-S2, Omg/L PFOS,no aoil.. 22 tO10123-004 10% E00-1311-3009-S2, Omg/L PFoS,no soil.. 23 t010123-005 10% E00-1311-3009m-S2, Omg/L PFOS,no so.. 24 t010123-006 10% 600-1311-3010-S2, 5mg/L PFOS,no soil.. 25 t010123-007 250 ppb FC Mix 00002-104-10 26 t010123_OOB MeOH Blank, TN-A-4740, Aliq. 12/04/00 27 t010123_009 MeOH Blank, TN-A-4740. Aliq. 12/04/00 28 t010123 010 10% E00-1311-3011-S2, 5 m g / L PFOS,no soil.. 29 t010123~Oll 10% HO0-1311-3012-S2, Omg/L PFOS,no soil.. 30 t010123-012 10% EOO-1311-3012m-S2, Omg/L PFOS,no so.. 31 tO10123-013 lox E00-1311-3022-S2, OmglL PFOS.1:l cla.. 32 t010123_014 10% i300-1311-3023-S2, Omg/L PFOS.1:l cla.. 33 to10123 015 250 ppb FC Mix 00002-104-10 34 t0101231016 MeOH Blank, TN-A-4740, Aliq. 12/04/00 35 t010123-017 MeOH Blank, TN-A-4740, Aliq. 12/04/00 36 t010123~018 101 E00-1311-3024-S2, Omg/L PFOS.1:l cla.. 37 t010123-019 lox E00-1311-3024ms-S2, Omg/L PFOS,l:l c.. 38 t010123-020 10% E00-1311-3025-52, Omg/L PFO5,l:S cla.. 39 t010123-021 10% E00-1311-3026-S2, OmglL PFoS.1:5 cla.. 40 t010123-022 lox E00-1311-3027-S2, Omg/L PFOS,1:5 cla.. 41 tOlOl23-023 250 ppb FC Mix 00002-104-10 42 tO10123-024 MeOH Blank, TN-A-4740, Aliq. 12/04/00 43 t010123-025 MeOH Blank. TN-A-4740. Aliq. 12/04/00 44 t010123-026 10% 600-1311-3027ms-S2, Omg/L PEOS.1:) c . , 45 t010123-027 lox H00-1311-3020-S2. Oma/L PFo5.1:25 cl.. 46 `~ ~0~ 10~~~ 1230.28 lox E00-1311-3029-S2; Omg/L PF05,1:25 cl.. 47 t010123I029 48 t010123-030 49 t010123-031 10% 10% .. E00-1311-3030-S2, OmglL PFOS,1:25 cl.. E00-1311-3030ms-S2, Omg/L PFOS,1:25 250 ppb FC Mix 00002-104-10 50 to10123 032 MeOH Blank, TN-A-4740. Aliq. 12/04/00 51 t0101231033 MeOH Blank, TN-A-4740. Aliq. 12/04/00 52 t010123-034 10% E00-1311-3094-S2, 5 m g / L PFOS.1:l cla.. 53 t010123-035 5 4 t010123_036 55 t010123-037 10s H00-1311-3095-SZ, Smg/L PFOS,l:l cla.. lox 800-1311-3096-S2, 5 m g l L PFOS,I:I cla.. lox E00-1311-3096ma-S2, 5mgll PFOS.1:l c.. 56 t010123-038 5 7 t010123-039 lox EOO-1311-3097-52, 5rng/L PF05.1:5 cla.. 250 ppb FC MIX 00002-104-10 58 t010123-040 MeOH Blank. TN-A-4740. Alia. 12/04/00 59 t010123-041 MeOH Blank; TN-A-4740; Alii. 1;/04/00 60 t010123_042 10% E00-1311-3098-S2, 5 m g / L PFOS,1:5 cla.. 61 t010123-043 lox E00-1311-3098ms-S2, 5mg/L PFOS,1:5 c.. 62 t010123-04t lox E00-1311-3100-S2, 5 m g l L PFOS,1:25 cl.. 63 t010123-045 10% E00-1311-3101-S2, 5 m g l L PFOS,1:25 cl.. 64 t010123-046 10% E00-1311-3102-S2, 5mg/L PFOS,1:25 cl.. 65 t010123-047 250 ppb FC Mix 00002-104-10 66 t010123-048 MeOH Blank, TN-A-4740. Aliq. 12/04/00 67 t010123-049 68 t010123-050 69 t010123-051 .. MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-3102as-S2, 5 m g / L PFOS.1:ZS 10% E00-1311-3166-S2, 5mg/L PFOS,l:l Sed.. 70 t010123-052 lox 600-1311-31668-52, 5 m g l L PFoS.1:l Se.. 71 t010123-053 lox E00-1311-3168-S2, 5 m g / L PFOS.1:l Sed.. 72 t010123-054 10% E00-1311-3168ms-S2, 5 m g / L PFOS,l:l S.. 73 t010123_055 250 ppb FC Mix 00002-104-10 74 t010123-056 MeOH Blank, TN-A-4740, Aliq. 12/04/00 75 t010123-057 MeOH Blank, TN-A-4740, Aliq. 12/04/00 76 to10123 058 MeOH Blank, TN-A-4740. ALiq. 12/04/00 0 ppb FC Mix 00002-104-01 2 . 5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 25 ppb FC Mix 00002-104-05 82 t010123I064 40 ppb FC Mix 00002-104-06 RT 6.242 6.383 6.192 6.389 6.217 6.249 6.367 6.390 6.232 6.266 6.253 6.316 6.266 6.181 6.231 6.385 6.240 6.363 6.988 6.334 6.250 6.346 6.383 6.374 6.326 6.193 6.097 6.037 6.069 6.061 6.047 6.049 6.048 6.059 6.146 6.393 6.046 6.046 6.046 6.037 6.046 6.040 6.191 6.371 6.308 6.170 6.336 6.119 6.175 6.418 6.112 6.290 6.351 6.289 6.303 6.169 7.166 6.205 6.202 6.262 6.204 6.338 6.254 6.350 6.387 6.142 6.086 6.095 6.060 6.025 6.156 6.312 6.322 6.095 6.063 6.179 6.346 6.335 6.324 6.294 Area 691 560 661 118951 103945 104129 106331 106157 105084 94464 91385 87246 72111 56656 62640 49733 95 1 553 548 109593 103586 103996 83590 105510 72867 675 0 108447 113341 79040 122235 118145 79028 1325 1759 114179 94750 122184 119139 124601 84017 1533 1451 96699 110681 108861 110999 103222 73553 1245 531 120000 124613 107886 82200 109439 71896 0 4534 101980 75026 109899 102412 107149 74784 661 520 72220 127941 125584 124884 90938 89412 677 595 2000 123326 118124 107803 105770 104192 100354 Rnsponse 690.849 560.268 660.914 118951.328 103945.063 104129.148 106330.531 106156.602 105083.742 94464.391 91385.258 87246.352 72111.070 56656.000 62640.102 49132.637 951.098 552.916 547.605 109593.180 103586.234 103995.594 83589.734 105510.461 72866.516 675.222 1.08..447.039 113340.656 79039.930 122235.211 118145.313 79027.961 1325.487 1758.722 114179.469 94750.258 122184.172 119139.492 124601.102 84016.813 1532.789 1451.493 96698.766 110680.852 108861.070 110999.161 103221.789 73552.547 1245.197 530.664 119999.648 124612.836 107886.336 82199.563 109439.414 71896.141 4533.709 101980.344 75025.750 109899.039 102411.563 107149.367 74783.500 661.374 520.055 72._ 719...969 12794 1.430 125583.922 124883.797 90937.609 89412.344 676.734 595.368 2000.157 123326.328 118123.727 107803.281 105770.016 104191.516 100354.180 ppb 1.95 1.58 1.87 336.00 293.61 294.13 300.35 299.85 296.82 266.83 258.13 246.44 203.69 160.03 176.94 140.48 2.69 1.56 1.55 309.56 292.59 293.75 236.11 298.03 205.82 1.91 nag. bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb M bb bb bb bb bb bb bb M 306.32 bb 320.15 bb 223.26 bb 345.27 bb 333.72 bb 223.23 bb 3.74 bb 4.97 bb 322.52 bb 267.64 bb 345.13 bb 336.53 bb 351.95 bb 237.32 bb 4.33 bb 4.10 bb 273.14 bb 312.63 bb 307.49 bb 313.53 bb 291.57 bb 207.76 bb 3.52 bb 1.50 bb 338.96 bb 351.99 bb 304.71 bb 232.18 bb 309.13 bb 203.08 bb 12.81 bb 288.06 bb 211.92 bb 310.43 bb 289.28 bb 302.66 bb 211.24 bb 1.87 bb 1.47 bb 204.00 bb 361.39 bb 354.73 bb 352.75 bb 256.87 bb 252.56 bb 1.91 bb 1.68 bb 5.65 bb 348.35 bb 333.66 bb 304.51 bb 298.76 bb 294.30 bb 283.47 bb brmv 34 17 18 20 20 19 7 3 -1 -19 -36 -29 -44 24 17 18 -6 19 -18 23 28 -11 38 33 -11 29 7 38 35 41 -5 9 25 23 25 17 -17 36 41 22 -7 24 -19 15 -15 24 16 21 -16 -18 45 42 41 3 1 39 33 22 20 18 13 Dags 3 Guantitated and Printed by a4C om 24 Jan 01 Study # E00-1311 3M Environmental Laboratory i LJ-.i/c i Page 486 of 703 BACK TO MAIN Gvanbfy C e o u n d S - r y mort PFOS Add.orb/Wsorb Study, L C M Instrument: TUOkeL (-52) S w l e Irst: C : \ l a R s s L n a t \ ~ a o a t u r . P R o \ s ~ l ~ \ t O l o l 2 3 - Last mdLf3e.d: Wed Jan 24 07:48:32 2001 tkthod: C:\HnssLYNx\Dccatur.PRO~thDB\PFOS THPWS h s t aoclfmd: W e d Jan 2 4 06:53:49 2001 Job Code: &=tad: Wed Jan 2 4 07:54:16 2001 Coqdund 2: I.S. (TH-PEOS) (427) I N83 t010123-065 84 t010123-066 85 t010123-067 86 to10123 068 87 t010123-069 88 t010123I070 89 t010123-071 90 t010123-072 91 t010123-073 S a a D l a l i s t Text 50 ipb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 iib FC Mix 00002-104-11 750 ibb FC Mix 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-I740. Aliq. MeOH Blank, TN-A-4740. Aliq. 12/04/00 12/04/00 RT 6.242 6.302 6.251 6.279 6.102 6.091 6.095 6.092 6.069 )ma 97580 99827 92725 78172 59689 62522 57521 1502 1802 Response 97579.789 99827.031 92724.766 78171.930 59689.027 62521.754 57521.328 1502.362 1801.890 ppb 275.63 281.98 261.91 220.81 168.60 176.60 162.18 4.24 5.09 Flags bb bb bb bb bb bb bb bb bb 6 D w ad 10 13 5 -1.2~ -2.3~ -29 -35 Cammt Page 4 Quantitated and Printed by PIC on 24 Jan 01 Study 8 E00-1311 3M Environmental Laboratory BACK TO MAIN h w t a f y c w n u r d summary Repart PPOS Msorb/Dssorb Study, L.c/bfS Inrtruaant: T w k a r (LAO52) Sample Last: Last -&fled: Method: Last -&fled: Job C&: C:\saassL~~x\~eaatur.~~O\S~l~~\tOlOl24 - Wed Jan 24 08:lA:OS 2001 c : \ M A S S L Y N X \ D e e a t u r . P R O ~ ~ \ P P O S THPEOS Wed Jan 24 06:53:49 2001 Prmtui: Thu Jan 25 07:47:21 2001 CDmpdnrd 1: PFoS(499) 3 t010123-059 4 t010123-060 5 t010123-061 6 t010123-062 7 t010123-063 8 t010123-064 10 t010123-066 11 tO10123-067 12 t010123-068 13 t010123-069 14 to10123 070 15 tOI01231071 16 t010123-072 17 t010123-073 18 t010124-001 19 tOlOl24 002 20 t0101241003 21 t010124 004 ~ ~ ~~~ ~ ~ 22 t010124I005 23 t010124-006 24 t010124 007 25 t010124-008 26 t0101241009 27 t010124~010 28 to10124 011 29 t0101241012 30 t010124-013 31 t010124-014 32 t010124-015 33 t010124-016 34 t010124-017 35 t010124~018 36 t010124-019 37 t010124-020 38 t010124~021 39 t010124-022 40 t010121-023 41 t010124-024 42 t010124-025 43 t010124-026 44 t010124 027 4 5 t010124I028 46 tOl0124-029 47 t010124-030 48 to10124 031 49 t010124I032 50 t010124 033 51 t0101241034 5 2 t010124-03.5 53 t010124-036 54 toioiza-037 55 t010124-038 56 t010124-039 57 t010124-040 58 t010124 041 59 t0101241042 60 t010124-043 61 t010124-044 62 tO10124-015 63 tOl0124-046 64 tO10124-047 65 t010124-048 66 t010124-049 67 t010124-050 S-lelist T e x t MeOH Blank, TN-A-4140. Aliq. 12/04/00 MeOH Blank, TN-A-4140, Aliq. 12/04/00 0 ppb FC Mix 00002-104-01 2.5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 25 ppb FC Mix 00002-104-05 4 0 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb F C Mix 00002-104-10 . _ ~ 500 ppb FC Mix 00002-104-11 750 oob F- C- Mix 00002-1~ 04-1~ 2 . 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank. TN-A-4740. Alia. 12/04/00 . lox EOO-1311-3169-S2, O.Smg/L PFOS,1:5 S.. lox ~~~~ E~ O0-1.3.11.-~ 31~ 70-S~ 2. 0 . 5- m- =d L PFOS.1:5 S . ~~ lox E00-1311-3171-S2, O.Smg/L PFOS;l:5 S.. lox lox .. BOO-1311-3171rmr-SZ. 0.5mg/L PFOS,1:5.. E00-1311-3172-S2, 0.5mg/L PFOS,1:25 2 5 0 ppb FC Mix 00002-104-10 MeOH-Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 .. lox 800-1311-3173-S2, 0.5mg/L PFOS,1:25 .. lox EOO-1311-3174-S2, 0.5mg/L PFOS,1:25 lox E00-1311-3174ms-S2, 0.5mg/L PFOS,1:2.. lox E00-1311-3184-S2, Omg/L PFOS,l:l Sed.. lox E00-1311-3185-S2, Omg/L PFOS, 1:l S e d . . 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-3186-S2, Omg/L PFOS.1:l Sed.. lox E00-1311-3186ms-S2, Omg/L PFOS,l:l S.. lox E00-1311-3187-S2, Omg/L PFOS,1:5 Sed.. lox E00-1311-3188-S2, OmglL PFOS,1:5 Sed.. lox EOO-1311-3189-52, Omg/L PFOS,1:5 Sed.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 lox E00-1311-3189ms-S2..~OmolL PFOS.1:5 S.. lox E00-1311-3190-S2, Omg/L PFOS,1:25 Se.. lox E00-1311-3191-S2, OmglL PFOS,1:25 Se.. lox lox .. E00-1311-3192-S2, Omg/L PFOS,1:25 Se.. E00-1311-3192m-S2, Omg/L PFOS,1:25 250 ppb F C Mix 00002-104-16 MeOH Blank. TN-A-4740. Alia. 12/04/00 MeOH Blank; TN-A-4740. Alii. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 0 ppb FC Nix 00002-104-01 2 . 5 ppb FC MIX 00002-101-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 25 ppb FC nix 00002-104-05 4 0 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 7 5 ppb FC Mix 00002-104-08 100 ppb F C Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 RT 6.382 6.156 6.159 6.457 6.431 6.408 6.396 6.355 6.303 6.374 6.300 6.340 6.150 6.163 6.156 6.164 6.141 6.622 6.174 6.555 6.124 ~~ 6.325 6.122 6.542 6.098 6.541 6.265 6.540 6.253 6.533 6.227 6.483 6.278 6.409 6.328 6.317 6.507 6.290 6.580 6,216 6.420 6.218 6.565 6.386 6.361 6.218 6.592 6.193 6.543 6.528 6.204 6.375 6.123 6.102 6.134 6.159 6.541 6.086 6.363 6.111 6.516 6.121 6.325 6.121 6.360 6.118 6.553 Area 174436 154736 107657 179721 196874 231081 314548 396613 463216 623373 740153 1392032 2222555 3363541 4161343 137404 141494 329160 148405 2008353 2978378 2091729 3089729 2749532 1690139 211382 186560 2974252 2~ 78~ 90.63~ 3375943 174753 183066 1492375 185832 192377 189635 1332791 1~9 0.6 0.4.. 202180 176278 1440653 166888 209975 1789138 201659 1.111.4.7202407 1351244 1589633 188064 173176 189146 107963 195139 170706 230314 325950 393053 426687 615435 678046 1475797 2194012 3224378 3953019 137693 185417 bspnSl, 0.000 0.000 218.235 380.367 456.559 546.187 754.734 988.034 1186.763 1561.132 1995.565 4451.828 9308.893 13449.481 18086.088 0.000 0.000 0.000 0.000 3510.085 6104.627 4018.001 8684.097 5030.908 4406.001 0.000 0.000 5340.462 5395.878 7580.041 331.804 351.811 4495.674 0.000 0.000 378.275 3109.357 369.223 369.266 344.860 4259.849 0.000 0.000 3571.515 408.113 343.872 372.116 3603.727 3743.216 0.000 0.000 0.000 223.595 442.196 359.205 504.877 684.561 91~ 3..309 1007.082 1636.708 1616.410 4437.320 9228.069 13956.302 16771.422 0.000 0.000 Ppb Flags 0.00 bb 0.00 bb 7.77 bb 16.28 bbX 20.28 bbX 24.99 bbX 35.96 bbX 4 8 . 2 7 bb 58.76 hb 78.59 bb 101.69 bb 234.06 bb 505.39 bb 748.03 bb 1034.13 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 186.19 bb 324.90 bb 210.45 bb 469.73 bb 265.72 bb 231.56 bb 0.00 bb 0.00 bb 282.72 bb 285.76 hb 407.27 bb 13.73 bb 14.78 hb 236.45 bb 0.00 bb 0.00 bb 16.17 bb 161.33 bb 15.69 bb 15.70 bb 14.42 bb 223.60 bb 0.00 bb 0.00 bb 1~86~.~ 26.~b~~ b 17.74 bb 14.36 bb 15.85 bb 188.01 bb 195.55 hU 0.00 bb 0.00 bb 0 . 0 0 bb 8 . 0 5 bb 19.53 bbX 15.17 bbX 22.82 bbX 32.27 bbX 44.32 bb 49.27 bb 82.61 bb 81.53 bb 233.27 bb 500.77 bb 778.52 bb 951.32 bb 0.00 bb 0.00 bb SDav od c0mm-k 551 306 150 44 21 18 5 2 -6 1 -0 3 -7 -5 -11 -22 b 681 203 128 29 11 -1 10 -18 -7 0 4 -5 Page 1 puantitated and Printed by cM2 on 25 Jan 01 study I E00-1311 3M Environmental Laboratory Page 488 of 703 BACK TO MAIN Quantify Compound Stxmury Report PPOS Msorb/Desorb Study, Ic/MS IMt-t: T u o k e r (IAo52) S-le LISt: C : \ a a a s S L Y N x \ D e ~ ~ t u r . P R O \ S ~ l s D B \ t 0 1 0 1 2 4 - Last modified: W e d Jan 24 08:14:06 2001 Wthod: c:\aaasSLnat\Deoatur.pRo~ulne\PwS last &fled: Wed Jan 24 06:53:49 2001 THPPOS Job Code: Pr-ted: Thu Jan 25 07:47:21 2001 C & u m d 2: 1 . 8 . (m-PFOS) (427) 1 t010123-057 2 t010123-058 3 t010123-059 4 t010123-060 5 to10123 061 6 t010123I062 7 t010123-063 8 t010123-064 9 t010123-065 10 t010123-066 11 t010123-067 12 t010123-068 13 t010123-069 14 t010123-070 15 to10123 071 21 t010124~004 22 t010124-005 23 t010124-006 24 t010124-007 25 t010124-008 26 t010124-009 27 tOlOl24-0l,O 28 t010124-011 29 tO10124-012 30 t010124-013 31 t010124-014 32 t010124-015 3 3 t010124-016 34 t010124-017 35 t010124-018 36 t010124-019 37 t010124-020 38 t010124-021 39 t010124-022 40 t010124 023 46 t010124I029 47 to10124 030 48 t0101241031 49 t010124-032 50 t010124-033 51 t010124-034 52 t010124 035 53 t010124-036 54 f010121~037 55 t010124-038 56 to10124 039 57 t010124I040 58 t010124-041 59 t010124 042 60 t0101241043 61 t0o10124-004444 62 t01100112244-~040545 63 t010124-046 64 t010124-047 65 t010124-048 66 t010124-049 67 tOlO124-050 S m p l d i s t Text MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 ppb FC Mix 00002-104-01 2 . 5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 25 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 lox E00-1311-3169-S2, 0.5mg/L PFOS,1:5 S.. lox E00-1311-3170-S2, O.Smg/L PFOS,1:5 S.. lox E00-1311-3171-S2, 0.5mg/L PFOS.l:5 S.. lox lox .. E00-1311-3171ms-S2, O.Smg/L PFOS,1:5.. E00-1311-3172-S2, 0.5mg/L PFOS,1:25 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 .. lox E00-1311-3173-S2, 0.5mg/L PFOS.1:25 .. lox E00-1311-3174-S2, 0.5mg/L PFOS,1:25 lox E00-1311-3174ma-S2. 0.5mg/L PFOS,l:2.. lox E00-1311-3184-S2, Omg/L PFOS,l:l Sed.. lox E00-1311-3185-S2, Omg/L PFOS,l:l Sed.. 2 5 0 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-3186-S2, Omg/L PFOS,1:1 Sed.. l o x E00-1311-3186ms-S2, OmqlL PFOS.1:l S.. 10x E00-1311-3187-S2, Omg/L PFOS,1:5 Sed.. lox 600-1311-3188-52. Omg/L PFOS,l:5 Sed.. lox E00-1311-3189-92, Omg/L PFOS,1:5 Sed.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 lox E00-1311-3189ms-S2, Omg/L PFOS,1:5 S.. lox E00-1311-319042. Omq/L PFOS,1:25 S e . . lox E00-1311-319142. Omg/L PFOS,1:25 Se.. lox lox .. E00-1311-319242. OmglL PFOS,1:25 Se.. E00-1311-3192ms-S2, Omg/L PFOS,1:25 250 ppb PC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 0 ppb FC Mix 00002-104-01 2.5 ppb BC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 2 5 ppb FC M i x 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC nix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Nix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Nix 00002-104-12 1000 ppb FC M i x 00002-104-13 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq, 12/04/00 RT 6.322 6.095 6.063 6.179 6.346 6.335 6.324 6.294 6.242 6.302 6.251 6.279 6.102 6.091 6.095 6.092 6.069 6.067 6.102 6.338 6.075 6.144 6.073 6.301 6.038 6.420 6.157 6.396 6.145 6.280 6.131 6.206 6.230 6.192 6.161 6.387 6.145 6.351 6.120 6.347 6.122 6.408 6.192 6.277 6.122 6.315 6.121 6.338 6.239 6.131 6.315 6.039 6.329 6.074 6.051 6.323 6.037 6.170 6.074 6.275 6.048 6.264 6.049 6.167 6.046 6.252 Area 595 2000 123326 118124 107803 105770 104192 100354 97580 99827 92725 78172 59689 62522 57521 1502 1802 84 6 1760 140638 121972 130147 88948 136632 95900 566 1457 139232 129222 111343 131669 130088 82989 704 0 125329 107160 129058 136880 127790 84548 1735 722 125237 123531 129002 135984 93739 106168 913 1535 521 120713 110321 118808 114045 119036 107590 105922 94005 104869 83147 59439 57758 58925 1483 612 Rnapmur 595.368 2000.157 123326.328 118123.727 107803.281 105770.016 104191.516 100354.180 97579.789 99827.031 92724.766 78171.930 59689.027 62521.754 51521.328 1502.362 1801.890 846.302 175 9.64 9 140637.594 121972.141 130147.320 ~~ 88947.891 136631.984 95899.828 566.227 1456.896 139231.969 129221.938 111343.148 131668.844 130088.313 82989.492 703.963 125328.508 107159.664 129057.625 136879.719 127789.961 84548.352 1735.427 721.528 125236.625 123531.180 129002.477 135984.188 93739.367 106167.570 913.271 1535.103 521.492 120713.117 110323.898 118807.953 114044.594 119036.070 107590.352 105921.656 94005.047 104869.109 83146.836 59438.539 57758.453 58924.914 1482.589 612.205 ppb 1.61 5.41 333.59 319.52 291.60 286.10 281.83 271.45 263.95 270.03 250.82 211.45 161.46 169.12 155.59 1.06 4.87 2.29 4.76 380.42 329.93 352.04 240.60 369.58 259.41 1.53 3.94 376.62 349.54 301.18 356.16 351.08 224.48 1.90 Flag. bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb * D w od C-t 33 28 17 14 13 9 6 8 0 -15 -35 -32 -38 52 32 41 -4 48 4 51 40 20 42 41 -10 339.01 bb 36 289.86 bb 16 349.10 bb 40 370.25 bb 48 345.67 bb 38 228.70 bb -9 4.69 bb 1.95 bb 338.76 bb 36 334.15 bb 34 348.95 bb 40 367.83 bb 47 253.56 bb 1 287.18 bb 15 2.47 bb 4.15 bb 1.41 bb 326.52 bb 31 298.42 bb 19 321.37 bb 29 308.49 bb 23 321.99 bb 29 291.03 bb 16 206.51 bb 15 254.28 bb 2 283.67 bb 13 224.91 bb -10 160.78 bb -36 156.23 bb -38 159.39 bb -36 4.01 bb 1.66 bb Page 2 puantitated and Printed by UE on 25 Jan 01 Study I E00-1311 3M Environmental Laboratory BACK TO MAIN Quantify colpound - r y Repart PFOS Adsorb/Desorb Study, Khls Instrunmnt: W k e z lLA052) Sanple List: Last modified: Msthmi: L a s t modified: Job Code: c:\sdnssLrx\Dao.tur.PRO\SanplY1B\t010125 - Thu Jan 25 10:45:39 2001 C:\sdnsSL~\Daoatul.PRO~uloB\PFOS THPFOS Wed Jan 31 07:38:20 2001 Printed: Wed Jan 31 07:42:18 2001 c-smd 1: PFOS(499) # N1 t010125-001 2 t010125-002 3 t010125-003 4 t010125-0Q4 5 t010125-005 6 t010125-006 1 t010125~007 8 t010125-008 9 t010125-009 10 t010125-010 11 t010125-011 12 t010125-012 13 to10125 013 19 t010125I019 20 to10125 020 26 t010125I026 21 to10125 021 34 to101251034 35 t010125-035 36 t010125-036 31 t010125 0 3 1 43 t010125I043 41 t010125-044 45 t010125-045 46 t010125-046 41 t010125-041 18 t010125-048 49 t010125-049 50 t010125-050 51 t010125-051 52 t010125-052 53 t010125-053 5 4 tO10125-054 55 t010125-055 56 t010125-056 51 t010125-057 58 t010125-058 59 t010125-059 60 t010125-060 61 t010125-061 62 t010125-062 63 t010125-063 64 tO10125-064 65 t010125-065 66 t010125-066 61 t010125-061 68 t010125 068 69 t0101251069 10 t010125-010 11 t010125-011 12 t010125 012 13 t0101251073 14 t010125-014 75 t010125-015 1 6 t010125-076 71 t010125~011 18 t010125-018 I9 tOl0125-079 80 t010125-080 81 t010125-081 02 t010125-082 S-ldlst TUt MeOH Blank, TN-A-4140, Aliq. MeOH Blank, TH-A-1110. Aliq. 1000 ppb FC Mix 00002-104-13 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-1140. Aliq. MeOH Blank, TN-A-4740. Aliq. 0 ppb FC Mix 00002-101-01 2.5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-01 25 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 15 ppb FC Mix 00002-104-08 100 ppb F C Mix 00002-104-09 250 ppb FC Mix 00002-101-10 500 ppb FC Mix 00002-104-11 150 ppb k C Mix 00002-104-12 1000 ppb FC Mix 00002-101-13 MeOH Blank, TN-A-4140. Aliq. MeOH Blank, TN-A-4140. Aliq. MeOH Blank, TN-A-1140. Aliq. MeOH Blank. TN-A-1140. Aliq. 0 ppb FC Mix 00002-104-01 2.5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-101-04 25 ppb FC Mix 00002-104-05 10 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-101-01 15 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-1140. Aliq. MeOH Blank, TN-A-4140. Aliq. MsOH Blank, TN-A-4140. Aliq. lox 600-1311-0016 lox E00-1311-0011 lox EOO-1311-0018 10% EOO-1311-0019 10% EOO-1311-0020 250 ppb F C Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4140. Aliq. lox EOO-1311-0021 lox E00-1311-0022 10% EOO-1311-0023 lox EOO-1311-0024 lox EOO-1811-0025 250 ppb FC Mix 00002-104-10 HeOH Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-4740, Aliq. 1Ox 800-1311-0026 1Ox EOO-1311-0021 lox EOO-1311-0028 lox E00-1311-0029 lox EOO-1311-0030 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4140. Aliq. MeOH Blank, TN-A-9140. Aliq. lox EOO-1311-0031 10% EOO-1311-0032 lox E00-1311-0033 lox E00-1311-0034 lox EOO-1311-0035 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4190. Aliq. MeOH Blank, TN-A-4740, Aliq. 10% 00-1311-0036 lox EOO-1311-0037 lox 600-1311-0038 10% E00-1311-0039 10x EOO-1311-0040 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4140. Aliq. MeOH Blank, TN-A-4710, Aliq. 10% E00-1311-0011 lox 600-1311-0042 lox EOO-1311-0043 12/04/00 12/04/00 12/04/00 12/01/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/01/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/01/00 12/04/00 12/04/00 RT 6.450 6.241 6.119 6.542 6.108 6.543 6.121 6.520 6.156 6.388 6.111 6.292 6.388 6.011 6.483 6.134 6.509 6.398 6.265 6.101 6.531 6.265 6.352 6.146 6.349 6.121 6.302 6.110 6.458 6.110 6.156 6.341 6.050 6.520 6.543 6.050 6.590 6.013 6.410 6.121 6.500 6.169 6.675 6.110 6.458 6.049 6.561 6.062 6.590 6.101 6.662 6.108 6.192 6.095 6.626 6.111 6.612 6.012 6.135 6.110 6.445 6.039 6.460 6.025 6.508 6.035 6.505 6.035 6.532 6.614 6.108 6.315 6.012 6.458 6.086 6.325 6.096 6.205 6.519 6.254 6.109 6.501 Area 831200 296113 5181701 5239132 251189 296161 190383 228013 209827 256016 321643 122644 508823 625655 696012 1601022 2411999 3324924 3625888 140546 175160 150113 160830 132405 181926 110151 223063 298612 400141 169182 601584 144115 1484003 2300138 3223153 3992950 178960 106658 168111 84682 162860 141596 188330 141421 1301101 125026 161718 104841 110430 138631 193349 134611 1353855 139866 198325 139108 198174 146148 55629 145556 1369261 122300 151469 2808141 2511874 2834724 2425654 2148880 1418330 59950 138121 2531391 2161946 2545826 2801459 2632713 1501011 148933 114595 2612098 2687648 2610315 Response 831200.000 296143.250 5181107.000 5239132.000 251188.984 296161.125 190383.219 228073.438 209821.018 256076.359 321642.656 422643.563 508823.188 625654.688 696012.313 1601021.750 2171998.150 3324921.000 3625888.250 140546.016 115459.922 150113.141 168829.969 132101.518 181925.563 110150.612 223063.438 298612.031 400141.438 469181.844 604584.250 144174.150 1484002.500 2300131.500 3223152.500 3992949.500 118960.315 106658.201 168116.119 84681.828 162860.281 141596.422 188329.828 141420.531 1301100.500 125026.102 161111.181 104841.234 170429.656 138631.112 193349.112 131610.134 1353855.250 139866.328 198324.119 139101.166 198113.656 146448.291 55628.688 145555.625 1369261.315 122300.242 151468.953 2808143.500 2511814.250 2834124.000 2425654.250 2148880.250 1418330.250 59950.008 138126.672 2531397.000 2161945.500 2545825.750 2807459.250 2632112.150 1501071.125 148933.156 114594.859 2612098.000 2681647.500 2610315.000 ppb Flagr 125.20 bb 9.40 bb 1495.43 bb 1521.41 bb 0.05 bb 9.40 bb 0.00 bb 0.00 bb 0.00 bb 0.95 bb 14.19 bb 36.21 bb 54.16 bb 80.04 bb 95.10 bb 304.22 bb 525.01 bb 161.38 bb 862.14 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bbX 0.00 bbX 0.00 bbX 9.92 bbX 31.41 bb 16.24 bb 75.46 bb 105.91 bb 214.84 bb 411.90 bb 136.43 bb 986.15 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 231.89 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 214.20 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 211.80 bb 0.00 bb 0.00 bb 615.66 bb 531.11 bb 623.15 bb 511.02 bb 599.06 bb 259.33 bb 0.00 bb 0.00 bb 539.31 bb 602.10 bb 543.28 bb 615.46 bb 566.96 bb 278.90 bb 0.00 bb 0.00 bb 561.30 bb 582.06 bb 560.81 bb Wav 50 53 -100 -100 -91 -4 1 -9 10 1 -5 22 5 2 -I1 -100 -100 -100 -60 -21 -8 1 6 10 -4 -2 -1 -1 -2 -1 4 12 od c-t Puantitated and Printed by CMC on 31 Jan 01 Study 0 EOO-1311 3M Environmental Laboratory Page 490 of 703 BACK TO MAIN lcm h w t i f y Compound Summary Rsport PFOS Adsorb/Derorb Study, Instrumm%t:T w k e r (LAo52) S q l e List: c:~SLrx\Dsoatur.PRD\Ssrpla~~\tO10125 - Last mdzfied: Thu Jan 25 10:45:39 2001 bw: C:\aaasSLnrX\~oatur.pRo\HsthDB\PFOS TWlOS Last m d i f i e d : Wed Jan 31 07:38:20 2001 Job Code: Printed: Wed Jan 31 07:42:18 2001 (I Nama S - l d i s t Text RT Area IhSporuO ppb F l a p tDar od t-C 03 t010125-003 lox EOO-1311-0014 6.073 2858584 2858584.250 629.91 bb 84 t010125-004 lox EOO-1311-0045 6.324 2564991 2564990.500 518.47 bb 85 t010125-085 250 ppb FC Mix 00002-104-10 6.047 1595213 1595213.250 301.30 bb 21 86 t010125-086 MeOH Blank, TN-A-4740. Aliq. 12/04/00 6.578 179270 179270.266 0.00 bb 87 t010125-007 MeOH Blank, TN-A-4740. Aliq. 12/04/00 6.036 113308 113300.227 0.00 bb 88 t0101251088 lox EOO-1311-0046 6.313 2646930 2646937.500 570.84 bb 89 t010125-089 lox EOO-1311-0047 6.119 2804164 2804164.000 614.54 bb 90 t010125-090 lox EOO-1311-0048 6.299 2570387 2570306.500 549.94 bb 91 t010125-091 lox EOO-1311-0049 6.098 2079210 2879210.250 635.77 bb 92 tO10125-092 lox EOO-1311-0050 6.170 2533023 2533023.250 539.81 bb 93 t010125-093 250 ppb FC Mix 00002-104-10 6.050 1333005 1333005.000 239.33 bb -4 94 t010125 094 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.373 146205 146204.059 0.00 bb MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.059 70603 70603.414 0.00 bb lox EOO-1311-0051 6.363 2005065 2005864.625 402.35 bb lox EOO-1311-0052 6.099 2065654 2065653.500 417.47 bb lox EOO-1311-0053 6.120 1833231 1833230.750 359.31 bb lox 600-1311-0054 6.100 1920545 1920544.625 300.97 bb 100 t010125~100 lox E00-1311-0055 6.331 2704784 2704704.000 609.10 bb 101 t010125-101 250 ppb FC Mix 00002-104-10 6.046 1582417 1582416.750 298.31 bb 19 102 t010125-102 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.448 180976 100975.719 0.00 bb 103 t010125-103 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.051 126826 126826.359 0.00 bb 104 t010125-104 lox EOO-1311-0056 6.541 2766212 2766211.500 603.90 bb 105 t010125-105 lox E00-1311-0057 6.493 2534908 2534900.000 540.32 bb 106 t010125-106 lox EOO-1311-0058 6.040 3035705 3035785.000 680.00 bb 107 t010125~10.7 lox E00-1311-0059 6.348 2548403 2540402.500 543.97 bb 108 t010125-108 lox EOO-1311-0060 6.071 2013637 2013637.000 617.20 bb 109 t010125-109 250 ppb FC Mix 00002-104-10 6.460 1387797 1387796.500 252.15 bb 1 110 t010125~110 MeOH Blank, TN-A-4740. Aliq. 12/04/00 6.024 125005 125004.563 0.00 bb 111 t010125-111 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.552 174696 174695.734 0.00 bb 112 t010125-112 lox E00-1311-0061 6.322 2567028 2567027.750 549.02 bb 113 t010125-113 lox EOO-1311-0062 6.071 2770300 2770308.000 605.04 bb 114 t010125-114 lox EOO-1311-0063 6.507 2493961 24 93960.500 529.29 bb 115 t010125-115 lox E00-1311-0064 6.061 2801319 2801310.750 613.74 bb 116 t010125-116 lox EOO-1311-0065 6.535 2516190 2516190.000 535.27 bb 117 t010125-117 250 ppb FC Mix 00002-104-10 6.503 1357075 1357075.125 244.95 bb -2 110 to10125 118 MeOH Blank. TN-A-4740, Alia. 12/04/00 6.050 103976 103975.977 0.00 bb MeOH Blank; TN-A-4740; Aliq. 12/04/00 6.520 175921 175920.563 0.00 bb lox EOO-1311-0066 6.385 2561146 2561146.000 547.43 bb lox E00-1311-0067 6.033 1697580 1697500.000 326.10 bb lox E00-1311-0060 6.160 2221049 222104 0.750 457.52 bb lox EOO-1311-0069 6.050 2703500 2703579.500 586.47 bb lox E00-1311-0070 6.436 2045503 2045503.000 412.39 bb 125 t0101251125 250 ppb FC Mix 00002-104-10 6.157 1373129 1373120.625 248.71 bb -1 126 t010125-126 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.060 131690 131689.594 0.00 bb 127 t010125-127 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.662 209049 2~ 09.0~ 4 R. .59.4 ~ ~ .0..00 bb 128 t010125-120 lox EOO-1311-0071 6.026 2281647 2281647.250 473.07 bb , 129 t010125-129 130 t010125-130 lox E00-1311-0072 lox 600-1311-0073 6.543 6.156 1994915 1994914.500 2107328 2107328.000 399.60 bb 420.08 bb 131 t010125-131 lox BOO-1311-0074 6.073 2275225 2275224.500 411.39 bb 132 t010125-132 10x EOO-1311-0075 6.263 2070615 2070675.125 418.75 bb 133 to10125 133 250 ppb PC Mix 00002-104-10 6.135 1410906 1410906.000 259.46 bb 4 134 i0101251134 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.576 189572 189572.422 0.00 bb 135 t010125-135 136 t010125 136 MeOH Blank, TN-A-4740. Aliq. 12/04/00 HeOH Blank, TN-A-4740, A l i q . 12/04/00 6.070 6.581 77009 77009.250 188258 188257.766 0.00 bb 0.00 bb 137 t0101251137 0 ppb FC Mix 00002-104-01 6.095 177973 177972.719 0.00 bb 138 t010125-138 139 t010125-139 2.5 ppb FC Mix 00002-104-02 5 ppb FC nix 00002-104-03 6.450 6.101 191704 191004 191704.063 191884.234 0.00 bbX 0.00 bbX -100 -100 140 to10125 140 10 ppb FC Mix 00002-104-04 6.326 235222 235222.219 0.00 bbX -100 25 ppb FC Mix 00002-104-05 6.096 308328 300328.469 11.98 bbX -52 40 ppb FC Mix 00002-104-06 6.312 387661 307661.406 20.81 bb -28 50 ppb FC Mix 00002-104-07 6.240 479692 479691.563 48.49 bb -3 75 ppb FC Mix 00002-101-08 6.530 578191 578191.375 69.74 bb -7 100 ppb FC Mix 00002-104-09 6.109 700577 700576.875 114.00 bb 14 46 t010125- 250 ppb FC Mix 00002-104-10 6.424 1300449 1380448.075 250.42 bb 0 147 t010125-147 500 ppb FC Mix 00002-104-11 6.039 2466444 2466444.250 521.91 MM 4 a 140 t010125-140 750 ppb FC Mix 00002-104-12 6.528 3197643 3197642.500 728.76 bb -3 149 t010125-149 1000 ppb FC Mix 00002-104-13 6.040 4125592 4125591.750 1034.37 bb 3 150 t010125-150 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.556 205462 205461.656 0.00 bb 151 t010125-151 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.674 71219 71219.266 0.00 bb Quantitated and Printed by on 31 Jan 01 Study * E00-1311 3M Environmental Laboratory Page 491 of 703 BACK TO MAIN huntify C c q a m d Sumary bport PFOS Msorb/Desorb Study, L C M Inrt-t: W k e r (LA0521 sa@e List: c:\bUISSLW\Dt.atUr.m\S.qlsDB\t010125 - Last modified: Tim Jan 25 10-45:39 2001 Method: C:\acasSLW\D.oatur.prto~ulo0\PFOS THPFOS Last uedifisd: Wed Jan 31 07:38:20 2001 Job Code: Printed: Wed Jan 31 07:42:18 2001 C&md 2: I.S. (TW-PPOS) (4271 a N1 to10125 001 7 t010125-007 8 t0101251008 9 t0o10112255-000099 10 t010125-010 11 t010125-011 12 t010125-012 13 t010125-013 I4 t010125-014 15 t010125-I015 16 to10125 016 17 t010125-017 23 t010125I023 24 t010125-024 25 t010125-025 26 t010125-026 27 tO10125-027 28 t010125-028 29 t010125-029 30 t010125-030 31 t010125-031 32 t010125-032 33 t010125-033 34 t010125-034 35 tO10125-035 36 t010125-036 37 t010125-037 38 t010125-038 39 t010125-039 40 t010125-040 41 t010125-041 42 t010125-042 13 t010125-043 44 t010125-044 45 t010125-045 46 t010125-096 47 t010125-047 48 t010125-048 49 tO10125-049 50 t010125-050 51 t010125-051 52 tO10125-052 53 t010125-053 54 t010125-054 55 t010125-055 56 tO10125-056 57 t010125-057 58 t010125-058 59 t010125-059 60 t010125-060 61 t010125-061 62 tO10125-062 63 t010125-063 61 t010125-064 65 tO10125-065 66 t010125-066 67 t010125-067 68 t010125-068 69 t010125-069 70 t010125-070 71 to10125 071 72 t010125-072 79 t010125y079 80 t010125-080 81 t010125-081 82 t010125-082 Samplelist Text MeOH Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-1740. Aliq. 1000 ppb FC Mix 00002-104-13 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4710, Aliq. 0 ppb FC Mix 00002-104-01 2.5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 25 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-101-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb FC Mix 00002-101-13 MeOH Blank. TN-A-4740, Aliq. MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-4740. Aliq. 0 ppb FC Mix 00002-104-01 2.5 ppb IC Mix 00002-101-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-01 25 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-101-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb F C Mix 00002-104-13 MeOH Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-4740, Aliq. lox EOO-1311-0016 lox 800-1311-0017 12/01/00 12/04/00 1210000 12/04/00 12/04/00 12/01/00 12/04/00 12/04/00 12/04/00 12/04100 12/04/00 MeOH Blank. TN-A-4740, Aliu. MeOH Blank, TN-A-4740. Aliq. lox 800-1311-0021 lox E00-1311-0022 lox E00-1311-0023 lox E00-1311-0024 10x EOO-1311-0025 250 ppb FC Mix 00002-104-10 HeOa Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-1740, Aliq. lox BOO-1311-0026 lox EOO-1311-0021 lox EOO-1311-0028 lox EOO-1311-0029 lox E00-1311-0030 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740. Aliq. lox EOO-1311-0031 lox EOO-1311-0032 lox EOO-1311-0033 lox EOO-1311-0034 10n 500-1311-0035 250 ppb FC Mix 00002-104-10 MeOM Blank, TN-A-1740. Aliq. MeOH Blank, TN-A-4740, Aliq. lox E00-1311-0036 lox EOO-1311-0037 lox EOO-1311-0038 lox E00-1311-0039 lox E00-1311-0040 250 ppb FC Mix 00002-104-10 MeOM Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-4740, Aliq. 108 E00-1311-0041 lox E00-1311-0042 lox E00-1311-0043 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 12/04/00 RT 6.209 7.132 6.071 6.325 6.048 6.012 6.061 6.231 6.096 6.159 6.063 6.135 6.328 6.026 6.230 6.073 6.400 6.193 6.217 6.046 6.410 6.120 6.292 6.086 6.145 6.061 6.109 6.061 6.206 6.062 6.035 6.280 5.990 6.399 6.362 5.990 6.000 6.169 6.025 6.380 6.108 6.072 6:110 6.157 5.952 5.990 6.265 6.047 6.121 6.048 6.179 6.035 6.145 6.084 6.082 6.012 5.978 6.109 6.144 5.966 5.977 6.207 5.963 6.204 5.975 6.303 6.000 6.048 6.050 5.952 6.133 6.037 6.085 5.987 6.157 6.037 6.049 6.206 ..rA 5373 11729 70045 75600 2522 519 126675 117847 118679 112125 109100 107613 99745 102506 96942 82354 73659 62381 46986 1691 511 1019 503 118013 106158 109910 105112 101461 99250 91592 96662 84852 76758 76238 70176 53632 0 1428 603 118872 112733 110966 114288 109119 86705 1081 0 124529 122964 117237 117726 116042 92444 2050 712 113810 119108 252894 186886 185019 92634 1567 0 108803 119501 113016 119626 107200 103229 1198 1922 116019 108681 119125 108263 115063 89852 607 0 116893 106721 122748 Rsspponre 5372.521 11728.611 70045.336 75600.156 2522.483 519.195 126675.086 117846.625 118679.031 112125.469 109100.398 107613.313 99744.711 102505.703 96911.961 82353.539 73659.094 62380.656 46985.852 1690.943 514.222 1019.106 503.462 118013.289 106157.750 109909.656 105111.656 101460.953 99250.172 97591.688 96662.000 84852.133 76757.734 76237.547 70176.188 53631.707 1127.568 603.102 118872.305 112733.109 110965.875 114288.406 109118.742 86705.156 1080.741 121529.161 122964.258 117236.961 117725.922 116041.797 92414.066 2050.362 712.336 113810.109 119407.734 252894.094 186885.938 185019.078 92633.828 1567.286 108802.805 ~ ~~ 119501.391 113015.695 119626.469 107199.844 103228.611 1198.204 1922.064 116048.961 108683.570 119124.578 108263.000 115063.258 89851.828 606.992 116893.242 106720.656 122748.484 ppb 14.48 31.62 188.83 203.80 6.80 1.40 341.49 317.69 319.93 302.27 294.11 290.10 268.89 276.33 261.33 222.01 198.57 168.16 126.66 4.56 1.39 2.75 1.36 318.14 286.18 296.29 283.36 273.52 267.56 263.09 260.58 228.74 206.92 205.52 189.18 144.58 Flags bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb W bb bb bb bb bb bb bb bb bb bb bb bb bb bb bb *Dm -24 -18 37 27 28 21 18 16 8 11 5 -11 -21 -33 -49 27 14 19 13 9 7 5 4 -9 -17 -18 -24 -42 od t-C 3 . 8 5 bb 1.63 bb 320.45 bb 28 303.90 bb 22 299.14 bb 20 308.10 bb 23 291.16 bb 18 233.74 bb -7 2 . 9 1 bb 335.70 bb 34 331.49 bb 33 316.05 bb 26 317.36 bb 27 312.82 bb 25 249.21 bb -0 5 . 5 3 bb 1.92 bb 306.81 bb 23 321.90 bb 29 681.75 bb 173 5 0 3 . 8 0 bb 102 498.77 bb 100 249.72 bb -0 4.23 bb 293.31 bb 17 322.15 bb 29 301.67 bb 22 322.19 bb 29 288.99 bb 16 278.28 bb 11 3 . 2 3 bb 5.18 bb 312.84 bb 25 292.99 bb 11 321.13 bb 28 291.85 bb 17 310.19 bb 24 242.22 bb -3 1.61 bb 315.12 bb 26 287.70 bb 15 3 3 0 . 9 0 bb 32 Quantitated and Printed by cw2 on 31 Jan 01 study E00-1311 3M Environmental Laboratory Page 3 BACK TO MAIN Quantify conpound S u m m a q Paport P W S Adsorb/msorb Study, L C M Inst-t: Tuoker (LAO521 S a z ~ l sList: last mdificd: Method: last a f i e d : Job Code: C:\MnsSLYNX\Daoatur.PRO\SamplsDB\t010125 - Thu Jan 25 10:45:39 2001 C : \ M n s S L ~ \ D ~ . t u r . P R O ~ ~ B \ P P O S THPPOS Wed Jan 31 07:38:20 2001 Printad: Wed Jan 31 07:42:1E 2001 & C 2: 1,s. (RI-PFOS)(427) E.l- ~ RT mu Ppb Flags WDOVod comment 83 t010125-003 lox EOO-1311-0014 6.013 105324 10532i.10; 283.93 bb 14 84 t010125-084 l o x EOO-1311-0045 6.072 116901 116900.750 315.11 bb 26 85 t010125-OB5 250 ppb FC Mix 00002-104-10 5.999 83072 83072.023 223.94 bb -10 86 to10125 086 MeOH Blank, TN-A-4710. Aliq. 12/04/00 0 87 t0101251087 MeOH Blank, TN-A-1140, Aliq. 12/04/00 5.976 1668 1668.148 4.50 bb 88 t010125-008 lox 800-1311-0046 6.253 106186 106186.273 286.26 bb 15 89 t010125-089 lox EOO-1311-0047 6.070 103150 103150.477 278.07 bb ~~ 11 90 t010125-090 10% EOO-1311-0048 6.070 112295 112295.242 ~ ~ ~ 302.72 bb 21 91 t010125-091 6.049 96921 96921.016 261.28 bb 5 92 t010125-092 6.038 102624 102624.383 276.65 bb 11 93 t010125-093 5.986 71867 71867.242 193.74 bb -23 94 t010125-094 12/04/00 0 95 t010125-095 MeOH Blank; TN-A-4740. Aliq. 12/04/00 5.975 1056 1055.913 2 . 8 5 bb 96 t010125-096 lox EOO-1311-0051 6.291 68517 60546.523 184.79 bb -26 97 t010125-097 10% E00-1311-0052 6.039 62273 62273.418 167.88 bb -33 98 t010125-098 10% E00-1311-0053 5.999 68098 68097.969 183.58 bb -27 99 t010125-099 lox EOO-1311-0054 6.120 53704 53704.141 144.77 bb -42 100 t010125-100 10% EOO-1311-0055 6.271 104842 104842.320 282.63 bb 13 101 t010125-101 250 ppb FC Mix 00002-101-10 5.998 81701 81701.250 220.25 bb -12 102 t010125-102 MeOM Blank, TN-A-4740, Aliq. 12/04/00 6.376 695 695.141 1.87 bb 103 to10125 103 MeOH Blank, TN-A-4740, Aliq. 12/04/00 5.990 2071 2071.462 5.58 bb 10% EOO-1311-0056 6.361 123699 123699.145 333.47 bb 33 lox EOO-1311-0057 6.168 114165 114164.625 307.76 bb 23 108 EOO-1311-0058 5.988 101409 101408.508 273.38 bb 9 10% EOO-1311-0059 6.071 109000 109000.341 293.84 bb 18 10% EOO-1311-0060 6.011 98029 98029.047 264.27 bb 6 ! 109 t010125I109 250 ppb FC Mix 00002-101-10 6.372 81428 81428.047 219.51 bb -12 110 to10125 110 MeOH Blank, TN-A-4710, Aliq. 12/01/00 5.952 1436 1435.502 3.87 bb MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 lox EOO-1311-0061 6.262 99050 99049.680 267.02 bb 7 10% 600-1311-0062 6.023 96206 96205.742 259.35 bb 4 lox BOO-1311-0063 6.170 112143 112143.391 302.31 bb 21 10% EOO-1311-0064 6.001 97979 97978.953 264.13 bb 6 10% 600-1311-0065 6.245 115602 115601.617 311.64 bb 25 250 ppb FC Mix 00002-104-10 6,203 94374 94374.211 254.41 bb 2 MeOH Blank, TN-A-4740, Aliq. 12/04/00 5.986 1721 1720.759 4.64 bb MeOH Blank, TN-A-4740, Aliq. 12/01/00 6,383 530 530.416 1.43 M 120 t0101251120 10% EOO-1311-0066 6.313 102207 102207.177 275.53 bb 10 121 t010125-121 10% EOO-1311-0067 5.985 207435 207135.231 559.20 bb 124 122 tO10125-122 10% EOO-1311-0068 5.999 209218 209218.359 564.01 bb 126 123 t010125-123 10% EOO-1311-0069 5.966 222164 222163.859 598.91 bb 140 124 t010125-124 10% EOO-1311-0070 6.351 131563 131562.906 354.67 bb 42 125 to10125 125 250 ppb FC Mix 00002-104-10 6.000 88381 88380.602 238.26 bb -5 126 t0101251126 MeOM Blank, TN-A-4740, Aliq. 12/04/00 6.000 1806 1806.316 1.87 bb 127 to10125 127 MeOH Blank, TN-A-4740. Aliq. 12/04/00 6.084 1088 1088.456 2.93 ~ b~b - 10% EOO-1311-0071 5.965 159566 159565.938 430.16 bb 72 lox EOO-1311-0072 6.267 128245 128214.859 345.72 bb 38 10% E00-1311-0073 5.999 173139 173139.297 466.75 bb 87 10% EOO-1311-0074 5.977 176159 176158.922 471.89 bb 90 10% E00-1311-0075 6.203 141018 141078.141 380.32 bb 52 133 t0101251133 250 ppb FC Mix 00002-104-10 6.086 77577 77576.617 209.13 bb -16 134 t010125-131 MeOH Blank, TN-A-4700, Aliq. 12/01/00 0 135 t010125-135 MeOH Blank, TN-A-4740. Aliq. 12/04/00 5.962 1240 1240.172 3.34 bb 136 t010125-136 HsOH Blank, TN-A-4740, Aliq. 12/04/00 0 137 t010125-137 0 ppb FC Mix 00002-104-01 5.975 118927 118927.320 320.60 bb 28 138 tO10125-138 2.5 ppb PC Mix 00002-104-02 6.354 107193 107192.914 288.97 bb 16 139 t010125-139 5 ppb FC Mix 00002-104-03 6.121 110172 110171.938 297.00 bb 19 140 tO10125-140 10 ppb FC Mix 00002-104-01 6.085 113811 113810.570 306.81 bb 23 141 tO10125-141 25 ppb FC Mix 00002-104-05 6.048 115567 115567.383 311.54 bb 25 142 t010125-142 40 ppb FC Mix 00002-104-06 6.108 110021 110021.266 296.59 bb 19 143 t010125-143 50 ppb FC nix 00002-104-07 6.192 97363 97363.398 262.47 bb 5 144 tO10125-144 75 ppb FC Mix 00002-104-08 6.240 111681 111684.203 301.08 bb 20 145 t010125-145 100 ppb FC Mix 00002-104-09 6.061 94649 94649.477 255.15 bb 2 146 t010125-146 250 ppb FC Mix 00002-104-10 6.159 90408 90107.883 213.72 bb -3 147 t010125-147 500 ppb FC Mix 00002-104-11 5.979 67716 67715.648 182.55 bb -27 148 t010125-148 750 ppb FC Mix 00002-104-12 6.288 73108 73708.352 198.70 bb -21 149 t010125-119 1000 ppb FC Mix 00002-104-13 5.979 55605 55605.203 149.90 bb -40 150 t010125-150 MeOH Blank, TN-A-4740, Aliq. 12/04/00 5.953 578 578.391 1.56 bb 151 t010125-151 MeOH Blank, TN-A-4740, Aliq. 12/04/00 5.988 1101 1101.073 2.97 bb Quantitated and Printed by (Mc on 31 Jan 01 Study b E00-1311 3M Environmental Laboratory ch?c ( pI i C l Page 493 of 703 BACK TO MAIN Quantify C-und Sumnary Report PFOS AdsorblDssorb EOO-1311 comp.mnd 1: PFOS ( 4 9 9 > 9 9 ) , fYnE 1 I; N1 s00120~001 2 s00120~002 ntudY M samplelist Text E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA me Analyte Analyte S t d Con= RT 7.141 7.117 Area 259 30961 llpb %L%vFlaps Wd co 0.00 bb bbl 3 ~00120-003 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA Analyte 7.118 30002 4 ~00120-004 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 Analyte 7.130 213 5 ~00120-005 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 Analyte 7.118 148 6 ~00120-006 EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 MLA Analyte 7.119 691 7 ~00120-007 E00-1311 2.47ppb PFOS 00002-86-02. Aliq. 11-03-00 MLA Analyte 7.117 1222 8 s00120~008 E00-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA Analyte 7.131 1468 9 ~00120-009 E00-1311 9.9 ppb PFOS 00002-86-04, Aliq. 11-03-00 MLA Analyte 7.131 1566 0.00 -100 bb 10 ~ 0 0 1 2 0 ~ 0 1 0 E00-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA Analyte 7.118 2745 17.72 -28 bb 11 s0012O~Oll 12 s00120~012 13 ~00120-013 14 ~00120-014 E00-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA E00-1311 74.26 ppb PFOS 00002-86-08. Aliq. 11-03-00 MLA E00-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA Analyte Ana1yte Analyte Analyte 7.118 7.119 7.117 7.107 3508 3899 5352 6795 34.55 (3.26 76.26 110.02 -13 bb -13 bb 3 bb 11 bb 15 .500120~015 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA Analyte 7.105 12561 257.10 4 bb 16 ~00120-016 E00-1311 495.9 ppb PFOS 00002-86-12 Alia. 11-03-00 MLA Analyte 7.106 19155 460.85 -7 bb 17 ~00120-017 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA Ana1yte 7.107 28597 974.59 -2 bb 18 s00120~018 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 Ana1yte 7.119 144 0.00 bb 19 ~00120-019 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16100 Blank 7.118 123 0.00 bb 20 *00120~020 E00-1311 MeOH Blank, TN-A-4715, Aliq, 11/16/00 Blank 7.129 124 0.00 bb 21 s00120~021 E00-1311 0 ppb PFOS 00002-86-01. Aliq. 11-03-00 MLA Analyte 7.117 604 0.00 bb 22 s00120~022 E00-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA Standard 2.47 7.106 1095 0.00 -100 bbX 2 3 ~00120-023 EOO-1311 4.95 ppb PFOS 00002-86-03, Alia. 11-03-00 MLA Standard 4.95 7.118 1354 0.00 -100 bbX 2 4 900120-024 E00-1311 9.9 ppb PFOS 00002-86-04, Alia. 11-03-00 MLA Standard 9.90 7.106 1454 0.00 -100 bbX 2 5 ~00120-025 E00-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA Standard 24.75 7.117 2683 16.35 -34 b b 26 ~00120-026 E00-1311 39.6 ppb PFOS 00002-86-06. Aliq. 11-03-00 MLA Standard 39.60 7.107 3390 31.91 -19 bb 27 ~00120-027 E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA Standard 49.50 7.106 3889 43.05 -13 bb 28 s00120~028 E00-1311 74.26 ppb PFOS 00002-86-08. Aliq. 11-03-00 MLA Standard 74.26 7.106 5282 14.65 1 bb 29 ~00120-029 EOO-1311 99.2 ppb PFOS 00002-86-09. Aliq. 11-03-00 MLA Standard 99.20 7.106 6720 108.24 9 bb 30 ~00120-030 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 M L A Standard 247.90 7.106 12653 259.63 5 bb 31 ~00120-031 E00-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA Standard 495.90 7.106 19151 460.70 -7 bb 3 2 ~00120-032 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 nLA Standard 991.78 7.107 28429 955.43 4 bb 3 3 ~00120-033 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 Analyte 7.130 207 0.00 bb 34 ~00120-034 E00-1311 MeOH Blaqk, TN-A-4715, Aliq. 11/16/00 Analyte 7.128 133 0.00 bb 3 5 ~00120-035 E00-1311 E00-1311-1001 Ohr Analyte 7.131 110 0.00 bb 36 ~00120-036 E00-1311 EOO-1311-1002 Ohr Analyte 7.142 161 0.00 bb 37 ~00120-037 EOO-1311 B00-1311-1003 Ohr Ana1yte 7.132 119 0.00 bb 38 ~00120-038 E00-1311 EOO-1311-1004 Ohr Analyte 7.133 2652 15.68 bb 39 ~00120-039 EOO-1311 EOO-1311-1005 Ohr Analyte 7.138 2598 14.50 bb 4 0 ~00120-040 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA QC 247.90 7.131 12431 253.52 2 bb 41 ~00120-041 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 Analyte 7.143 119 0.00 bb 42 ~00120-042 E00-1311 MeOH Blank. TN-A-4715. Alio. 11/16/00 Analyte 7.144 90 0.00 bb 43 s00120_043 E00-1311 EOO-l~il-lO06 O h r - . ~~ ma1yte 7.131 2578 14.07 bb 44 S00120-044 E00-1311 E00-1311-1007 Ohr Analyte 7.143 19884 486.97 bb 45 ~00120~045 Analyte 7.142 20845 523.02 bb 46 ~00120-046 Analyte 7.133 21384 544.09 bb 47 ~00120-047 Analyte 7.130 3116 25.86 bb 48 ~00120~048 QC 247.90 7.130 12536 256.40 3 bb 49 ~ 0 0 1 2 0 ~ 0 4 9 Analyte 7.142 100 0.00 bb I 50 600120~050 Ana1yte 7.142 e1 0.00 bb 51 ~00120-051 EOO-1311 E00-1311-1011 24 hour, OmgiL, S1, C - l Analyte 7.141 1084 0.00 bb 52 ~00120-052 E00-1311 E00-1311-1012 24 hour. OmgIL. S1. C-l Analyte 7.143 540 0.00 bb 53 ~00120-053 E00-1311 E00-1311-1012 2 4 hour, OmglL, SI. C-1, MS Analyte 7.131 11095 217.61 bb 54 ~00120-054 E00-1311 E00-1311-1013 24 hour, O.lOmg/L, S1, C-l Ana1yte 7.143 2562 13.72 bb 55 s00120~055 E00-1311 E00-1311-1014 2 4 hour, O.lOmglL, S1. c-1 Analyte 7.142 2834 19.66 bb 56 ~00120-056 E00-1311 247.9 ppb PFOS 00002-86-10. Allq. 11-03-00 MLA Q 247.90 7.131 12793 263.50 6 bb 57 ~00120-057 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 Analyte 7.130 133 0.00 hb 58 ~ooi20_058 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 59 900120-059 E00-1311 EOO-l3ll-1015 * 4 hour, 0 10mg,L, 51. c-1 Analyte illa1yte 7.138 7.141 143 0.00 bD 2667 16.01 bb 60 ~00120-060 E00-1311 E00-1311-1015 24 hour, O.lOmg/L, S1. C-1, MS Ana1yte 7,141 12420 253.23 bD 61 ~00120-061 E00-1311 E00-1311-1016 2 4 hour, l.Oma/L. S1. C-l Analyte 7.144 19190 462.08 bb 62 ~00120-062 E00-1311 E00-1311-1017 24 hour. 1 . 0 G l L . S1, C-l Analyte 7.142 19557 475.12 bb 63 ~00120-063 E00-1311 E00-1311-1018 2 4 hour. l.Omg/L, S1, C - l Analyte 7.140 20389 505.67 bb 64 ~00120-064 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA Q 247.90 7.133 12905 266.61 bb 65 ~ 0 0 1 2 0 ~ 0 6 5 EOO-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 Analyte 7.132 160 0.00 bb 66 ~00120-066 E00-1311 MeOH Blank. TN-A-4715. Alla. 11/16/00 Analyte 7.142 89 0.00 bb 67 ~00120-067 EOO-1311 E00-1311-1018 2 4 hour. l.O&/L, S1. C-1 MS Analyte 7.131 25186 719.03 hb 68 sOO120-068 E00-1311 E00-1311-1010 2 4 hour, OmglL, S2. C-l AnLna1yte 7.142 3 0 3 3 24.03 bb 69 ~00120-069 E00-1311 E00-1311-1011 2 4 hour, OmgIL. SZ, C - l Analyte 7.141 1052 0.00 bb 70 ~00120-070 E00-1311 E00-1311-1012 2 4 hour, OmgIL. SZ. C-1 Analyte 7.142 438 0.00 bb 71 ~00120-071 E00-1311 E00-1311-1012 2 4 hour, OmglL. SZ, C-1, MS Analyte 7.141 12229 248.01 bb 72 ~00120-072 EOO-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA QC 247.90 7.127 13639 287.25 I bb 73 ~00120-073 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Analyte 7.154 106 0.00 bb 74 ~ 0 0 1 2 0 ~ 0 7 4 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Analyte 7.141 91 0.00 bb 75 ~00120-075 EOO-1311 E00-1311-1013 2 4 hour. 0.lOmglL. S2. C-1 Analyte 7.143 1425 0.00 bb 76 ~00120-076 EOO-1311 EOO-l3ll-lOl4 24 hour, O.lOr&/L. 52,. C-1 Analyte 7.130 1186 0.00 bb 77 s00120_077 E00-1311 E00-1311-1015 2 4 hour, 0.lOmglL. S2. C-l Analyte 7.131 1470 0.00 bb 78 ~00120-078 E00-1311 E00-1311-1015 2 4 hour, O.lOmg/L. S2. C-1. MS Analyte 7.129 12466 254.50 bb 79 ~00120-079 E~ 00~ -1-3~11 E00-1~ 311.-.10.16 2 4 hour. l.Om/L. SZ. C-1 Analyte 7.133 6830 110.87 bb 80 .s00120~080 E00-1311 247.9 ppb PFOs~OOO62-i6-lO.~Aliq.11-03-00 MLA QC 247.90 7.119 13880 294.14 19 bb 81 ~00120-081 EOO-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 Analyte 7.140 e1 0.00 bb 82 s00120~082 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Analyte 7.128 79 0.00 bb 83 SOO120-083 E00-1311 E00-1311-1017 2 4 hour. l.Omg/L, S2, C-1 Analyte 7.130 7145 118.37 bb 8 4 ~00120-084 E00-1311 E00-1311-1018 24 hour, l.Omg/L. 52. C-1 Analyte 7.132 7928 137.30 bb e5 sooi20-085 E00-1311 E00-1311-1018 2 4 hour, l.Omg/L, S2, C-1. MS Analyte 7.130 15596 344.75 bb 86 s00120_086 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Analyte 7.127 109 0.00 bb 87 s00120_087 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 Analyte 7.142 81 0.00 bb 88 SOOIZO-088 E00-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 MLA Analyte 7.120 625 0.00 bb 89 ~ooizo-089 E00-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA Standard 2.47 7.115 1061 0.00 -100 bbX SOUP 020199: wantitared and printad by CDc on 01/11/01 3M Environmental Laboratory Page 494 of 703 BACK TO MAIN Quantify compound SUmMrY neD0l-t PPOS M s o r b l m s o r b ~ 0 0 - 1 3 1 1 6-1- List: Last d i f i e d : Method: Last modified: Job COde: C:\Hn~~l~\~OUp~20199.D~O\S~lEDB\~00112Oa Tbu Jan 11 0 1 : 0 0 : 0 6 2001 C:\nasslynx\.ouD020199.pro\nathDB\.001120 Wad Nov 22 06:41:05 2000 Printad: Thu J.n 11 0 7 : 0 3 : 2 1 2001 90 ~00120-090 91 ~00120-091 92 800120~092 9 3 s00120I093 94 ~00120-094 9s S O O I ~ O - 0 9 5 96 ~00120-096 97 sOO120-097 98 so0120 098 99 sOOl2OI099 100 ~00120-100 101 ~00120-101 102 ~00120-102 E00-1311 4.95 ppb PFOS 00002-86-03. Aliq. 11-03-00 MLA E00-1311 9.9 ppb PFOS 00002-86-04, Aliq. 11-03-00 MLA EOO-1311 24.75 DDb PFOS 00002-86-05. Alia. 11-03-00 MLA E00-1311 39.6 pi& PFOS 00002-86-06. Aliq: 11-03-00 MLA E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA EOO-1311 74.26-ppb PFOS 00002-86-08. Aiiq. 11-03-00 MLA EOO-1311 99.2 ppb PFOS 00002-86-09. Aliq. 11-03-00 EILA E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA E00-1311 495.9 DDb PFOS 00002-86-12 Alia. 11-03- -00 MLA ~~~ ~~ EOO-1311 991.78'ppb PFOS 00002-86-13. aliq. 11-03-00 M U E00-1311 MeOX Blank, TN-A-4715, Aliq. 11/16/00 600-1311 MeOX Blank. 'I?-A-4115. Aliq. 11/16/00 BOO-1311 HeOn Blank. TN-A-4715. Aliq. 11/16/00 e**. 2 Standard Standard Standard Std Con0 4.95 9.90 24.75 Standard 39.60 Standard 49.50 Standard Standard 14.26 99.20 Standard 247.90 St~ and~ ard ~.49.5~.90 Standard 991.78 Analyte Analyte Analyte RT 7.118 7.116 7.118 7.111 7.115 7.117 7.115 7.129 7 . 1- 1 '. 1 _ 7.118 7.125 7.126 7.142 1382 1491 3542 4013 5604 6903 13256 1- 9- R-o-4_ 29264 137 87 92 0.00 -100 bbX 0.00 -100 bbX 35.30 45.81 ~ ~~ 82.08 112.60 276.43 d- -a_d. "nI s 1080.65 0.00 0.00 0.00 -11 bb -7 b_h_ 11 bb 14 bb -12 bb _I) LL L" 9 bb bb bb bb SOUP 020199: m a n t i t a t 4 and Printed by Mc On 01111101 3M Environmental Laboratory Page 495 of 703 BACK TO MAIN Ouantify CampOund sullrrmry Report PFOS MsorblDssorb E00-1311 ___-__ __ Slmpl. List: Laet mdified: Method: Last mdified: Job code: C:\MaS~lynu\~ouD02019~.D~\S~~~DB\.001120~ Thu Jan 11 07:00:06 2001 C:\Ma~s~~\~OUDO20199.D~O\M~thDB\~001120 Wad Nov 22 06:41:05 2000 Printed: Thu Jan 11 07:03:22 2001 #N m study M S-1eli.t Text 1 s00120~001 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 2 r00120~002 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 3 so012 E00-1311 991.78 ppb PFOS 00002-86-13. aliq. 11-03-00 MLA E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 0 ppb PFOS 00002-86-01. Aliq. 11-03-00 MLA EOO-1311 2.47ppb PFOS 00002-86-02. Aliq. 11-03-00 MLA 8 P00120I008 E00-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA 9 s00120~009 E00-1311 9.9 ppb PFOS 00002-86-04, Aliq. 11-03-00 MLA 10 s00120~010 E00-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 11 s00120~011 E00-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA 12 P00120~012 E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA 13 ~00120-013 E00-1311 74.26 ppb PPOS 00002-86-08. Aliq. 11-03-00 M U 14 ~00120-014 E00-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA 15 ~00120-015 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 16 ~00120-016 E00-1311 4 9 5 . 9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 17 ~00120-017 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 18 900120~018 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 19 ~00120-019 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 20 s00120~020 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 21 s00120~021 E00-1311 0 ppb PFOS 00002-86-01. Aliq. 11-03-00 MLA 22 s00120~022 E00-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA 23 ~00120-023 EOO-1311 4.95 ppb PPOS 00002-86-03. Aliq. 11-03-00 MLA 2 4 ~00120-024 E00-1311 9.9 ppb PFOS 00002-86-04. Aliq. 11-03-00 MLA 25 ~00120-025 EOO-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 26 ~00120-026 EOO-1311 39.6 ppb PFOS 00002-86-06. Aliq. 11-03-00 MLA 21 ~00120-027 E00-1311 4 9 . 5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA 28 POO120~028 E00-1311 74.26 ppb PFOS 00002-86-08. Aliq. 11-03-00 MLA 29 ~00120-029 EOO-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA 30 ~00120-030 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 31 ~00120-031 E00-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 32 ~00120-032 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 33 ~00120-033 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 34 500120-034 E00-1311 MeOH Blank, TM-A-4715, Aliq. 11/16/00 35 ~00120-035 E00-1311 E00-1311-1001 Ohr 36 ~00120-036 E00-1311 E00-1311-1002 Ohr 37 S00120-037 E00-1311 E00-1311-1003 Ohr 38 ~00120-038 E00-1311 E00-1311-1004 Ohr 39 S00120-039 E00-1311 E00-1311-1005 Ohr 40 ~00120-040 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 41 ~00120-041 E00-1311 MeOM Blank. TN-A-4715. Aliq. 11/16/00 42 ~00120-042 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 43 ~00120-043 E00-1311 E00-1311-1006 Ohr 44 ~00120-044 E00-1311 E00-1311-1007 Ohr 45 ~00120-045 E00-1311 E00-1311-1008 Ohr 46 ~00120-046 E00-1311 E00-1311-1009 Ohr 47 ~00120-047 EOO-1311 E00-1311-1010 24 hour, OmglL, S1. C-l 48 ~00120-048 EO0 - 1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 4 9 ~00120-049 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 50 ~00120-050 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 51 ~ 0 0 1 2 0 ~ 0 5 1 EOO-1311 E00-1311-1011 24 hour, OmgIL, S1. c-l 52 SOO120-052 E00-1311 EOO-1311-1012 2 4 hour, OmglL. S1, C-l 53 ~00120-053 E00-1311 E00-1311-1012 24 hour. OmglL, S1, C-1, MS 54 ~00120-054 E00-1311 E00-1311-1013 2 4 hour, 0.10mglL. S1, C-1 55 ~00120-055 EOO-1311 E00-1311-1011 2 4 hour, 0.lOmglL. S1, C-1 56 ~00120-056 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 57 ~00120-057 EOO-1311 58 ~00120-058 E00-1311 59 s00120~059 E00-13ll 60 ~00120-060 EOO-1311 61 800120-061 E00-1311 62 ~00120-062 800-1311 63 ~00120-063 BOO-1311 64 ~00120-064 E00-1311 65 ~00120-065 BOO-1311 66 ~00120-066 E00-1311 67 ~00120-067 E00-1311 68 ~00120-068 E00-1311 69 ~00120-069 E00-1311 70 ~ 0 0 1 2 0 ~ 0 7 0 E00-1311 E00-1311-1012 24 hour, O&/L, SZ. C-1 71 ~00120-071 E00-1311 E00-1311-1012 2 4 hour. O G / L . 52. C-1, MS 72 ~00120-072 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 73 SOO120-073 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 74 SOO120-074 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 75 S00120-075 76 ~00120-076 77 ~00120-077 E00-1311 E00-1311-1013 24 hour. 0.lOmolL. 52 C - l E00-1311 EOO-1311-1014 24 hour: O.iO&/L: 52: C-i E00-1311 EOO-1311-1015 2 4 hour. O.lO$/L, SZ. C-1 78 ~00120-078 E00-1311 EOO-1311-1015 2 4 hour. O.lOmg/L, 82. C-1, MS 79 ~00120-079 E00-1311 EOO-1311-1016 2 4 hour, l.Omg/L, SZ. C-l 80 s00120~080 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 81 900120~081 E00-1311 MeOH Blank. TN-A-4715. Alin. 11~ /~ 16/.n.O 82 s00120~082 E00-1311 L1/16/00 83 ~00120-083 E00-1311 EOO-1311-1017 24 hour. l:O&/l Ir 52 c-1 84 SOO120-084 E00-1311 E00-1311-1018 2 4 houz, l.O&/L: 52: C-1 8 5 s00120~085 E00-1311 E00-1311-1018 2 4 hour, l.Omg/L, 12, C-1, MS 86 ~00120-086 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 87 500120-087 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 88 s 0 0 1 2 0 ~ 0 8 8 EOO-1311 0 ppb PFOS 00002-86-01. Aliq. 11-03-00 MLA 89 *00120~089 E00-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA SOUP 020199: (yumtitated and Drinted by CMC on 01/11/01 3M Environmental Laboratory ~ __ Page 3 TyDe Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Blank Blank Ana1yte Standard Standard Standard Standard Standard Standard Standard Standard standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Qc Analyte Analyte Analyte Anblyte Analyte Analyte Analyte QC Analyte Analyte Anblyte Analyte Analyte Anslyte Analyte Qc Analyte Allalyte Analyte Analyte Ana1yte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Ana1yte Analyte Analyte Analyte Analyte Analyte Qc Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Standard Std cone RT 6.938 6.938 6.927 6.926 6.952 6.940 6.938 6.927 6.939 6.926 6.926 6.926 6.926 6.927 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 6.925 6.927 6.939 6.926 6.938 6.928 6.927 6.926 6.927 6.926 6.926 6.926 246.10 6.951 6.951 6.953 6.953 6.941 6.951 246.10 6.952 6.951 6.962 6.953 6.951 6.951 246.10 6.948 6.964 6.951 6.951 6.962 6.939 246.10 6.961 6.962 6.965 6.963 6.962 6.954 246.10 6.951 6.962 6.949 6.951 6.962 6.947 246.10 6.951 6.950 6.952 6.950 6.954 6.939 6.950 6.952 6.938 246.10 6.941 6.935 Are* 2930 2763 m b 8-v F l a g ~ lMod co 257.53 242.81 5 bb -1 bb 2812 3382 3449 3103 3256 2928 2648 2677 2711 2632 2501 2412 247.17 291.23 303.13 272.69 286.20 257.37 232.71 235.32 238.30 231.34 220.31 211.97 0 bb 21 bb 23 bb 11 bb 16 bb 5 bb -5 bb - 4 b~ b . -3 bb -6 bb -10 bb -14 bb 2702 3155 3245 2865 3119 2791 2618 2621 2590 2611 2488 2506 237.45 277.28 285.19 251.77 274.08 245.25 230.10 230.34 227.66 229.43 218.68 220.25 -4 bb 13 bb 16 bb 2 bb 11 bb -0 bb -7 bb -6 bb -7 bb -7 bb -11 bb -11 bb 3530 3521 3549 3518 3496 2489 310.26 309.43 311.94 309.20 307.26 218.76 2 4 bb 24 bb 25 bb 2 4 bb 2 3 bb -11bb 3489 3477 3270 3371 3432 2527 306.60 305.55 287.41 296.83 301.61 222.08 23 bb 22 bb 15 bb 19 bb 21 bb -10 bh 3519 3536 3401 3448 3526 2535 309.27 310.79 298.93 303.03 309.91 222.78 2 4 bb 2 4 bb 20 bh 21 bb 24 bb -9 bb 3578 3434 3445 3409 3431 2461 314.44 301.76 302.81 299.65 301.57 216.30 26 bb 21 bb 21 bb 20 bb 21 bh -12 bb 3345 3773 7994 4614 4514 3079 294.00 331.60 702.58 405.48 396.76 270.57 18 bb 33 bb 181 bb 62 bb 59 bb 10 bb 4590 4334 4403 4276 4318 2941 403.42 380.88 386.94 375.79 379.46 258.51 61 bh 52 bb 55 bb 50 bb 5 2 bh 5 bb 4117 4161 3976 361.83 365.66 349.41 45 bb 46 bb 40 bb 2849 3166 250.36 278.28 2 bb 13 bb cmc I / h / O ( Page 496 of 703 BACK TO MAIN Quantify C m v o u n d S u m ~ r yReport Pros Msorb/rmrorb E00-1011 8-1. List: Last mxlified: Method: Last mdified: Job code: C:\~~s1~\~0~D020199.pr0\8~1~D8\9001120a Thu Jan 11 01:00:06 2001 C:\~lsl~\loup020199.p~O\M~t~B\.001120 wed NOV 22 06:41:05 2000 Printed: Thu Jan 11 07:03:22 2001 I; uame 90 ~00120-090 91 000120-091 92 ~00120-092 93 ~00120-093 94 ~00120-094 95 s00120~095 96 ~00120-096 91 ~00120-091 98 s00120~098 99 ~00120-099 100 s00120~100 101 n00120-101 102 900120~102 study no E00-1311 E00-1311 EOO-1311 EOO-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 Samplelist Text 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 HLA 9.9 ppb PPOS 00002-86-04, Aliq. 11-03-00 MLA 24.15 ppb PFOS 00002-86-05, Aliq. 11-03-00 M U 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA 49.5 ppb PFOS 00002-86-01 Aliq. 11-03-00 M U 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA 99.2 ppb PFOS 00002-86-09. Aliq. 11-03-00 MLA 241.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 991.78 ppb PFOS 00002-86-13, eliq. 11-03-00 MLA MeOH Blank, TN-A-4715, Aliq. 11/16/00 MeOH Blank, TN-A-4115. Aliq. 11/16/00 MeOH Blank. TN-A-4115. Aliq. 11/16/00 -0 standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte AKlLna1yte Analyte std cone 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 RT 6.938 6.931 6.938 6.931 6.936 6.938 6.936 6.931 6.937 6.925 -ea 3315 2919 3231 2840 2615 2116 2669 2317 2568 2460 vvb %Dav Flags Mod Co 291.36 18 bb 261.80 6 bb 2 8 3 . 9 8 15 bb 249.60 1 bb 235.11 -4 bb 238.13 -3 bb 234.51 -5 bb 208.93 -15 bb 225.66 - 8 bb 216.11 -12 bb SOUP 020199: mantitilted and printed by CMC On 01/11/01 3M Environmental Laboratory C b 7 C ( / I ( /o( Page 497 of 703 BACK TO MAIN huntify c w o u n d sumnary Report PFOS Adsorb/Dasorb Study, L C W Inst-t: Tuokar (LA052) S a q l a List: c:\HnssLYNx\Daoatur.PRO\Saql&B\t010122 - L a s t r o d r f i e d : Man Jan 22 15:03:42 2001 kkulod: C : \ H n s S L Y N x \ ~ ~ ~ t u r . ~ ~ ~ ~ \ WP FFOOS S Last modxfied: Wad Jan 24 06:53:49 2001 Job Code: hinted: ' W e d Jan 24 07:06:18 2001 co& 1: PMS(409) I N- S-ldist Text RT kea Rnspons. ppb F l a g s 1 t010122~OOl MeOH Blank, TN-A-4710, Aliq. 12/04/00 0 2 t010122~002 MeOH Blank, TN-A-4740, Aliq. 12/04/00. 6.471 1418177 0.000 0.00 b~b- 3 t010122-003 1000 ppb PFOS 00002-104-13 6.518 5443742 19342.259 1092.32 bb 9 4 t010122-004 1000 ppb PFOS 00002-104-13 6.494 4872953 17296.191 917.26 bb -2 5 t010122-005 MeOH Blank, TN-A-1740. Aliq. 12/04/00 6.302 666738 0.000 0.00 bb 6 t010122-006 MeOH Blank, TN-A-1710, Aliq. 12/01/00 6.278 188374 0.000 0.00 bb 7 tO10122-007 MeOH Blank, TN-A-4710, Aliq. 12/04/00 6.304 163484 0.000 0.00 bb 8 t010122~008 0 ppb FC Mix 00002-104-01 6.278 117782 277.506 2 . 8 5 bb 9 t010122~009 2 . 5 ppb FC Mix 00002-101-02 6.351 135145 342.973 6.66 bb 167 10 t010122~010 5 ppb FC Mix 00002-104-03 6.529 161293 425.429 11.46 bb 129 11 t010122~011 10 ppb FC Mix 00002-104-04 6.603 196372 539.114 18.07 bb 81 12 t010122-012 25 ppb FC Mix 00002-101-05 6.467 266693 820.039 34.41 bb 38 13 t010122-013 40 ppb PC Mix 00002-101-06 6.565 338161 1459.014 71.53 bb 79 14 t010122-011 50 ppb FC Mix 00002-101-07 6.483 131898 1818.543 92.39 bb 85 15 t010122 015 75 ppb FC Mix 00002-101-08 6,423 513753 1730.299 87.27 bb 16 100 ppb FC Mix 00002-104-09 6.531 594588 1936.961 99.26 bb -1 250 ppb FC Mix 00002-104-10 6.337 1275366 ~~ 1921.492 271.87 b-~b 9 500 ppb FC Mix 00002-104-11 6.277 2007741 9491.826 534.29 bb 7 750 ppb FC Mix 00002-104-12 6.457 2763803 13604.815 768.53 bb 2 1000 ppb FC Mix 00002-104-13 6.556 3645079 17205.562 972.14 bb -3 21 t010122~021 MeOH Blank, TN-A-4740, Aliq. 12/01/00 6.423 131577 0.000 0.00 bb 22 to10122 022 MeOH Blank, TN-A-1740. Aliq. 12/04/00 6.507 129156 0.000 0.00 bb 23 t0101221023 MeOH Blank, TN-A-1740, Aliq. 12/04/00 6.217 112678 0.000 0.00 bb 24 t010122-021 0 ppb FC Mix 00002-104-01 6.266 107071 252.335 1.39 bb 25 t010122-025 2 . 5 ppb FC Mix 00002-104-02 6.242 127936 303.081 4.31 bbX 74 26 t010122-026 5 ppb FC Mix 00002-104-03 6.241 141180 344.029 6.72 bbX 34 27 t010122-027 10 ppb FC Mix 00002-104-01 6.212 174501 415.631 10.89 bbX 9 28 t010122-028 25 ppb FC Mix 00002-104-05 6.292 278888 692.659 27.00 MU 8 b 29 tOlOl22 029 1 0 ppb FC Mix 00002-104-06 6.278 388285 944.455 41.64 MU 4 b 30 t0101221030 50 ppb FC Mix 00002-104-07 6.253 146576 1120.035 51.84 hN 1 b 31 t010122-031 75 ppb FC Mix 00002-104-08 6.212 570014 1520.355 75.09 MU O b 32 t010122-032 100 ppb FC Mix 00002-104-09 6.228 744606 2028.656 104.58 5 b 3 3 t010122-033 2 5 0 ppb FC Mix 00002-104-10 6.195 1386363 4620.568 254.51 bb 2 31 t010122-034 500 ppb FC Mix 00002-104-11 6.269 500.86 bb 0 35 tOlOl22-035 750 ppb FC Mix 00002-101-12 6.252 789.27 bb 5 36 t010122-036 1000 ppb FC Mix 00002-101-13 6.242 1033.68 bb 3 37 t010122-037 MeOH Blank, TN-A-1740, Aliq. 12/01/00 6.289 0.00 bb 3 8 t010122-038 MeOH Blank, TN-A-4740. Aliq. 12/04/00 6.192 124131 0.000 0.00 bb 39 t010122-039 MeOH Blank, TN-A-4740. Aliq. 12/01/00 6.278 117983 0.000 0.00 bb 40 t010122-040 E00-1311-2001, Oug PFOS, control,l/22/01.. 6.240 118400 ~~~ 269.982 2 . 4 2 bb 41 t010122-041 EOO-1311-2002. Oug PFOS, contro1,1/22/01.. 6.241 120731 283.170 3.18 bb 42 tOlOl22-042 E00-1311-2003, Oug PFOS, control,l/22/01.. 6.241 120322 275.218 2.72 bb 43 t010122-043 E00-1311-2003ms, Oug PFOS, control,l/22/.. 6.204 1168835 3577.816 194.28 bb 44 t010122-014 EOO-1311-2004. 0.75ug PFOS, control,1/22.. 6.205 813735 1879.338 95.92 bb 45 t010122-045 250 ppb FC Mix 00002-101-10 6.336 1424150 4176.378 228.87 bb -8 1 6 t010122 046 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.172 135069 0.000 0.00 bb MeOH Blank, TN-A-4710, Aliq. 12/01/00 6.412 137576 0.000 0.00 bb EOO-1311-2005. 0 . 7 5 ~ 9PFOS, control,l/22.. 6.459 813677 1895.496 96.85 bb 800-1311-2006. 0.75ug PFOS, control,l/22.. 6.542 893031 1870.228 95.39 bb E00-1311-2006ms, 0.75~9 PFOS, control,l/.. 6.325 1715684 5961.233 331.91 bb E00-1311-2007. 7.5ug PFOS, control,l/22/.. 6.338 5378311 11195.194 802.01 bb E00-1311-2008, 7.5~9PFOS, control,l/22/.. 6.348 4162893 10426.933 587.71 bb . . 2 5 0 ppb FC Mix 00002-104-10 MeON B l a n k , TN-A-4740. Aliq. 12/04/00 6.264 1217079 4483.933 2'16.63 bb -1 6.386 136322 0.000 0 . 0 0 bb MeOH Blank. TN-A-4710. Alia. 12/01'/00 6.433 139432 0.000 0.00 bb E00-1311-2009. 7.5ug PFOS, control,l/22/.. 6.241 4515612 11893.660 671.30 bb E00-1311--2009ms, 7.5ug PFOS, control.ll2.. 6.508 4776306 13117.657 757.91 bb EOO-1311-2010. Oug PFOS, Clay,1/22/01 M C 6.146 159367 358.722 7.58 bb E00-1311-2011, Oug PFOS, Clay,1/22/01 M C 6.386 136483 291.362 3.66 bb EOO-1311--2012. Oug PFOS, Clay, 1/22/01 M C 6.314 132405 278.898 2.93 bb 2 5 0 ppb FC Mix 00002-101-10 6.298 1319212 4478.412 216.31 bb -1 62 t010122-062 MeOH Blank, TN-A-4740. Aliq. 12/04/00 6.410 136755 0.000 0.00 bb 63 t0101221063 64 t010122-064 65 L010122_065 _ . M~ s~ OH~~B~ ~ lan.~ k.. TN-A-1740., ~Al-i-o.> 12./04~/.00 E00-1311--2012ms, Oug PFOS, Clay,1/22/01 E00-1311-2013, 0 . 7 5 ~ 9PFOS, Clsy,1/22/01.. 6.350 6.206 6.212 138103 1.2-29..867 708722 0.000 3235.341 1321.360 0.00 bb 174.17 bb 63.71 bb 66 tO10122-066 EOO-1311-2014. 0.75~9PFOS, Clay,1/22/01.. 6.253 808319 1521.178 75.13 bb 67 t010122 067 68 tO10122-068 . EOO-1311-2015. 0.75~9 PFOS, Clay,l/22/01.. ~oo-i3ii-2oi5ms, o.75ug PFOS, ciay.i/22/. 6.254 6.231 814123 1813512 1514.113 4986.936 71.71 bb 275.64 bb 250 ppb FC nix 00002-101-10 6.336 1423318 1035.575 220.74 bb -12 MeOH Blank, TN-A-4710, Aliq. 12/04/00 6.579 141495 0.000 0.00 bb MeOH Blank, TN-A-4740, Aliq, 12/04/00 .. EOO-l311-2016. 7.5~9PFOS. Clay,1/22/01 .. EOO-1311-2017, 7.5ug PFOS, Clay,1/22/01 .. E00-1311-2018, 7.5ug PFOS, Clay,1/22/01 E00-1311-2018m. 7 . 5 ~ 9 PFOS, Clay,l/ZZ/O.. 6.423 6.312 6.361 6.289 6.331 139217 4604516 5217586 3567801 5013902 0.000 11133.142 izoag.igo 8221.149 15883.856 0.00 bb 627.98 bb 682.43 bb 161.56 bb 897.56 bb EOO-1311-2019. Oug PFOS, Sediment,l/22/0.. 6.403 167395 318.587 6.99 bb 77 t010122-077 2 5 0 ppb FC Mix 00002-104-10 6.251 1438106 4448.547 211.58 bb -2 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.576 114134 0.000 0.00 bb MeOH Blank, TN-A-1740, Aliq. 12/01/00 6.183 149923 0.000 0.00 bb E00-1311-2020, Oug PFOS, sediment,1/22/0.. 6.568 173961 365.458 8.03 bb E00-1311-2021. Oug PFOS, Sediment,l/ZZ/O.. 6.409 168116 374.703 8.51 bb E00-1311-202lms. Oug PFOS, Sediment,l/22.. 6.388 1139314 3540.157 192.10 bb Quantitated and P r i n t e d by Qx: on 24 Jan 0 1 Study I E00-1311 page 1 3M Environmental Laboratory Page 498 of 703 BACK TO MAIN PIlantify Corpouncl S - q Wrt PFOS Adsorb/Deaorb S t u d y , LC/bfS h - t : T u c k e r (LA052) Smple L i s t : C:\MlssLm\hatur.PRO\Smpl~B\t010122 - Last modified: k n Jan 22 15:03:42 2001 New: c:\MlssLm\hatur.m~thDB\Pws L a s t d f i s d : Wed Jan 24 06:53:49 2001 THPPOS Job C&: Printed: W d Jan 24 07:06:18 2001 C A 1: PFoS(499) .I N- Sanplelirt Text 83 t010122-083 600-1311-2022, 0.75~9 PFOS. Sediment,l/2.. 84 t010122-084 600-1311-2023. 0.75~9 PFOS, Sedirnent.ll2.. 85 t010122-085 250 ppb FC Mix 00002-104-10 86 t010122-086 MeOH Blank, TN-A-4740. Aliq. 12/04/00 87 t010122-087 MeOH Blank, TN-A-4740, Aliq. 12/04/00 88 t010122-088 BOO-1311-2024. 0.75119 PFOS, Sedirnent,l/L.. 89 tO10122-089 E00-1311-2024ms. 0.75ug FFOS, Sediment.1.. 90 t010122-090 E00-1311-2025, 7 . 5 ~ 9 PFOS, Sediment,l/22.. 91 t010122-091 800-1311-2026. 7 . 5 ~ 9 PFOS, Sediment,l/ZZ.. 92 t010122-092 E00-1311-2027, 7.5ug PFOS, Sedinent,l/22.. 93 to10122 093 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 B00-1311-2027~, 7 . 5 ~ 9 FFOS, Sediment,l/.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 99 t0101221099 MeOH Blank, TN-A-4740. Aliq. 12/04/00 100 t010122~100 MeOH Blank, TN-A-4740, Aliq. 12/04/00 101 to1.012~ 2 10~ 1 .~ 0 ppb FC Mix 00002-104-01 102 t010122~102 2 . 5 ppb FC Mix 00002-104-02 103 t010122-103 5 ppb FC Mix 00002-104-03 104 t010122-104 10 ppb FC Mix 00002-104-04 105 t010122~105 25 ppb PC Mix 00002-104-05 106 t010122 106 40 ppb FC Mix 00002-104-06 107 t010122~107 50 ppb FC Mix 00002-104-07 108 t010122-108 75 ppb FC nix 00002-104-08 109 t010122-109 100 ppb FC Mix 00002-104-09 110 t010122~110 250 ppb FC Mix 00002-104-10 111 t010122~111 500 ppb FC M i x 00002-104-11 112 t010122~112 1 5 0 ppb FC Mix 00002-104-12 113 t010122-113 1000 ppb FC Hix 00002-104-13 114 t010122-114 MeOH Blank, TN-A-4740. Aliq. 12/04/00 115 t010122-115 MeOH Blank, TN-A-4740, Aliq. 12/04/00 RT 6.252 6.315 6.396 6.577 6.326 6.216 6.326 6.542 6.291 6.362 6,241 6.434 6.518 6.372 6.543 6.290 6.443 6.241 6.546 6.278 6.309 6.452 6.186 6.460 6.326 6.313 6.376 6.314 6.229 6.472 6.469 6.529 6.436 Area 1026372 866060 1372822 150111 142252 813373 1607159 4488760 4178850 4349355 1303467 148641 152985 5663187 1365566 149480 155378 144563 164749 166221 181623 212615 292832 353915 439196 583060 690084 1303673 2036643 3110621 3415199 185076 151445 Resppons. 2118.433 1772.460 3983.564 0.000 0.000 1752.210 4550,4 69 10086.002 10795.713 11084.279 4587.499 0.000 0.000 16464.124 3642.34 0 0.000 0.000 0.000 346.252 399.780 436.052 499.891 689.623 84 1.984 11 62.333 1595.061 1977.399 4519.670 8986.881 12414.655 17167.793 0.000 0.000 ppb 109.78 89.72 217.73 0.00 0.00 88.54 250.93 568.24 608.75 625.20 252.60 0.00 0.00 930.32 198.01 0.00 0.00 0.00 6.85 9.97 12.08 15.79 26.82 35.68 54.30 79.42 101.61 248.69 505.41 700.94 970.01 0.00 0.00 Flags bb bb bb bb bb bb bb bb MM bb bb bb bb bb bb bb bb bb bb bbX bbX bbX bb MM bb bb bb bb bb MM bb bb bb *De-, -13 1 299 142 58 7 -3 d Comment b Guantitatsd and P r i n t e d by CXC on 2 4 Jan 01 S t u d y # E00-1311 3M Environmental Laboratory BACK TO MAIN Quantxfy Corpovnd Svmcary b p r t PFOS AdsorbIDesorb Study, Lclsas Instrmwnt: Tucker (LAO52) s q 1 e L1St: Last d f z e d : . Mesthod: Last d f r e d : Job Code: c:wsLYNx\D~atur.PRO\SanplaDB\tOl0122 - h b n Jam 22 15:03:42 2001 C:\MnSSL~\Dooatur.PRO~U1DB\PFOS TWFOS Wed Jan 24 06:53:49 2001 Prmtad: W d Jan 24 07:06:18 2001 Conp'md 2: I.S. (TH-PFOS) (427) I Name 1 to1.0~ 122 001 ~ 2 t010122~002 3 t010122-003 4 t010122-004 5 t010122 005 6 t0101221006 7 t010122 007 12 t010122~012 13 t010122~013 14 tOlOl22 014 15 t0101221015 16 t010122-016 17 t010122-017 18 t010122~018 19 t010122-019 20 t010122~020 21 tOlOl2Z 021 22 t010122~022 23 t010122-023 24 t010122-024 25 t010122-025 26 t010122-026 27 t010122-027 28 t010122-028 29 t010122-029 30 t010122-030 31 t010122-031 32 t010122-032 33 t010122-033 31 t010122-034 35 t010122-035 36 t010122-036 37 tO10122-037 38 to10122 038 44 t0101221044 45 t010122-045 46 t0101222-0466 47 t010122I-047 48 t010122-048 49 t010122-049 50 t010122~050 51 t0o10122-051 52 t010112222-005522 53 t010122-053 59 t0101221059 60 tO10122-060 61 t010122-061 62 t010122-062 63 t010122-063 64 t010122-064 65 t010122-065 66 tO10122-066 67 t010122-067 68 t010122-058 69 t010122-069 70 t010122-070 71 t010122-071 72 t010122-072 73 t010122-073 74 t010122-074 75 t010122-075 76 t010122-076 77 t010122-077 78 t010122-078 19 t010122-079 80 t010122~080 81 t010122~081 82 t010122-082 Sanpldist Toit MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 1000 ppb FFOS 00002-104-13 1000 ppb PFOS 00002-104-13 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 0 ppb FC Mix 00002-104-01 2.5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb FC Mix 00002-104-04 2 5 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb PC Mix 00002-104-13 MeOH Blank, TN-A-4740. Aliq. lZl04lOO MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 ppb FC Mix 00002-104-01 2 . 5 ppb FC Mix 00002-104-02 5 ppb FC Mix 00002-104-03 10 ppb PC Mix 00002-104-04 25 ppb FC Mix 00002-104-05 40 ppb FC Mix 00002-104-06 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 250 ppb FC Mix 00002-104-10 500 ppb FC Mix 00002-104-11 750 ppb FC Mix 00002-104-12 1000 ppb FC Mix 00002-104-13 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank. TN-A-1740, Aliq. 12/04/00 MeOH Blank, TN-A-4740. Aliq. 12/04/00 E00-1311-2001. Oug PFOS, control,ll22/01.. E00-1311-2002, OUg PFOS, control,l/22/0l.. E00-1311-2003, Oug PFOS. control,l/22/01.. 600-1311-2003ms. Oug PFOS, control,l/22/.. 600-1311-2004. 0.75ug PFOS, control.1122.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 E00-1311-2005, 0.75ug PFOS, control,1/22.. E00-1311-2006. 0.75~9 PFOS, control,l/22.. E00-1311-2006rrm, 0 . 7 5 ~ 9PFOS, control,l/.. 600-1311-2007. 7.519 PFOS, control,l/22/.. E00-1311-2008, 7 . 5 ~ 9 PFOS, control,l/22/.. 250 DDb FC Mix 00002-104-10 M e o H ' i l a n k , TN-A-4740, Aliq. 12/01/00 NeOH Blank, TN-A-4740. Aliq. 12/04/00 BOO-1311-2009. 7 . 5 ~PF~OS, control,l/22/.. 600-1311-2009rrm. 7 . 5 ~ 9 PFOS, control, 112.. 600-1311-2010. Oug PFOS, Clay,1/22/01 M C E00-1311-2011, Oug PFOS, Clay,l/ZZ/Ol M C E00-1311-2012, Oug PFOS, Clay,l/22/01 M C 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740, Aliq. 12/04/00 .. MeOH Blank. TN-A-4740, Aliq. 12/04/00 E00-1311-2012ms, Oug FFOS, Clay,l/22/01 E00-1311-2013, 0.75ug PFOS, Clay,l/22/01.. GOO-1311-2014, 0.75ug PFOS, Clay,l/22/01.. GOO-1311-2015, 0.75ug PFOS, Clay,1/22/01.. E00-1311--2015ma, 0.75~9 PFOS, Clay,1/22/.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 .. 800-1311-2016. 7 . 5 ~ 9 PFOS, Clay,1/22/01 .. GOO-1311-2017. 7 . 5 ~ 9 PFOS, Clay,1122/01 .. GOO-1311-2018, 7 . 5 ~ 9 PFOS, Clay,1/22/01 E00-1311-2018ms, 7.5ug FFOS, Clay,l/22/0.. GOO-1311-2019, Oug FFOS, Sediment,l/22/0.. 250 ppb FC Mix 00002-104-10 MeOH Blank, TN-A-4740. Aliq. 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 E00-1311-2020, Oug PFOS, Sediment,l/ZZ/O.. 600-1311-2021. Oug PFOS, Sediment.1/22/0.. B00-1311-2021ms, Oug PFOS, Sediment.l/ZL.. RT 6.386 6.361 6.386 6.158 6.170 6.208 6.181 6.206 6.289 6.374 6.395 6.360 6.411 6.255 6.313 6.289 6.229 6.397 6.423 6.351 6.157 6.169 6.158 6.169 6.151 6.183 6.182 6.181 6.193 6.168 6.147 6.185 6.180 6.182 6.193 6.132 6.182 6.155 6.169 6.169 6.156 6.145 6.216 6.255 6.243 6.255 6.421 6.277 6.277 6.276 6.215 6.372 6.181 6.292 6.373 6.314 6.242 6.250 6.350 6.134 6.170 6.180 6.170 6.159 6.204 6.252 6.301 6.241 6.274 6.319 6.202 6.311 6.399 6.291 6.325 6.327 *ea 0 3928 70361 70433 2936 1130 1051 106107 98510 94782 91062 81305 57943 59374 74229 76742 64786 52881 50787 52964 694 0 756 106080 105530 104773 104963 100658 102780 99679 93730 91761 75010 64556 55314 50107 727 1541 1224 109637 106589 109297 81672 108248 85250 811 744 107317 119375 71916 94721 99811 71203 0 530 94916 88993 111066 117108 118685 73643 613 0 95034 133786 132844 134396 92417 88175 0 0 103397 107898 108495 78915 120053 80836 623 547 118677 112367 80456 3928.481 70360.727 70432.680 2936.239 1130.456 1051.464 106107.367 98510.055 94782.305 91062.211 81304.906 57913.418 59374.168 74228.898 76742.336 64785.551 52880.7ai 50787.223 52963.672 694.074 755.682 106080.023 105529.836 104773.352 104963.086 100658.469 102780.266 99678.969 93730.359 91761.063 75010.414 64555.895 55314.195 50107.137 727.358 1544 .lSI ~~ 1224.169 109637.445 106589.008 109296.547 81672.383 108247.570 85250.313 810.623 743.885 107317.102 119374.625 71915.523 94720.633 99811.055 71203.055 529.970 94916.367 a899z.914 111065.523 117107.781 118685.422 73642.852 612.897 95033.773 133785.656 132844.172 134395.797 92417.078 88175.039 103397.258 107897.750 108494.609 78915.063 120052.766 80835.727 623.047 547.122 118677.195 112366.523 80456.438 ppb Flags 6D.v od C-t 11.28 bb 202.11 bb -19 202.32 bb -19 8.43 bb 3.25 bb 3.02 bb 304.80 bb 22 282.97 hb 13 272.27 bb 9 261.58 bb 5 233.55 bb -7 166.44 bb -33 170.55 bb -32 213.23 bb -15 220.45 bb -12 186.10 bb -26 151.90 bb -39 145.89 bb -42 152.14 bb -39 1.99 bb 2.17 bb 304.72 bb 22 303.14 bb 21 300.97 bb 20 301.51 bb 21 289.15 bb 16 295.24 bb 18 286.33 bb 15 269.24 bb 8 263.59 bb 5 215.47 bb -14 185.44 bb -26 158.89 bb -36 143.93 bb -42 2.09 bb 4...P.P. b-b 3.52 bb 314.94 bb 26 306.18 bb 22 313.96 bb 26 234.61 bb -6 310.95 bb 24 244.88 bb -2 2.33 bb 2.14 bb 308.27 bb 23 342.91 bb 37 206.58 bb -17 272.09 bb 9 286.71 bb 15 204.53 bb -18 1.52 bb 272.65 bb 9 255.64 bb 2 319.04 bb 28 336.40 bb 35 340.93 bb 36 211.54 bb -15 1.76 bb 272.99 bb 9 384.30 bb 54 381.60 bb 53 386.06 bb 54 265.47 bb 6 253.29 bb 191 297.01 bb 309.94 bb 24 311.66 bb 25 226.69 bb -9 344.86 bb 38 232.20 bb -7 1.79 bb 1.57 bb 340.90 bb 36 322.78 bb 29 231.11 bb -8 Quantitated and Printed by (1wc on 24 Jan 01 Study 0 E00-1311 Paga 3 3M Environmental Laboratory Page 500 of 703 BACK TO MAIN pllantafy Compound S - r y &port PFOS Adsorblossorb Study. L C W Inst-t: Tucker (LA0521 Sample L i s t : bst m l f i s d : Method: Last nuolfred: Job Code: C:\aansSLYNx\D~atur.~\Smpl~B\tOlOl22 Xon Jan 22 15:03:42 2001 C:\aanssLm\Dsoatur.PRO\WstMB\PFOS - RlpFos Wed Jan 24 06:53:49 2001 Printed: W a d Jan 24 07:06:16 2001 C& 2: I.S. (TH-PFOS)(427) I N- Samplelist T e x t 11l Aeea ppb Flags %DN od c m t a3 ~ o i o m - 0 8 3 800-1311-2022, 0.75~9 PFOS, sediment,1/2.. 6.180 121124 12112'3.969 347.93 bb 39 84 t010122-084 EOO-1311-2023. 0 . 7 5 ~ 9 PFOS, Sedirnent,l/Z.. 6.182 122155 122155.006 350.90 bb 40 65 tOlO122-085 250 ppb FC Mix 00002-104-10 6.240 66155 86155.375 247.48 bb -1 86 t010122 086 MeOH Blank, TN-A-4740. Aliq. 12104100 0 87 t0101221087 HeOH Blank, TN-A-4740. Aliq. 12/04/00 7.181 24442 24442,334 70.21 bb 88 to10122 088 EOO-1311-2024. 0 . 7 5 ~ 9PFOS, Sediment.ll2.. 6.168 116050 116049.539 3 3 3 . 3 6 bb 33 89 C010122~089 E00-1311-2024ms, 0.75~9 PFOS, Sediment.1.. 6.193 88141 88141.375 253.19 bb 1 90 t010122-090 BOO-1311-2025, 7.519 PFOS, Sediment,l/22.. 6.325 111262 111262.109 319.60 bb 28 91 t010122-091 E00-1311-2026, 7.5ug PFOS, Sediment,1/22.. 6.230 96771 96771.055 277.90 bb 11 92 to10122 092 E00-1311-2027, 7 . 5 ~ 9 PFOS, Sediment.1122.. 6.302 98097 98097.375 281.79 bb 13 93 t010122I093 250 ppb FC Mix 00002-101-10 6.193 71034 71033.633 204.05 bb -18 94 t010122 094 HeOH Blank, TN-A-4740, Aliq. 12/04/00 0 95 C010122I095 HeOH Blank, TN-A-4740, Aliq. 12/04/00 0 96 t010122-096 600-1311-2027ms. 7 . 5 ~ 9 PFOS. Sediment.l/.. 6.216 85993 85992.a36 241.02 bb -1 97 t010122_097 250 ppb FC Mix 00002-104-10 6.386 93729 93728.602 269.24 bb 8 98 tO10122-098 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.242 691 690.849 1.99 bb 99 to10122 099 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.363 560 560.268 1.61 bb 100 t010122~100 HeOH Blank, TN-A-4740, Aliq. 12/04/00 6.192 661 660.914 1.90 bb 101 t010122~101 0 ppb FC Mix 00002-104-01 6.389 116951 116951.328 341.69 bb 37 102 t010122~102 2.5 ppb FC Mix 00002-104-02 6.217 103945 103945.063 298.59 bb 19 103 t010122-103 5 ppb PC Mix 00002-104-03 6.249 104129 101129.118 299.12 bb 20 104 t010122~104 10 ppb FC Mia 00002-104-04 6.367 106331 106330.531 305.44 bb 22 105 t010122-105 25 ppb FC Mia 00002-104-05 6.390 106157 106156.602 304.94 bb 22 106 t010122-106 40 ppb FC Mia 00002-104-06 6.232 105084 105083.742 301.86 bb 21 107 t010122-107 50 ppb PC Mix 00002-104-07 6.266 94464 94164.391 271.35 bb 9 I 108 t010122-108 109 t010122-109 75 ppb FC Mix 00002-104-08 100 ppb FC Mix 00002-104-09 6.253 91385 91385.258 262.51 bb 5 6.316 87206 87246.352 250.62 bb 0 110 t010122~110 250 ppb FC Mix 00002-104-10 6.266 72111 72111.070 207.11 bb -17 111 t010122~111 500 ppb FC Mix 00002-104-11 6.181 56656 56656.000 162.75 bb -35 112 to10122 112 ~~ 750 ppb FC Mix 00002-104-12 6.231 62640 62640.102 179.94 bb -28 113 t.010122~113 1000 ppb FC Mix 00002-104-13 6.385 49133 49732.637 142.66 bb -43 111 t010122-114 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.240 951 951.098 2.73 bb 115 t010122_115 MeOH Blank, TN-A-4740, Aliq. 12/04/00 6.363 553 552.916 1.59 M Page 4 G u m t i t a t e d and Printed by C-lC on 2 4 Jan 01 Study M' EOO-1311 3M Environmental Laboratory c f i c ( /3q/Ol Page 501 of 703 BACK TO MAIN t N- study M Samplelist Text 1 sOO12Za-001 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 2 s00122a 002 E00-1311 991.78 ppb PFOS 00002-86-13. aliq. 11-03-00 M L A 3 ~ 0 0 - 1 3 1 1991.78 ppb PFOS 00002-86-13. aliq. 11-03-00 MLA 4 r00122a~004 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 5 soo122Poo5 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 6 a00122a-006 E00-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 M L A 7 s00122a-007 e soouza-ooe 9 900122a-009 E00-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA E00-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA EOO-1311 9.9 ppb PFOS 00002-86-04, Aliq. 11-03-00 MLA 10 s00122a~010 E00-1311 24.75 ppb PFOS 0 0 0 0 2 - 8 6 - 0 5 , Aliq. 11-03-00 MLA 112 s00l22a~0ll E00-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA so01229012 E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA 13 ~ 0 0 1 2 2 ~ 0 1 3Eoo-1311 74.26 ppb PFOS 0 0 0 0 2 - 8 6 - 0 8 , Aliq. 11-03-00 MLA 14 s00122a~014 E00-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 M L A 156 sO0122a-015 E00-1311 247.9 ppb PFOS 00002-86-10. Alip. 11-03-00 MLA s00122a-016 E00-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 HLA 1is7 s00122a~017 E00-1311 991.78 ppb PFOS 00002-86-13. aliq. 11-03-00 HLA sooiz2a-oie E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 19 sOOl22a-019 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 20 s00122a-020 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 21 so0122a-021 E00-1311 0 ppb PFOS 00002-86-01. Aliq. 11-03-00 MLA 232 s00122a~022 E00-1311 2.47ppb PFOS 00002-86-02. Aliq. 11-03-00 MLA a00122a-023 E00-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA 2 4 s00122a-024 E00-1311 9.9 oob PFOS 00002-86-04. Alia. 11-03-00 MLA 2 5 sOO122a-025 EOO-1311 24.7j-ppb PFOS o o o o 2 - e ~ - o s ~ ~ A i iiqi.loi-00 MLA 26 s00122a-026 E00-1311 39.6 ppb PFOS 0 0 0 0 2 - 8 6 - 0 6 , Aliq. 11-03-00 MLA 27 r00122a-027 E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA 298 sOO122a-028 E00-1311 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA s00122a-029 E00-1311 99.2 ppb PFOS 00002-86-09. Aliq. 11-03-00 M I A 30 800122a-030 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 31 sOO122a-031 E00-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 32 sooi22a-a32 EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MU 3 3 s00122a-033 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 354 sOOl2Za-034 s00122a-035 36 s00122a-036 37 s00122a-037 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 E00-1311 E00-1311-1019 24 hour, O m g i L , S2, C-2 . 800-1311 E00-1311-1020 24 hour, OmglL, S2. C-2 EOO-1311 E00-1~ 311.-~ 102~~ 1 2..4 h.o~ur~ .., O~~ mo_/.r-.. S2. C--2- 38 s00122a-038 E00-1311 E00-1311-1021 24 hour, OmglL, 92. C-2, MS 4309 sOO122a-039 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA r00122a-040 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 41 s0012Za-041 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 4623 s00122a-062 E00-1311 E00-1311-1022 24 hour, O.lOmg/L, S Z . C-2 s00122a-043 E00-1311 E00-1311-1023 24 hour, O.lOmg/L. S2, C-2 4 4 s00122a-046 E00-1311 E00-1311-1024 24 hour. O.lOmg/L, S2, C-2 45 rOO122a-045 EOO-1311 EOO-l311-1024 24 ~~ h.o~ur.. 0.l~ O.m..a.l-.L.. 52. C - 2 ~~ MS 66 saoi22a-046 E00-1311 E00-1311-1025 24 hour, l.Omg/L, S2. C-2 487 sO0122a-047 SOo 122LO 4 e 49 s00122a-049 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 HLA EOO-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 600-1311 MeOH Blank, TN-A-4715, Alii. 11/16/00 50 s00122a-050 E00-1311 E00-1311.1026 24 hour. l.Omg/L, S 2 , C-2 51 s00122a-051 E00-1311 E00-1311.1027 24 hour, l.Omg/L. 6 2 , C-2 52 s00122a~052 EOO-1311 E00-1311-1027 2 6 hour. l.Omo/L. S2. C-2. MS 53 s00122a~053 Eoo-1311 ~ 0 0 - 1 3 i i - 1 0 ~284 hour. ami. 5 2 . c-3 54 r00122a-054 EOO-1311 E00-1311-1029 24 hour, OmilL, 5 2 . C-3 55 s00122a-055 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 56 s00122a-056 E00-1311 MeOH Blank, TN-A-47 15. Aliq. 11/18 57 s00122a-057 E00-1311 MeOH Blank, TN-A-4715. 58 so0122PO58 E00-1311 E00-1311-1030 24 hour. 59 r00122P059 E00-1311 EOO-l3ll-1030 2d hour. 60 a00122a~060 E00-1311 E00-1311-1031 24 hour. 61 s00122a~061 EOO-1311 E00-1311-1032 24 hour, O.lOG/L; S2: C - 3 632 s00122a-062 E00-1311 1100-1311.1033 24 hour. O.lOmg/L. S 2 , C-3 s00122a-063 E00-1311 ;!47.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 64 sOo122a-064 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 65 a00122n-065 EOG-1311 MeOH Blank. TH-A-4715, Alii. 11/16/00 66 sOO122a-066 EOO-1311 E00-1311-1033 24 hour. O.lOmg/L, S Z . C-3 M S 67 s00122a-067 E00-1311 E00-1311-1034 24 hour. l.Omg/L. S2, C-3 68 7609 ~ 0 0 1 2 2 ~ 0 6 eE00-1311 sOO122a-069 EOD-1311 E00-1311-1035 EoO-i3il-l036 24 24 hour. hi&: li..DOmGo/;Li;. 52. s2: C-3 c-i s00122b-070 E00-1311 EOO-1311.1036 24 hour, l.Omg/L. 5 2 . C-3 MS 712 sOO122a-071 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA s00122a1_072 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 73 sO0122a-073 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 754 SOO122a-074 E00-1311 E00-1311-1037 24 hour, Omg/L, S Z . C-4 s00122a-075 E00-1311 E00-1311-1038 24 hour. O m / L 5 2 . C-4 76 ~ 0 0 1 2 2 ~ 0 7 6 77 s00122a1077 E00-1311 E00-1311-1039 26 hour, O&/L. S Z . C-4 MS 78 ~ooi22a-078 EOO-1311 E O O - L ~ ~ L - 2~4Oh~ouOr. o . i o m / L , s z . c-4 79 SOO122a-079 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 80 s00122a-080 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 - 81 s~ o01~ 22~ 1 0.81 EOO-1311 M ~ O HBlank. T N - A - ~ ~ ~AsI.~ O .11/16/00 oTiiwiL, e2 ~ 0 0 1 2 2 ~ 0 e 2EOO-1311 ~ o o - i S I i - 1 o ~2i4 hour; sz, c-4 e 3 S O O ~ ~ Z L O~~o o~- i 3 i i~oo-i3ii-i04224 hour, o.iomg/~, s z . c-4 e4 soo12~a-oe4 ~00.1311 EOO-1311-1042 24 hour. o.iomg/~,sz, c-4 MS 85 s00122a-OB5 E00-1311 E00-1311-1043 24 hour. l.Omg/L, S2. C-4 86 s00122a-086 E00-1311 E30-1311-1044 24 hour. l.Omg/L, S 2 , C-4 e7 ~ o o i 2 ~ ~ 0 ~8007.1311 247.9 ppb PFOS 00002-86-io. Aliq. 11-03-00 MLA 88 sOO122a-088 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 89 s00122a-089 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 soup 020199: puantitated and printed by CElC on 11/27/00 ma Analyte Analyte Analyte Analyte Analyte Ana1yte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Blank Blank Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Qc AM1yte Analyte Ana1yte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Ana1yte QC Analyte Analyte A~lyte Analyte Analyte Analyte Analyte Qc Analyte Analyte Analyte Analyte Analyte Analyte Analyte ac Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte AnLnalyte Analyte anaiyte Analyte Analyte Qc Analyte Analyte Std COILC 2.47 4.95 9.90 24.75 39.60 49.50 74.26 99.20 247.90 495.90 991.78 247.90 247.90 247.90 247.90 247.90 247.90 247.90 RT 7.156 7.118 7.117 7.130 7.130 7.117 7.118 7.118 7.116 7.117 7.115 7.117 7.116 7.115 7.117 7.115 7.117 7.130 7.128 7.129 7.117 7.103 7.115 7.117 7.106 7.104 7.106 7.115 7.103 7.105 7.103 7.103 7.128 7. lie 7.117 7.131 7.124 7.118 7.104 7.128 7.129 7.116 7.118 7.119 7.115 7.118 7.106 7.129 7.129 7.116 7.119 7.106 7.116 7.127 7.105 7.104 7.103 7.129 7.113 7.117 7.117 7.128 7. lie 7.127 7.141 7. lie 7.128 7.118 7.129 7.117 7.117 7.142 7.143 7,128 7.142 7.139 7.132 7.130 7.129 7.144 7.142 7.130 7.130 7.130 7.129 7.130 7.130 7.140 7.150 *.a 202 37418 36717 423 197 926 1416 1776 1900 3566 4431 4984 6826 8679 16310 24541 35819 263 198 186 e55 1461 1761 ieeo 3414 4497 5027 7129 e453 16335 23694 34689 201 161 237 156 159 19144 14927 154 128 728 601 859 19389 5002 14912 147 136 6414 5781 20890 198 146 15212 544 373 15.5 19173 124s 1124 883 15129 321 134 19397 12990 10723 7873 22076 14963 158 139 226 190 168 19233 783 15169 166 165 1328 1062 19629 2728 5894 15343 174 133 PDb %Cev ?lags Hod Co 0.00 bb bbI bb1 0.00 bb 0.00 bb 0.00 bb 0.00 -100 bb 1.57 -68 bb 3.32 -66 bb 27.40 11 bb 40.26 2 bb 68.62 -2 bb 77.36 4 bb 107.79 9 bb ~ 256.64 4 bb 565.92 14 bb bb1 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 -100 bbX 1.08 -78 bbx 3.03 -69 bbX 25.60 3 bb 41.26 4 bb 49.28 -0 bb 82.23 11 bb 104.00 5 bb 257.22 4 bb 502.61 1 bb bbX1 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 128.62 bb 225.85 -9 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 335.59 bb 48.91 bb 225.53 -9 bb 0.00 bb 0.00 bb 70.82 bb 60.90 bb 382.11 bb 0.00 bb 0.00 bb 232.03 -6 bb 0.00 bb 0.00 hb o.ao bb 329.42 bb 0.00 bb 0.00 bb 0.00 bb 230.22 -7 bb 0.00 bb 0.00 bb 335.81 bb 186.09 bb 143.63 bb 96.36 bb 425.37 bb 226.63 -9 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 331.12 bb 0.00 bb 231.09 -7 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 362.57 bb 15.18 bb 62.65 bb 234.87 -5 bb 0.00 bb 0.00 bb 3M Environmental Laboratory Page 502 of 703 BACK TO MAIN puantify C ~ u n Bdunmaw Report E00-1311 PPOS Add.orb/Desorb 8-1. List: Last Wdified: Method: Last Wdifiad: Job Cod.: C:\~~~1~\~aUPO20199.DrO\O~lsDB\~00112~a Wad NOV 22 07:23:55 2000 C:\~~~lyN(\~oUp020199.~~~\~t~B\~OO1122~ Man N W 27 07:42:34 2000 Printed: Man nov 27 07:50:41 2000 ( 4 9 9 > 9 9 ) , fupE 1 mtudy no Samplelist Text E00-1311 E00-1311-1045 24 hour, l.Omg/L, S2. C-4 E00-1311 EOO-1311-1015 24 hour. l.Omcr/L. S2. C-4 MS E00-13Il 247.9 PPb PFOS 00002-~6-10,-Al~q1.1-03-00 MLA 93 s00122az093 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 94 sOO122a-094 EOO-1311 HeOH Blank, TN-A-4715, Aliq. 11/16/00 95 s00122a-095 E00-1311 HeOH Blank, m-A-4715. Aliq. 11/16/00 96 sOO122a-096 EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 HLA 97 s001221)-097 E00-1311 2.47ppb PFOS 00002-86-02. Aliq. 11-03-00 MLA 98 ~ O o l 2 2 a ~ a 9 8E00-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA 99 n00122a-099 EOO-1311 9.9 Doh PFOS 00002-86-04. Alio. 11-03-00 MLA 100 900122a-100 EOO-T3yy 24:75'~ppb PFOS OOOO2I86-05: Aiiq. 11103-00 M U 101 s00122a~lOl E00-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 HLA 102 s00122a-102 E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA 103 sOO122a-103 E00-1311 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA 104 s00122a-104 E00-1311 99.2 ppb PFOS 00002-86-09. Aliq. 11-03-00 MLA 105 sOO122a-105 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 106 s00122a-106 EOO-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 HLA 107 a00122a-107 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 108 s00122a-108 E00-1311 MeOH Blank, Tt-A-4715, Aliq. 11/16/00 109 ~ 0 0 1 2 2 p 1 0 9 EOO-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 110 s00122a-110 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 we Analyte Analyte QC Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Std Con0 247.90 2.47 4.95 9.90 24.75 39 60 49.50 74.26 99.20 247.90 495.90 991.78 RT 7.123 7.128 7.114 7.139 7.148 7.149 7.117 7.118 7.121 7.124 7.122 7.113 7.117 7.121 7.117 7.116 7.117 7.128 7.142 7.143 7.150 Araa 3002 20271 15179 140 ~~ 149 164 803 1332 1713 1795 3284 4210 4728 6565 8022 15354 23693 34251 241 189 150 19.14 362.03 231.29 0.00 0.00 0.00 0.00 0.00 0.67 1.84 23.25 36.96 44.74 73.21 96.81 235.13 491.10 0.00 0.00 0.00 -7 -100 -86 -81 -6 -7 -10 -1 -2 -5 -1 bb bb bb b_ b_ bb bb bb bbX bbX bbX bb bb bb bb bb bb bb bbX1 bb bb bb SOUP 020199: wantitate6 and printed by CMC on 11/27/00 3M Environmental Laboratory Page 503 of 703 BACK TO MAIN S a l w h List: Last modifid: Method: Last maifiea: Job Code: C:\Idarllynx\.oUp020l99.pro\salwl~~B\*ooll22a Wed Nov 22 07:23:5S 2000 C:\Ida~~l~\~o~D020199.prO\M~~MB\~001122~ on NOV 17 07:42:34 2000 Printed: Hon NOY 27 07:50:41 2000 1 Campound 2: TllP108 (427,801. fUnC 2 1 s00122a-001 E00-1311 Meoi Blank, TN-A-4715, Aliq. 11/16/00 2 sOO122a-002 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 3 s00122a-003 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 4 sOO122a-004 E00-1311 MeOH Blank, TN-A-4715, Aliqo. 11/16/00 5 s00122a 005 600-1311 MeOH Blank. TN-A-4715. AIlia. 11/16/00 6 sOOl22a-006 E00-1311 0 Dnb PFOS 00002-86-01 A l k 11-03-00 MLA 7 s00122a~007 EOO-1311 2.ijppb PFOS 00002-86-02. Aiiq. 11-03-00 MLA 8 s00122a~008 E00-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA 9 sOO122a-009 E00-1311 9.9 ppb PFOS 00002-86-04, Aliq. 11-03-00 MLA 10 s00122a~010 E00-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 11 s00122a-Oll E00-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA 123 soo122a-012 E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 HLA sOO122a-013 E00-1311 74.26 ppb PFOS 00002-86-08. Aliq. 11-03-00 MLA 154 s00122a-014 E00-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA s00122a-015 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 16 SO 0122a-0 16 E00-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 17 s00122a-017 E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 18 500122a~018 600-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 19 s00122a-019 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 20 s00122a-020 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 21 100122a~021 E00-1311 0 ppb PPOS 00002-86-01, Aliq. 11-03-00 M U 22 n00122a-022 E00-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA 23 s00122a-023 E00-1311 4 . 9 5 ppb PFOS 00002-86-03. Aliq. 11-03-00 MLA 24 s00122a-024 EOO-1311 9.9 ppb PFOS 00002-86-04, Aliq. 11-03-00 MLA 25 s00122a-025 E00-1311 24.75 ppb PFOS 00002-86-05. Aliq. 11-03-00 MLA 26 sOO122a-026 E00-1311 39.6 ppb PFOS 00002-86-06. Aliq. 11-03-00 HLA 287 ~ 0 0 1 2 2 ~ 0 2 7E00-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA sOO122a-028 E00-1311 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA 29 sOO122a-029 EOO-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 HLA 30 s00122a-030 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 31 s00122a-031 E00-1311 4 9 5 . 9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 32 s00122pq32 E00-1311 991.78 ppb PFOS 00002-86-13. aliq. 11-03-00 MLA 3 3 sOO122a-033 BOO-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 34 s00122a-034 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 35 sOO122a-035 E00-1311 E00-1311-1019 24 hour, OmgIL, S2. C-2 36 s00122a-036 E00-1311 EOO-1311-1020 24 hour. OmglL. 52, C-2 37 s00122a-037 E00-1311 EOO-1311-1021 24 hour, OmgIL, S2, C-2 38 sOO122a-038 E00-1311 E00-1311-1021 24 hour, OmglL, 52, C-2, MS 39 s00122a-039 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 40 s00122a-040 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 421 s00122a-041 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 s00122a-042 E00-1311 600-1311.1022 24 hour, 0.lOmglL. 82, C-2 43 s00122.a-043 E00-1311 E00-1311.1023 24 hour, O.lOmg/L, S2. C-2 44 600122a_044 E00-1311 EOO-1311-1024 24 hour, O.lOmo/L, S2. C-2 4 5 s00122aI045 EOO-1311 800-1311-1024 24 hour, O.lOm~/L.S2, C-2, MS 4 6 s00122a-046 E00-1311 E00-1311-1025 24 hour, l.OmgiL, S2, C-2 47 sOO122a-047 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 48 sOO122a-048 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 4 9 50012211 0 4 9 E00-1311 MeOH Blank. TN-A-47lS. Alia. 11/16/00 50 s00122a1050 E00-1311 EOO-l3;l-l026 24 hour: l . O & / L y S2, C-2 51 sO0122a~051 E00-1311 E00-1311-1027 24 hour. 1.OmglL. S2. C-2 E00-1311 E00-1311.1027 24 hour, l.Omg/L. S2, C-2. MS 600-1311 E00-1311-1028 24 hour, OmglL. 82. C-3 E00-1311 800-1311-1029 2 4 hour. OmglL, 52, C-3 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA ~ ~~~ E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 57 soo122a-os7 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 58 s00122aI058 E00-1311 E00-1311-1030 24 hour. Omg/L. s2, C-3 59 soo122a-059 E00-1311 E00-1311-1030 24 hour. O m g l L . 5 2 . C-3 MS 60 sOO122a-060 E00-1311 E00-1311-1031 24 hour, 0.lOmglL. S2. C-3 61 500122a-061 E00-1311 EQO-1311-1032 24 hour. 0.lOnwlL. S2. C-3 E00-1311 E00-1311.1033 24 hour. O . l O & / L . S2, C-3 E00-1311 247.9 ppb PFOS 00002-86-10, 1119. 11-03-00 MWL E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 E00-1311 E00-1311-1033 24 ho~u.r. O.lOmo-/L.. S2.. C-3 MS 67 s00122aI067 EOO-1311 800-1311-1034 24 hour. l.Omo/L. 82. C-3 68 sOO122a-068 E00-1311 E00-1311-1035 24 hour, l.O&/L. S2, C-3 69 rO0122a-069 E00-1311 E00-1311-1036 24 hour, l.Omg/L, 52. C-3 70 s00122a-070 E00-1311 E00-1311.1036 24 hour, l.Omg/L, S2, c-3 MS 71 sOO122a-071 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 72 sOO122a-072 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 73 s00122a-073 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 74 s00122a-074 E00-1311 E00-1311-1037 24 hour, OmgIL. 52. C-4 75 sOO122a-075 E00-1311 EOO-1311.1038 24 hour. OmglL, S2. C-4 76 s00122a-076 E00-1311 E00-1311-1039 24 hour, OmgIL. S Z , C-4 77 sOO122a-077 E00-1311 E00-1311-1039 2 4 hour, OmgIL. S2, C-4 MS 78 sOO122a-078 E00-1311 E00-1311-1040 24 hour. 0.lOmglL. 52, C-4 79 s00122a-079 E00-1311 247.9 ppb PFOS 00002-86-10. Aliq. 11-03-00 MLA 80 900122.~080 EO0 -1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 81 s00122a~O.81 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 82 so0122a-082 E00-1311 E00-1311-1041 24 hour, 0.lOmglL. S2. C-4 83 ~ 0 0 1 2 2 ~ 0 8 3E00-1311 E00-1311-1042 24 hour. O.lOmg/L, S2, C-4 84 s00122a-084 E00-1311 EUO-1311-1042 2 4 hour, O.lOmg/L. S2, C-4 M! 85 ~001228.-085 E00-1311 E00-1311-1043 24 hour, l.Omg/L. S2, C-4 86 a00122a-086 E00-1311 E00-1311-1044 24 hour. l.Omg/L, S2. C-4 87 s00122a-087 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 88 s00122a-088 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 89 s00122a-089 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 SOUP 020199: quantitated and Drinted by CMC O n 11/27/00 P.S. 3 Tm. Analyte Analyte Analyte Analyte Analyte Analyte Analyte Ana1yte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Anna1yte Analyte Analyte Blank Blank Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Ana1yte Analyte Analyte Analyte Analyte Q Analyte Analyte Analyfe Analyce Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte AM1yte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Eta conc RT 6.939 6.937 6.938 6.939 6.940 6.938 6.939 6.935 6.937 6.937 6.936 6.926 6.936 6.926 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 6.939 6.924 6.924 6.925 6.926 6.925 6.926 6.923 6.924 6.926 6.924 6.924 246.10 6.937 6.927 6.932 6.927 6.925 246.10 6.925 6.926 6.927 6.936 6.926 6.926 246.10 6.925 6.926 6.926 6.924 6.935 6.926 246.10 6.939 6.934 6.938 6.938 6.937 6.939 246.10 6.938 6.936 6.938 6.937 6.938 6.938 246.10 6.937 6.938 6.949 6.940 6.951 6.937 246.10 6.938 6.938 6.951 6.949 6.937 6.939 Area 3051 3040 m 217.69 216.91 ria^^ Hod co -12 bb -12 bb 3421 3762 4037 3673 4110 3660 3241 3276 3264 3307 3143 3129 244.07 268.38 288.03 262.10 293.25 261.13 231.28 233.72 232.91 235.96 224.24 223.23 -1 bb 9 bb 17 bb 6 bb 19 bb 6 bb -6 bb -5 bb -5 bb -4 bb -9 bb -9 bb 3449 4070 4333 3650 4008 3746 3326 3445 3451 3421 2921 2813 246.08 290.39 309.17 260.43 285.94 267.24 237.33 245.81 246.25 244.07 208.41 200.70 -0 bb 18 bb 26 bb 6 bb 16 bb 9 bb -4 bb -0 bb 0 bb -1 bb -15 bb -18 bb 2593 2607 2649 2468 3004 184.99 185.98 189.00 176.07 214.36 -26 bb -26 bb -24 bb -30 bb -13 hb 2680 2654 2684 2550 2669 3101 191.25 189.34 191.51 181.94 190.42 221.29 -24 bb -24 bb -23 bb -27 bb -24 bb -10 bb 2687 2648 2546 2726 2708 3128 191.68 188.95 181.67 194.48 193.23 223.18 -23 bb -24 bb -27 bb -22 bb -23 bb -9 bb 2729 2641 2702 2695 2687 3115 194.71 188.46 192.79 192.30 191.73 222.22 -22 bb -25 bb - 2 3 bb -23 bb -23 bb -10 bb 2598 2577 2600 2635 2502 3063 185.34 183.88 185.A9 187.99 178.55 218.57 -26 bb -26 bb -26 bb -25 bb -29 bb -11 bb 2707 2802 2718 2612 2728 3086 193.17 199.93 193.94 186.40 194.65 220.15 -23 bb -20 bb -22 bb -25 bb -22 bb -11 bb 2750 2815 2704 2728 2773 3103 196.21 200.86 192.91 194.61 197.84 221.43 -22 bb -20 bb -23 bb -22 bb -21 bb -10 bb 3M Environmental Laboratory Page 504 of 703 BACK TO MAIN Last m d i f i e d : W e d NOY 22 07:23:55 2000 Method: C:\~~LI1~\~oUpO2Ol99.prO\~tMB\~001122~ Last M i r i e a : MOD NOV 27 07:42:34 zoo0 Job Code: Printed: MOD Nov 27 07:50:41 2000 C-und 2: THPFOS l417W801, fuuc 2 0 NUM 90 s00122a-090 91 s00122a-091 92 s00122a-092 93 s00122a-093 94 sOO122a-094 95 s00122a-0.95 96 s00122a-096 97 s00122a-097 98 s00122a-098 99 s00122a-099 100 s00122a~100 101 s00122a-101 102 s00122a-102 103 600122a-103 104 s00122a-104 105 s00122a-105 106 sOO122a-106 107 s00122a-107 108 aO0122a-108 109 s00122a-109 110 s00122a~110 atudy no EOO-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 - E00-1311 EO0 1311 E00-1311 - E 0 0 4 3 1 1 EO0 1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 S-lelfSt T a t E00-1311-1045 24 hour, l.Ow/L. S2, C-4 E00-1311-1045 24 hour, l.OG/L, S2, C-4 MS 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA MeOH Blank. TN-A-4715. Aliq. 11/16/00 MeOH Blank, TN-A-4715. Aliq. 11/16/00 HeOH Blank. TN-A-4715. Alia. 11/16/00 0 11-03-00 M U 2.iqppb PFOS 00002-86-02, Aiiq. 11-03-00 MLA 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA 9.9 ppb PFOS 00002-86-04. Aliq. 11-03-00 MLA 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 NLA 74.26 ppb PFOS 00002-86-08. Aliq. 11-03-00 MLA 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MIA MeOM Blank, 'R-A-4715. Aliq. 11/16/00 MeOH Blank, TN-A-4715. Aliq. 11/16/00 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Type Analyte Analy te QC Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Std Corm 246.10 246.10 246.10 246.10 246.10 246.10 RT 6.944 6.949 6.935 6.938 6.939 6.941 6.945 6.938 6.949 a.2748 2591 3076 m b %De.v Flaws Hod Co 196.05 -22 bb 184.90 -26 bb 219.46 -11 bb 3265 3759 4012 3443 3774 3346 3009 3152 3125 3159 3013 2906 232.93 268.23 286.25 245.67 269.26 238.73 214.72 224.87 222.98 225.42 214.96 207.36 -5 bb 9 bb 16 bb -0 bb 9 bb -3 bb -13 bb -9 bb -9 bb -8 bb -13 bb -16 bb SOUP 020199: wuantitatsd and Printed by CMC an 11127fOO 3M Environmental Laboratory BACK TO MAIN '0 fPn) 0 0 Inj Dale 8sW SmpTyp Fils Sample Name M21012053 D.WsmWurh.WJ10222.b SAMPLE 2N10121:M D.WemWurh.!W010222.b CALlB-1 2R2/0121:16 0 WemWurh.ilR010222.b W l B - 2 2R210121.27 0 WemWurh.N(OlCI222.b CALIB-3 2122101 21.38 DWemWurh.iiROl0222.b CALIB-4 2122101 21 49 DWemWurh.iW010222.b CALK-5 212/01 22.03 D~~.~m~~~"r*.iWC!O22C2K.IbB-6 2/221C12211 0:bhsmWush 1W010222.b CALIB-7 2/22/012222 D WemWurh.iW010222.b CALIB-8 2/22/0122.34 0 khemWuih.iW010222.b CALIB-9 2/22/0122 45 0 khemU(urh iW010222.b CALK-10 2122101 22.56 D WemWurh.iW010222.b SAMPLE 212UO123.07 D.WsmWurh.iW010222.b SAMPLE 2123/01 1.32 D.WemWurh.iiR010222.b CCALlB-1 2123101 1.43 DWemWurh.iW010W.b CCALIB-1 2/23/014.08 DkhemWurh.iW010222.b CCALIB-1 2/23/014.20 D:WsmWurh.iW010222.b CCALIB-1 2RM16 45 DkhamWurh.iW010222.b CCALlE-1 2R3016-56 DWemWurh.iW010222.b CCALIB-1 2R3/01 B21 D:WemWush.iW010222b CCALIB-1 RUSH0022.D OOW2-1Mol RUSHW23.D WW2-10442 RUSHW24.D woO2-laM3 RUSHW25.D WW2-1MM RUSHW26.D wOO2-10445 RUSH0027 D OwO2-1Mo6 RUSH0028.D W 2 - 1 M 0 7 RUSH0029.0 WW2-1Mo8 RUSH0030.0 WW2-1MO9 RUSHW31.D WW2-1M10 RUSH0032.D woO2-1Ml1 RUSH0033.0 W002-1Ml2 RUSHOOY.0 OW02.1M13 RUSHO(U7.0 wW2-1M43 RUSHWI8.0 WWZ-1M-IO RUSHWB1.D wO02-1ou)3 RUSH0062.D W002-1MlO RUSHW750 woO2-1Mo3 RUSH0076.0 WW2-1MlO RUSHW89 0 WOOZ-lMo3 2/23/01933 2/23/01 1158 2123101 12 09 2/23/01 14.35 2/23/01 1446 2/23/01 16.49 2/23/01 17.W 2/23/01 1734 u23/01 1745 2/23/01 1756 2/23/01 18 07 2/23/01 1818 2/23/01 18 29 2/23/01 1841 2:23/01 16.52 2/23/01 19 03 2/23/01 19.14 2/23/01 19.25 2/23/01 19 36 2/23/01 19.48 DWemWush.iW010222.b CCALIB-1 OhhamWurh1W010222.b CCALIB-1 0 WemWurh.#W010222.b CCALlB-1 D WemWurh.iWO10222.b CCALlB-1 D'khemWush IW010222.b CCALlB-1 D.bhemWurh8W010222.b CCALIB-1 D WemWush.ii010222.b CCALIB-1 D.WemU(ush xW010222b SAMPLE O.WemWurh.iW010W b CALlB-1 D Wem!Rush.iW010222.b CALK-2 D WemWurh.oU(010222.b CALIB-3 D.khemWush.iW010222.b W B - 4 D.WemWurh.iiR010222.b CALIB-5 D.WcmWurh.rW010222.b CALIB-6 0 Shem~Wuih.iW010222.bCALlB-7 DWemWurh.iW010222.b CALIB-8 D.!&hemWurh iW010222.b CALlB-9 D WemWurh iW010222.b CALIB-10 D bhemWUih.iW0102Z2.b SAMPLE DWemWuihoWO10222.b SAMPLE RUSHW90.0 RUSH0103 D RUSHO1M.D RUSH0117 D RUSHO118.D RUSHOl29.D RUSH0130.D RUSH0133.D RUSHO1Y.D RUSHO1U.D RUSH0136.D RUSH0137.D RUSHO138.D RUSH0139.D RUSH0140.D RUSH0141.D RUSH0142.D RUSH0143.D RUSHOlU D RUSH0145.D WWZ-1MlO WW2-1Mo3 WW2-lM10 OOW2-1Mo3 woO2-lMlO OwO2-1M43 WWZ-1MlO WW2-1Mo1 WW2-1M02 WW2-104-03 WW2-lMo4 WW2-1M-05 OOW2-1Mo6 WW2-lW7 OwO2-1Mo8 OwO2-lM09 00W2-1M10 WWZ-lMll WWZ-lM12 WW2-1M13 J Misc Info ComwndNam Ldnolmsatacwnqrsquinmml Cal sld 2 (LW) C1. .Id 3 Cal .Id 4 Cal std 5 Cal *Id 6 Cal s l d 7 CaI s l d 8 CaI sld 9 CaI sld 1 0 excluded IO kner 61d a b u d u d o d l o klter 61dab did ml m e l amno, nquinmsnl Cal *Id lz(L0Q) Calsld13 Cal sld 1 4 C1. .Id 1 s Cal s l d 1 6 Cal 'Id 1 7 CaI s l d 1 8 CaI s l d 19 C d .Id 20 excluded IO teller M dstl exdudsd IO M e r fit d a b THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFDS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT Ana 5.553 5.561 5.55.8 5 554 5.545 5.54 5 539 5.552 5.567 5.56 5.551 5.569 5.555 5.561 5.567 5.555 5.547 5.545 5.539 5.54 688380 604164 889138 679632 671308 684907 876783 674589 68747 6uBo2 619576 595985 576693 713865 652248 716157 659416 723145 654913 557797 5.532 5.507 5.51 5.537 5.536 5.5w 5.511 5.507 5 454 5.505 5 499 5.51 5.502 5.519 5.509 5.513 5.511 5.512 5.508 5.505 avenge sld deviation %Cy 649228 714024 640235 748169 662e45 729420 637769 718171 728159 734029 723187 711239 704611 705699 702051 85302 6r16270 610214 573664 562318 672404 45783 6.8% h w n t CompoundNanis RT ndmL ,-- ha munl ndmL % De" 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249 3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 0 5.185 56147 5.775 93148 5.778 104431 5.769 401765 5.764 664873 5 756 856165 5.776 1276020 5.784 1657895 5.777 3779794 5.775 6765120 5.773 95011% 0 0 5.779 94822 5.785 3452407 5.78 93243 5.771 3887395 5.769 92534 5.763 3872492 5.771 94512 check standard>30%due lo 5.763 3834030 5.731 91142 5.741 3727210 5.768 94563 5.76 3860610 5.733 94353 5.728 n 3687433 0 5.735 50380 5.729 89391 5.716 165120 5.727 385518 5.719 629059 5 729 832703 5 726 1248638 5 13 1612642 5 728 3713608 5 722 606551 5 725 9143085 5 722 11281687 00 00 X 50 00% 100 00% 250 00% 401 0 3% 502 0 4% 748 0 3% 995 0 5% 249s 0 0% 5W1 0 0% 7765 X 00 X 53 59% 251 6 0 6% 52 3 6% 2497 0 1% 51 2 1% 251 9 0 7% 67 34 6% lowTHPFos rctponre 251 5 0 6% 51 1 8% 2477 0 9% 50 0 9% 2479 0 9% 52 3 2% 2458 11% 00 26 X 50 0 3% 105 4 7% 221 11 5% 304 8 9% 483 3 5% 732 2 4% 982 1 8% 2505 0 2% 4998 0 0% 7764 X 10176 X P BACK TO MAIN 73 9) rn (D sVI 0 -J -J 0 0 2/22/01 2341 D chemP.ulh 1P.010222 b SAMPLE RUSHW37 D 13114052S1 2r2M123 52 D chemlRvln 1R010222b SAMPLE RUSHW38 D 1311405M1 2125010 03 D LChemRuIn1P.010222 b SAMPLE RUSh0039 D 13114054S1 M Y 0 10 14 D Cnem\Rurh16010222b SAMPLE RUSHOMOD 131140YMS s f M310l 025 DWsmP.urh1P.010222b SAMPLE RUShC.31D 13114051s1 u 2 L O l 036 DkhemP.urh1P.010222b SAMPLE RUSkW42D 131140Msl 2R310l 0 47 D LChsmP.ushhR010222b SAMPLE RLShC.33 D 13114057S1 212M1 0 59 D WcmlR.sh UU10222b W P . E R U S H WD 13114057MSSl 2123011 10 DWemlRah 1P.010222~SAMPLE RUSrlOM5D 1~114056Sl 2!2301 4 24 D LChemWuih 1R.010222D SAMPLE RLSd0048 D 1311405951 2123012 17 DWemP.urnkR010222 b SAMPLE RUSd0051D 1311.406C-Sl 2R301 2 28 0 WemWurn 1P.010222b SAMPLE RUSHW52D 1311MWMSS1 2RM1 239 D\chcmP.ulh1P.010222b SAMPLE RUShW53D 13114061S1 212M12 50 DkhtmP.~rh~P.01022b2 SAMPLE RUSH0054D 13114062Sl 2RM13 01 D memP.ush&3010222 b SAMPLE RUShW55D 1311406?-Sl 2123013 13 D WrmR.rh iW010222b SAUPLE RUSHW56D 13114063MSSl 2R301 3 24 DWemRdih 1P.0102220 SAMPLE RUSH0057D 1311406cS1 2~31013 35 D memflusn N10102220 SAMPLE R J S ~ W So 13114065-s1 212301346 D~ncmP.urh1R010222b SAMPLE RUSdW59D 13114066.Sl 212301 3 57 DYhemRuih1P.010222 b SAMPLE RUSHW60 D 13114066M5S1 2123014 53 D WemRurh 1R.010222b SAMPLE RUSrl0065D 1311406751 21231015 M D khsmR.rh 1R.010222b SAMPLE RUShW6BD 1311406851 21238015 16 DWcmR.rh1W010222 b SAMPLE RUSHW67D 13114069-Sl 2RLO15 27 D WemP.ush lW010222b SAMPLE RUShW68D 13114069USSl 212301538 D WomU7urh1U1010222D SAMPLE RbSHW69D 1311407C-S1 2123401 5 49 D WsmlRush1P.010222D SAMPLE RUSH0070D 13114071S1 2123016 W D mcmlRurh 4P.010222 b SAMPLE RuSHW7l D 13114072S1 21231016 11 D WcmP.urh 1P.010222b SAMPLE RUSr(0072D 13114072MSSl 212301623 DWernP.uih P.010222 b SAMPLE RJSH0073 D 1311407bSl M 3 0 16 34 D WchemP.,sh fR.OlOu2b SAMPLE RUSh0074 D 1311407cSl 2 2 M 1 7 30 D WomW.sh N(010222b SAMPLE RUSh0079 D 13114075Sl MU017 41 DkhemlRush1P.010222~SAMPLE RUShOO6OD 13114075MSSl 2RUOl 7 52 D WemP.sh1lR010222D SAMPLE RLShW8l D 13114076Sl u231018 03 D memWYih1P.010222b SAMPLE RLSHW82 D 1311407751 2nUol 8 14 D memP.urh iW010222b SAMPLE RUSH0083D 13114078-S1 W231018 25 D WemWurh 1R.010222b SAMPLE RUSH00840 13114078MSSt 21231018 37 D WemP.uih 1W010222b SAMPLE RUSH0085D 13114079-Sl M M 1 848 D WemWush tW010222 b SAMPLE RUSH00860 1311438&S1 2QM1 8 59 D khemU7urhiW010222b SAMPLE RUSH0087D 13114081-51 2/23/019 10 D WemWulih iW010222b SAMPLE RusHooaaD 1 3 i i ~ o a i ~ ~ s i 21231011006 D WemR.urh 1P.010222b SAMPLE RUSH0093D 1311482.S1 212301 10 17 D WemP.uih 1P.010222 b SAMPLE RUSHW94 D 1311408551 2IZ301 1028 D WemWuih iW010222b SAMPLE RUSH0095D 1311408cs1 2123011040 D.WemR.ush.iR.OlO222.b SAMPLE RUSmM96.D 13114WMSS1 2nM1 1051 D!chemWush iP.OlM22.b SAMPLE RUSH0097D 13114085S1 21231011132 DWemP.ush.iW010222.b SAMPLE RUSHOW8.D 1311-4086.Sl 2R3101 11:13 D ~hemP.uih.iWOlO222.b SAMPLE RUSHW99 D 13114087Sl 212301 1124 D Wem\Rush iW010222b SAMPLE RUSH0100D 13114087MSSl 21231011135 D WemRush rR.010222b SAMPLE RUSH0101D 13114088-Sl Z M 1 1747 D WemRurh ,lRO10222b SAMPLE RUSHO102D 13114089-S1 2 n M 1 1243 D WemR.urh 1P.010222b SAMPLE RUSH0107D 13114090S1 212301 1254 D WemWurh iP.010222 b SAMPLE RUSH0106D 13114090MS-S1 m 3 m l 1305 D WemiRvrh iW010222b SAMPLE RUSH0109D 13114091-51 2 n M 1 1316 D WemR.urh iW010222b SAMPLE RUSH0110D 13114092-S1 21231011327 OWemLQurh 1P.010222b SAMPLE RUSH0111D 1311409bSl 2123/01 13 39 D:khemP.ush.#P.010222.b SAMPLE RUSHO1jZ.D 13114093MS-S1 21231011350 D.\chemR.ush.iP.OlO222.b SAMPLE RUSHO113.D 1311.409441 2/2310114:01 O.WemP.u~h.iP.010222.bSAMPLE RUSH0114.D 13114095S1 212310114.12 O\chemP.ushiR.010222b SAMPLE RUSHO115.D 1311.4096S1 21231011423 D.!chemP.urh iR.010222b SAMPLE RUSHOll8.D 1311409SMS-Sl 212301 1519 DW~mP.ushRRO1OW.bSAMPLE RUSHOl2l.D 13114W761 2/23/0115'30 0 k h W u S hiW010222b SAMPLE RUSH0122.D 13114098-51 212301 15:42 D.WemR.urh.iW010222.b SAMPLE RUSH0123.D 13114099-51 2 n M 1 15.53 D.Wem\Rurh.lP.010222 b SAMPLE RUSH0124D 13114099MSS1 2123101 16 04 D.WemR.urh.1P.010222.b SAMPLE RUSH0125.0 1311.4lO&S1 2123101 1615 DWemP.urh iP.010222.b SAMPLE RUSH0128D 1311.4101Sl 212301 18.28 DWemR.urh.iW010222b SAMPLE RUSH0127.D 13114102-Sl 2n301 1638 D khemlRurh.~R.Ol0222.bSAMPLE RUSH0126.D 1311.4102MSSl THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.561 5.565 5.567 5.567 5.559 5.56 5 565 5 567 5.568 5.561 5.558 5.561 5.555 5.559 5.561 5.554 5.544 5.537 5.555 5.554 5.533 5 525 5.539 5.539 5.541 5.54r 5.54 5.54 5.547 5.547 5 548 5.541 5.554 5.545 6.551 5.539 5 537 5.543 5.528 5.528 5.527 5.528 5.513 5 509 5 5M 5.506 5.505 5.51 5.518 5 502 5.511 5.521 5 521 5.503 5 505 5.525 5.531 5.547 5.533 554 5 523 5 529 5.528 5.52 5.515 5.515 5.518 5.51 738374 729881 748027 MBMO 720087 718694 713613 650599 898677 697037 712727 623982 713961 722949 717685 625622 893953 703230 883158 601504 715149 718563 721833 626695 723074 713569 710887 826987 719422 721925 721018 830748 721U5 713442 714470 827930 716587 706703 787134 825739 711683 705320 711370 817162 702007 701896 704199 818234 883319 878063 87Mx)9 594782 696138 702240 713218 817233 706887 708135 705249 81W7 727274 722539 724260 611327 714433 712382 699621 606960 249.3 249.3 249.3 249.3 249.3 249.3 240 3 249.3 249.3 249.3 249.3 249.3 240.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249 3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249 3 249 3 249 3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249 3 249.3 249.3 249.3 249 3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249 3 249.3 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.792 5.789 5.791 5.798 5.79 5.792 5.797 5.791 5.797 5.785 5.775 5 785 0 5.783 0 5.778 0 0 0 5.785 5.75 5.749 5.783 5.783 5.758 5 759 5.757 8.757 5.m 5.m 5.779 5.772 5.778 5.789 5.775 5.758 5.781 5.787 5 752 5.757 5.751 5.743 5.73 5.733 5.728 5.73 5.729 5.734 5.74 5.719 5.735 5.746 0 0 0 5.742 0 0 0 5.784 5.747 5.753 5 757 5 751 5.739 5.74 5.735 5 734 210932 lsB367 214795 32735% 162434 159201 4M553 3223948 199972 le4182 188818 3147881 0 52969 0 3039824 0 0 0 2944564 708991 738565 483585 3383101 353028 401704 385139 3324237 368061 377219 3w 3329105 4W719 3M833 391323 3308122 327587 32608553 3277776 359433 317521 322509 3238116 275759 289371 598587 3378059 296195 292811 286C64 3043722 0 0 0 2959556 0 0 0 2967005 379645 387810 572801 3364903 266964 280369 248736 3069584 11.3 10.1 11.3 212.3 8.9 8.8 22.4 208.2 11.3 10 4 10.5 212.2 0.0 3.0 0.0 203.5 00 0.0 0.0 m.5 39.3 40.8 26.5 228.3 19.3 22.2 21.4 223.9 20 1 20 8 19.5 2Z.8 21.9 21.3 21.6 222.3 18.1 18 1 31.4 221.0 19.9 17.8 179 221.4 155 18 3 33.7 232.1 17.1 17 1 18 8 215.5 0.0 00 0.0 201.0 0.0 0.0 0.0 200.7 20 8 21.2 31.3 233 1 14 8 15 5 14.0 212.8 BACK TO MAIN 212UO12042 DWemWurh.iW010222b SAMPLE 212210123.18 D.khamWush.~W010222.bSAMPLE 2/22/012329 D WamWurhiW010222.b SAMPLE 2/231011.54 D.\chsmWushiWO10222.b SAMPLE 2/23/012:ffi D.WemWurh.iW010222.b SAMPLE 2/23/01 4 31 D.WrmWurh.iW010222b SAMPLE 2123101 4.42 D.WemWush.i\R010222.b SAMPLE 2123101 7.07 O.MemWurh.tWOlOZZ2.b SAMPLE 2/23101718 D'khemWurh.iWO10222.b SAMPLE 2123101 9:44 D.WemWurh.iWO10222.b SAMPLE 2123101 9.55 DkhemWurh.iW01022.b SAMPLE 2/23/01 1220 DWsmWurh.iW010222.b SAMPLE 2/23/01 1232 D:WlemWush.1W010222.b SAMPLE 2/23/01 1457 D:WemWush.i\ROlO222.b SAMPLE 2/25/01 1508 D.\chemWurh.iW010222.b SAMPLE 2123101 1711 O:WamWurh.lW010222.b SAMPLE 2R31011722 D:WemW~~h.1W010222.SbAMPLE 2/23/01 1959 DWcmWurh.rWOlO222.b SAMPLE 2/23/012010 DkhsmWurh.i\R010222.b SAMPLE RUSHW21.D TN-A4755 MsOH RUSHW35.D TKA4755 MeOH RUSHW36.D TN-A4755 MsOH RUSH0049.D TKA 4755 MsOH RUSH0050.D TN-A4755 MsOH RUSH0063.D TKA4755 MsOH RUSHW64.D TN44755 MsOH RLISHW77.D TKA4755 MeOH RUSHW78.D TKA4755 MsOH RUSHW91.D TN-A4755MeOH RUSHW92.D TUA4755 MeOH RUSHOlO5.D TN-A4755 MsOH RUSHO1OB.D TN-A4755 MeOH RUSHO119.D TN-A4755 MeOH RUSH0120.D TN-A4755 MeOH RUSHO131.D TN-A4755 MeOH RUSHO132.D TN-A4755 MeOH RUSHOl46.D TN-A4755 MeOH RUSH0147.0 TN-A4755 MaOH THPFOS 0 0.0 PFOS 5.802 13952 0.0 THPFOS 0 PFOS 5.794 23163 00 THPFOS 0 0 0 PFOS 0 0 00 THPFOS 0 0 0 PFOS 0 0 00 THPFOS 0 0 0 PFOS 0 0 0.0. THPFOS 0 0 0 PFOS 0 0 0.0 THPFOS 0 0 0 PFOS 0 0 0.0 THPFOS 0 0 0 PFOS 0 0 00 THPFOS 0 0 0 PFOS 0 0 0.0 THPFOS 0 0 0 PFOS 0 0 0.0 THPFOS 0 0 0 PFOS 0 0 0.0 THPFOS 0 0 0 PFOS 0 0 0 0 ~~ THPFOS 0 0 0 PFOS 0 0.0 THPFOS 0 0 0 PFOS 0 0.0 THPFOS 0 0 0 PFOS 0 0.0 THPFOS 0 0 0 PFOS 0 0.0 THPFOS 0 0 0 PFOS 0 0 0.0 THPFOS 0 0 0 PFOS 5.733 25813 0.0 THPFOS 0 0 0 PFOS 5.735 18305 0.0 BACK TO MAIN HOIMO2b.xls Sample Batch HOlW2.b. analyzedon Hlllary ocO201. PFOS AdsorblDesorbsamples. Matrix: SolUSlglSed. Standardcuwe range used for calibration OF sampler: 5-1002 nghnL Batch method H010402b.m In] Date Batch Samplype File SamDle Name 4/3/01 3 14 D ChemWillary\H010402b SAMPLE HILL0077D 0 n&L PFOS in MeOH 413/01 3 28 D\ChemWillaryW010402b 4/3/013 43 D ChemWdlary\HOIC4Mb CALIBIZ CALIB 1 HILL0078D 2 5 ngmL PFOS In MeOH HILL0079D 5 ngm. PFOS m MeOH 413/013 57 D\ChemWillaryWO10402b CALIB-3 HILL0080D IOnghnl PFOSm MSOH 4/3/014 11 D ChemWdlaryWOlC402b CAUB-4 HILL0081D 25 ngmL PFOS m MeOH 4/3/01 4 26 D ChemWillaryW010402b SAMPLE HILL0082D 40n#mL PFOS in MeOH 4/3/014 40 D \CChemWdlaryW010402b CALIB-5 HILL0083D 50 1ngmL PFOS in MeOH 4/3/014 54 D\ChemWiIlary\HO10402b CALIB-6 HILL0084D ?5 1 ngmL PFOS In MeOH 4/3/01 5 09 D \ChemWillwyWOlM02b CALIB-7 HILL0085D 1002 nglmL PFOS in MeOH 4/3/01 5 23 D\ChemWiIlaryW010402b CALIB-8 HILL0086D 250 5 n@mLPFOS In MeOH 4LW1 5 38 D ChemWillaryWOlM02b SAMPLE HILL0087D 4W 8 ngmL PFOS in MeOH 413/01 5 52 D\ChemWdIaryW010402b CALlE-9 HILLW88D 501 ngmL PFOS In MeOrl 4/3/01606 DChemWiIIaryWOIM02b CALIB-IO HILLWB9D loo2 nglmL PFOS in MeOH 4f3/0123 24 D ChemWillaryWO10402b SAMPLE HILL0161D OWmL PFOS in MeOH 4/3/0123 39 DChemWillaryWOlM02 b CALIB-11 HILL0162D 2 5ngmL PFOS in MeOH 4/3/0123 53 D ChemW1llaryW010402b CALIB-12 HILL0163D 5 ngmt PFOS in MeOH 4/4/01 0 07 D \ChemWillaryW010402b CALIB-13 HILLO164D IOngmL PFOS in MeOH 4/4/010 2 2 D ChemWillaryWO10402b CALIB-14 HILL0165D 25 ngmL PFOS in MeOH 414101 0 36 D\ChemWillaryW010402b SAMPLE HILLOIE6D 40 ngmL PFOS in MeOH 4/4/01 0 50 D \ChemWllaryWO10402b CALIB-15 HILL0167D 50 1ngmL PFOS in MeOH 4/4M1 105 D ChemWilla~WOl0402b CALIB-16 HILL0168D 75 1 n#mL PFOS in MeOH 4/4/01 I19 ~ \ C h e m ~ 1 I l a r y ~ 0b1 0 4C~ALIB-17 HILL0169D 1W 2 namL PFOS in MeOH 4/4/01 134 D\ChemWillaryW010402b CALIB-18 HILL0170D 2% 5 ngmL PFOS ~1MeOH 4/4/01 1 48 D \ChemWillaryW010402b SAMPLE HILL0171D 4W 8 ngmL PFOS In MeOH 4/4/012 02 D ChemIHdlaryW10402b CALIB-19 HILL0172D 501 n@mLPFOS in MeOH 4/4/012 17 DChemWillaryW010402b CALIB-20 HILL0173D 501 ngmL PFOS in MeOH THPFDS MI% InfComnoundNI RT Ana Amount 5106 1211876 254 THPFOS 5105 1169631 254 THPFOS 5108 1115864 254 THPFDS 5097 1128520 254 THPFOS 5105 1132730 254 THPFOS 5104 1144180 254 THPFOS 5112 1088719 254 THPFOS 5105 10M910 254 THPFOS 5107 1034615 254 THPFOS 5105 86924a 254 THPFOS 5105 988215 254 THPFDS 51Og 1060823 254 THPFOS 5107 928336 254 THPFOS 5105 1337731 254 THPFOS 5 1 1311179 254 THPFOS 5097 1236112 254 THPFOS 5101 1272114 254 THPFOS 5087 1204745 254 THPFOS 5 1 1303887 254 THPFOS 50% 1207553 254 THPFOS 5Q99 1208046 254 THPFOS 5101 1167221 254 THPFOS 509 1093910 254 THPFOS 5091 1097069 254 THPFOS 5091 1175367 254 THPFOS 5104 1023103 254 Compound NInUT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 5322 5325 5321 5 322 5329 5336 5322 5331 5329 5329 533 5331 0 531 5307 5 311 5308 531 5306 5309 5318 5307 5309 5309 5321 Area Amount 0 0 76308 3386026 108804 5067026 209068 9618429 565907 26 00359 929336 4242639 1114128 5358744 1636985 8209443 2152918 1103641 4767587 2698584 7513403 4302713 9712588 5273099 15404980 1041642 0 0 76978 3057097 107847 4535542 208869 8524792 W 7 1 4 2270129 928989 3717265 I099646 4762208 1590311 6917822 2147218 972829 4811322 2398238 7530799 3852073 9910075 4816606 15786129 9510902 1487085 +30%: 800738 30%: 101% 96% 104% 106% 107% 109% t*O% 108% 107% 105% 104% 91% 05% 91% 93% 95% 92% 97% 96% %% 96% 95% 0 -h page r of 3 BACK TO MAIN In] Date Batch 4nm1 2 45 O\ChemWillaryW010402b SamPTYF,e SAMPLE 4/3/012 59 0\ChemWdIaryW010402b SWPLE 4/3/016 21 D \ChemWillaiyW010402b SAMPLE 4133101 6 35 0\ChemWillaryv1010402b SAMPLE 4 ~ m7i 04 D \ChemWillaryWO104OZb SAMPLE 4/3/017 33 0 \ChemWillaryWo10402b SAMPLE 40mi 8 02 0 !ChemWillaryW010402b SAMPLE 4/3/01 8 30 D \ChemWillaryW010402 b SAMPLE 4 n m i 8 59 0 \ChemWillaryWO10402b SAMPLE 4/3/01 9 28 D\ChemWdIaryW010402b SAMPLE 4/3/01 9 57 D \ChemWillaryW010402b SAMPLE 4/3/01 10 26 OU)hemWillaryW010402b SAMPLE 4/3/01 10 55 O\ChemWillary\HOl0402b SAMPLE 413101 11 52 O\ChemWillaryW010402b SAMPLE 4/3/01 1207 O!ChemWiIlary\H01040202 b SAMPLE 4 n m i 12 35 0 \ChemWillaryWOl0402b SAMPLE 4/3/01 13 04 0 \ChemWillaryW010402b SAMPLE 4/3/01 13 33 0 \ChemWillaryW010402b SAMPLE 4/3/01 14 02 D \ChemWillaryWOl0402b SAMPLE 4nm1 14 31 o \ C h e m ~ ~ I l a r y ~ O l WbO Z SAMPLE 4/3/01 1500 D\ChemWillaryW010402b SAMPLE 413101 15 26 D\ChemWilIaryWOlC402b SAMPLE 4/3/01 15 57 D \ChemWillaryW010402b SAMPLE 4 n m i 16 26 D \Cham~llaryV1010402b SAMPLE 4/3/01 17 24 D \ChemWillaryW010402b SAMPLE 413101 17 36 D ChemWtllaryW010402b SAMPLE 40mi 18 07 D \ChemWilIaryW010402b SAMPLE 4/3/01 18 36 O\ChemWilla~W010402b SAMPLE 4/3/01 19 05 D \ChemWillaryW010402b SAMPLE 4/3/0119 33 O!ChemWillaryW010402b SAMPLE 4/3/012002 O\ChemW~llary\HO1040b2 SAMPLE 4/3/0120 31 D !ChemWillaryW010402b SAMPLE 4/3/0121 00 O\ChemWillaryW010402b SAMPLE 4 n m i 21 29 O\ChemWillaryW010402b SAMPLE 41301 21 58 \ChemWillaryW010402b SAMPLE 4/3/04 22 55 0 !ChemWilleryW010402b SAMPLE 4nmi 23OI D \ChemWillaryW010402b SAMPLE 4 ~ m2i 31 0 \ChemWillaryWO10402b SAMPLE 4/4/012 45 D \ChemWilla~WO1040b2 SAMPLE flle HILL0075 D HlLLW76.D HILLOO9O.D HILLW91.D HILLOW3 D HlLLW95.0 HILL0097.D HILLWQ9.D HILL0101 D HILLO103.D HILL0105 D HILL0107.D HlLL0109.D HILLO113.D HlLL0114.D HILLO1IG.D HlLL0118.D HILL0120 D HILL0122 0 HILL0124.D HILL0126.D HILLO128.0 HILLO130.D HILL0132.D HILL0136.D HlLL0137.D HILL0139.D HILL0141.0 HILL0143.D HILL0145 0 HILL0147.0 HILL0149.D HILLOl51.D HILL0153 D HILL0155 0 HILL0159.D HILL0160 D HILL01740 HILL0175.D Sample Name TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4602 MeOH TN-A 4802 MeOH TN-A 4602 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TNA 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TNA 4802 MeOH TNA 4802 MeOH TNA 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TNA 4802 MeOH TNA 4802 MeOH TNA4602 MeOH TN-A 4802 MeOH TNA 4602 MeOH TN4 4602 MeOH TNA4802 MeOH TN-A 4802 MeOH TNA4602 MeOH TN4 4802MeOH TN-A 4802 MeOH TN4 4802 MeOH TN-A 4802 MeOH TNA 4802 MeOH TN-A4802 MeOH TN-A 4602 MeOH TNA4802 MeOH TN-A 4802 MeOH TNA 4602 MeOH H010402b.xls Miss lnfcompound Na UT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS A*. 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 '0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound NanRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A 0 0 5425 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 m Amount 0 0 0 0 56059 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 page 2 of 3 BACK TO MAIN . H010402b.xls C' Inj Date Batch 4/3/01 6 49 D \ChemWillaryW010402b 4i-31017 18 DChemWillaryW010402b 4/3/01 7 47 D \Chem\HillaryW010402b 4/3/01 8 16 DChemWillaryWOl0402b 4/3/01 8 45 D\ChemWillaryW010402b 4/3/01 9 14 D\ChemWillaryW010402b 4 1 3 ~ 1 942 D ChemVlillwjWO10402 b 4/3101 10 11 DChemWilIaryW010402b 4/3/01 1040 DChernW1llaryWO10402b 4/3/01 11 09 DChemWilIaryW010402b 4/3/01 1123 DChemWIIlaryW010402b 4/3101 11 38 DChemWillaryWOl04OZb 4/3/01 12 21 DChemWillaryW010402b 4nm1 12 50 DChemWillaryW010402b 4/3/01 13 19 DChemWillaryW010402b 4/3/01 1348 DChemW1llaryW010402b 4/3/01 14 17 DChemWillaryW010402b 4/3/01 14 45 D ChemWillaryW010402b 4/3/01 15 14 DChemWillaryWOlO402b 4/3/01 1543 D ChemWilIaryW010402b 413101 16 12 D ChemVlill~Wo10402b 4/3/01 16 40 D ChemWillaryW010402b 4/3/01 1655 D ChemWillaryW010402b 4/3/01 1709 DChernW1llaryW010402b 4/3/01 1752 DChemUiiIIaryWOl0402b 4/3/01 1821 D ChemWillaryW010402b 4/3/01 1850 D ChemWillaryW010402b 4/3/01 19 19 DChemWillaryW010402b 4/3101 1948 D\ChemWllla1yW010402b 4/3/0120 17 D\ChernW1UaryWO10402b 4/3/0120 46 D ChemWillaryWOl0402b 4/3/01 21 14 D\ChemWlllaryW010402b 4/3/01 21 43 DChemW1IIa~Ol040b2 4/3/0122 12 D \ChemWillaryW010402b 4/33/0122 27 D \ChemWillaryW010402b 4/3/0122 41 D\ChemWillayW01~02b SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File HILL0092.D HILLW94.D HILL0WG.D HILL0098.D HlLLOlW.D HtLW102.0 HILL01M.D HILL0106.D HILL0108.D HILLOl1O.D HILLO1ll.D HILL0112.D HILL0115.D HILLO117.D HlLLOl19.D HILLO12l.D HlLL0123.D HILL0125.D HILL0127.D HILL0129.D HILLO131.0 HILL0133.D HILL0134.D HILL0135 D HILL0138.D HILL0140D HILL0142D HILL0144 D HILL0148D HILL0148D HILLOISOD HILL0152D HILL0154D HILL0156 D HILL0157 D HILL0158 D SimDle Name 5 m g i PFOSSudy Number E001311 5mgA PFOS Study Number E00-1311 5mgA PFOS Study NJmber E001311 5mgA PFOSShdy Number EW-1311 5mgA PFOS SlLdy Number E001311 smgh PFOS Study Number EW-1311 5Wk PFOS Sludy Nlul?OwEW-1311 5mgA PFOS Study Number EW-1311 5mgA PFOS Study Nurnber EW-1311 5mgk PFOSSlddy humber E00-1311 5 ndmL PFOS In MeOH 2% 5 q / m L PFOS in MeOH Smgk PFOSStudy Number EW-1311 5W PFOS SlLdy Number EW-1311 5mgA PFOS Study Ndmber EW-1311 5mgll PFOSStudy Number EW.1311 S M PFOS Study Number EW-1311 5mgA PFOS Study Numbsr E001311 5mgA PFOSS M y Numwr E001311 smen 5mgL PFOS Saay NJmber EW-1311 PFOSstudy N ~ EW W-I~II 5 M PFOS S M y Nmber EW-1311 5nprmL PFOS In MeOH 2% 5 ngmL PFOS on MeOH Smpll PFOS Sludy Number EW-1311 5mgk PFOS Study Number EW-1311 5mgA PFOS Study Number EW-1311 5mgll PFOS Study Number EW-1311 SmgA PFOS Study Number E00-1311 5mgA PFOS Study Number E00-1311 5mgllPFOS Study NurnberEW-1311 5mgllPFOSStudyNumberE00-1311 Smgk PFOS Study Number EW-1311 5mgA PFOS Study Number EM)-1311 5 n$mL PFOS in MeOH 250 5 ngmL PFOSin MeOH Mire InfCompound Na RT nmr Am o u n t Compound NanRT Am Amount THPFOS 5106 1643044 254 ISTD>130% PFOS 533 209598 6621818 THPFOS 5112 1594154 254 ISTD>130% PFOS 5329 3430184 1142188 THPFOS 5106 1605329 254 ISTD>130% PFOS 5323 73592 2392023 THPFOS 5097 1598522 254 ISTD>130% PFOS 5314 58889 1919775 THPFOS 5103 1558836 254 ISTD>lM% PFOS 5321 63584 2 130565 THPFOS 5105 1574536 254 ISTD>130% PFOS 5322 3247504 1093654 THPFOS 5105 1563077 254 IST0>130% PFOS 5329 72818 2430454 THPFOS 5098 1582850 254 lSTD>l30% PFOS 5322 99365 3268414 THPFOS 5098 1574580 254 ISTD>13O% PFOS 5323 173732 5731799 THPFOS 5099 1545068 254 ISTD>130% PFOS 5323 3282444 1127346 THPFOS 5105 1418003 254 PFOS 5322 111688 4096218 THPFOS 5105 1327511 254 PFOS 5322 4689629 190655 THPFOS 5087 1772997 254 ISTD>130% PFOS 5319 178540 5232697 THPFOS 5091 1580363 254 ISTD>130% PFOS 5309 143612 472336 THPFOS 509 1599960 254 ISTD>130% PFOS 5314 73070 2363101 THPFOS 5098 1583275 254 ISTD>130% PFOS 5322 3194485 1069281 THPFOS 5093 1507671 254 ISTD>l3O% PFOS 531 74289 2569598 THPFOS 5 1 1613223 254 ISTD>l3O% PFOS 5317 73272 2370152 THPFOS 5099 1542538 254 ISTD>130% PFOS 5316 125073 4216276 THPFOS 50% 1558630 254 ISTD>130% PFOS 5316 3322158 1131153 THPFOS 5097 1638237 254 ISTD>130% PFOS 5314 132485 420529 THPFOS 5104 1636599 254 ISTD>13O% PFOS 5314 188089 5969764 THPFOS 5103 1485841 254 PFOS 5313 102882 3603134 THPFOS 5112 1395726 254 PFOS 5322 4803174 1855252 THPFOS 5093 1654266 254 ISTD>130% PFOS 531 189555 595208 THPFOS 5099 1604691 254 ISTD>130% PFOS 5318 3364843 1112337 THPFOS 5 1 1567626 254 ISTD>130% PFOS 5317 70689 2353252 THPFOS 5098 1657152 254 ISTD>130% PFOS 5315 150169 4710199 THPFOS 5098 1628130 254 ISTD>13O% PFOS 5308 256726 8 187031 THPFOS 5105 1586581 254 ISTD,130% PFOS 5315 3420939 1144608 THPFOS 5106 1594869 254 ISTD>130% PFOS 5316 197132 641957 THPFOS 5105 1613975 254 ISTD>130% PFOS 5315 178892 5757917 THPFOS 5104 1847163 254 ISTD>130% PFOS 5314 88721 2807077 THPFOS 5098 1616736 254 ISTD>130% PFOS 5308 3291692 1079254 THPFOS 5097 1495313 254 ISTD>130% PFOS 5308 111995 3895974 THPFOS 5099 1408690 254 PFOS 5309 4791463 1832822 82% 76% 72% 74% 78% 73% page 3 of 3 BACK TO MAIN R010404 extemai sld quantds LG, Sample Batch R010404.b, analyzedon Hillary 044441. PFOSAdsorbmesorb sampler. Matrix: SolllSlplSed. Standard cuwe range used for calibration01 samples: IO-lW2 n#mL Batch method: UO1MM.m (ENrn.1 Standard Quat) Inj Date Batch 4/4/01 17 33 D \Chem\RurhW010404 b SampTyP SAMPLE 4/4/01 1748 D \ChemWurhW010404b CALlB-1 414101 18 02 DChemWushW0104M b CALIB-2 4/4/01 16 16 D \Chem\RurhW010404b CALIB-3 4/4/01 18 31 D C h e ~ ~ R ~ s ~ ' i ? 0b1 0 4C~ALiB-4 4/4/01 18 45 D ChemWurh\R010404 b SAMPLE 4/4/01 18 59 D Chem\RushW010404b cALiB-5 4/4/01 19 14 D \Chern\RurhW010404b CALIB-6 4/4/01 19 28 D Chem\Rurh\R010404 b CAUB-7 4/4/011943 DChem\Rush\ROlD404b CALIB-8 4/4/01 19 57 D ChemRushW0104C-i b SAMPLE 4/410120 11D \Chem\Rush\RO10404b CALIB-9 4/4/0120 26 D \ChemRush\RO10404b CALIB-IO 4/5/01 14 08 D ChemWurhW010404 b SAMPLE 4/5/01 1422 D ChemWush\R010404b CALIB-11 4/5/01 14 36 D \ChemWurh\R010404b CALIB-12 4/5/01 1451 D CtvemWushW010404b CALIB-13 4/5/01 1505 D \ChemWurh\R010404b CALIB-14 415101 15 19 D\Chem\Rush\R010404b SAMPLE 4/5/01 15 34 D ChemRushW010404 b CALlB-15 4/5m11548 D \ChemWurh\R010404b CALIB-18 4/5/01 16 03 DChemRush\R010404 b CAUB-17 4/5/01 16 17 D \Chem\RushW010404b CAUB-18 4151011631 D \ChsmWush\RO10404b SAMPLE 4/5/01 1646 D Chem\RushW010404b CALlB-19 4/5/01 17 00 D lChemRushW010404b CALIB-20 nl. RUSH0017 D RUSH0018 D RUSHW19 D RUSH0020 D RUSH0021 D RUSH0022 D RUSH0023 D RUSH0024 D RUSH0025 D RUSH0026 D RUSHW27 D RUSH0026 D RUSHW29 D RUSHW96 D RUSH0099 D RUSH0100 D RUSH0101 D RUSH0102 D RUSH0103 D RUSH0104 D RUSH0105 D RUSH0108 D RUSH0107 D RUSH0108 D RUSHOlO9.D RUSHOl1O.D Sample Name 0 ngmL PFOS in MeOH 2.5 n@mLPFOSin MeOH 5 nglmL PFOS in MeOH 1 0ndmL PFOSin MeOH 25 N m L PFOSin MeOH 4 0 ngimLPFOSin MeOH 50.1 n$mL PFOSin MeOH 75.1nglmLPFOSin MeOH 100.2nglmL PFOSin MeOH 2M5 nUmLPFOSin MeOH 400.8n&nL PFOSin MeOH M1ngmL PFOSin MeOH 1002ngImLPFOSin MeOH 0 ngmL PFOS in MeOH 2.5 n#mL PFOSinMeOH 5 nglmL PFOS in MeOH 10n#mL PFOSin MeOH 25 n p L PFOSin MeOH 40 WmL PFOSinMeOH 50.1nglmLPFOSin MeOH 75.1 WmL PFOS in MeOH 100.2nNmL PFOSin MeOH 250 5 n#mL PFOSin MeOH 4W.8 nglmL PFOS in MeOH 501 ngmL PFOSinMeOH 1W2 nglmLPFOSIn MeOH Miss IniCompOundNaRT THPFOS THPFDS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Ana 5.582 5 579 5 591 5 595 5 569 5 587 558 6 588 5 598 5 569 5 585 5 588 5 581 5 574 5 579 5 581 5 567 5 573 5 585 5 578 5 577 5 565 5 588 5 589 5584 5 561 Amount 583312 254 598272 254 61sB09 254 603517 254 a229 254 607817 254 012230 254 820258 254 614982 254 641474 254 615848 254 625082 254 640512 254 567197 254 573134 254 587603 254 566302 254 587276 254 550302 254 571777 254 568082 254 565114 254 573672 254 560876 254 557017 254 575273 254 Compound N i R T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A 0 5.789 5 801 5 805 5 792 5 79 5 79 5 799 5 799 5 792 5 788 5 798 5 784 0 5 782 5 764 5 777 5 783 5 788 5 781 5 787 5 768 5771 5 772 5 707 5 764 m Amount 0 0 170517 0 216580 OW3813 300075 5901514 587394 2529359 825934 4428921 998065 5734062 1408399 88 63623 174Mx9 114 5699 3758226 2843931 5347186 4324344 6357305 533 1193 11034302 1065 901 0 0 147436 0 189460 0 258280 290194 519265 21 77576 736331 3773328 897827 49 75867 1258308 77.07207 1578440 1018738 ~ ~ 5 0 4 22248 4373 4782617 378.3062 5638078 4609056 9804704 9152275 1% 53% 101% 111% 114% 118% 114% 114% 108% 106% 106% 0% 29% 87% 94% 99% 103% 102% 99% 94% 92% 91% Averam: 591028,653 20847.711Q XRSD: 4.5% 708337 +30%: 413720 -30%: Inj Date Batch 4 1 4 ~ 137 05 DChemWushW010404b 4/4/01 17 19 DChemWurhW010404 b 41410120 40 D\chem~ushWO10404b n i 4/4/01 20 54 DChemWurhW010404 b 4/5/010 01 D\Chem\Rurh\R010404b 4/5/01 0 15 D ChemWurhW010404 b 2 i n 4/5/013 22 D \Chem\Rush\R010404b 4/5/013 37 D ChemWurhWO10404b 4/5/016 54 D \Chem\RushW010404b 4/5/01 7 08 D ChemWush\R010404b 4/5/01 10 15 DChem\RushW0104W b 4/5/01 10 30 D \ChemWurh\ROlM04 b 4l5101 12 25 D\Chem\Rurh\R010404b 415101 13 39 D EhemWurhW010404 b 41510113 53 D Chem\Rush\R010404b 4/5/01 17 14 DChemWushW010404 b 4/5/01 17 29 D ChemWurhW010404 b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File RUSH0015 D RUSH0016 D RUSH0030 D RUSH0031 D RUSH0044 D RUSHM)45 D RUSH0058 D RUSH0059 D RUSHW72 D RUSH6373 D RUSH0086 D RUSH0067 D RUSHW95 D RUSHW96 D RUSHW97 D RUSH0111 D RUSH0112 D Sample Name TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 M ~ O H TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH MISC lnkompound NaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS AIU 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amwnt 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound N a R l PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Ana 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 4 0 w page 1 of 2 BACK TO MAIN -0 9) (P (D ROIMM external6td q ~ n L x l i Inj Date Batch 4/4/0121.09 D.\Chem\Rush\R010404.b 4/4/01 21:23 D'\Chem\RuSh\R0104M.b 4/4/0121 37 D \Chem\Ruih\R010404b 41410121 52 D \Chern\Rush\R010404 b 41410122 06 D \ChemiRushW010404b 4/4/0122 20 D \Cham\Rush\R010404b 4/4/0122 35 D \Chern\Rurh\R010404b 4'4/0l 22 49 0 Ciiem8ushW010404 b 4/5/0123 03 D \Chem\RurhW010404b 4/5/01 23 18 D \Chern\RurhW010404b 4/5/0123 32 D \Chem\RurhW010404b 4/5/0123 47 D \Chem\Ru5hR010404b 415/01030 D ~hem~urh\R01040b4 4/5/01 0 44 D \Chem\Rurh\ROIMM b 4/5/010 58 D\Chem\Rurh\R010404b 4/5/01 1 13 D \Chern\Rush\R010404 b 4/5/01 127 D \ChemRush\R010404b 4/5/01 1 42 D \Chem\Rurh\R010404b 4/5/01 156 D \ChemWurhW010404b 4/5/012 10 D \Chem\Rush\R010404b 4/5/012 25 D \Chem\Rush\R010404b 4/5/012 39 D \Chem\Rush\R0104M b 4/5/01 2 53 D \Chem\Rush\R010404 b 4/5/01 3 08 D \ChemWurh\RO10404 b 4/5/013 51 D \Chern\Rurh\R010404b 4/5/014 06 D \Chem\Rush\ROlMMb 4/5/014 20 D \Chem\Rurh\R010404b 4/5/014 34 D \Chem\Rurh\R010404b 4/5/014 49 D \ChemRurh\R010404b 4/5/01 5 03 D \Chem\Rurh\R010404b 4/5/015 17 D \Chem\Rurh\R010404b 4/5/01 5 42 D \Chem\Rush\R010404b 4/5/015 56 D \Chem\RushW010404b 415101 6 11D \ChemWush\R010404b 4/5/016 25 D \Chem\Rurh\R010404b 4/5/016 39 D Chem\RushWO10404b 4/5/017 23 D ChernWurhW010404b 4/5/017 37 D Fhem\Rush\R010404b 4/5/01 7 51 D \Chem\Rurh\R010404b 415/018 06 D \Chem\Rush\R010404b 4/5/01 8 20 D \Chem\Rurh\R010404b 4/5/01 8 34 D \Chem\Rurh\R010404b 4/5/01 8 49 D \ChemWurh\R010404 b 4/5/01 9 03 D \Chem\Rurh\R010404b 4/5/01 9 18 D\Chem\Rurh\R010404 b 4/5/019 32 D ChemWuShiR010404b 4/5/019 46 D \Chem\Rurh\ROIMMb 415101 1001 D \Chem\Rurh\R010404b 4/5/01 1044 D \Chsm\Rurh\R010404b 4/5/01 10 58 D \Chern\RurhW0104Mb 4/5/01 11 13 D \ChemWush\R010404 b 4l5101 1127 D \Chem\Rush\R010404b 4/5/01 1142 D \Chem\RurhW010404b 4/5/01 1156 D\Chem\Rush\R010404b 4/5/01 12 10 D \Chern\Rurh\R010404b SampTyyp SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE Flle RUSHW32.D RUSHW33 D RUSH0034 D RUSHW35 D RUSH0036 D RUSH0037 D RUSH0038 D RUSH0039 D RUSH0040 D RUSH0041 D RUSH0042 D RUSH0043 D RUSH0046 D RUSH0047 D RUSH0048 D RUSH0049 D RUSHOOM D RUSH0051 D RUSHW52 D RUSHW53 D RUSH0054 D RUSHW55 D RUSH0056 D RUSH0057 D RUSHOOM) D RUSHWel D RUSHW62 D RUSHWe3 D RUSH0064 D RUSHM)65 D RUSHW68 D RUSHW67 D RUSHWeB D RUSHW69 D RUSH0070 D RUSH0071 D RUSHW74 D RUSH0075 D RUSHW76 D RUSH0077 D RUSHW78 D RUSHW79 D RUSH0080 D RUSH0081 D RUSHM)82 D RUSH0083 D RUSH0084 D RUSHCQ85 D RUSHW88 D RUSH0089 D RUSHW90 D RUSH0091 D RUSH0092 D RUSH0093 D RUSH0094 D Simple Name Study Number EW-1311 Study NumberE001311 Study Number E00-1311 Study Number EW-1311 Study Number EW-1311 Study Number E001311 Study Number EW-1311 Study Number EM)-1311 Study Number E001311 Study NumberEm1311 5 ng/mLPFOS in MeOH 250 5 n g h L PFOS in MeOH Study Number E00-1311 Study Number EW-1311 Study Number EW-1311 Study Number EM)-1311 Study Number EW-1311 Study Number EW-1311 Study Number EW-1311 Study Number E00-1311 Study Number EW-1311 Study NumberEm1311 5 nWmL PFOS m MeOH 250 5ng/mL PFOSin MeOH Study Number E00-1311 Study Number EW-1311 Study Number E00-1311 Study Number EW-1311 Study Number UX)-1311 Study Number E001311 Study NumberE00-1311 Study Number E00-1311 Study Number E00-1311 Study NumberEm1311 5 n@mLPFOSm MeOH 250 5 ng/mL PFOS in MeOH Study Number E001311 Study NumberE001311 Study NumberEW-1311 Study NumberEm1311 Study Numbar E001311 Study Number EW-1311 Study NumberEW-1311 Study Number EW-1311 Study NumberEW-1311 Study Number E00-1311 5 ngimL PFOS m MeOH 250 5 WmL PFOSm MsOH Study NumberE001311 Study NumberE001311 Study NumberEM)-1311 Study Number E00-1311 Shdy Number EOO-1311 5 nUmLPFOSm MeOH 250 5 ng/rnL PFOSm MeOH Mlrc InfCompound NaRT Ama ' THPFOS 5 589 THPFOS 5 589 MPFOS 5 574 THPFOS 5 596 THPFOS 558 THPFOS 5 574 THPFOS 5 581 THPFOS 5 578 THPFOS 5 579 THPFOS 5 575 THPFOS 5 575 MPFOS 5 582 THPFOS 5 57 THPFOS 5 58 THPFOS 5 608 THPFOS 5 586 THPFOS 5 565 THPFOS 5 587 THPFOS 5 578 THPFOS 5 578 THPFOS 5 588 THPFOS 5 594 THPFOS 5 589 THPFOS 5 589 THPFOS 5 579 MPFOS 5 581 THPFOS 5564 THPFOS 5 565 THPFOS 5 565 THPFOS 5 567 THPFOS 5 575 THPFOS 5 635 THPFOS 5 596 THPFOS 5 614 THPFOS 5 616 THPFOS 5 598 THPFOS 5 581 THPFOS 5 581 THPFOS 5 596 THPFOS 5 59 THPFOS 5 582 MPFOS 5 594 THPFOS 5 603 THPFOS 5 597 THPFOS 5 585 THPFOS 5 582 MPFOS 5 589 THPFOS 5 5e4 MPFOS 5 574 THPFOS 5 575 THPFOS 5 574 THPFOS 5 581 THPFOS 5 582 THPFOS 5 586 THPFOS 5 571 Amount 867461 254 843971 254 856577 254 103366g 254 7.84276 254 797188 254 753794 254 795069 254 817238 254 860427 254 566116 254 559850 254 862542 254 787133 254 934664 254 863820 254 1126734 254 942383 254 808043 254 978478 254 1316674 254 899797 254 619700 254 583040 254 904765 254 896633 254 902428 254 898486 254 913892 254 958949 254 747595 254 953521 254 921327 254 956257 621485 591317 672912 921483 254 914616 254 929161 254 924098 254 903461 254 884953 254 998451 254 941330 254 1193912 254 681210 254 626988 254 789982 254 1022922 254 970087 254 999735 254 808526 254 685035 254 844837 254 Compound NaRT ARa Amount ISTDrlJO% PFOS 0 0 '0 ISTD>130% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD,130% PFOS 0 0 0 ISTD,13Wb PFOS 0 D O ISTD430% PFOS 0 0 0 PFOS 0 0 0 ISTD>13O% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 PFOS 0 0 0 PFOS 5.785 3853083 275.043 ISTD>130% PFOS 0 0 0 ISTD430% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD113Wb PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTDr1309L PFOS 0 0 0 I S T D 1 3 W PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD>l30% PFOS 0 0 0 PFOS 0 0 0 PFOS 5.792 3610058 271.2329 ISTD>l30% PFOS 0 0 0 ISTDz13046 PFOS 0 0 0 ISTD>13O% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 tSTD>130% PFOS 0 0 0 ISTDz130% PFOS 0 0 0 PFOS 5.778 2604047 184.7008 ISTDrl30% PFOS 5.845 267284 3.547403 ISTD>130% PFOS 0 0 0 0 0 0 0 0 0 5.801 3590033 269.4627 5.792 3440014 256.2652 ISTD>130% PFOS 0 0 0 ISTDr130% PFOS 0 0 0 ISTD,130% PFOS 0 0 0 ISTDrl3O% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTDrl30% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD>13O% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 PFOS 0 0 0 PFOS 5.794 3481787 259.9287 ISTD>130% PFOS 5.777 2772186 I98 8805 ISTDz130% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD>130% PFOS 0 0 0 ISTD>130% PFOS 5.785 225U127 1555797 PFOS 0 0 0 PFOS 5.775 3467170 258.6458 0.0% 109.8% 0.0% 108.3% 0.0% 107.6% 0.0% 103.8% 0 0% 103.3% page 2 of 2 BACK TO MAIN Sample Batch HOlO329.b, analyzed on Hillary 03-29-01. PFOS AdsorblDesorb samples. Matrix: SoillSlglSed. Standard CUNB ranae used for calibration of samples: 5-1002 ng/mL (2.5 nglmL s l d not included due to (he higher sample concentration range). Batch method H010329.m In1Date Batch SampType File Sample Name MisC InfCompounb(T 3R9/01 17 54 D \ChemUiillaSAMPLE HILLWIG D 0 ndmL PFOS in THPFOS 3/29/01 1809 D:\Chem\HillCALlB-l HILLOO17.D 2.5 &lmL PFOS I THPFOS 3/29/01 1823 D:\ChemiHillCALIE-l HILL0018.0 5 ng/mL PFOS in THPFOS 3/29/01 18:38 C?!Chem\HiII CALlE-2 HILL0019.D 10nglmL PFOS i THPFOS 3129101 1852 D:\Chem\HillCALlB-3 HlLL0020.D 25 nglmL PFOS in THPFOS 3/29/01 19 06 D \Chem\H liaSAMPL.5 HILLOO~I 0 4 0 n@mLPFOS in THPFOS 3/29/01 1921 O\Chem\HillCALIE-4 HILLO0ZZ.D 50.1 nglmL PFOS THPFOS 3/29/01 1935 D:\Chem\HillCALIE-5 HILL0023.D 75.1 n@mLPFOS THPFOS 1/29/01 19:49 D:\Chem\HillCALIE-6 HlLL0024.D 100.2 nglmL PFO THPFOS 3/29/01 20:M D:Chem\HillCALlB-7 HILLOO25.D 250.5 nglmL PFO THPFOS 3/29/01 2O:t8 D:\Chem\HillCALIE-8 HILL0026.D 400.8 ng/mL PFO THPFOS 3/29/01 20:33 D:\Chem\HillCALIE-9 HILL0027.D 501 nglrnL PFOS THPFOS 3/29/01 2047 D:\Chem\HillCALlE-10 HILL0028.D 1002 ng/mL PFOS THPFOS 3/31/01 16 58 0 \Chem\HhSAMPLE HILL0212 D 0 n@mLPFOS m THPFOS 3/31/01 1713 D:\Chem\HillCALIB-11 ~iLL0213.D2.5 ng1mL PFOS I THPFOS 3131101 1727 D:\Chem\HillCALIB-11 HILL0214.D 5 nglmL PFOS in THPFOS 3/31/01 17:41 D:\Chcm\HillCALIB-12 HILL0215.D 10nglmL PFOS i THPFOS 3131101 1756 D.\Chem\HillCALIB-13 HILLO216.D 25 nglmL PFOS in THPFOS 3/31/01 18 10 D\ChemWr.laSAMPLE HILL0217 D 4 0 n@mLPFOS in THPFOS 3131101 1825 D : \ C ~ ~ ~ \ H I I ~ C A L I EH-IL~L~0218.D 50.1 nglmL PFOS THPFOS 3/31101 1839 D.\Chem\HillCALIB-15 HlLLOZl9.D 75.1 nglmL PFOS THPFOS 3/311011853 D:\Chem\HillCALIE-l6 HILL0220.D 100.2 nglmLPFO THPFOS 3/31101 19:08 D:\Chem\HillCALlE-17 HILL0221.D 250.5 nglmL PFO THPFOS ~ 3 1 1~9221 D:\Chem\HillCALIB-18 HILL0222.D 400.8 nglmL PFO THPFOS 3/31/01 19:36 D:\Chcm\HillCALIE-19 HILL0223.D 501 nglmL PFOS THPFOS 3/31/01 1951 D:\ChemWillCALIE-ZO HILL0224.D 1002nglmL PFOS THPFOS Area Amount 5.098 960831 254 5.098 970141 254 5.098 1088770 254 5.088 954633 254 5.093 962518 254 5.092 969520 254 5.098 976505 254 5.093 967966 254 5.094 957847 254 0 0 0 5.091 969149 254 5.092 973244 254 5.093 1000466 254 5.07 842487 254 5.on 835488 254 5.078 850162 254 5.07 814436 254 5.071 813666 254 507 800797 254 5.076 805652 254 5.07 799837 254 5.071 789814 254 5.073 812044 254 5.079 775631 254 5.07 783605 254 5.077 814065 254 CompounRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 5.323 5.315 5.312 5.324 5.316 5.315 5.317 5.318 0 5.316 5.316 5.31 0 5.308 5.302 5.301 5.295 5294 5.294 5.294 5.295 5.29 5.303 5.288 5.294 Amount 0 0 68338 0.677157 154846 3.650955 209554 6.883663 550443 2260741 874302 37.47291 1094742 47.43103 1620491 72.81732 2093623 96.65124 0 0 7386300 370.5128 B ~ ~ O D Mm . 6 5 a s 17048775 914.463 0 0 W J ~ I 0.85a56i 109759 2.805341 179020 7.088001 495753 24.4548 779905 4089347 981753 52.01963 1483559 81.31145 1929027 108.8196 4679248 272.5867 6867611 437.8109 8368086 541.0708 15279147 1050.288 73.0% 68.8% 90.4% 93.7% 94.7% 97.0% 96.5% 0.0% Sample level i n Vial too low 92.4% 90.8% 93.3% 58.1% 70.9% 97.8% 102 2% 103.8% 108.3% 108.6% 68.0% 109.2% 108.0% 104.8% Averaqe: 857280.5 _ Std D_ ev: _ 1962_ 00.6 _XRS_D:-22.9% 1114465 +30%: 6W096 -30%: BACK TO MAIN In1 Date Batch SampType 3/29/01 17 26 D \Chem\HdIaSAMPLE 3/29/01 17 40 0 \ChemWillaSAMPLE 3/29/01 21 01 0 \Chem\HillaSAMPLE 3/29/01 21 16 D \Chem\HtllaSAMPLE 3/29/01 21 30 D \Chem\HdlaSAMPLE 3/30/01 0 23 0 \ChemWillaSAMPLE 3/30/01 0 37 0 Charmnti~aSAMPLE 3/30/01 3 44 D \Chem\HillaSAMPLE 3/30/01 3 59 D \ChemWillaSAMPLE 3/30/01 7 06 D \ChemWillaSAMPLE 3/30/017 20 D \ChemWdlaSAMPLE 3/30/01 10 28 D \ChemWillaSAMPLE 3/30/01 10 43 D \Chem\HillaSAMPLE 3/30/01 13 50 D \Chem\HillaSAMPLE 3/30/01 14 05 D\ChemWillaSAMPLE 3/30/01 17 12 D \ChemUlillaSAMPLE 3/30/01 17 27 0 \ChemWillaSAMPLE 3/30/01 20 34 0 \Chem\HillaSAMPLE 3/30/01 20 48 D \ChemWdlaSAMPLE 3/31/01 23 27 o \ChemWilIaSAMPLE 3/31/01 2341 0 \ChemWiIIaSAMPLE 3/31/01 2 48 D \Chem\HtllaSAMPLE 3/31/01 3 03 D\Chem\HillaSAMPLE 3/31/01 6 24 D \Chem\HillaSAMPLE 3/31/01 6 39 D \Chem\HillaSAMPLE 3/31/01 9 46 D \ChemWillaSAMPLE 3/31/01 10 00 D \ChemWillaSAMPLE 3/31/01 13MI D \Chem\HillaSAMPLE 3/31/01 13 22 D \Chem\HillaSAMPLE 3/31/01 16 30 D\Chern\li~llaSAMPLE 3/31/01 16 44 D \Chem\HillaSAMPLE 3/31/01 20 05 D \Chem\HillaSAMPLE 3/31/01 20 20 D \Chem\HillaSAMPLE File Sample Name MIS:( InfCornpound3T HILL0014 D TN-A 4802 MeOH THPFOS HILL0015 D TN-A4802 MeOH THPFOS HILL0029 D TN-A 4802 MeOH THPFOS HILL0030 D TN-A4802 MeOH THPFOS HILLW31 D TNA4802 MeOH THPFOS HILLW43 D TN-A 4802 MeOH THPFOS hlL&O44 D IN-A 4802 MeOH THPFOS HILL0057 D TN-A 4802 MeOH THPFOS HILL0058 D TN-A 4802 MeOH THPFOS HILL0071 D TN-A4802 MeOH THPFOS HILL0072 D TN-A4802 MeOH THPFOS HILL0085 D TNA4802 MeOH THPFOS HILL0086 D TNA4802 MeOH THPFOS HILL0099 D TN-A 4802 MeOH THPFOS HILL01W D TN-A 4802 MeOH THPFOS HILLO113D TN-A4802 MeOH THPFOS HILL0114 D TN-A 4802 MeOH THPFOS HILL0127 D TN-A4802 MeOH THPFOS HILL0128 D TNA4802 MeOH THPFOS HILL0139 D TNA4802 MeOH THPFOS HILL0140 D TN-A 4802 MeOH THPFOS HILL0153 D TN-A 4802 MeOH THPFOS HILL0154 D TN-A 4802 MeOH THPFOS HILL0168 D TN-A 4802 MeOH THPFOS HILL0169 D TN-A4802 MeOH THPFOS HILL0182 D TN-A4802 MeOH THPFOS HILL0183 D TN-A 4802 MeOH THPFOS HILL0196 D TN-A 4802 MeOH THPFOS HILL0197 0 TN-A 4802 MeOH THPFOS HILL0210 D TN-A4802 MeOH THPFOS HILL0211 D TN44802 MeOH THPFOS HILL0225 D TN-A 4802 MeOH THPFOS HILL0226 D TN-A 4802 MeOH THPFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0' 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 CompounRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area Amount 5392 13019 0 0 0 0 5386 23896 0 0 0 0 0 0 0 0 0 0 0 0 0 D 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 BACK TO MAIN In] Date Batch SampType File Sample Name Mlrc InfCompoundXT Area Amount CompounRT Area Amount 3/29/01 21 45 D \Chem\HillaSAMPLE HILL0032 D lOmg/mL PFOS Study NumTHPFOS 5092 941565 254 PFOS 5317 7685289 3998253 3/29/01 21 59 D \Chem\HillaSAMPLE HILL0033 D IOmg/mL PFOS Study NumTHPFOS 5 092 955051 254 PFOS 5316 8722101 4533549 3/29/01 22 13 D \Chem\HillaSAMPLE HILL0034 D lOmg/mL PFOS Study NumTHPFOS 5091 947677 254 PFOS 5315 7434958 3826G37 3/29/01 22 28 D \Chem\HillaSAMPLE HILL0035 D 10mglmL PFOS Study NumTHPFOS 5093 777892 254 PFOS 5 3 1 9661038 6436158 3/29/01 22 42 D \Chem\HillaSAMPLE HILL0036 D 50mglmL PFOS Study NumTHPFOS 5085 I089404 254 PFOS 5302 5246893 2244704 3/29/01 22 56 0 \Chen'Hi"aSAMPLE HILL0037 D 5OnglmL PFOS Study NumTHPFOS 5083 1w0640 254 PFOS 5308 5197203 221 9073 3/30/01 23 11 D \ChemWdlaSAMPLE HILL0038 0 50mgmL PFOS Study NumTHPFOS 5084 1030788 254 PFOS 5308 4771646 2150835 3/30/01 23 25 D \Chem\HillaSAMPLE HILL0039 D 50mglmL PFOS Study NumTHPFOS 5077 1073111 254 PFOS 5301 9471261 4363103 3/30/01 23 40 D \ChemWillaSAMPLE HILL0040 D OmglmL PFOS Study NumWHPFOS 5085 918338 254 PFOS 5309 540709 233661 3/30/01 23 54 D \ChemWillaSAMPLE HILL0041 D 5 nglmL PFOS in MeOH THPFOS 5085 1091788 254 PFOS 5302 162150 3734831 74.7% 3/30/01 0 08 D \ChemWillaSAMPLE 3/30101 0 52 D \Chem\HillaSAMPLE 3/30/01 1 06 D \Chem\HIIIaSAMPLE 3/30/01 1 20 D \Chem\H!llaSAMPLE 3/30/01 1 35 D \ChemWillaSAMPLE 3/30/01 1 49 0 \Chem\HillaSAMPLE HILL0042 D 250 5 ngmL PFOS inMeOTHPFOS HILL0045 D OmglmL PFOS Study NumWHPFOS HILL0046 D OmglmL PFOS Study NumWHPFOS HILL0047 D hng/mL PFOS Study NumbTHPFOS HILL0048 D 0 5mglmL PFOS Study NunTHPFOS HILL0049 D 0 5mglmL PFOS Study NunTHPFOS 0 5091 5086 5092 5092 5085 0 893965 871748 746435 887622 872024 0 lST&ZQ% PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS 254 PFOS 0 5315 531 5316 5316 5309 0 126502 88651 3303886 620867 520023 0 3424213 166155 2049582 2834021 2370488 0.0% Sample levelinVial too low 3/30/01 2 04 0 \Chem\HillaSAMPLE HILL0050 D 0 5mg/mL PFOS Study NunTHPFOS 5083 867832 254 PFOS 5307 582795 2708401 - 3/30/01 2 18 0 \Chem\HillaSAMPLE HILL0051 D 0 5mglmL PFOS Study NunTHPFOS 5091 727915 254 3/30/01 2 32 D \Chem\HillaSAMPLE HILL0052 D 2mglmL PFOS Study NumbTHPFOS 5083 854851 254 3/30/01 2 47 D \ChemWillaSAMPLE HILL0053 D 2mglmL PFOS Study NumbTHPFOS 5083 857430 254 PFOS PFOS PFOS 5300 5307 5307 3691790 237353 2353605 1234773 2593339 1364485 3/30/01 3 01 D \Chem\HillaSAMPLE HILL0054 D 2mglmL PFOS Study NumbTHPFOS 5 0 9 854499 254 PFOS 5314 2562398 1352093 3/30/01 3 16 D \Chem\HillSAMPLE 3/30/01 3 30 D \Chem\HdlaSAMPLE HILL0055 D 5 nglmL PFOS in MeOH THPFOS HILL0056D 250 5 nglmL PFOS inMeOTHPFOS 0 0 0 ISTD<70% PFOS 0 0 0 ISTD<70% PFOS 0 0 0 0 0% Sample level In Vial too low 0 0 0 0 0% SamplelevelIn Vial too low 3130/01 4 13 D \Chem\HillaSAMPLE HILL0059 D 2mglmL PFOS Study NumWHPFOS 5084 749219 254 PFOS 5308 5345747 3444726 3/30/01 4 28 D \Chem\HillaSAMPLE HILLWGOD 5mglmL PFOS Study NumWHPFOS 5084 876417 254 PFOS 5300 1620046 8090241 3/30/01 4 42 D \ChemWiIWAMPLE HILL0061 D 5mglmL PFOS Study NumWHPFOS 5077 906862 254 PFOS 5301 1503995 7209314 3/30/01 4 56 D \Chem\HillaSAMPLE HILL0062 D 5mglmL PFOS Study NumbTHPFOS 5085 901113 254 PFOS 5309 1497426 7224531 3/30/01 5 11 0 \Chem\HillaSAMPLE HILL0063 D 5mglmL PFOS Study NumWHPFOS 5084 755376 254 PFOS 5 301 4532655 280 4432 3/30/01 5 25 D \Chem\HillaSAMPLE H I L L W D IOmglmL PFOS Study NumTHPFOS 5086 913312 254 PFOS 5303 3057247 1520074 3/30/01 5 40 D \ChemWillaSAMPLE 3/3/01 5 54 D \ChemWillaSAMPLE 3/30/01 6 08 D \Chem\HiIIBAMPLE 3/30/01 6 2 3 D \Chem\HillaSAMPLE 3/30/01 6 37 0 \Chem\HillaSAMPLE HILL0065 D IOmglmL PFOS Study NumTHPFOS HILL0066 D 10mglmL PFOS Study NumTHPFOS HILL0067 D IOmglmL PFOS Study NumTHPFOS HILL0068 D 5OmglmL PFOS Study NumTHPFOS HILL0059 D 5 ng/mL PFOS in MeOH THPFOS 5086 5079 5083 5088 0 973798 911827 781459 979507 0 - 254 PFOS 254 PFOS - 254 PFOS - 254 PFOS 0 lST&ZQ% PFOS 531 5303 5307 5312 0 3260951 3051917 5989063 2234423 0 1520686 151 9884 372804 101 1328 0 0 0% Sample levelin Vial too low 3/30/01 6 51 D \ChemWtllaSAMPLE - 3/30/01 7 35 D \Chem\HillaSAMPLE - 3/30/01 7 49 D \Chem\HillaSAMPLE - 3/30/01 8 03 D \Chem\HillaSAMPLE - 3/30/01 8 18 D \ChemWillaSAMPLE - 3/30/01 8 32 0 \ChemWillaSAMPLE - 3/30/01 8 46 D \Chem\HillaSAMPLE 3/30/01 9 01 D \Chem\HillaSAMPLE - 3/30/01 9 15 D \Chem\HillaSAMPLE - 3/30/01 9 30 D \Chem\HillaSAMPLE - 3/30/01 9 45 D \Chem\HillaSAMPLE 3/30/01 9 59 0 \Chem\HillaSAMPLE 3/30/01 10 14 D\ChemWillaSAMPLE - 3/30/01 10 57 D\ChemWdlaSAMPLE - 3/30/01 11 12 D \Chem\HillaSAMPLE - 3/30/01 11 26 D \Chem\HillaSAMPLE - 3/30/01 1141 D \Chem\HillaSAMPLE - 3/30/01 11 55 D \Chem\HillaSAMPLE - 3/30/01 12 09 0 \Chem\HillaSAMPLE - 3/30/01 12 24 D \Chem\HillaSAMPLE - 3/30/01 12 38 D \Chem\HillaSAMPLE s - 3/30/01 12 53 D \Chem\HillaSAMPLE HILL0070 D 250 5 nglmL PFOS in MeOTHPFOS HILL0073 D 50mglmL PFOS Study NumTHPFOS HILL0074 D 50mglmL PFOS Study NumTHPFOS HILL0075 D SOmghL PFOS Study NumTHPFOS HILL0076 D OmglmL PFOS Study NumbTHPFOS HILL0077 D OmglmL PFOS Study NumWHPFOS HILL0078 0 OmglmL PFOS Study NwWHPFOS HILL0079 D OmglmL PFOS Study NumbTHPFOS HILL0080 D 0 5mglmL PFOS Study NunTHPFOS HILLW81 D 0 5mglmL PFOS Study NunTHPFOS HILL0082 D 0 5mglmL PFOS Study NuBHPFDS HILL0083 D 5 nglmL PFOS in MeOH THPFOS HILL0084 D 250 5 ng/mL PFOS m MeOTHPFOS HILLW87 D 0 5mglmL PFOS Study NunTHPFOS HILL0088 D 2mglmL PFOS Study NumWHPFOS HILL0089 0 2mglmL PFOS Study NumWHPFOS HILL0093 D 2mglmL PFOS Study NumWHPFOS HILL0091 D ZmglmL PFOS Study NurnWHPFOS HILL0092 D 5mglmL PFOS Study NumbTHPFOS HILL0093 D 5mglmL PFOS Study NumWHPFOS HILL0094 D 5mglmL PFOS Study NumWHPFOS HILL0095 D 5mglmL PFOS Study NurnWHPFOS 0 5079 5084 5077 5076 5084 5085 5083 5077 5084 5087 0 0 5083 5086 508 5078 5077 5072 5077 5078 5078 0 967155 990636 924192 868541 862422 848676 712693 830763 838359 817463 0 0 723549 829574 810539 813653 698202 870788 833403 865160 732175 0 lST&ZQ% PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 ~ PFOS 254 PFOS 254 PFOS 254 PFOS 0 &?J&GO% PFOS 0 &?J&GO% PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 0 5296 5301 5294 5307 0 0 53 5295 5309 5311 0 0 5314 5303 5297 5295 5301 5297 5294 5 302 5302 0 0 1999273 9109713 1896764 839824 5706884 2939526 199968 7359762 0 0 0 0 3185982 2071555 2350237 1270906 1735740 9124829 2751710 1529141 0 0 0 0 5581843 3755325 7796382 4682081 7782923 4796898 7488962 4573479 9920061 7529404 4681978 2528436 4589661 2595041 4617034 250 8006 7091269 4843771 0.0% Samplelevelin Vial too low 0 0% Sample levelin Vial too low 0.0% Sample ISVEinI Vial too low BACK TO MAIN 3/30/01 1307 D \ChemWillaSAMPLE 33W01 13 21 0 \Chem\HillaSAMPLE 3/30/01 13 36 D \Chem\HillaSAMPLE 3130101 14 19 D \Chem\HillaSAMPLE 3/30/01 14 34 D\ChemWillaSAMPLE 3/30/011448 D \Chem\HillaSAMPLE 3/30/01 15 02 D \Chem\HillaSAMPLE 3/30/01 15 17 D\Chem\HillaSAMPLE 3/30/01 15 31 D \Chem\HiIlaSAMPLE 313010115 46 D\Chem\HilIaSAMPLE 3/30/01 16 00 D \ChemWillaSAMPLE 3/30/01 16 15 D \ChemWillaSAMPLE 3/30/01 16 29 D \Chem\HillaSAMPLE 3130101 16 43 D \ChemWillaSAMPLE 3/30/01 16 58 D \Chem\HillaSAMPLE 3/30/01 17 41 D \Chem\HillaSAMPLE 3/30/01 17 56 D \Chem\HdlaSAMPLE 3130101 18 10 D\Chem\HilWAMPLE 3/30/01 18 24 D \Chem\HdaSAMPLE 3130101 18 39 D \Chem\HillaSAMPLE 3/30/01 18 53 D \ChemWillaSAMPLE 3/30/01 I 9 08 D \Chem\HillaSAMPLE 3/30/01 19 22 D \Chem\HillaSAMPLE 3/30/01 19 36 D \Chem\HillaSAMPLE 3/30/01 19 51 D \Chem\HdlaSAMPLE 3/30/0120 05 D \ChemWillaSAMPLE 3/30/01 20 20 D \Chem\HillaSAMPLE 3130101 21 03 D \ChemWillSAMPLE 3/30/01 21 17 D \Chem\HdlaSAMPLE 3/30/01 21 32 D \Chem\HillaSAMPLE 3/30/01 21 46 D\ChemWillaSAMPLE 330101 22 00 D \Chem\HillaSAMPLE 3/30/01 22 15 D \Chem\HillaSAMPLE 3/30/01 22 29 D \Chem\HillaSAMPLE 3/30/01 22 44 D \Chem\HillaSAMPLE 3/30/01 22 58 D \Chem\HllaSAMPLE 3/31/01 23 12 D \Chem\HillaSAMPLE 3/31/01 23 56 D \ChemWillaSAMPLE 3/31/01 0 10 D \ChemWillaSAMPLE 3/31/01 0 24 D \Chem\HillaSAMPLE 3/31/01 0 39 D \ChemWdlaSAMPLE 3/31/01 0 53 D \ChemWillaSAMPLE 313'1101108 D \Chem\HllaSAMPLE 3/31/01 1 22 D\ChemWtllaSAMPLE 3/31/01 1 36 D \Chem\HiIIaSAMPLE 3/31/01 1 51 D\ChemWillaSAMPLE 3/31/012 05 D \Chem\HilIaSAMPLE 3/31/01 2 20 D \Chem\HillaSAMPLE 3/31/01 2 34 D \Chem\HillSAMPLE 3/31/01 3 17 D \Chem\HiIWAMPLE 3/31/01 3 32 D\Chem\HllaSAMPLE 3/31/01 3 46 D \Chem\HillaSAMPLE 3/31/014 00 D \Chem\HillaSAMPLE 3/31/01 4 15 D\Chem\HillaSAMPLE 3/31/01 4 29 D \ChemWillaSAMPLE 3/31/01 4 44 D \ChemWillaSAMPLE 3/31/01 4 58 D \ChemWdlaSAMPLE 3/31/01 5 12 D \Chem\HillaSAMPLE 3/31/01 5 27 D \Chem\HdlaSAMPLE HILL0096D 10mgmL PFOS Study NumTHPFOS HILL0097 D 5 ngmL PFOS in MeOH THPFOS HILL0098 D 250 5 ngmL PFOS IllMeOTHPFDS HILL0101D 10mgmL PFOS Study NumTHPFOS HILL0102 D IOmgmL PFOS Study NumTHPFOS HILL0103 D lOmg/mL PFOS Study NumTHPFOS HILL0104 D 50mg/mL PFOS Study NumTHPFOS HILL0105 D 5OmgmL PFOS Study NumTHPFOS HILL0106 D 5OmgmL PFOS Study NumTHPFOS HILL0107 D 50mglmL PFOS Study NumTHPFOS HILL0108 D OmgmL PFOS Study NumWHPFOS HILL0109D CmgmL PFOS Study NumWHPFOS HILL0110 D h g m L PFOS Study NumWHPFOS HILL0111D 5 nglmL PFOS in MeOH THPFDS HILL0112 D 250 5 ngmL PFOS inMeOTHPFOS HlLLOl 15 D OmgmL PFOS Study NumWHPFOS HILL0116 D 0 5mglmL PFOS Study NunTHPFOS HILL0117 D O5mglmL PFOS StudyNunTHPFOS HlLLOlI 8 D 0 5mgmL PFOS Study NunTHPFOS HILL0119 D 0 5mgmL PFOS Study NunTHPFOS HILL0120 D 2mglmL PFOS Study NumWHPFOS HILL0121 D 2mg/mL PFOS Study NumWHPFOS HILL0122 D 2mg/mL PFOS Study NumWHPFOS HILL0123D ZmglmL PFOS Study NumWHPFOS HILL0124 D 5mglmL PFOS Study NumWHPFOS HILL0125 D 5 ngfmL PFOS m MeOH THPFOS HILL0126D 250 5 ngmL PFOS inMBOTHPFOS HILL0129D 5mgmL PFOS Study NumWHPFOS HILL0130 D 5mgmL PFDS Study NumbTHPFOS HILL0131 D 5mgmL PFOS Study NumWHPFOS HILL0132 D 10mgmL PFOS Study NumTHPFOS HILL0133 D IOmgmL PFOS Study NumTHPFOS HILL0134 D 1OmglmL PFOS Study NumTHPFOS HILL0135 D 10mg/mL PFOS Study NumTHPFOS HILL0136 D 5OmglmL PFOS Study NumTHPFOS HILL0137 D 5 ngmL PFDS in MeOH THPFOS HILL0138 D 250 5 ngmL PFOS in MeOTHPFOS HILL0141 D 50mgmL PFOS Study NumTHPFOS HILL0142 D 5OmglmL PFOS Study NumTHPFOS HILL0143 D 50mgmL PFDS Study NumTHPFOS HILL0144 D OmslmL PFOS Study NumbTHPFOS HILL0145D OmgmL PFOS Study NumWHPFOS HILL0146D DmgmL PFOS Study NumWHPFOS HILL0147 D OmglmL PFOS Study NumbTHPFOS HILL0148 D 0 5mg/mL PFOS Study NuriWPFOS HILL0149 D 0 5mUmL PFOS Study NunTHPFOS HILL0150D 0 5mgmL PFOS Study NuniHPFOS HILL0151 D 5 ng/mL PFOS in MeOH THPFOS HILL0152 D 250 5 ngmL PFOS in MeOTHPFOS HILL0155 D 0 5mglmL PFOS Study NunTHPFOS HILL0156D ZmplmL PFOS Sludy NumWHPFOS HILL0157 D Zmg/mL PFOS Study NumWHPFOS HlLLOl58 D Zmg/mL PFOS Study NumWHPFOS HILL0159 D 2mg/mL PFOS Study NumbTHPFOS HILL0160 D 5mgmL PFOS Study NumWHPFOS HILL0161 D 5mglmL PFOS Study NumbTHPFOS HILL0162 D 5mglrnL PFOS Study NmbTHPFOS HILL0163 D 5mglmL PFOS Study NumbTHPFOS HILL0164 D IOmglmLPFOS Study NumTHPFOS 507 507 507 5075 507 507 5083 5076 5081 5071 5079 5084 5083 5079 5071 5084 5085 5077 5085 5079 5084 5077 5071 5077 5078 5085 5076 5078 5077 5075 507 5069 5078 5077 5077 5077 5084 5078 5077 5077 507 507 0 0 0 0 5059 5077 507 5063 5057 0 5055 5055 5062 507 5069 507 5071 871278 1031178 935555 877270 893385 742701 907624 931206 919670 796555 849151 829076 821979 913364 935372 706581 824542 816173 807718 699831 788878 809256 794520 683431 846191 899639 916782 862439 872248 730684 853720 867572 825915 705375 891448 947052 930968 900440 896344 785271 1517034 1519670 0 0 0 0 1378137 I127307 10.57386 1222595 1394294 0 1405167 1264058 1123797 1170021 1140248 892226 1049855 254 PFOS 254 PFOS 254 PFDS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFDS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFDS 254 PFOS 254 PFOS 254 PFDS 254 PFOS 254 PFOS 254 PFOS 254 PFDS 254 PFDS 254 PFOS 254 PFDS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFO.S. 254 Ma PFOS 254 &zbaLu PFOS 0 &ZDQ.C% PFOS 0 IfTprzo?L PFOS 0 IfTprzo?L PFOS 0 IfTprzo?L PFOS 254 sw4a.b PFOS - 254 &zbaLu PFOS 254 PFOS 254 &zbaL'u PFOS 254 &zbaLu PFOS 0 &ZDQ.C% PFOS 254 uzn43Lu PFOS 254 &zbaLu PFOS 254 &zbaLu PFDS 254 uzn43Lu PFOS 254 ST&bWXb PFOS - 254 PFOS - 254 PFOS 5294 5287 5287 5 292 5294 5287 5307 5308 5298 5296 5311 5301 5307 5303 5288 5308 5302 5294 5302 5303 5308 5295 5295 5301 5302 5309 5307 5309 5294 5299 5294 53 5302 5301 8976434 165503 4930244 12899537 13256112 15131931 5518080 5108086 5181946 7665976 742763 183483 107928 119662 4919934 3248594 1502753 1724356 1736346 4688064 5634498 5717625 5974646 8405232 3725697 122088 4879273 3516962 3677170 6262922 6519410 6622791 6587808 83758505705483 5194978 4265778 2474028 783 9937 7924273 1161 188 2890022 2583954 2660334 4809168 3624765 6963474 2972255 2 959401 2468948 2135081 7969637 9322899 9496021 3213717 3448627 3407597 3650473 6363714 2037979 3167352 2500647 1877001 1945103 4222447 3713232 371 1742 3897087 61485332466657 5301 5308 5295 5 288 5294 5294 5294 5283 5294 5288 5286 5283 5301 5294 5294 5288 5295 5286 5286 5294 5301 5293 5294 5 295 121133 4866574 3499027 3507729 6226527 607465 161015 102458 2813295 123415 245088 154022 104248 4570480 2934417 298977 308066 261303 3012214 256463 268126 138591 3214850 12043940 2821811 2452477 1782918 179 6005 387 1451 1493697 1850082 0 0 0 0 2107086 1253723 1997993 1067379 6657971 0 5394641 1059273 7269909 7312199 2540176 164426 587 354 85.3% 98.8% 59.2% 98.6% 63.3% 99.8% 56.4% 97.9% 25.1% 79.8% BACK TO MAIN 3/31/01 5 41 0 1CnemWlISAMPLE HILL0165 D IOmglmL PFOS Study NumTHPFOS 3/31/01 5 56 D \Chem\H ,ISAMPLE HILL0166D 5 nglmL PFOS in MeOH THPFOS 3/31/01 6 10 0 \Cnem\HdiaSAMPLE HILL0167 D 250 5 ng/rnL PFOS in MeOTHPFOS 3131101 6 53 D \Chem\H ll&AMPLE HILL0170D lOmglmL PFOS Study NumTHPFOS 3/31/017 08 0 \Cnem\HibaSAMPLE HILL0171 D 10mglmLPFOS StudyNumTHPFOS 3/31/01 7 22 D \Chem\ii IISAMPLE HILL0172 D 50mglmL PFOS Study NumTHPFOS 3131M1 7 36 D \Cnem\H,I SAMPLE HILL0173D 5OmglrnL PFOS StudyNumTHPFOS 3/31/01 7 51 D \Chem\HdaSAMPLE HILL0174 D 50mglmL PFOS Study NumTHPFOS 3131/@18 05 0 Che!--lu 'ISAMPLE HILL0175 D 5OmglmL PFOS Study NumTHPFOS 3/31/01 8 20 D \Chem\HIISAMPLE HILL0176 D Omg/mL PFOS Study NumbTHPFOS 3/31/01 8 34 D \Chem\HrllaSAMPLE HILL0177 D OmglmL PFOS Study NumbTHPFOS 3/31/01 8 48 D \Cnem\Hd &AMPLE HILL0178 D CmglmLPFOS StudyNumWHPFOS 3131101 9 03 D \Cnem!htiaSAMPLE HILL0179 D OmglmL PFOS Study NumWHPFOS 3/31/01 9 17 D \Chem\H IlaSAMPLE HILLOlBO D 5 nglmL PFOS in MeOH THPFOS 3/31/01 9 32 D ChemWdlaSAMPLE HILL0161D 250 5 nglmLPFOS~1MeOTHPFOS 3/31/01 10 15 O \ C ~ ~ ~ W I M A M P L EHILL0184 D 0 5mglmL PFOS StudyNunTHPFOS 3/31/01 10 29 D \Chem\HdaSAMPLE HILL0185 D 0 5mglrnL PFOS Study NunTHPFOS 3/31/01 10 44 D \Cnem\H#iSAMPLE HILL0186D 0 5mglmL PFOS StudyNunTHPFOS 3/31/01 10 58 D \ChsmWalaSAMPLE HILL0187 D 0 5mg/mL PFOS Sludy NunTHPFOS 3/31/01 11 13 D \Chern\HillaSAMPLE HILL0188D 2mglmL PFOS Study NumbTHPFOS 3/31/01 11 27 0 \ChemW#PaSAMPLE HILL0189D ZmglmL PFOS Study NumWHPFOS 3131101 11 41 D \Chem\HillSAMPLE HILL0190 D ZmglmL PFOS Study NumtXHPFOS 3/31/01 11 56 0 \CnemWdlSAMPLE HILL0191D 2mglmL PFOSStudy NumWHPFOS 3/31/01 12 10 D \Chem\H6ilSAMPLE HILL0192 D 5mglmL PFOS Study NumWHPFOS 3/31/01 12 25 O \ C ~ ~ ~ \ H I I S A M P L EHILL0193D 5mg/mL PFOS Study NumWHPFOS 3/31/01 12 39 D \Cnem\HllaSAMPLE HILL0194 D 5 ng/mL PFOS in MeDH THPFOS 3/31/01 12 53 D \Chem\H IlaSAMPLE HILL0195 D 250 5 nglmL PFOS in MeOTHPFOS 3/31/01 13 37 D\Chem\HiISAMPLE HILL0198D 5mglmL PFOS Study NumWHPFOS 3/31/01 13 51 D\Cnem\HillaSAMPLE HILL0199 D 5mglmL PFOS Study NumbTHPFOS 3/31/01 14 05 D \Chem\HdlaSAMPLE HILL0200 D 10mglmLPFOS Study NumTHPFOS 3/31/01 14 20 D\ChemWiI&AMPLE HILL02010 tOmglmL PFOS Study NumTHPFOS 3/31/01 14 34 0 lCnem\H.&MMPLE HILL0202 D 10mglmLPFOS Study NumTHPFOS 3/31/01 14 49 D lChem\H.llSAMPLE HILL0203 0 10mglmLPFOS Study NumTHPFOS 3131101 15 03 D \Cnem\HdlaSAMPLE HILL0204 D 5OmglmLPFOS Study NumTHPFOS 3/31/01 15 17 O\Cnem\H #ISAMPLE HILL0205D SOmg/mL PFOS Study NumTHPFOS 3/31/01 15 32 0 \Chem\H IlaSAMPLE HILL0206 D 56nglmL PFOS Study NumTHPFOS 3/31/01 15 46 0 lChemlHiISAMPLE HILL0207 0 5OmglmL PFOS Study NumTHPFOS 3131101 16 01 0 \Chem\H1laSAMPLE HILL0208D 5 nglmL PFOS inMeOH THPFOS 3/31/01 16 15 D \Chem\HillaSAMPLE HILL0209D 250 5 ndmL PFOS in MeOTHPFOS 507 5077 5078 5078 5062 5077 5073 5078 5078 507 0 5077 507 5077 5077 0 0 5071 0 0 0 5056 5056 5057 5072 5055 5062 507 5074 5077 5071 5077 5077 5077 5084 5077 5078 5077 507 1029270 1045844 961392 983111 781444 863043 848190 958369 699825 1475601 0 1496086 1338136 1319457 1233038 0 0 1471417 0 0 0 1464319 1287803 1254007 1222970 1252112 1233786 1196708 940569 1165476 1154702 1154514 936013 1005094 1020410 970721 844704 937393 9- - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS -254 PFOS 0 lETpLzosL PFOS -254 a PFOS -254 &TbllLb PFOS 254 JsTbuCu PFOS 254 PFOS O S T L u M PFOS 0 lETpLzosL PFOS 254 l s b l a c u PFOS O S T L u M PFOS O S T L u M PFOS 0 lETpLzosL PFOS 254 SUWSQ% PFOS 254 ksUw3U PFOS 254 ksUw3U PFOS 254 PFOS 254 lSTb&N% PFOS 254 szbu&*b PFOS 254 254 4 s b-u L b PFOS PFOS 254 PFOS 254 lSTb&N% PFOS 254 ksUw3U PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS - 254 PFOS 5294 5301 5302 5302 5294 5294 5297 5302 5309 0 53 0 5294 0 5301 5296 5296 0 5294 5294 5288 5287 5288 5288 5289 0 5286 5294 5298 5301 5302 5301 5301 5294 5301 5309 5302 5 295 5294 7942166 113187 4685914 11897888 13471666 547258 371026 502489 3544102 0 15403 0 2562313 0 4581504 106080 88413 0 2763394 243781 191714 184484 2856662 314686 267523 0 4563196 188759 3245571 335088 525297 550957 3645184 256482 233790 231102 3674257 112408 4662409 3756283 195061 227378 6246515 9475747 2540056 1658928 204758 2369754 0 0 0 8398912 0 1699125 0 0 0 0 0 0 2736832 9817581 8279809 6849741 0 1690775 4143137 1570094 990566 1737075 1836785 1782599 6468139 7309995 7707909 2011561 2 468054 242609 39.0% 90.8% 0.0% 67.8% 0.0% 67.5% 49.4% 96.8% . .. BACK TO MAIN 9 0 ? 5 I' rn 00 3 Batch Sample List. Curve and CalibrationChecks Acquiotm InslrumentlSequence: Hilla1y/HOlO319~a) DatelAnalystof Reprocessing: 02 Apr 01 / M I A Batch Method: R010319a.m OuantitationRange: 2.5 to 1002 n g h L lnj Date 3/19/2001 20:05 3/19/2001 2O:i9 3/19/2001 20.33 3/19/2001 20:48 3/19/2001 21:02 3/19/2001 21:16 3/19/2001 21.31 3/19/2001 21:45 3/19/2001 22:OO 3/19/2001 2 2 1 4 3/19/2001 2 2 2 8 3/19/2001 2 2 4 3 3/20/2001 2:04 3/20/2001 2:18 3/20/20015:l I 3/20/2001 5.25 3/20/2001 832 3/20/2001 8:47 3/20/2001 11:25 3/20/2001 1 1 3 9 3/20/2001 14:18 3/20/2001 14.32 Batch SampType File Sample Name C:\CHEMWillary.iWOIO319-a.b CALIB-1 C:\CiiEM',Hillary.i\J-IC10319-a.b CALIB-2 C.\CHEMWillary.iWO1031S-a.b CALIB-3 C:\CHEMWillary.iWO10319-a.b CALIB-4 C\CHEM\Hillary.iWO1031S-a.b CALIB-5 C:\CHEMWillaiy.iWOIO319-a.b CALlB-6 C:\CHEMWillarf.rWO10319-a.b CALIB-7 C:\CHEMWillary.iW010319-a.b CALlB-8 C:\CHEMWillary.iWO1031S-a.b CALIB-9 C:\CHEMWillary.iWO1031S-a.b CALIB-IO C:\CHEMWillary.iWOlO3lS-a.b CALIB-I 1 C:\CHEMWillary.iWO1031Pa.b CALlB-12 C:\CHEMWillary.iWOIO319-a.b CCALIB-I C:\CHEMWillary.iWOl0319-a.b CCALIB-1 C:\CHEMWillary.iWOIO319-a.b CCALIB-I C.\CHEMWillary.iWO10319-a.b CCALlB-I C : l C H E M ~ i ~ i ~ . i ~ O l O C3 Cl ~AL~L.-1b C:\CHEMWillary i\H010319-a.b CCALIB-1 C:\CHEMWillary.iW0103lS-a.b CCALIB-1 C:\CHEMWillary.iWOlO3l!&a.b CCALIB-I C:\CHEM\HiIlary.iWOiO319-a.b CCALIB-I C:\CHEMWillary.iWOIO319-a.b CCALIB-1 HILL0017.D HILL00IB.D HILL0019 D HILLW20.D HILL0021.D HILLW22.D HILL0023.D HILL0024.D HILL0025.D HILL0026.D HILL0027.D HILL0028.D HILL0042.D HILL0043.D HILL0055.D HtLL0056.D HILL0lW.D HILL0070.D HILLOOB1.D HILL0082.D HILL0093.D HILL0094.D 2.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 1 0 ng/mL PFOS in MeOH 25 ng/mL PFOS in MeOH 4 0 nglmL PFOS in MeOH 50.1 ng/mL PFOS in MeOH 75.1 ng/mL PFOS in MeOH 100.2 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 400.8 ng/mL PFOS in MeOH 501 ng/mL PFOS in MeOH 1002 ng/rnL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 5 n g h L PFOS in MeOH 250.5 n g h L PFOS in MeOH 5nghL PFOS h MeOH 250.5 ng/mL PFOS in MeOH 5 n g h L PFOS in MeOH 250.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH Yisc. Info. 01003-07-02 01003-07-03 01003-07-04 0100M7-05 0100M7-06 01003-07-07 0100347-08 01003-07-09 0100307-10 01003-07-11 01003-07-12 01003-07-13 01003-07-03 01003-07-10 01003-0703 0100507-10 01003-07-03 01003-07-10 01003-07-03 01OOM7-10 0100307-03 0100307-10 Compound Name THf+ec THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Avengeha: S1d b v : %RSD: RT 4.96 4.97 4.96 4.96 4.97 4.96 4.96 4.97 4.97 4.97 4.97 4.96 4.97 4 97 4.97 4.97 4.98 4.99 4.96 4.96 4.98 4.98 887103 67424.5 8% Area 952704 958659 946379 954921 955330 958316 961545 961218 963600 945005 937041 930802 869312 865137 854600 852353 828170 821673 792949 787755 795135 793444 Amount 254 ~ 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 -.- Compound Name PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS RT M 5.18 5.18 5.19 5.18 5.19 5.19 5.19 5.18 5.19 5.19 5.19 5.18 5.19 5.19 5.20 5.20 5.20 5.21 5.19 5.19 5.20 5.20 Area n 63092 108976 207712 553295 871355 1084605 1595162 2149447 5065486 7558280 9061046 15880052 107823 4962586 104397 4950256 111868 4958647 108119 4876204 111428 4914110 Amount 3.2 5.2 9.8 25.4 40.0 49.8 73.7 100.4 250.5 401.6 500.7 1002.0 5.7 275.9 5.6 279.7 6.2 291.9 6.2 300.3 6.4 300.5 Theoretical 27.7% 4.5% 2.4% 1.4% 0.1% 0.6% 2.0% 0.2% 0.0% 0.2% 0.1% 0.0% 13.4% 10.1% 11.8% 11.7% 22.8% 16.5% 23.9% 19.9% 27.2% 20.0% E001311 PFOS AdsoW/oeso* BACK TO MAIN 9 ?(D 5 I m ' Y0- 0 3 2 -0 II) (0 (D VI Iu 0 0 =+I 0 -4 0 Batch Sample List. SarnDles Onlr Acquistion InstrumentlSequence: Hillary/HOIO319(a) Date/Analyst of Reprocessing: 02 A p r 0 1 I MLA Batch Method. R010319a.m Quantitation Range: 2.5 t o 1002 ng/mL Inj Date 3/19/2001 23:40 3/19/2001 2354 3/20/2001 0:09 3/20/2001 0 2 3 3/20/2001 0:38 3/20/2001 0:52 3/20/2001 1:06 3/20/2001 1 2 1 3/20/2001 1:35 3/20/2001 1:49 3/20/2001 3:01 312012001 3.16 3/20/2001 3:30 3/20/2001 3:44 3/20/2001 3 5 9 3/20/2001 4: 13 3/20/2001 4 2 8 3/20/2001 4:42 3/20/2001 4:56 3/20/2001 6:08 3/20/2001 6 2 3 3/20/2001 6.37 3/20/2001 6 5 1 3/20/2001 7:06 3/20/2001 7 2 0 3/20/2001 7:35 3/20/2001 7:49 3/20/2001 8:03 3/20/2001 8:18 3/20/2001 9:30 3/20/2001 9:44 3/20/2001 9 59 3/20/2001 10 13 3/20/2001 10:27 3/20/2001 10:42 3/20/2001 1056 3/20/2001 1 1 : l l 3/20/2001 1223 3/20/2001 12.37 312012001 12 51 3/20/2001 13 06 3/20/2001 13 20 3/20/2001 13:35 3/20/2001 13 49 3/20/2001 14 03 Batch SampType C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i!HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.RHO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hilla~.i\HO10319-a.b SAMPLE C:\CHEM\Hilla&\HO10319-a.b SAMPLE C~\CHEM\Hillary.i\H010319-a.b SAMPLE C:\CHEM\Hillary.i\H010319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\HilIary.i\HO10319-a.b SAMPLE C:\CHEM\Hillarv.i\HO10319-a.b SAMPLE C:\CHEM\Hilla~.i\HO10319-ab. SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C \CHEM\Hlllary i\H010319-a b SAMPLE C \CHEM\Hillary AH010319-a b SAMPLE C \CHEM\Hillary iAH010319-a b SAMPLE C \CHEM\Hillary i\H010319-a b SAMPLE C \CHEM\Hillary AH010319-a b SAMPLE C \CHEM\Hillary i\H010319-a b SAMPLE C \CHEM\Hillary iAH010319-a b SAMPLE C \CHEM\Hillary 1\H010319-ab SAMPLE C \CHEM\Hillary iAH010319-a b SAMPLE C \CHEM\Hillary ilH010319-a b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.RHO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C \CHEM\Hillary i\H010319-a b SAMPLE C \CHEM\Hillary 1\H010319-ab SAMPLE C:\CHEMWillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C:\CHEM\Hillary.i\HO10319-a.b SAMPLE C \CHEM\Hillary 1\H010319-ab SAMPLE C \CHEM\Hillary i\H010319-a b SAMPLE C \CHEM\Hillary iAH010319-a b SAMPLE C \CHEM\Hillary.i\HO10319-a.b SAMPLE C \CHEM\Hillary 1\H010319-ab SAMPLE C \CHEM\Hillary AH010319-a b SAMPLE File HILL0032.D HILL0033.D HILL0034.D HILL0035.D HILL0036.D HILL0037.D HILL0038 D HILL0039.D HILLW0.D HILL0041.D HILL0046.D HILL0047.D HILL0048.D HILL0049.D HILL0050.D H I L L 0 0 5 1. D HILLW52.D HILL0053.D HILLW54.D HILL0059.D HILL0060.D HILL0061.D HILL0062.D HILL0063.D HILL0064.D HILL0065.D HILL0066.D HILL0067.D HILL0068.D HILL0073.D HILL0074.D HILL0075 D HILL0076 D HILL0077.D HILL0078 D HILL0079.D HILL0080.D HILL0085.D HILL0086.D HILL0087 D HILL0088 D HILL0089 D HILL0090.D HILL0091 D HILL0092 D Sample Name 131 1-4124-SZ 1311-4125-S2 131 1-4126-SZ 1311-4148-S2 131 1-4149-SZ 131 1-4150-52 1311-4124-53 1311-4124-53 13114126-53 1311-4148-S3 1311 - 4 1 4 9 4 3 1311-415O-S3 131 1-4124-S4 131 1-412 5 4 4 131 1-4148-S4 1311-4149-54 131 1-4150-54 1311-4124-S5 13114125-55 1311-4126-S5 131 1-4148-S5 1311-4149-S5 1 3 11 - 4 15 0 - S 5 1311 4 1 2 4 - 5 6 1311-4125-56 13 11-4 12 6 - S 6 13114126MS-S6 1311-4148-S6 1311-414946 1311-4150-S6 1311-4150MS-S6 1311-4124-S7 1311-4125-S7 1 3 11 - 4 1 2 6 4 7 1311-414847 1311-4149-57 1311-4150-57 1311-4124-S8 1311-4125-58 1311-4126-S8 13114126MS-S8 1311-4148-S8 1311-4149-S8 1311-4150-S8 1311-4150MS-S8 Compound N a m e THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT 4.97 4.97 4.96 4.97 4.97 4.97 4.97 4.97 4.96 4.97 4.97 4.97 4.97 4.97 4.97 4.97 4.97 4.97 0.00 4.98 4.99 4.99 4.99 4.99 4.99 4.99 4.99 4.99 4.99 4.97 4.97 497 497 4.97 4.97 4.97 4.97 4.97 4.98 497 4 98 497 4.98 498 4 98 Area 912437 929948 896524 912022 896921 864432 851789 760590 855770 815449 799794 795722 778881 829069 831754 822782 783261 832109 0 870389 818725 813491 836794 794532 935394 819696 682208 824967 796443 790214 671901 833453 781273 822529 788804 839982 766667 873274 851164 794047 720378 819035 837526 867770 765928 Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 0 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Compound Name PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS RT 0.00 0.00 5.19 5.19 5.19 5.19 0.00 5.11 0.00 5.19 5.19 5.20 5.20 5.19 5.20 5.19 5.19 5.21 0.00 5.20 5.21 5.21 5.22 5.22 5.21 5.21 5.22 5.22 5.21 5.20 5.20 520 520 5.25 5.20 5.20 5.19 5.20 5.20 521 520 520 5.20 521 521 Area 0 0 24098 634921 662089 600651 0 11390 0 725638 701086 791683 18545 88450 2403148 1442298 3545457 19220 0 20928 1344937 1158276 1492192 22539 16342 12441 3391548 1104066 1163274 1145873 4132085 38789 22919 79060 1077441 1199443 1234169 28965 41619 20502 3590912 1087596 1189179 720004 4692081 Amount 0.0 0.0 1.5 30.5 32.4 30.4 0.0 1.0 0.0 39.1 38.5 43.7 1.4 4 9 131.4 780 212.6 1.4 00 1.4 72.9 63.0 79.4 1.6 1.1 1.0 235.6 59.1 64.6 64.2 298.1 24 16 4.5 60.4 63.2 71.4 1.8 2.5 15 2363 586 628 364 2968 3rd Environmental Laboratory EW-1311PFOS AdsorblDesorb BACK TO MAIN Batch Sample List: Methanol Blanks s Acquistion Instrumentlsequence: Hillary/HOlO3lS(a) Date/Analystof Reprocessing: 02 Apr 01 / MLA 9 Batch Method: R010319a.m 3. Quantitation Range: 2.5 to 1002 ng/mL 3 ;i; 3 Inj Date Batch SampType File Sample Name Compound Name RT Area Amount Compound Name RT Area Amount ? 3/19/2001 19:22 C:\CHEM\Hillary.i\HOIO319-a.b SAMPLE HILL0014.D TN-A 4802 MeOH THPFOS 00 0 ICm-T 33//1199//2200001121295: 7s CC::\\CCHHEEMM\\HHiillllaarryy..ii\\HHOOIIOO331199--aa..bb SSAAMMPPLLEE HHlILLLLO00O2195..DD TTNN--AA 44880022 MMeeOOHH TTHHPPFFOOSS 00 00 00 0 3/19/2001 2 3 : l l C:\CHEM\Hillary.i\HO10319-a.b SAMPLE HILL0030.D TN-A 4802 MeOH THPFOS 00 0 3 3/19/2001 23:26 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0031.D TN-A 4802 MeOH THPFOS 00 0 PFOS PFOS PFOS PFOS PFOS 5.22 14278 0 0.00 0 0 5.21 27267 O 5.25 11603 0 0.00 0 0 3/20/2001 2:33 C:\CHEM\Hillary.i\HO10319-a.b SAMPLE HILL0044.D TN-A 4802 MeOH THPFOS 00 0 3/20/2001 2:47 C:\CHEM\Hillarv.i\HO10319-a.b SAMPLE HILL0045.D TN-A 4802 MeOH THPFOS 00 0 3/20/2001 5 4 0 C:\CHEM\Hilla&.i\HO10319-a.b SAMPLE HILL0057.D TN-A 4802 MeOH THPFOS 00 0 PFOS .P.FO_ S_ PFOS 0.00 0 0 ooo n- n- 0.00 0 0 3/20/2001 5-54 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0058.D TN-A 4802 MeOH THPFOS 00 0 PFOS 0.00 0 0 3/20/2001 9:Ol C:\CHEM\Hillary.i\HOIO319-a.b SAMPLE HILL0071.D TN-A 4802 MeOH THPFOS 00 0 PFOS 0.00 0 0 3/20/2001 9:15 C:\CHEM\Hillary.i\HOIO319-a.b SAMPLE HILL0072.D TN-A 4802 MeOH THPFOS 00 0 PFOS 0.00 0 0 3/20/2001 1154 C:\CHEM\Hillary.i\HO10319-a.b SAMPLE HILL0083.D TN-A 4802 MeOH THPFOS 00 0 PFOS 0.00 0 0 3/20/2001 12:08 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0084.D TN-A 4802 MeOH THPFOS 00 0 3/20/2001 14:47 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0095.D TN-A 4802 MeOH THPFOS 00 0 PFOS PFOS 0.00 0 0 0.00 0 0 3/20/2001 15:Ol C:\CHEM\Hillary.i\HOIO319-a.b SAMPLE HILL0096.D TN-A 4802 MeOH THPFOS 00 0 PFOS 0.00 0 0 3M EnvironmentalLaboratoly E00-1311 PFOS Adsorb/Desoib BACK TO MAIN I' a, e 0 GI Batch Samole List: Curve and Calibration Checks Acquislion InsWmenVSequence: Rush I R010312 OatelAnalystof Reprocessing: 27-28 Mar 01 / MIA Batch Method R010312.m Ouantitation Range: 5 to 501 ng/mL, Quadratic fit, lniernalStandard W a n t Inj Date Batch , SampType File Sample Name 3/13/2001 1 2 5 9 3/13/2001 13:lO 3/13/2001 13:21 3/13/2001 1 3 3 3 3/13/2001 1 3 4 4 3/13/2001 1 3 5 5 3/13/2001 1 4 0 7 311312001 14:18 3/13/2001 1 4 2 9 3/13/2001 14:41 3/13/2001 17:08 3/13/2001 17:19 31132001 19:47 3/13/2001 1 9 5 8 3/13/2001 2226 3/13/2001 2 2 3 7 3/14/2001 1:05 3/14/2001 1:16 3/14/2001 3:44 3/14/2001 3 5 5 3/14/2001 6 2 3 3/14/2001 6:34 3/14/2001 9 9 2 3/14/2001 9:14 3/14/2001 11:07 C:\CHEMRush.i\RO10312.b CALIB-1 C:\CHEMRush.i\RO10312.b CALIB-2 C:\CHEM\Rush.iR010312.b CALIB-3 C:\CHEM\Rush.i\R010312.b CALiB-4 C:\CHEMRush.iRO10312.b CALIB-5 C:\CHEM\Rush.i\RO10312.b CALIB-6 C:\CHEMRush.i\RO10312.b CALiB-7 C:\CHEM\Rush.i\ROl0312.b CALlB-8 C:\CHEMRush.i\RO10312.b CALlB-9 C\CHEM\Rush.iRO10312.b CALlB-IO C:\CHEM\Ruoh.iR010312.b SAMPLE C:\CHEM\Rush.iUiOl0312.b SAMPLE C:\CHEM\Rush.iUiO10312.b SAMPLE C:\CHEMRush.iRO10312.b SAMPLE C\CHEMRush.i\RO10312.b SAMPLE C:\CHEMRush.iRO10312.b SAMPLE C:\CHEMRush.i\RO10312.b SAMPLE C:\CHEMWush.i\RO10312.b SAMPLE C:\CHEM\Rush.i\RO10312.b SAMPLE C:\CHEM\Rush.iROl0312.b SAMPLE C:\CHEM\Rush.iRO10312.b SAMPLE C:\CHEMRush.iROl0312.b SAMPLE C:~HEM\Rush.i~O10312.b SAMPLE C\CHEMRush.iRO10312.b SAMPLE C:\CHEMRush.iWO103f2.b SAMPLE SAMPLE RUSH0018.D RUSH0019.D RUSH0020.D RUSH0021.D RUSH0022.D RUSHW23.D RUSH0024.D RUSH0025.D RUSH0026.D RUSH0027.D RUSHW40.D RUSH0041.D RUSH0054.D RUSHW55.D RUSHOOB8.D RUSHOffi9.D RUSHW82.D RUSHOOB3.D RUSHOO96.D RUSH0097.D RUSHOl 10.D RUSH0111.D RUSH0124.D RUSH0125.D RUSH0135.D RUSHO1X.D 5 ng/mL PFOS In MeOH 1 0 ng/mL PFOS in MeOH 25 ng/mL PFOS in MeOH 4 0 ng/mL PFOS in MeOH 50.1 nghnL PFOS in MeOH 75.1 nghnL PFOS in MeOH 100.2 ng/mL PFOS in MeOH 250.5 nghL PFOS in MeOH 400.8 ng/mL PFOS in MeOH 501 ng/mL PFOS in MeOH 5 ng/mL PFOS In MeOH 250.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 nghnL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ng/mLPFOS in MeOH 5 n g h L PFOS in MeOH 250.5 nghnL PFOS in MeOH 5 ng/mL PFOS in MeOH 250.5 ndmL PFOS In MeOH Misc Info Compound Name RT 01003-07-03 010034744 01003-07-05 0100307-08 01003-07-07 010 0 3 0 7 4 8 01003-07-09 0100307-10 0100507-11 0100307-12 01003-0743 01003-07-10 010030743 01003-07-10 01003-0743 01003-07-10 01003-07-03 01003-07-10 010030743 01003-07-10 01003-0743 01W3-07-10 01003-07-03 01003-07-10 010034743 01003-07-10 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.52 5.52 5.51 5.52 5.51 5.50 5.52 5.51 5.51 5.51 5.50 5.51 5.50 5.50 5.48 5.48 5.49 5.47 5.46 5.48 5.47 5.46 5.47 5.47 5.47 5.47 Area lawx 1175891 1179538 1182584 1170614 1181798 1181055 1158213 1161020 1178672 1183842 1100680 1104166 1077492 1087960 1078955 1102376 1038142 I024757 1028518 1029337 1016043 1008141 1011902 990965 Besgss 995410 Amount 2;; 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Compound Name "I ," .A I PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS RT w 5.73 5.73 5.72 5.73 5.72 5.72 5.73 5.73 5.73 5.73 5.71 5.73 5.71 5.71 5.70 5.69 5.70 5.69 5.87 5.87 5.68 5.68 5.68 5.68 5.69 5.69 Area Amount Theoretical " 204920 357143 891797 1351707 1872821 2422605 3017918 6654469 9884645 11780946 199857 6579760 203470 6288787 191841 6376911 211733 6137149 188604 6114459 197545 6034586 189737 6021739 187812 6061624 3.5 8.1 24.7 39.9 50.0 75.5 98.8 246.3 393.6 490.1 3.8 258.1 4.0 248.8 3.6 249.0 4 6 259.6 3.8 257.1 4.2 260.1 4 .O 264.3 4.0 284.9 70.1% 81.1% S8.7% 99.7% 99.8% 100.6% 98.6% 98.3% 98.2% 97.8% 75.3% 103.0% 80.5% 99.3% 72.5% 99.4% 91.3% 103.7% 76.6% 102.6% 84.5% 103.8% 79.5% 105.5% 80.3% 105.8% 3/14/2001 1 2 1 5 C:\CHEMWush.W010312.b CALIB-11 RUSH0141.0 3/14/2001 1 2 2 6 C:\CHEMRush.iROl0312.b CALlB-12 RUSHOl42.D 3/14/2001 1 2 3 8 C:\CHEM\Rush.i\ROlO3lZ.b C U B - I 3 RUSH0143.D 3/14/2001 1 2 4 9 C:\CHEM\Rush.iW01031Z.b CALlB-14 RUSH0144.D 3/14/2001 1 3 0 1 C:\CHEM\Rush.i\R010312.b CALiB-IS RUSH0145.D 3/14/2001 1312 C:\CHEM\Rush.i\R010312.b CALIB-16 RUSH0146.D 3/14/2001 1 3 2 3 C:\CHEMlRush.iR010312.b CALIB-17 RUSH0147.0 3/14/2001 1 3 3 5 C:\CHEM\Rush.iR010312.b CALlB-18 RUSH0148.D 3/14/2001 1346 C \CHEMRush i\R010312 b CALlBIl9 RUSH0149D 3/14/2001 13 57 . C L \CHEM\Rush i d a*ullt.0. iW010312 b pol"" y. M ,"CALIB-20 "..d ,rU I I D RUSH0150 D O I O n Ws"ldo". 5 ng/mL PFOS in MeOH 1 0 nglmL PFOS in MeOH 25 ng/mL PFOS in MeOH 4 0 ng/mL PFOS in MeOH 50.1 nglmLPFOSin MeOH 75.1 ng/mLPFOS in MeOH 100.2 nghnL PFOS in MeOH 250.5 nghnL PFOS in MeOH 400.8 n m L PFOS in MeOH 501 nglmLPFOS in &OH 010030743 0100307-04 01003-07-05 010030748 aiw3-07-07 0100307-08 01003-07-09 01003-07-10 0100307-11 0100367-12 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.46 5.48 5.46 5.46 5.46 5.46 5.47 5.46 5.48 5.48 1010117 999012 1013523 1000910 1019495 1013642 1007297 1010097 995285 1019903 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS m m l r O . w . - . -1 ,=,4r a m - 7 JOI 5.68 5.68 5.88 5.68 5.68 5.68 5.69 5.67 5.67 5.67 184884 324179 787488 1203328 1495911 2154462 2739039 5867202 8617452 10475418 3.8 8.9 25.5 41.7 52.0 78.8 103.8 250.2 409.9 510.6 76.3% 89.0% 102.1% 104.2% 103.9% 104.6% 103.4% 99.9% 102.3% 101.9% EOO-1311PFOS AdsMblDBsolb BACK TO MAIN Balm Sem~lqLis1 SamDles Only Acqulsbon lnswrnenVSequenw RushI R010312 DalslAnalyn ol Reprocessing 27-28 Mar 01 I MLA Balm Meinoa R010312.m Ouanurauon Range 6 lo 501 n@mL, Quadratic fit,lniemalStandard Quint. In1 Date Batch Flla SampleNima CompoundNamc RT AN. Amour4 Compoundname RT A n a Amount 3/13/2001, 1535 C:\CHEM\Rush.i~010312.b RUSHW30.D 1311-5088S1 THPFOS 551 1385664 254 PFOS 5.73 9084269 289.8 3/13/200115:26 3/13/2001 1537 3113,2001 16:00 C:\CHEMWush.l\R010312.b RUSH0031.D C:\CHEMWushhR010312.b RUSHW32.D C5CHEM\Rush.i\R010312.b RUSHWM.D 13115089 1311-5090 13115091 THPFOS THPFOS THPFOS -5.51 1477514 254 5.50 1191529 254 5.51 1269217 254 PFOS -" PFOS ^^ PFOS 5.72 9108410 268.9 5.72 7388008 269.9 5.73 1291151 34.6 3/13/2001 16:11 C:~HEM\Rush.i\R010312.b RUSH0035.D 13115092 THPFOS 5.51 1192069 254 PFOS 5.72 334372 7.3 3/13/2001 1623 C:\CHEM\Rush.i\RO10312.b RUSH003B.D 1311-5093 THPFOS 5.51 1150399 254 PFOS 5.72 177340 2.8 3/13/2W1 1634 C:\CHEM\Rush.i\RO10312.b RUSH0037.D 13115093MS THPFOS 5.50 1021896 254 PFOS 5.72 4988078 203.3 3/13/2001 l6:45 C:\CHEM\Rushl\RO10312.b RUSH0038.D 1311-5094 THPFOS 5.51 1149765 254 PFOS 5.72 1598584 49.0 3/13/2001 1657 C:\CHEM\Rush.iW010312.b RUSH0039.D 13115095 THPFOS 5.50 1187956 254 PFOS 5.72 1827571 54.8 3/13/2001 1754 C:~HEM\Rush.i\R010312.b RUSH0044.D 13115096 THPFOS 5.51 1190238 254 PFOS 5.72 1567771 46.2 3/13RW1 18:05 C:\CHEM\Rush.iAR010312.b RUSHW45.D 13115096MS THPFOS 5.51 1010278 254 PFOS 5.73 8130982 263.8 3/13/2001 18:16 C:\CHEM\Rush.i\R010312.b RUSHW46.D 13115097 THPFOS 5.51 1151402 254 PFOS 5.72 5335559 191.2 3113RWl 18:28 3/13/2001 18:39 C:\CHEM\Rush.i\R0103lZ.b RUSHW47.D C:\CHEM\Rush.RR010312.b RUSHW48.D 13115098 13115099 THPFOS THPFOS - 5.51 1115232 254 5.50 1102724 254 *I -.. PFOS PFOS -" 5.72 6471149 249.9 5.71 6167800 239.1 3/13/2001 19:M 3/13RO01 19:13 3/13/2W1 1924 3/13,2001 19:36 3/131200120:32 3/13/200120:44 3/13/200120:55 C:\CHEM\R~sh.l\R010312.b C\CHEM\Rush.iWO10312.b C:5CHEM\Rwh.l\R010312.b C:\CHEM\Rush.i\R010312.b C:\CHEM\Rush.i\R010312.b C:\CHEM\Rurh.i\RO10312.b C:\CHEM\Rush.l\R010312.b RUSH005O.D RUSH0051.D RUSHCM52.D RUSHW53.D RUSHW58.D RUSHW59.D RUSHW60.D 1311-5100 1311-5101 13114102 1311-5102MS 13115103 13115104 13115105 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.50 1062217 254 5.49 1091409 254 5.49 1089550 254 5.49 954668 254 5.49 1117174 254 5.50 1116804 254 5.48 1088708 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.71 4081880 153.8 5.71 3885689 140.8 5.71 3812836 1380 5.71 7834048 370.7 5.70 7957940 321.0 5.71 7667501 306.8 5.69 7435595 305.4 u- Y13/200121:18 C:\CHEM\Rush.i\RO10312.b RUSHWB2.D 13115106 THPFOS 5.49 1197459 254 PFOS 5.71 5272348 180.1 3/13/200121:29 C:\CHEM\Rush.i\R010312.b RUSHW63.D 13115107 THPFOS 5.49 1180945 254 PFOS 5.69 5098549 176.0 3/13/200121:41 C:\CHEM\Rush.l\ROl0312.b RUSHW64.D 13115108 THPFOS 5.49 1203215 254 PFOS 5.70 5046570 170.2 3/13/200121:52 C:\CHEM\Rush.i\R01031Z.b RUSH0065.D 13115108MS THPFOS 5.48 1052179 254 PFOS 5.70 9075493 407.9 3/13/2W122:03 C\CHEM\Rush.iWO10312.b RUSH0OSB.D 13115109 THPFOS 5.49 1065391 254 PFOS 5.70 478603 134 i 3/13/2W12215 C:\CHEM\Rush.l\R010312.b RUSHW67.D 13115110 THPFOS 5.48 1166374 254 PFOS 5.89 154573 2.0 3/13/200123:ll C\CHEM\Rush.N1010312.b RUSH0072.D 13115111 THPFOS 5.48 1179002 254 PFOS 0.00 0 0.0 3/13/200123:23 C:\CHEM\Rushi\R010312.b RUSH0073 D 1311S111MS THPFOS 5.48 956166 254 PFOS 5.69 4711542 205.6 Y13Rw121.34 C:\CHEM\Rush.i!R010312.b RUSH0074.D 1311-5112 THPFOS 5.48 1126349 254 PFOS 5.69 1945796 62.4 3/13/2001 23:45 C\CHEM\Rush,i\RO10312.b RUSHW75.D 13115113 THPFOS 5.48 1133593 254 PFOS 5.69 1923182 61.1 3/13/20012357 C:\CHEM\Rush.i\R010312.b RUSH0076.D 13115114 THPFOS 5.48 105W97 254 PFOS 5.69 1911701 66.1 3/14ROO10:08 C:\CHEM\Rush.i\R010312.b RUSH0077.D 1311-5114MS THPFOS 5.48 913903 254 PFOS 5.69 5785268 277.7 3/14Roo1 0.20 C:\CHEM\Rush.l\R010312.b RUSHW78.D 13115115 THPFOS 5.47 1051871 254 PFOS 5.M) 7556059 324.3 U14/2W10:31 C5CHEM\Rush.iW010312.b RUSH0079.D 1311-5116 THPFOS 5.48 1005648 254 PFOS 5.69 7453080 337.1 3/14R0010:42 C:\CHEM\Rush.i\R010312.b RUSH0080.D 1311-5117 THPFOS 547 1064813 254 PFOS 5.88 7243851 303.4 31~0011:50 3/14RWl 2 0 2 3/14RW12:13 3/14/20012:25 3/14R0012:36 3/1412001 2 4 7 3/14/2001 2 5 9 3/14/2001 3 3 0 3/14/2001 3 2 1 3/14/20013:33 3/14/2001 4 2 9 311412001 4:41 3/14120014:52 3/14/2W15:04 Y14R001 515 3/14/2001 526 3/14/2W15:38 3/14/20015:49 3/14/2001 6:00 3/14/2W16:12 3/14/2001 7:08 3/14/20017:20 3/14/2001 731 3/14/2w17:43 3/14/2W1 7 5 4 3/14/2001 8:05 3/14/2001 8:17 3/14/2001 8:28 3/14RW1@39 3/14/2001 8 5 1 3/14/2001 9:48 311412001 9:59 3/14/2001 10:lO 3/14/2001 1022 W1412Wl 1033 3/14/2001 10:44 311412001 10:56 _. C\CHEM\RushiW010312b RUSH0086 D RUSH0087.D RUSH0068.D RUSH0089.D RUSH0090.D RUSH0091.D RUSHOW2.D RUSHCG93.D RUSHCG94.D RUSHW95.D RUSHO1W.D RUSHOlD1.D RUSHOlO2.D RUSH0103.D RUSH01W.D RUSHO105.D RUSH0106.D RUSH0107.D RUSHO108.0 RUSH0109.D RUSH0114.D RUSH0115.D RUSHO116.D RUSH0117.D RUSH0118.D RUSHO119.D RUSHOl2O.D RUSHO121.D RUSH0122.D RUSH0123.D RUSH0128.D RUSH0129 D RUSHO13O.D RUSHO131.D RUSH0132.D RUSH0133.D RUSH0134.0 13115118 13115119 1311-5120 1311-5120MS 1311-5019-SZ 1311-5020 13115021 1311-5021MS 13115022 13115023 1311-5024 13115024MS 1311-5025 13115028 1311-5027 13115027MS 13115028 13115029 13115030 1311-5030MS 13115031 1311-5032 13115033 13115033MS 1311-5034 1311-5035 13115036 1311-5036MS 1311-5055 13115055 13116057 13115057MS 1311-5058 1311-5059 1311-5060 13115060MS 1311-5061 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.48 1069400 254 5.48 1071246 254 5 47 1053796 254 5 47 906343 254 5.47 1068914 254 5.47 1035621 254 5.46 1058784 254 5.46 908983 254 5.48 1047722 254 5.47 1044074 254 5.47 1027244 254 5.47 900913 254 5.46 1034605 254 5.47 1024646 254 5.46 1017504 254 5.48 879952 254 5.49 997963 254 5.48 1030844 254 5.47 1022445 254 5.48 879426 254 5.46 1025535 254 5.47 1025203 254 5.47 1029469 254 5.47 880742 254 5.47 1023217 254 5.47 1012932 254 5.47 1026080 254 5.47 earn 254 5.47 987998 254 5.47 968034 254 5.48 691221 254 548 855978 254 5.48 897688 254 5.47 958286 254 5.47 975732 254 5.46 840001 254 5.47 967423 254 .. PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS ... 569 5 69 5 68 566 5 68 OW OW 5 67 5 69 5 68 5 69 5 68 5 68 5 68 5 68 5 69 5 70 5 69 5 69 5 70 5 68 5 68 568 5 69 5 68 5 68 5 68 5 68 5 68 588 ow 5 69 5 69 5 69 5 68 5 68 5 68 ...-. 5158635 4682505 5171543 e4%68 237607 0 0 4336124 413339 390331 420991 4492622 862953 009216 730970 4918144 1584024 970831 1650112 5622153 1856815 1884859 2002764 5840312 3730551 5585758 4711539 7998407 395287 166967 0 4243033 380@42 391761 847418 4805368 1987989 200.5 17i.7 204.6 460.9 5.2 00 0.0 197.9 11.4 10.7 12.0 208.5 27.7 28 9 23.3 238.9 56.0 31.7 57.8 281.1 65.7 66.9 71.2 293.9 144.7 235.1 189.2 448.9 11.6 34 0.0 206.8 10.9 11.9 29 0 245.7 75.7 3M Environmental Laboratory EO@-1311 PFOS AdsoMDsaorb P a w 4 of 5 Page 523 of 703 BACK TO MAIN ,9 7 s. 0 3 zI- Pe , 0 3 Batch SarnDle List MeOH Blanks Acquistion InstrumenffSequence: R u s h IR010312 DatelAnalystof Reprocessing: 27-28 Mar 01 I M U Batch Method: R010312.m Quantitation Range: 5 t o 501 ng/mL, Quadratic f&Internal Standard Q U m t lnj Date 3/13/2001 12:13 3/13/2001 1225 3/13/2001 14:52 3/13/2001 15:03 3/13/2001 17:31 3/13/2001 17:42 3/13/2001 20:lO 3/13/2001 20:21 3/13/2001 2249 3/13/2001 23:OO 3/14/2001 1 2 8 3/14/2001 1:39 3/14/2001 4:07 3/14/2001 4:18 3/14/2001 6:46 3/14/2001 6 5 7 3/14/2001 9:25 3/14/2001 9:36 3/14/2001 11:30 3/14/2001 11:41 3/14/2001 14:09 3/14/2001 2420 Batch C:\CHEM\Rush.i\R010312.b C:\CHEM\Rush.i\R010312.b C:\CHEMUiush.iRO10312.b C:\CHEM\Rush.iWOl0312.b C:\CHEM\Rush.i\RO10312.b C:\CHEMRush.i\RO10312.b C:\CHEM\Rush.iWOl0312.b C:\CHEM\Rush.i\RO10312.b C:\CHEM\Rush.i\RO10312.b C:\CHEMRush.iRO10312.b C:\CHEM\Rush.i\ROl0312.b C:\CHEM\Rush.iWO10312.b C:\CHEMWush.iWOl0312.b C:\CHEM\Rush.iW010312.b C:\CHEMRush.iW010312.b C:\CHEM\Rush.i!RO10312.b C:\CHEM\Rush.i\RO10312.b C:\CHEM\Rush.i\RO10312.b C:\CHEM~ush.iWO10312.b C:\CHEMWush.i\RO10312.b C:\CHEM\Rush.i\RO10312.b C:\CHEM\Rush.i\R010312. b SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File RUSH0014.D RUSH0015.D RUSHOO28.D RUSH0029.D RUSHOO42.D RUSH0043.D RUSH0056.D RUSH0057.D RUSH0070.D RUSH0071.D RUSHO064.D RUSHO085.D RUSHOO98.D RUSHO099.D RUSH0112.D RUSH0113.D RUSHO126.D RUSH0127.D RUSH0137.D RUSH0138.D RUSH0151.D RUSH0152.D Sample Name TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Compound Name RT THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 THPFOS 0 Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound Name PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS RT 5.76 5.69 5.74 5.67 5.68 5.66 5.70 5.70 5.70 5.69 5.66 5.64 5.62 5.63 5.63 5.64 5.64 5.64 5.64 5.63 5.70 5.63 Area 38880 28954 39944 31045 30703 26910 71679 67134 72663 87507 72910 27715 30881 26667 29144 26564 31899 27859 29497 25940 41235 31551 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 3M EnvironmentalLabwatwy EDO-1311PFOS AdrorbDescd Page 5 of 5 LG, -0 P) (P (D PFOS AdslDes E00-1311 BACK TO MAIN Intcml Slindard 9usnI. Rsproctrslns method H0~0222t.m.callbntlon hndards 6-250 nplmL 2.6 npPFOSImL standarddld not meet accuracy requlnnents. 500.750 and 1000nWmL standards exclud*d t o better fit th. data. 9uadratic cuwe fit Inj Date 2/2210120:51 2/22/0121.02 2/22/01 2133 2/22D1 21.24 2N101 21:35 2Rm121.46 21221012158 2/2m122:09 2122/0122:20 2/22/012231 2R2101 22:42 2Rm122:53 2R210123:04 2R3/01 1:29 2/23/01 1:40 2/23/014:05 2t23Dl 4:16 2/23/01 6.41 2123101 632 2/23/01 9:17 2/23/01 9:28 2/23101 1153 2R3/01 12:04 2/23/01 1430 22301 14:41 2123D1 16.44 2R301 16:55 2/23/01 17:28 2R301 17:39 m 3 m i 17:s 2/23/01 1802 2i23/01 18:13 2/2310118'24 22301 1835 2/23/01 18:46 2RJ101 18.57 2 R M 1 19:08 2/23/01 19.20 2R301 1931 ZRYOl 19:42 Batch D:WemWiilary.iW01OW.b D:khemWillary.WOlOW b D:WemWillaIy.iWOlOW.b D.WemWillary.iW01022.b D:WemWillary.iWO10222.b O.WemUliliary.iWO10222.b D:WemWlllary.iWOIOW.b D:WemWillary.iWO10222.b D:WemWiliary.iWOlM22.b D.WemWillary.RHO10222.b D:WemWillaryiW010W.b D WlemWilia1y.RH010222.b D.~mWillary.iV1010222.b D:WemWillary.iW010222.b D.WemWiilary.RH010222.b D.\chemWillary.iWO10222.b D:WlamWillary.WOl02222.b D:WemWiliary.iWO10222.b DWemWillary.iWO10222.b DWemWillary.iWO10222.b D:WemWiliary.iW01022.b D:WemWillary.iWO10222.b D.WamWillary.iWO10222.b D:WamWillary.iWOIO222.b D:'~~emWiliary.WO10222.b D.WemWlllary.iWO10222.b O.WemWillary.iWO10222.b D:WemWillary.iWO10222.b D.WemWillary.iWO10222.b D;Wem\Hillwy.RHO10222.b D:WlemWiilary.RHOlM22.b D:WemWiilary.iWOIO222.b D:WemWillary.iWO10222.b D:#emWillary.iWO10222.b D.WemWillary.iWO10222.b DWemWillary.iUl010222.b D:WemWillary.iWO10222.b D:WemWiilary.iWOlOW.b D.WemWilla~.~O10222.b D:WemW~llary.iW010222.b SampType Fila SAMPLE HILLW22 D CALIB-1 HlLW23 D CALlB-2 HILLW24.D CALIB-3 HILLW25.D CALIB-4 HILLW26.D CALIB-5 HILLW27.D CUB-6 HtLLCQ28.D CALlB-7 HILLW29.D CALlB-8 HILLW30.D CALIB-9 HILL0031.D CALlB-IO HILLW32.D SAMPLE HiLLW33.D SAMPLE HlLLW34.D CCALIB-1 HILLOM7.D CCALIB-1 HiLLOM8.D CCALIB-1 HILL00gl.D CCALIB-I HILL0062.D CCALIB-1 HILL0075.D CCALIB-1 HILLW76.D CCALIB-I HILL0089.D CCALlB-1 HILL0090.D CCALIB-I HILL0103.D CCALIB-I HILL0104.D CCALlB-1 HILL0117.0 CCALIB-1 HILL0118.D CCALIB-I HILL0129.D CCALIB-1 HILL0130.D SAMPLE HILL0133.D CALIB-I1 HILL0134.D CALlB-12 HILL0135D CALIB-I3 HILL0136.D CALIB-14 HILL0137.D CALIB-15 HILL0138.D CALIB-16 HILL0139.D CALIB-17 HILL0140.D CALlB-I8 HILL0141.D CALlB-19 HILL0142.D CALlB-20 HILL0143.D SAMPLE HILL0144.D SAMPLE HILL0145.D Sample Name 00002-10401 00002-10402 WW2-lM43 WW2-10404 woO2-10405 W002-10406 MxKJ2-10407 00002-10408 00002-10409 m2-104-10 WW2-104-11 00002-104-12 0~-104-13 00002-10403 m2-104-10 woO2-10443 MXx)2.104-10 WW2-10403 W002-104-10 m2-10403 w002-104-10 oooO2-10403 m2-104-10 00002-1oeo3 ww2-104-10 oooO2-10443 00002-104.10 00002-10441 00002-10402 W2-10443 m2-10404 WOO2-10445 m2-10406 00002-10447 m02-10608 m2-10408 00002-104-10 M)o2-1M.11 00002-104-12 00002-104-13 Miac Info Compound N8me S M a m. t_~ n ~ L l 2.5 THPFOS THPFOS 5 THPFOS 10 THPFOS 25 THPFOS 40 THPFOS 50 THPFOS 75 THPFOS I00 THPFOS 250 THPFOS 500 THPFOS 750 THPFOS lW0 THPFOS 5 THPFOS 250 THPFOS 5 THPFOS 250 THPFOS 5 THPFOS 250 THPFOS 5 THPFOS 250 THPFOS 5 THPFOS 250 THPFOS 5 Twos 250 THPFOS 5 THPFOS 250 THPFOS (0 SW) 2.5 THPFOS THPFOS 5 THPFOS 10 THPFOS 25 THPFOS 40 THPFOS 50 THPFOS 75 THPFOS 1W THPFOS 250 THPFOS 500 THPFOS 750 THPFOS I000 THPFOS RT 4.945 4.938 4.945 4 945 4.945 4.938 4.944 4.937 4.937 4.945 4.932 4.905 4.948 4.944 4.928 4.937 4.938 4.903 4.934 4.933 4.904 4 921 4.914 4.93 4.818 4.91 4.909 4.909 4.917 4.9 4.897 4.902 4.902 4.91 4.902 4.903 4.902 4.902 4.903 4.904 Area 882637 883313 890555 879564 886135 877054 863584 863923 861128 819727 777086 727981 725193 938494 843674 954179 843825 955094 854940 972449 a46048 9MO% 841012 w76a 843661 965275 849853 960603 970213 975322 962803 955202 931719 913224 908508 891910 835096 767261 726914 710125 Averaae: 877~02 Std Dev: 75930 Y R S D 8.7% Amount Compound Name 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS 249.3 PFOS QC IS range (+I3-0% averaps): 1140493 +30%: 614112 30%: RT 5.169 5.162 5.169 5.169 5.169 5.162 5.168 5.161 5.162 5169 5.156 5.171 5.163 5.168 5.153 5.154 5.162 5.155 5.151 5.157 5.163 5.145 5131 5154 5.147 5135 5.134 5.133 5.134 5.124 5.121 5.126 5.127 5.134 5.127 5.113 5.119 5.126 5.127 5.128 Area 87135 71W7 130540 254321 527419 838037 10948% 1627972 2166581 5046746 9079135 12908429 16080347 128463 5084843 130987 5117167 124712 5115342 128458 5100493 126306 50014W 127270 5032612 123647 4974770 80947 70306 123635 246680 509141 809392 1075245 1576634 2094348 4914708 8822276 12478371 15773542 Amount 4.2 3.4 6.2 12.1 24.8 39.7 52.7 78.3 104.4 255.1 483.2 731.9 913.8 5.8 249.8 5.8 251.3 5.5 248.0 5.6 249.8 56 246.5 5.4 247.2 5.4 242 6 3.6 3.1 53 10.7 22.2 36.1 48 9 72.1 97.5 243.9 475.6 708.7 915.4 % meweucai X 123 1% 120 7% 99 1% 99 3% 105 4% 1043% 104 4% 102 1% X X 1151% 888% 1154% 1005% 109 8% 99 2% 111 1% 99 8% 111 8% 98 6% 108 5% 98 9% 107 8% 97 0% X 106 7% 107 I % ea 8% 90 3% 97 9% 96 1% 97 5% 97 6% 95 1% X X Page 1 of 4 BACK TO MAIN PFOS AdsDes Em-1311 Internal Standard Quint, Reprocessing method: H01022nm, calibrationstandards 5 - I O n#mL 2.5 ngPFOSlmLstandard did not meet accuracy requlrments, 500.750 and 1000 nglmL standards excludedto better Mthe data. Quadrauc CUNC M In1D a b Batch SampType File Sample Name MissInfo Compound Name RT 2R2101 23 38 2/2210123 49 2123101 o 00 2/23/01 o 11 2/23/01 0 22 2/23/010 33 2123m10 45 2123771 0 56 2231011 0 7 2123m1118 2/23/01 2 14 2/23/012 25 212Nl12 36 2/23/012 47 2/23/012 58 2/2M13 w 2/23/01 3 20 2R31013 32 2R31013 43 2123101354 m 3 m i 4 50 2/23/01 5 01 2,23/015 12 2113101 5 23 2/23/015 34 2 R M 1 5 45 2123/01556 2R3iU16 08 M u 0 1 6:lS 2 R M 1 6 30 2,23101 7 26 2,231017 37 Z n M l 7:48 m m 1 759 m~m8ii o 2/23/018 21 Z R M l 812 2/23/018 44 2 / 2 M 1 8 55 2/23/01906 D:khemWillary.iWO10222.b D \memWil!ary.iW@1~222.b D:WemWillary.WOl0222.b D.WemWillary.iW010222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLW37D 13114001Sl HILL0038D 13114W2S1 HILL0039D 13114W3S1 HILL0040D 13114W3MS-Sl D:WemWillary.iW010222.b D:Wem\Hillary iW010222.b D WemWillary.iW010222.b D:WemWillary.iWO10222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLW41D 13114W4S1 HILLW420 13114W5S1 HILL0043D 13114006s1 HILLW44D 13114006MSSl D'WlemWillary.iW010222.b D.WemWillary iWO10222.b D WemWillary.iWOlO222.b D.WemWllary.iWO10222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLWX5D 13114W7S1 HILL00460 1311400Bs1 HILL00510 1311400991 HILL0032D 13114009MSSl D.WemWillary.iW010222.b D.WemWillary iW010222.b D WemWillary.iW010222.b D.WemW3lary.iWO10222.b SAMPLE SAMPLE SAMPLE SAMPLE HILL00530 13114010S1 HILLW540 13114011S1 HILL0055 D 13114012Sl HILL0056D 13114012MSS1 D.WemWillary.iWO10222.b 0 WemWBlary.iW010222.b D.WemWillary.iWO10222.b D.WmWillary.iWO10222.b SAMPLE SAMPLE SAMPLE SAMPLE HILL00570 1311401391 H I U 5 8 0 13114014-S1 HILL00590 1311401541 HlLLW60 0 13114015MS-S1 D.WemWillary.iW010222.b D.WemWillary.iWO10222.b D.WemWillary.iWO10222.b D.WemWillary.iW010222.b SAMPLE SAMPLE SAMPLE SAMPLE H I L L M D 1311-401E-S1 HILLOW60 1311401791 HlLLW67D 13114018S1 HlLLW68 D 13114018MSSl D'WemWillary.iWO10222.b D.WemWillary.iWO10222b D:WemWillary.iW010222.b D:WemWillary.iWOl0222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLW69D 1311401991 HILLW70D 13114MDs1 HILLW71 D 13114UZ191 HILLW72 0 1311-4021MSS1 D:khsmWillrry,NIOl0222.b D.WemWillaiy.iWO10222b D WemWillary.iW010222.b D.WmWiilary.i~O10222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLW73.D 1311-4022-S1 HILL0074D 13114023-S1 HILL0079D 1311402491 HILLODBOO 13114024MS-S1 D:lchemWilkry.MolO222.b D:lchemWillary..lWO10222.b D WlemWillary.iW010222.b D.WemWillary.iWO10222.b WPLE SAMPLE SAMPLE SAMPLE HlLL0081.D 1 3 l l M 2 5 - S I HULW82.D 13114026S1 HILL083 D 1311402791 HILL0084D 13114027MS-S1 O:lchemWillary.MOlO222.b DWemWillary iW010222b D WemWillary.iW010222.b D.WemWillary.tWO10222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLW8S.D 1311-4028-S1 HILL0086D 13114029Sl HILLW87D 13114030-S1 HILL0088D 13114030MSS1 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 4.943 4.931 4.944 4.937 4.939 4.937 4.937 4.929 4.937 4.938 4.939 4.93 4.937 4.936 4.935 4.931 4.929 4.936 4.937 4 938 4.93 4.93 4.936 4.931 4 93 4.939 4932 4.925 4.933 4 931 4.929 4.937 4.947 4.938 4.93 4.932 4.937 4.929 4.931 4.929 Area 944393 963890 942003 ern32 945739 932519 933232 816057 944645 933140 965150 833273 871260 963096 966343 839415 971971 978257 958983 831850 1012423 1057231 1128229 879406 994786 1005038 995117 855713 1145409 1017422 996024 995047 1162201 1169445 1007177 949165 1167037 985447 1123074 866592 Samples E00-4Wl-SI mru4 0 5 1 9 1 *'. Amount 249.3 249.3 249.3 249.3 249.3 249.3 240.3 249 3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 248.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249 3 249.3 mpoundName RT Area Amount %Theoretical PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS was PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 0 0 5.161 0 0 0 4102327 0 0 0 5.153 0 0 0 4020982 5.161 5.162 5.17 5.154 1164609 1239235 1999524 5149900 5161 5.16 5.16 5.155 1233408 1214963 1183400 5007271 5.154 5.16 5.162 5162 1195984 1232516 1212915 5041035 5.154 5.154 5.16 5.155 1263565 1276111 1396036 5215525 5.154 5.163 5.1% 5149 1172949 1226450 1202381 5111162 5.15 5.155 5153 5.161 1537684 1206313 1250887 5936492 5.f65 5.162 5.162 5.163 1453734 1398064 1265770 5704109 5.168 5.161 5162 5.16 1418355 1267363 1377526 5191492 0.0 0.0 0.0 204.7 0.0 0.0 0.0 204.3 51.2 55.2 86.0 256.1 52.8 52.4 50.9 247.2 51.1 52.4 52.6 251.1 51.9 50.2 51.4 245.8 490 50.7 50.2 247.5 55.8 49.3 52.2 247.3 52.0 49.7 52.2 249.1 50.5 53.4 51.0 248.3 Page2 of4 PFOS Adsmes 00-1311 BACK TO MAIN Sampler E W 4 W I S l thrd 4051-51 -3- InternalStandardQuint, Reprocerrlng method: H01022~m.Callbmlon standards6-250 nglmL 2.6 ngPFOSlmLstandard did not meet accuracy requlnnentr, 600,760 and 1000nNmL standards excluded to better Mthe data. QuadmUc curve M In) Date Batch SampType File Sample Name MI% Info Compound Name RT Am. m3m11002 2 m m i 10'13 m 3 m 1 10.24 2/23/01 10.35 D:WlemWillary.iWO10222.b D.WemWillary.IW010222.b O:WemWillary.iWO10222.b D:WemWillary.iWOl0222.b SAMPLE SAMPLE SAMPLE SAMPLE HlLL0093.D 13114031S1 HILLWM D 13114032S1 HILL0095D 1311403341 HILLW98.D 13114033MSSl THPFOS THPFOS THPFOS THPFOS 4 925 4 923 4 93 4926 1015824 1079934 10551W 898829 2R3/01 10.46 2/23/01 10.57 2/23/01 11:09 2123/oi 11:zo D WemWillary.RHO1OW.b 0 WemWiliary.iW010222.b D:WemWillary.iW010222.b D:WernWillary.iWOlO222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLW97.D 13114034-51 HILLW98.D 1311403551 HILLW99.D 13114036S1 HILLO1W.D 13114036MSSl THPFOS THPFOS THPFOS THPFOS 4 923 4 924 4 915 4 918 987405 1090655 1031470 841990 m 3 m i 11'31 zmmi ii:m z m m i 12.38 2 R M 1 1249 D:tchemWiilary.iWOl0222b O:WemWillary.iW010222.b D:WemWillary.iWOlOW.b D.WlemWillary.iWO1OW.b SAMPLE SAMPLE SAMPLE SAMPLE HiLLO1Ol.D 13114037Sl HILL0102.D 13114038sl HILL0107.D 1311403851 HILL0108.D 13114039MSSl THPFOS THPFOS THPFOS THPFOS 4 922 4 922 4 918 4 915 995964 992751 985052 844071 2/23/01 13:W 2/23/01 13:12 2/23/01 1323 m 3 m i 1x34 D.WemWillary.iWO10222.b DWemWillary.lW010222.b D:WemWillary.iW0102.b D:WemWillary.iW010222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLOlD9.D 13114040-51 HILLO1lO.D 13114041Sl HILLO1ll.D 13114042Sl HILL0112.0 13114042MSSl THPFOS THPFOS THPFOS THPFOS 4 91 4 917 4 908 4 915 %lo932 986341 982392 873132 2R3D1 1S45 212331 13% 2/23/01 14.07 2/23/01 14.18 o:chernWillar/IWO10Z?2.b D:WemWillary.lW010222.b O.WemWillary.iWO10222.b D.WemWillary.iW010222.b SAMPLE SAMPLE SAMPLE SAMPLE HlLLO113.D 13114M3s1 HlLLO114.0 13114M4S1 HILLO115.D 1311-4045-Sl HILL0116.0 13114045MSSl THPFOS THPFOS THPFOS THPFOS 4 914 4 925 4 922 4 923 984852 999207 997394 861434 m3mi1 5 : ~ ~3101 5 : ~ 212301 1537 2/23/01 15:48 D:~mWilIary.i~10222.b D:WemWillary.iW010222.b D:WlemWillary.iW010222.b D.WemWillary.iW010222.b SAMPLE SAMPLE SAMPLE SAMPLE HILLO1Zl.D 1311404651 HILL0122.D 1311-4047-51 HiLL0123.D 13114MBSl HILL0124.D 13114048MSSl THPFOS THPFOS THPFOS THPFOS 4 923 4 92 4 923 4 91 1017804 993010 1007737 853140 2 ~ 3 mi5i :59 2/23/01 1610 m3mi 1 6 : ~ m3mi 1 6 : ~ ~ DtchemWillary.lWOlOZ~.b D.WemWillary.iWO10222.b D.WemWillary.iW010W.b D.WemWillary.iWO10W.b SAMPLE SAMPLE SAMPLE SAMPLE HILL0125.D 13114049S1 HILL0126.D 1311405041 HlLL0127.D 1 3 1 1 4 0 5 1 ~ 1 HILL0128.D 13114051MSSl THPFOS THPFOS THPFOS THPFOS 4 916 4 91 4 915 4911 986831 979691 955326 849190 AVeRqe: 972356 Std Dev: 85032 .XRSD: 8.7% Amouni 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 Compound Name RT Area Amount PFOS PFOS PFOS PFOS 0 0 0 0 0 0 5.15 4355290 0.0 0.0 0.0 2w.9 PFOS PFOS PFOS PFOS 0 0 0 5.149 0 0 0 4108751 0.0 0.0 0.0 202.3 PFOS PFOS PFOS PFOS 5.153 5.153 5.142 5.139 876072 768043 683545 4577937 J6.6 33.0 28.9 2248 PFOS PFOS PFOS PFOS 5.141 5.141 5.139 5.146 277725 246166 265448 4439371 11.7 10.4 11.3 210.8 PFOS PFOS PFOS PFOS 5.145 269994 5.1479 23462256227 5.154 4358791 11.5 1909.2 209.8 PFOS PFOS PFOS PFOS 5.147 5.144 5.148 5.134 330798 266017 312638 4357808 13.6 11.2 12.9 211.8 PFOS PFOS PFOS PFOS 5.14 5.141 5.139 5.135 223688 203407 237833 4290735 9.5 8.7 104 209.5 X meoreucal Page 3 of 4 BACK TO MAIN Quantity Compovnd RiipOrt E00-1311 P M 8 AdsorblDesOrb 8 - h List: Last wdified: Method: Last wdifisd: Job Code : C:\Mse~l~\:~oup020199.pro\8ampl~D8\~001207 Mon Dec 11 0'3:05:24 2000 C:\Msrlilynw\:10up020199.pro\MethD8\s001201 m n De0 11 0'):10:27 2000 Priqed: m n DOC 11 0 ! 3 : a 3 : 3 8 2000 C m s n u n d 1: P.08 1499,991. :Cum 1 # N- study no S.-lelirt Text 1 s001201~001 E00-1311 NeOH Blank, TN-A-4115, Aliq. 11/16/00 2 s001201_002 E00-1311 11101.7 ppb PFOS 00002-86-13. allq. 11-27-00 MLA 3 ~ 0 0 1 2 0 1003 E00-1311 1001.7 DDb PFOS 00002-86-13. alia. 11-27-00 MLA 4 E00-1311 L2OH Blank, TN-AL-4715,Aliq. ll/i6/00 5 E00-1311 MeOH Blank. TN-A-4115. Aliq. 11/16/00 6 E00-1311 0 ppb PFOS 00002-86-01, Aliq. 11-27-00 MLA 1 E00-1311 2.5 ppb PFOS 00002-86-02. Aliq. 11-21-00 MLA 8 E00-1311 5.00 ppb PFOS 00002-86-03. Aliq. 11-27-00 MLA 9 E00-1311 111.0 ppb PFOS 00002-86-04. Aliq. 11-27-00 MLA 10 EOO-1311 2'5.0 ppb PFOS 00002-86-05. Aliq. 11-27-00 MLA 11 E00-1311 411.0 ppb PFOS 00002-86-06. Aliq. 11-27-00 MLA 12 E00-1311 511.1 DDb PFOS 00002-86-01 Alia. 11-27-00 MLA 13 sOOl207I013 E00-1311 79.1 Pbb PFOS 00002-86-08. Alia. 11-21-00 MLA 14 ~ 0 0 1 2 0 1 ~ 0 1 4E00-1311 llJO.2~ipbPFOS 00002-86-09, Aliq. 11-27-00 MLA 15 ~ 0 0 1 2 0 1 ~ 0 1 5EOO-1311 2'50.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA 16 ~ 0 0 1 2 0 1 ~ 0 1 6E00-1311 5110.9 ppb PFOS 00002-86-11 Aliq. 11-21-00 MLA 17 a001201 011 E00-1311 11101.7 .o.Db PFOS 00002-86-13. alla. 11-21-00 MLA 18 ~ 0 0 1 2 0 1 ~ 0 1 8E00-1311 MlfOH Blank, TN-A-4115, Alla. ll/i6/00 19 ~ 0 0 1 2 0 1 ~ 0 1 9E00-1311 &?OH Blank, TN-A-4715, Alii. 11/16/00 20 ~ 0 0 1 2 0 7 ~ 0 2 0E00-1311 M*?OH Blank. TN-A-4115. Aliq. 11/16/00 21 ~001207-021 E00-1311 I1 ppb PFOS 00002-86-01, Aliq. 11-27-00 MLA 22 ~ 0 0 1 2 0 1 ~ 0 2 2E00-1311 2 5 ppb PFOS 00002-86-02. Aliq. 11-27-00 MLA 23 so01207 013 E00-1311 5 00 oob PFOS 00002-86-03. Alia. 11-21-00 MLA 24 ~001207--024 E00-1311 111.0 bbb PFOS 00002-86-04. All;. 11-21-00 MLA 25 s001207L025 E00-1311 25.0 PPb PFOS 00002-86-05. Alii. 11-27-00 MLA 26 ~ 0 0 1 2 0 1 ~ 0 2 6E00-1311 40.0 ppb PFOS 00002-86-06. Aliq. 11-27-00 MLA 27 s001201~021 E00-1311 511.1 ppb PFOS 00002-86-07 Aliq. 11-21-00 MLA 28 29 - s001201~028 E00-1311 ~ 0 0 1 2 0 1 ~ 0 2 9EO0 1311 7!;.1 ppb PFOS 0 0 0 0 2 - 8 6 - 0 8 . Aliq. 11-27-00 MLA 1110.2 ppb PFOS 00002-86-09. Aliq. 11-27-00 MLA 30 s001201_030 EOO-1311 2!50.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 31 ~ 0 0 1 2 0 1 ~ 0 3 1EO0 - 1311 500.9 ppb PPOS 00002-86-11 Aliq. 11-27-00 MLA 32 r001201 032 E00-1311 1001.7 ppb PFOS 00002-86-13. aliq. 11-27-00 MLA 33 sOOl201IO33 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 34 E00-1311 &:OH Blank, TN-A-4715, Alii. 11/16/00 356 37 38 39 40 41 42 43 44 45 46 41 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 732 74 75 76 s001207I016 71 18 19 eo 81 82 83 e4 e5 86 87 e8 e9 E00-1311 E00-1311 E00-1311 E00-1311 EOO-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 EOO-1311 E00-1311 ZOO-llll EOO-1311 E00-1311 E00-1311 EOO-1311 E00-1311 E00-1311 EOO-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 EOO-1311 E00-1311 E00-1311 250.4 ppb PFOS 00002-86-10. Aliq. 11-21-00 MLA MeOH Blank, TN-A-4115. Aliq. 11/16/00 MtiOH Blank, TN-A-4115. Aliq. 11/16/00 lllx E00-1311-3005-S1, 0.5mgIL. Ohr. NO soil. 12/01/00 lllx E00-1311-3006-S1, 0.5mgIL. Obr. NO soil. 12/01/00 lllx E00-1311-3006ms-S1,0.5mg/L, Ohr, NO soil, 12/07/00 lllx E00-1311-3013-S1, 0.OmglL. Ohr. 1:lclay. 12/01/00 lox E00-1311-3014-S1, O.Omg/L, Ohr, 1:lclay. 12/01/00 Zli0.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA M1:OH Blank. TN-A-4115, Aliq. 11/16/00 M<!OH Blank, TN-A-4115. Aliq. 11/16/00 l l l x E00-1311-3015-S1, O.Omg/L. Ohr, 1:lclay. 12/01/00 lllx E00-1311-3015ms-S1,0.Omg/L, Ohr. 1:lclay. 12/07/00 lllx E00-1311-3016-S1. O.Omg/L. Ohr, 1:5clay. 12/07/00 10x E00-l311-3017-S1, O.Omg/L. Ohr, 1:Sclay. 12/07/00 lOx E00-1311-3018-S1. O.Omg/L. Ohr. l:5clay, 12/07/00 2!>0.4 ppb PFOS 0 0 0 0 2 - 8 6 - 1 0 , Aliq. 11-27-00 MLA ":OH Blank. TN-A-4715. ALlrq. 11/16/00 MeOH Blank, TN-A-4715. Aliq. 11/16/00 lllx E00-1311-3018ms-S1.0.Omg/L. Ohr. 1:Sclay. 12/07/00 l l l x E00-1311-3019~S1,O.OmglL.Ohr. 1:25clay. 12/01/00 l l l x E00-1311-3020-S1,0.0mg/L, Ohr. 1:25clay, 12/07/00 l l l x E00-1311-3021S1.0.Omg/L. Ohr. 1:25clay. 12/07/00 l l l x E00-l3ll-3021ms-S1,0.Omg/L,Ohr. 1:25clay. 12/07/00 :!50.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA MeOH Blank. TN-A-4715. Aliq. 11/16/00 HeOH Blank, TN-A-4115, Aliq. 11/16/00 :Ox E00-1311-3031-S1.0.5mglL. Ohr, 1:lelay. 12/01/00 :Ilx E00-1311-3032-S1,0.5mg/L. Ohr. 1:lclay. 12/01/00 :Ox EOO-l311-3033-Sl,0.5mg/L. Ohr. l:lclay, 12/01/00 :Ox E00-l311-3033ms-S1,0.5~/L, Ohr, 1:Iclay. 12/01/00 lllx E00-1311-3034-S1,0.5mg/l.0hr. 1:Sclay. 12/07/00 250.4 ppb PFOS 00002-86-10. Aliq. 11-21-00 MLA Mt!OH Blank. TN-A-4115. Aliq. 11/16/00 MeOH Blank. TN-A-4115. Aliq. 11/16/00 l0x E00-1311-3035-S1.0.5mg/L,Ohr, 1:Sclay. 12/01/00 lllx E 0 0 - 1 3 1 1 - 3 0 3 6 - S 1 , 0 . 5 m g l L . O h r , 1:Sclay. 12/01/00 l(lx E00-1311-3036ms-Sl,0.5mg/L,0hr, 1:Sclay. 12/07/00 l(lx EOO-1311-303l-S1,0.5~/L,Ohr. 1:25clay, 12/07/00 l ( l x E 0 0 - 1 3 1 1 - 3 0 3 8 - S 1 , 0 . 5 ~ / L , O h r ,1:25clay. 12/01/00 2!#0.4 ppb PFOS 00002-86-10. Aliq. 11-21-00 MLA HeOH Blank, TN-A-4115, Aliq. 11/16/00 Mt!OH Blank, TN-A-4715. Aliq. 11/16/00 l(lx E 0 0 - 1 3 1 1 - 3 0 3 9 - S 1 , 0 . 5 m g l L . O h r , 1:25clay. 12/07/00 l(lx E00-1311-3039-S1,0.5mg/L,Ohr, 1:25clay. 12/07/00 EIr!OH Blank, TN-A-4115, Aliq. 11/16/00 MeOH Blank, TN-A-4715. Aliq. 11/16/00 MeOH Blank, TN-A-4715. Aliq. 11/16/00 0 ppb PFOS 00002-86-01, Aliq. 11-27-00 NLA Analyte Analyte Analvte Anal& Analyte Analyte Analyte Analyte Analyte Ana1yte Ane1yte Analyte Analyte Ana1yte Analyte Analyte Analyte Analvte Blank Blank Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Blank Blank Analyte Analyte Ana1yte Ana1yte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Blank Blank Analyte Std Conc 2.50 5.00 10.00 25.00 40.00 50.10 75.10 100.20 250.40 500.90 1001.70 250.40 250.40 250.40 250.40 250.40 250.40 RT 7.oeo 7.082 7.079 7.092 7.091 7.092 1.080 1.094 7.093 1.082 1.082 1.092 7.089 1.092 7.082 7.079 1.079 7.101 1.091 7.089 7.079 7.080 1.093 1.093 ~~ 7.092 1.094 7.080 7.080 7.082 7.081 7.091 7.091 7.104 1.091 7.092 7.089 7.105 1.105 7.093 1.103 1.093 1.093 7.094 1.094 1.086 7.105 7.098 7.109 7.094 7.106 7.115 1.106 1.105 7.104 7.106 1.103 7.104 7.092 7.091 1.106 7.106 7.092 1.104 7.105 1.093 1.091 7.106 1.103 1.103 1.106 1.131 1.106 1.103 7.105 7.105 1.092 1.104 1.100 1.106 1.107 1.092 7.091 1.091 1.104 1.092 1.101 PIDB 1 Area 92 50144 46601 ~~~~~ 364 102 131 pvb 0.00 0.00 0.00 0.00 5-v LOO LOO Flags Mod Co bb bb1 h_ hT _. bb bb bb bb bb 8189 9927 18824 29260 42301 262 123 18 111 534 805 1401 ~~ ~ 3018 4640 5541 1431 9561 18376 28180 40982 350 183 11 11 25 25 13130 227 14711 86 40 33 13912 61 13528 13 61 18197 91 53 23 13924 59 29 14015 18494 11814 e2 13420 14135 64 21 2906 4003 6024 17898 23398 20000 20428 15260 12 20562 20568 137 86 52 io8 86.02 15 bb 115.03 15 bb 269.69 8 bb 493.19 -1 bb bbI 0.00 bb ~~ 0.00 bb 0.00 bb 0.00 bb 0.00 -100 bbX 0.00 -100 bbx 0..0.0. -1..0.0 hhY 12.07 -52 bb 34.18 -13 bb 41.01 -6 bb 80.70 7 bb 115.12 15 bb 255.94 2 bb 469.41 -6 bb 848.10 -15 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 243.94 bb 0.00 bb 291.29 16 bb 0.00 bb 0.00 bb 0.00 bb 341.05 bb 0.00 bb 289.20 0.00 0.00 15 bb bb bb 463.23 bb 0.00 bb 0.00 bb 0.00 bb 272.53 9 bh 0.00 bb 0.00 bb 151.28 bb 398.29 bb 449.11 bb 0.00 bb 261.31 bb 281.45 12 bb 0.00 bb 0.00 bb 26.41 bb 47.72 bb 14.95 bb 541.85 bb 366.00 bb 211.32 11 bb 0.00 bb 0.00 bb 389.48 bb 390.30 bb 554.07 bb (27.38 bb 401.20 bb 214.95 10 bb 0.00 bb 0.00 bb 450.84 bb 441.93 bb 0.00 bb 0..0.0~ bb 0.00 bb 0.00 bb SOUP 020199: wantitated d l printed by chzc on 12/11/00 3M Environmental Laboratory Page 529 of 703 BACK TO MAIN Guantify Ccmuound sunmaw R e w r t E00-1311 PFO8 AdsorbIE0sorb S-le List: C:\lllsalynr.\~ou~020199.~ro\S~laDB\r001201 Method: C:\lll~~ly~1.\~0~~020199.~r0\l(atMB\~001201 Last mdified: I(on IMC 11 09:10:27 2000 Job Code : Prinded: I4on m c 11 09:23:38 2000 - _ - - - - I _ _ CaqpoUnd 1: PFOS ( 4 9 9 > 9 9 ) , fwrC 1 U Narm study M SaTwlelist Text 90 ~001207-090 E00-1311 2 . 5 ppb PFOS 00002-86-02, Aliq. 11-27-00 MLA 91 ~001207-091 EOO-1311 5.00 ppb PFOS 0 0 0 0 2 - 8 6 - 0 3 , Aliq. 11-27-00 MLA 92 ~001207-092 E00-1311 10.0 ppb PFOS 00002-86-04, Aliq. 11-27-00 MLA 93 ~001207-093 E00-1311 25.0 ppb PFOS 00002-86-05. Aliq. 11-27-00 MLA 94 ~001207-094 E00-1311 40.0 ppb PFOS 0 0 0 0 2 - 8 6 - 0 6 , Aliq. 11-27-00 MLA 95 ~001207-095 E00-1311 50.1 ppb PFOS 00002-86-01 Aliq. 11-21-00 MLA 96 ~001201-096 E00-1311 15.1 ppb PFOS 00002-86-08. Aliq. 11-27-00 MLA 91 ~001207-091 EOO-1311 100.2 ppb PFOS 00002-86-09, Aliq. 11-27-00 MLA 98 ~001207-098 E00-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA 99 s001207L099 E00-1311 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA 100 ~ 0 0 1 2 0 7 ~ 1 0 0E00-1311 1001.7 ppb PFOS 00002-86-13. aliq. 11-27-00 MLA 101 ~ 0 0 1 2 0 7 ~ 1 0 1E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 102 s001201~102 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 103 ~001207-103 E00-1311 MeOH Blank. TN-A-4115, Aliq. 11/16/00 104 ~ 0 0 1 2 0 1 ~ 1 0 4EOO-1311 lox E 0 0 - 1 3 1 1 - 3 0 4 0 - S 1 , 0 . 5 m g l L . 2 h r 105 ~001207-105 EOO-1311 lox E 0 0 - 1 3 1 1 - 3 0 4 1 - S 1 , 0 . 5 m g / L . 2 h r 106 ~001207-106 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 4 2 - S 1 , 0 . 5 m g / l . 2 h r 107 ~ 0 0 1 2 0 1 ~ 1 0 7E00-1311 250.4 ppb PFOS 00002-86-10, Aliq 108 ~001207-108 E00-1311 .YeOH Blank. TN-A-4115. Aliq. 11/16/00 109 ~001207-109 E00-1311 MeOH Blank, TN-A-4115, Aliq. 11/16/00 110 ~ 0 0 1 2 0 7 ~ 1 1 0E00-1311 lox E00-1311-3042ms-S1,0.5mg/L.Zhr. 1:lclay. 12/01/00 111 ~ 0 0 1 2 0 7 ~ 1 1 1~ 0 0 - 1 3 1 1lox E00-1311-3043-S1 112 ~001207-112 E00-1311 LOX E00-1311-3044-S1 113 ~001207-113 E00-1311 LOX E00-1311-3045-S1 114 ~001207-114 E00-1311 LOX E00-1311-3045ms- 115 ~001207-115 E00-1311 :250.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 116 ~001207-116 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 117 ~001207-117 E00-1311 MeOM Blank. lT-A-4715, Aliq. 11/16/00 118 ~001207-118 E00-1311 LOX E 0 0 - 1 3 1 1 - 3 0 4 6 - S 1 , 0 , 5 m g l l . 2 h r . 1:25clay 119 ~001207-119 E00-1311 .LOX E 0 0 - 1 3 1 1 - 3 0 4 7 - S 1 . 0 . 5 m J / L . 2 h r . 1:25clay 120 ~ 0 0 1 2 0 7120 E00-1311 LOX E 0 0 - 1 3 1 1 - 3 0 4 8 - S 1 . 0 . 5 m g / l . 2 h r . 1:25clay 121 s001201I121 E00-1311 :LOX E00-1311-3048ms-S1,0.5mglL.2br, l:25clay, 12/07/00 122 ~001207-122 E00-1311 .LOX E 0 0 - 1 3 1 1 - 3 0 4 9 - S 1 , 0 . 5 n g / L . 4 h r . l:lclay, 12/07/00 123 ~001207-123 E00-1311 :!SO.( ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA 124 ~001207-124 EOO-1311 MeOH Blank. TN-A-4115. Aliq. 11/16/00 125 ~001207-125 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 126 so01207 126 E00-1311 :.Ox E 0 0 - 1 3 1 1 - 3 0 5 0 - S l , 0 . 5 m g / l . d h r . l:lclby, 12/01/00 127 ~ 0 0 1 2 0 1 ~ 1 2 7E00-1311 :.Ox E 0 0 - 1 3 1 1 - 3 0 5 1 - S 1 , 0 , 5 m g / L . d h r , 1:lclay. 12/01/00 E00-1311 ].Ox E 0 0 - 1 3 1 1 - 3 0 5 1 m s - S 1 , 0 . 5 ~ l L . P h r . 1:lclay. 12/07/00 E00-1311 :.Ox E 0 0 - 1 3 1 1 - 3 0 5 2 - S 1 , 0 . 5 m g / L , 4 h r , 1:Sclay. 12/07/00 E00-1311 ].Ox E 0 0 - 1 3 1 1 - 3 0 5 3 - s 1 , 0 . 5 W / L . d h r . 1:5clay, 12/07/00 E00-1311 2150.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4115. Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4115. Aliq. 11/16/00 E00-1311 ].Ox E 0 0 - 1 3 1 1 - 3 0 5 4 - S 1 , 0 . 5 m g l L . d h r . 1:Sclay. 12/07/00 E00-1311 l o x E 0 0 - 1 3 1 1 - 3 0 5 4 m 4 - S 1 , 0 . 5 m g / L , 4 h r . l:5clay. 12/07/00 E00-1311 1 . 0 ~E 0 0 - 1 3 1 1 - 3 0 5 5 - S 1 , 0 . 5 m g l L . l h r , 1:25clay, 12/07/00 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 5 6 - S 1 , 0 . 5 m g l t . d h r . 1:25clay. 12/07/00 EOO-1311 lox E 0 0 - 1 3 1 1 - 3 0 5 7 - S 1 , 0 . 5 m g / L . ( h r . 1:ZSclay. 12/07/00 E00-1311 250.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 140 ~ 0 0 1 2 0 7 ~ 1 4 0E00-1311 MeOH Blank, TN-A-4715, Aliq. 11116/00 141 ~001207-141 E00-1311 EleOH Blank. TN-A-4715. Aliq. 11/16/00 142 ~001207-142 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 5 7 m a - S 1 , 0 . 5 m g / L . 4 h r . 1:25clay, 12/07/00 143 ~001207-143 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 6 7 - S 1 , 0 . 5 m e l L . 1 6 h r . 1:lclay. 12/07/00 144 ~001207-144 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 6 8 - S 1 , 0 . 5 m g / L , 1 6 h r . 1:lclay. 12/07/00 145 ~001201-145 E00-1311 l o x E 0 0 - 1 3 1 1 - 3 0 6 9 - S 1 , 0 . 5 m g / l . l 6 h r , 1:lclay. 12/07/00 146 s001207L146 E00-1311 lox E00-1311-3069ms~S1,0.5mglL.16hr. 1:Icle~. 12/07/00 147 5001207-1&7 E00-1311 2 5 0 . 4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA 148 ~001207-148 E00-1311 NeOH Blank, TN-A-4715, Aliq. 11/16/00 149 ~001207-149 E00-1311 lleOH Blank, TN-A-4115. Aliq. 11/16/00 150 ~001207-150 E00-1311 lox E00-1311-3070-S1,0.5mg/L.16hr, 1:Sclay. 12/07/00 151 ~001207-151 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 7 1 - S 1 , 0 , 5 m / L , 1 6 h r , 1:5clay, 12/07/00 152 ~001207-152 E00-1311 ]Ox E 0 0 - 1 3 1 1 - 3 0 7 2 - S 1 , 0 . 5 m g l l . l 6 h r , 1:Sclay. 12/07/00 153 ~001207-153 EOO-1311 l o x E00-1311-3072ms-S1,0.5~/L,l6h~,l:5clay. 12/07/00 154 ~001207-154 800-1311 l o x E 0 0 - 1 3 1 1 - 3 0 7 3 - S 1 , 0 . 5 m g l l . l 6 h r . 1:25clay. 12/07/00 155 ~001207-155 E00-1311 2 5 0 . 4 ppb PFOS 00002-86-10, Aliq. 11-21-00 MLA 156 s001207L156 E00-1311 BeOH Blank. TN-A-4715. Aliq. 11/16/00 EOO-1311 WeOH Blank, lT-A-4715. Aliq. 11116/00 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 7 4 - S 1 , 0 . 5 m g l L . 1 6 h r . 1:25clay. 12/01/00 E00-1311 lox E00-1311-3015-S1,0.5m91L.16hr. l:25clay. 12/01/00 E00-1311 lox E00-1311-3075ms-S1,0.5mg/L.16hr,1:25clay, 12/01/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 163 s001207I163 E00-1311 MeOH Blank. TN-A-4715. Alia. 11/16/00 ~ 0 0 1 2 0 1 ~ 1 6 4E00-1311 MeOH Blank. TN-A-4115. Alii. 11/16/00 65 E00-1311 0 ppb PFOS 00002-86 169 s001207I169 170 171 112 113 174 175 176 177 178 E00-1311 E00-1311 E00-1311 - E00-1311 EO0 1311 E00-1311 - E00-1311 EO0 1311 E00-1311 E00-1311 . ~ ~~ - ~~~ ~~ - - 25.0 bbb PFOS 00002-86-05. Alia. 11-21-00 MLA 4 0 . 0 &b PFOS 00002-86-06. Alii. 11-27-00 MLA 50.1 ppb PFOS 00002-86-07 Aliq. 11-27-00 MLA 75.1 ppb PFOS 00002-86-08. Aliq. 11-27-00 MLA 100.2 ppb PFOS 00002-86-09. Aliq. 11-27-00 MLA 250.4 ppb PFOS 00002-86-10, Aliq. 11-21-00 MLA 500.9 ppb PFOS 00002-86-11 Allq. 11-27-00 MLA 1301.7 ppb PFOS 00002-86-13. aliq. 11-27-00 MLA MeOH Blank, TN-1-4715. Aliq. 11/16/00 l a O H Blank. TN-A-4715, Aliq. 11/16/00 Type Standard Standard Standard Standard Standard Standard Standard Standard Standard S tandllrd Standard Analyte Blank Blank Ana1yte Ana lyte Analyte QC Ana1yte Analyte Analyte Analyte Ana1yte Analyte Anal& pc Analyte Analyte Analyte Analvte Anal& Analyte Analyte QC Analyee Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte Qc Analyte Analyte Analyte Analyte Analyte Ana1yte *n=.lYte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Ana1yte QC Analyte Analyte Anal& Analyte Standard Standard Standard Standard Standard Standard Standard Standard standard Standard Standard Analyte Analyte Std COnc 2.50 5.00 10.00 25.00 40.00 50.10 75.10 100.20 250.40 500.90 1001.70 250.40 250.40 250.40 2.50 5.00 10.00 25.00 40.00 1001.70 RT 7.091 7.093 7.103 7.093 7.092 7.093 7.093 7.078 7.080 1.094 1.091 7.094 7.102 1.093 7.092 7.018 ~~ 7.091 7.088 7.078 1.104 7.092 7.091 7.094 7.104 1.104 7.103 1.103 7.103 7.094 7.106 7.105 7.105 7.093 7.103 1.102 7.092 1.092 7.094 7.092 1.104 7.102 7.093 7.096 7.102 7.105 7.106 7.102 7.096 7.095 7.105 7.105 Area 419 621 1098 2371 3561 4481 5972 1587 14431 21888 33270 188 44 44 8077 6920 5280 14240 55 42 14422 1672 8831 8354 15956 14525 59 30 15297 15841 15684 20930 7184 14302 63 44 5740 6651 20690 7617 7312 15005 186 63 8406 Dub %E0v Flags Mod Co 0.00 -100 bbX 0.00 -100 bbX 0.00 -100 bbX 12.50 -50 bb 34.53 -14 bb 49.25 -2 bb 82.10 9 bb 112.16 12 bb 264.22 6 bb 181.43 -3 bb bbI 0.00 bb 0.00 bb 0.00 bb 144.29 bb 98.63 bb 68.87 bb 282.98 13 bb 0.00 bb 0.00 bb 250.89 bb 0.00 bb 155.70 bb 140.92 bb 351.48 bb 278.15 11 bb 0.00 bb 0.00 bb 311.10 bb 318.56 bb 326.30 515.02 bb 113.88 bb 266.08 6 bb 0.00 bb 0.00 bb 88.39 bb 92.13 bb 431.51 bb 126.40 bb 113.16 bb 273.98 9 bb 0.00 bb 0.00 bb 136.92 bb 113 91 23164 7812 6696 10698 212dO 15733 77 36 8898 9049 9463 11151 17176 16211 71 39 16614 11931 23217 16363 87 61 141 98 410 646 1176 2556 4700 6619 8118 15885 24335 36145 225 130 0.00 bb 0.00 bb 525.54 bb 119.29 bb 99.92 bb 166.04 bb d38.97 bb 276.31 10 bb 0.00 bb 0.00 bb 140.62 bb 136.17 bb 152.02 bb 313.61 bb 330.98 bb 273.69 9 bb 0.00 bb 0.00 bb 321.53 bb 346.78 bb 518.38 bb 279.58 12 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 -100 bbX 0.00 -100 bbX 0.00 -100 bbX 12.38 -50 bb 47.40 85.13 114.14 265.03 492.46 0.00 0.00 -5 bb 13 bb 14 bb 6 bb -2 bb bbI bb bb SOUP 020199: wantirated an4 Printed by CMC on 1 2 ~ 1 1 1 0 0 3M Environmental Laboratory a % C 1.3 / ( I /vc7 Page 530 of 703 BACK TO MAIN 0 NmlO study no samplelist Text 179 ~001207-179 E00-1311 MeOH Blank, TN-A--4715, Aliq. 11/16/00 TYVE Malyte Std COnc RT 7.105 Area 211 ppb ZIMV P I W S Mod Co 0.00 bb 3M Environmental Laboratory C1A1/7C i2AI /od Page 531 of 703 BACK TO MAIN p u m t i r y compound svnnary R a m r t 600-1311 PI08 Adsorblwnrorb 9-1s List: C:\Masslynw\s0up020199.pr0\~~l~DB\0001207 Last modified: l@n w c 11 09:05:24 2000 Method: C:\I*assl~\soup020199.pro\MathD8\sO0l207 Last modified:, m n Dec 11 09:10:27 1000 Job Code : C-und 2: T W F O S l427>80), fvnc 2 study no S-lmliat Text E00-1311 XeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 1001.7 ppb PFOS 00002-86-13, aliq. 11-27-00 MLA EOO-1311 1001.7 ppb PFOS 00002-86-13, aliq. 11-27-00 MLA E00-1311 YeOH Blank. TN-A-4715. Alia. 11/16/00 5 s001207I005 E00-1311 .*=OH Blank:.TN-A-4715. Alii. 11/16/00 6 ~001207-006 E00-1311 I ppb PFOS 00002-86-01, Aliq. 11-27-00 MLA 7 ~001207-007 E00-1311 1.5 ppb PFOS 00002-86-02. Aliq. 11-27-00 MLA 8 ~001207-008 E00-1311 '5.00ppb PFOS 00002-86-03. Aliq. 11-27-00 MLA 9 ~001207-009 E00-1311 10.0 ppb PFOS 00002-86-04, Aliq. 11-27-00 MLA 10 ~ 0 0 1 2 0 7 ~ 0 1 0E00-1311 .25.0 ppb PFOS 00002-86-05, Aliq. 11-27-00 MLA 11 ~001207-011 EOO-1311 ,10.0 ppb PFOS 00002-86-06. Aliq. 11-27-00 MLA 12 ~001207-012 E00-1311 '50.1 ppb PFOS 00002-86-07 Aliq. 11-27-00 MLA 13 4001207-013 E00-1311 ' 1 5 . 1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA 14 sOO1207-014 E00-1311 100.2 ppb PFOS 00002-86-09, Aliq. 11-27-00 MLA 15 ~001207-015 E00-1311 :!50.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 16 ~001207-016 E00-1311 !i00.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA 17 ~001207-017 E00-1311 :.001.7 ppb PFOS 00002-86-13, aliq. 11-27-00 MLA 18 SOO1207-018 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 19 ~001207-019 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 20 SOO1207-020 E00-1311 lIeOH Blank, TN-A-4715. Aliq. 11/16/00 21 ~001207-021 E00-1311 0 ppb PFOS 00002-86-01, Aliq. 11-27-00 MLA 22 ~001207-022 E00-1311 :!.5 ppb PFOS 00002-86-02. Aliq. 11-27-00 MLA 23 ~001207-023 EOO-1311 !,.OO ppb PFOS 00002-86-03. Aliq. 11-27-00 MLA 24 ~001207-024 E00-1311 10.0 ppb PFOS 00002-86-04, Aliq. 11-27-00 MLA 25 ~001207-025 ~ 0 0 - 1 3 1 1>5.0 ppb PFOS 00002-86-05, Aliq. 11-27-00 MLA 26 ~ 0 0 1 2 0 7 ~ 0 2 6EOO-1311 40.0 ppb PFOS 00002-86-06, Aliq. 11-27-00 MLA 600-1311 10.1 ppb PFOS 00002-86-07 Aliq. 11-27-00 MLA E00-1311 15.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA E00-1311 100.2 ppb PFOS 00002-86-09, Aliq. 11-27-00 MLA E00-1311 250.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA E00-1311 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA E00-1311 1001.7 ppb PFOS 00002-86-13. aliq. 11-27-00 MLA 3 3 ~ 0 0 1 2 0 7 ~ 0 3 3E00-1311 KeOM Blank, TN-A-4715. Aliq. 11/16/00 34 ~001207-034 E00-1311 HeOH Blank, TN-A-4715, Aliq. 11/16/00 35 ~001207-035 EOO-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 36 6001207-036 E00-1311 lox EOO-l3ll-3001-S1. 0.0mglL. Ohr. NO soil, 12/07/00 37 ~001207-037 E00-1311 lox E00-13ll-3002-S1, O.Omg/L, Ohr, NO soil, 12/07/00 3 8 SOO1207-038 EO0-1311 lox E00-1311-3003-S1, O.Omg/L. Ohr, No sail. 12/07/00 39 ~001207-039 E00-1311 lox E00-1311-3003ms-S1 O.Omg/L, Ohr. NO soil, 12/07/00 40 ~ 0 0 1 2 0 7 ~ 0 4 0E00-1311 lox E00-1311-3004-SI 0.5mglL. Ohr. No soil, 12/07/00 41 ~001207-041 E00-1311 250.4 xmb PFOS 00002-86-10. Alia. 11-27-00 MLA 42 5001207-042 E00-1311 MeOH Biink, TN-A-4715. Alia. llj16/00 43 ~001207-043 E00-1311 MeOH Blank, TN-A-4715. Alii. 11/16/00 44 SOO1207-044 E00-1311 lox E00-1311-3005-S1, 0.5mglL. Ohr. NO soil, 12/07/00 4 5 SOO1207-045 EOO-1311 lox EOO-l311-3006-S1, 0.5mgIL. Ohr. NO soil, 12/07/00 46 ~001207-046 E00-1311 lox E00-1311-3006ms-S1.0.5molL. Ohr. NO soil. 12/07/00 ~~ 47 r001207-047 E00-1311 lox E00-1311-3013-SI, O.OmgjL,'Ohr, 1:lclay. 12/07/00 48 ~001207-048 E00-1311 lox EO0-1311-3014-S1, O.Omg/L, Ohr. 1:lelay. 12/07/00 49 sOO1207-049 E00-1311 250.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 50 sOO1207-050 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 51 sOO1207-051 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 52 ~001207-052 E00-1311 10x E00-1311-3015-S1, O.Omg/L, Ohr. 1:lclay. 12/07/00 53 9001207-053 E00-1311 13x E00-1311-3015ms-S1,0.Omg/L. Ohr, 1:lclay. 12/07/00 54 ~001207-054 800-1311 llx E00-1311-3016-SI. O.Omg/L. Ohr, 1:Sclay. 12/07/00 55 ~001207-055 E00-1311 13x E00-1311-3017-S1, 0.OmglL. Ohr. 1:Sclay. 12/07/00 56 ~001207-056 E00-1311 1 . 1 ~E00-1311-3018-S1, 0.0mglL. Ohr. 1:5clav, 12/07/00 57 9001207_057 58 s001207~058 59 S001207-059 60 ~001207~060 61 ~001207-061 62 ~001207-062 ~. ~~ ~ ~ 63 ~001207-063 E00-1311 IIlx E O 0 - 1 3 1 1 - 3 0 2 l s 1. ~ b . O - m i L ~ ' O h r . ' ll25il.G. ~ _ . 12/07/00 E00-1311 lox E00-1311-3021ms-Sl,O.Omq/L,Ohr. 1:25clay, 12/07/00 800-1311 2!50.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 ~~. EO0-1311 lllx E00-1311-3031-S1,0.5mg/L, Ohr, 1:lclay. 12/07/00 69 ~001207-069 E00-1311 lox E00-1311-3032-S1,0.5mg/L, Ohr. 1:lclay. 12/07/00 70 5001207~070 E00-1311 lllx E00-1311-3033-Sll 0.5mg/L. Ohr, 1:lclay. 12/07/00 E00-1311 lllx E00-1311-3033ms-S1,0.5mg/L, Ohr. 1:lclay. 12/07/00 E00-1311 LClx E00-1311-3034-S1,0.5mgll.0hr, 1:Sclay. 12/07/00 E00-1311 250.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA EOO-1311 m!OH Blank. TN-A-4715, Aliq. 11/16/00 75 ~001207- E00-1311 &!OH Blank, TN-A-4715, Aliq. 11/16/00 76 S001207_076 E00-1311 l(lx E 0 0 - 1 3 1 1 - 3 0 3 5 - S 1 , 0 . 5 m g l L . O h r . 1:Sclay. 12/07/00 77 so0120 BOO-1311 l ( l x E00-1311-3036-Sl. 0.5mgIL. Ohr. 1:Sclay. 12/07/00 EOO-1311 l l l x E00-1311-3036ms-S1,0.Smg/L,Ohr, 1:Sclay. 12/07/00 E00-1311 l[lx E00-1311-3037-S1,0.5mg/L,Ohr, 1:25clay. 12/07/00 ~~. E00-1311 1.Cix E 0 0 - 1 3 1 1 - 3 0 3 8 - S 1 , 0 . 5 ~ / L , O h ~1,:25clay, 12/07/00 81 so0120 E00-1311 >50.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 82 ~ 0 0 1 2 0 7 ~ 0 8 2EO 0-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 8 3 t001207.083 E00-1311 MeOH Blank. TN-A-4715. Aliq. 11/16/00 E00-1311 I C x E00-1311-3039-S1,0.5mq/L,Ohr, 1:25clay, 12/07/00 E00-1311 1Cx E00-1311-3039-S1,0.5mg/L.Ohr. 1:25clay, 12/07/00 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 . ... E00-1311 McOH Blank. TN-A-4715, Aliq. 11/16/00 88 EOC E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 89 so1 E00-1311 0 ppb PFOS 00002-86-01, Aliq. 11-27-00 M L A TYD. Analyte Analyte Analyte Ana1yte Ana1yte Analyte Analyte Analyte Ana1yte Analyte Analyte Analyte Analyte Ana1yte Analyte Analyte Analyte Analyte Blank Blank Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Blank Blank Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte AnLna1yte Q Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC lVla1yte Analyte Analyte Ana1yte Analyte Ana1yte Analyte Qc Analyte Analyte Analyte Analyte Analyte AnalYte Ana& QC Analyte Analyte Analvte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Blank Blank Analyte Std Conc RT 6.889 6.899 6.900 6.900 6.902 6.914 6.903 6.904 6.900 6.898 6.900 6.903 6.900 6.901 248.60 248.60 6.900 6.901 6.901 6.901 6.900 6.902 6.901 6.901 6.903 6.902 6.912 6.899 248.60 6.909 6.912 6.913 6.915 6.912 6.913 248.60 6.914 6.917 6.907 6.913 6.914 6.907 248.60 6.914 6.915 6.924 6.913 6.914 6.912 248.60 6.925 6.913 6.912 6.914 6.926 6.913 248.60 6.914 6.910 6..~915 6.924 6.924 6.913 248.60 6.924 6.913 6.914 6.913 6.925 6.909 6.913 6.911 6.910 Area 2889 2593 DDb 339.35 304.55 37 bb 23 bb 3189 3064 3125 2657 2457 2712 2629 2467 2426 2401 2405 2355 374.53 359.92 367.01 312.11 288.56 318.54 308.79 289.75 284.94 282.02 282.49 276.59 51 bb 4 5 bb 48 ~ b~b - 26 bb 16 bb 28 bb 2 4 bb 17 bb 15 bb 13 bb 14 bb 11 bb 2386 2381 2451 2505 2411 2439 2467 2342 2328 2440 2397 2508 280.31 279.61 287.92 294.22 283.20 286.50 289.78 275.04 273.39 286.55 281.50 294.56 13 bb 12 bb 16 bb 18 bb 14 bb 15 bb 17 bb 11 bb 10 bb 15 bb 13 bb 18 bb 2239 2102 2149 1819 2059 1777 263.04 246.94 252.47 213.65 241.83 208.69 5 bb -1 bb 1 bb -15 bb - 3 bb -16 bb 1163 1560 1495 1851 1458 1636 136.65 183.26 175.58 217.42 171.19 192.17 -45 bb -27 bb - 3 0 bb -13 bb -32 bb -23 bb 1766 1570 1644 1719 1666 1762 207.41 184.45 193.06 201.96 195.68 2 0 6 93 -17 bb -26 bb -23 bb -19 bb -22 bb -17 bb 2804 1774 1570 1798 1733 1819 329.34 208.40 184.44 211.13 203.52 213.68 32 bb -17 bb -26 bb -16 bb -19 bb -14 bb 1756 1776 2006 1714 1832 1955 206.31 208.60 235.65 201.34 215.21 229.64 -17 bb -17 bb -6 bb -19 bb -14 bb -8 bb 1763 1742 1795 1825 1950 1918 207.11 204.64 210.87 214.36 228.99 225.26 -17 bb -18 bb -16 bb -14 bb -8 bb -9 bb 1808 1816 212.34 -15 bb 213.36 -15 bb 1949 228.98 -8 bb SOUP 020199: quantitated and printed by CMC On 12111100 3M Environmenfal Laboratory Page 532 of 703 BACK TO MAIN Quantify c-und B v m ~ a r yR e p r t E00-1311 Pros Adsorb/Daso:cb 8-1a List: C:\uai.slyn;~\soup020199.pro\Sam~leDB\r001207 Last Irodified: mn Dec 11 09:05:24 2000 Method: C:\ua8~1yr~~\~~~p020199.pr0\~thDB\~001207 Last mdified: mn Dec 11 09:10:27 2000 Job Code: Prinped: Elon De0 11 09:23:38 2000 Ccoqpovnd 1 : TXP1W S l427>801, tunc 2 x N- study M S w l a l i s t Text 90 ~001207-090 E00-1311 2.5 ppb PfOS 00002-86-02. Aliq. 11-27-00 MLA 91 ~ 0 0 1 2 0 7 ~ 0 9 1E00-1311 5.00 ppb PFOS 00002-86-03. Aliq. 11-27-00 MLA EOO-1311 10.0 ppb PfOS 00002-86-04, Aliq. 11-27-00 MLA E00-1311 25.0 ppb PfOS 00002-86-05, Aliq. 11-27-00 MLA E00-1311 40.0 ppb PFOS 00002-86-06. Aliq. 11-27-00 MLA EOO-1311 50.1 ppb PFOS 00002-86-07 Aliq. 11-27-00 MLA E00-1311 75.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA ~ ~~ E00-1311 100.2 ppb PfOS 00002-86-09, Aliq. 11-27-00 MLA 98 ~001207-098 E00-1311 250.4 ppb PfOS 00002-86-10, Aliq. 11-27-00 MLA 99 90012071099 E00-1311 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA 100 ~001207-100 E00-1311 1Op1.7 ppb PFOS 00002-86-13. aliq. 11-27-00 MLA 101 ~001207-101 EOO-1311 MeCH Blank. TN-A-4715. Aliq. 11/16/00 102 s00:207-102 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 103 so01207 103 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 104 ~ 0 0 1 2 0 7 ~ 1 0 4E00-1311 lox E00-1311-3040-S1,0.5mg/L.2hr. 1:lclay. 12/07/00 105 ~001207-105 E00-1311 lox E00-1311-3041-S1.0.5rm/L.2hr, 1:lclay. 12/07/00 106 ~ 0 0 1 2 0 7 ~ 1 0 6E00-1311 lox E00-l311-3042-Sl,O.5mg/L,2hr. 1:lclay. 12/07/00 107 ~001207-107 E00-1311 250.4 ppb PfOS 00002-86-10, Aliq. 11-27-00 MU. 108 ~001207-108 E00-1311 MeOH Blank, TN-A-4715. Aliq. 11/16/00 109 ~001207-109 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 110 ~ 0 0 1 2 0 7 ~ 1 1 0E00-1311 lox E00-1311-3042ms-S1,0.5mg/L,2hr, 1:lclay. 12/07/00 111 ~ 0 0 1 2 0 7 ~ 1 1 1E00-1311 lox E00-1311-3043-S1,0.5mg/L.Zhr, l:5clay. 12/07/00 112 ~001207-112 E00-1311 lox E00-1311-3044-S1,0.5mg/L,2hr. 1:5cIay, 12/07/00 113 ~001207-113 EOO-1311 lox E00-1311-3045-S1,0.5mg/L,2hr. 1:Sclay. 12/07/00 114 ~001207-114 E00-1311 lox E00-1311-3045ms-S1,0.5mg/L,2hr. 1:Sclay. 12/07/00 115 ~001207-115 116 ~001207-116 117 ~001207-117 118 ~001207-118 E00-1311 2 5 0 . 4 ppb PfOS 00002-86-10, Aliq. 11-27-00 MLA E00-1311 YeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 ,YeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 lox E00-1311-3046-Sl 0.5mg/L.2hr, 1:25clay. 12/07/00 119 ~001207-119 E00-1311 lox E00-1311-3047-S1 0.5mglL.2hr. 1:25clay. 12/07/00 120 ~001207-120 E00-1311 LOX EOO-1311-3048-51 0.5mglL.2hr. 1:25clay, 12/07/00 121 ~001207-121 E00-1311 LOX E00-l311-3048ms-S1,0.5~/L,2hr.1:25clay. 12/07/00 122 ~001207-122 EOO-1311 LOX E00-1311-3049-S1,0.5mg/L.4hr, 1:lclay. 12/07/00 123 ~001207-123 E00-1311 :250.4 ppb PfOS 00002-86-10, Aliq. 11-27-00 MLA 124 ~001207-124 E00-1311 I4eOH Blank, TN-A-4715, Aliq. 11/16/00 125 ~001207-125 EOO-1311 l4eoH Blank. TN-A-4715. Aliq. 11/16/00 126 ~001207-126 E00-1311 LOX E00-1311-3050-S1,0.5rng/L,4h~, 1:lclay. 12/07/00 127 ~001207-127 E00-1311 .LOX E00-1311-3051-S1,0,5rng/L,4hr. 1:lclay. 12/07/00 128 ~001207-128 E00-1311 :LOX E00-1311-3051ms-S1,0.5mg/L.4hr, 1:lclay. 12/07/00 129 9001207-129 EOO-1311 ..Ox E00-1311-3052-S1,0.5mg/L,4hr, 1:5clay, 12/07/00 130 ~001207-130 100-1311 :.Ox E00-1311-3053-S1,0.5mg/L.4hr. 1:Sclay. 12/07/00 131 ~ 0 0 1 1 0 7 ~ 1 3 1E00-1311 2!50.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA 132 so01207 132 E00-1311 BIeOH Blank. TN-A-4715, Aliq. 11/16/00 E00-1311 UeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 ].Ox E 0 0 - 1 3 1 1 - 3 0 5 4 - S 1 , 0 , 5 m g / L . P h r . 1:Sclay. 12/07/00 E00-1311 lox E00-1311-3054ms-S1,0.5ng/L.4hr, 1:5clay. 12/07/00 E00-1311 1Ox E00-1311-3055-S1,0.5~/L,4hr, 1:25clay. 12/07/00 E00-1311 l o x E00-1311-3056-S1,0.5mg/L,4hr. 1:25clay, 12/07/00 E00-1311 lox E00-13ll-3057-S1,0.5mg/L,4hr, 1:25clay, 12/07/00 139 ~ 0 0 1 2 0 7 ~ 1 3 9E00-1311 2 5 0 . 4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 140 s001207I140 141 9001207-141 142 ~001207-142 143 9001207-143 E00-1311 MeOH Bihnk, TN-A-4715, Aliq. lli16/00 E00-1311 l!eOH Blank, TI-A-4715, Aliq. 11/16/00 E00-1311 lox E00-1311-3057~-S1,0.5mglL.4hr. 1:25clay. 12/07/00 EOO-1311 lox E00-1311-3067-S1,0.5mg/L,16hr, 1:lclay. 12/07/00 144 ~001207-144 E00-1311 lox E00-1311-3068-S1,0.5mg/L,16hr. 1:lclay. 12/07/00 145 ~001207-145 E00-1311 lox E 0 0 - 1 3 1 1 - 3 0 6 9 - S 1 , 0 . 5 m g l l . l 6 h r . 1:lclay. 12/07/00 146 ~001207-146 E00-1311 lox E00-1311-3069rns-S1,0.5mg/L.16hr, 1:lclay. 12/07/00 1 4 7 ~001207-147 E O O - l 3 l l 2 5 0 . 4 ppb Pros 0 0 0 0 2 - 8 6 - 1 0 , Aliq. 11-27-00 M L I 148 ~001207-148 E00-1311 MeOH Blank. TN-A-4715, Aliq. 11/16/00 149 ~ 0 0 1 2 0 7 ~ 1 4 9E00-1311 MeOH Blank. TN-A-4715. Alia. 11/16/00 150 ~0012071150 E00-1311 lox EOO-l311-307O-S1.0.5rng;L. 16hr. l:5clay. 12/07/00 151 ~ 0 0 1 2 0 7 ~ 1 5 1E00-1311 lox E00-1311-3071-S1,0.5mg/L,16hr, 1:5clay, 12/07/00 152 ~001207-152 E00-1311 lox E00-1311-3072-S1,0,5rng/L,16hr. 1:Sclay. 12/07/00 153 ~001207-153 E00-1311 lox E00-1311-3072ms-S1,0.5mg/L.16hr. l:5clay. 12/07/00 154 so01207 154 E00-1311 lox E00-1311-3073-S1.0.5~/L.l6hr. 1:25clav. 12/07/00 155 s001207I155 156 s001207L156 157 sOOl207I157 158 ~001207-158 E00-1311 250.4 ppb PFOS 00002-86-1;. Aliq.'ll-27-00'MLA E00-1311 MeOH Blank. TN-A-4715, Alia. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Alii. 11/16/00 E00-1311 lox E00-1311-3074-S1.0.5mg16.16hr, 1:25clay. 12/07/00 159 ~001207-159 E00-1311 lox E00-1311-3075-Sl.0.5~/L,16hr. 1:25clay, 12/07/00 160 ~001207-160 E00-1311 lox E00-1311-3075ms-S1,0.5mg/L,16hr,l:25clay, 12/07/00 161 so01207 161 E00-1311 250.4 Dub PfOS 00002-86-10. Alia. 11-27-00 MLA 162 ~ 0 0 1 2 0 7 ~ 1 6 2Eoo-1311 M ~ O HBiHnk. TN-A-4715. Alib. llil6/00 163 s001207I163 EOO-1311 MeOH Blank. TN-A-4715, Alii. 11/16/00 164 ~001207-164 E00-1311 MeOH Blank. TN-A-4715. Alii. 11/16/00 165 ~ 0 0 1 2 0 7 ~ 1 6 5E00-1311 0 ppb PfOS 00002-86-01. Aliq. 11-27-00 MLA 166 ~ 0 0 1 2 0 7 ~ 1 6 6~ 0 0 - 1 3 1 12.5 ppb PfOS 00002-86-02, Aliq. 11-27-00 MLA 167 so01207 167 E00-1311 5 . 0 0 oob PFOS 00002-86-03. A110. 11-27-00 MLA 168 s001207I168 E00-;311 13.0 bbb PFOS 00002-86-04: Alii. li-27-00 MLA 169 ~0012071169 170 ~001207-170 171 ~001207-171 172 ~001207-172 173 ~001207-173 174 ~001207-174 175 ~001207-175 176 ~001207-176 177 ~001207-177 178 ~001207-178 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 E00-1311 25.0 PPb PfOS 00002-86-05. Alii. 11-27-00 MLA 481.0 ppb PFOS 00002-86-06. Aliq. 11-27-00 MLA 511.1 ppb PfOS 00002-86-07 Aliq. 11-27-00 MLA 7'5.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA 1110.2 ppb PfOS 00002-86-09. Aliq. 11-27-00 MLA 2'50.4 ppb PFOS 00002-86-10. Aliq. 11-27-00 MLA 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA LO01.7 ppb PfOS 00002-86-13. aliq. 11-27-00 MLA MBOH Blank. TN-A-4715, Aliq. 11/16/00 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Tnm Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Blank Blank Analyte Analyte Ana1;te Qc Analyte Analyte Analyte Analvte Analit. Analyte Analyte Qc Ana1yte Analyte Ana1yte Analyte Analyte Analyte Ana1yte QC Analyte Analyte Analvte Anal& AnLna1yte Analyte Analyte QC Ana1vte Analyte Analyte Analyte Ana1yte Analyte Analyte OC Analyte Analyte Analyte Analyte Analyte Analyte Analyfe Qc Analyte Analvte Anal& Analyte Analyte Analyte Analvte Qc Analvte Ana1;te Analyte Analyte Analyte OC Analvte Analhe Anal& Analyte Standard Standard Standard Standard Standard Standard Standard standard Standard Standard Standard Analyte Analyte Std Conc 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 RT 6.899 6.901 6.911 6.901 6.901 6.914 6.901 6.899 6.901 6.902 6.900 6.912 6.898 6.902 6.899 6.901 6.899 6.912 6.897 6.901 6.902 6.900 6.901 6.913 6.899 6.901 6.900 6.901 6.914 6.924 6.923 6.924 6.915 6.928 6.913 6.912 6.912 6.915 6.914 6.912 6.913 6.913 6.923 6.914 6.913 6~ .9.1.1 ~ 6.913 6.912 6.912 6.914 6.913 6.917 6.910 6.925 6.915 6.922 6.917 6.915 6.911 6.915 6.916 6.912 6.915 Aroa 1909 1930 1903 1875 1879 1941 1858 1889 1871 1822 1904 ppb %De" ?lags m d Co _ _ 224.21 -10 bb 2~~ 26.76. -9. hh 223.57 -10 bb 220.27 -11 bb 220.74 -I1 bb 227.93 -8 bb 218.26 -12 bb 221.85 -11 bb 219.71 -12 bb 214.03 -14 bb 223.61 -10 bb 1675 1902 1861 1751 196.76 223.44 218.60 205.65 -21 bb -11 bb -13 bb -17 bb 1955 2301 1728 1764 1677 1807 229.66 270.21 203.02 207.18 196.93 212.19 -8 bb 8 bb -19 bb -17 bb -21 bb -15 bb 1735 1792 1742 1683 1778 1843 203.84 210.44 204.56 197.65 208.90 216.49 -18 bb -16 bb -18 bb -21 bb -16 bb -13 bb 1706 1921 1875 1745 1819 1891 27 1814 1825 1846 1872 1929 ~~ 1943 200.35 225.66 220.25 204.99 213.63 222.11 3.18 213.05 214.36 216.79 219.93 2.2~6.~ 5.7 228.17 -20 bb -10 bb -12 bb -18 bb -15 bb -11 bb bb -15 bb -14 bb -13 bb -12 bb - 9~ bb ~~ -8 bb 1838 1869 1824 1993 1902 1970 215.90 219.50 214.19 234.12 223.44 a31.38 -14 bb -12 bb -14 bb -6 bb -11 hb -7 bh 1882 221.02 -12 bb 1961 230.30 -8 bb 1886 221.54 -11 bb 1723 202.41 -19 bb 1~ 887. .7.21~ .6.6. _ -~ 11 h_h_. 2045 240.24 -3 bb 1865 1903 1859 2030 219.09 223.51 218.32 238.49 -12 bb -11 bb -13 bb -4 bb 1997 2000 2051 2097 2028 2041 2082 2008 1995 2053 2004 2037 234.52 234.91 240.91 246.28 238.15 239.78 244.53 235.89 234.34 241.18 235.37 239.26 -6 bb -6 bb -3 bb -1 bb -4 bb -4 bb -2 bb -5 bb -6 bb -3 bb -5 bb -4 bb SOUP 020199: wantitared anU printed by CMC on 12/11/00 3M Environmental Laboratory Page 533 of 703 BACK TO MAIN QUu.nti.fY COmWUnd 6-ry RaEart E00-1311 ?PO8 AdsOrblDIIsoz'b 0 Name study no S - l a l i s t T a t 179 so01207279 E00-1311 MeOH Blank. TN-A-4715. A l i q . 11/16/00 TylM Analyte S t d conc DDb LWv Flags Hod Co SOUP 020199: quantitated and printed by CHC on 12/11/00 3M Environmental Laboratory BACK TO MAIN Pruntrfy Coolpound Suwmary I w o r t PFOS Adsorb/Desorb Study LWMS Ins-t: Tucker (uL052) S v ~ p l oIlst: C:\MRSSLYNX\Deoatur.PaO\SampleOB\t00l215 Last ao&fxsd: Uon D.a 1 8 L0:45:28 2000 Metbd: C:\MRSSLYNX\Dscatur.PRO~thDB\001215 last rodxfledd: Mon Do0 1 8 L0:SO:Ol 2000 Job Coda: Printed: Mon Do0 1 8 :L0:56:20 2000 Compound 1: PFOS(499) I N.a-1 t001215-001 2 t001215-002 3 t001215-003 4 to01215 004 5 t0012151005 6 t001215-006 7 t001215~007 8 tO01215-008 9 t001215-009 10 t001215 010 11 t0012151011 12 tOO1215-012 13 t001215-013 14 t001215-014 15 t001215-015 16 t001215-016 17 t001215-017 18 t001215-018 19 t001215-019 20 t001215-020 21 t001215-021 22 t001215-022 23 t001215-023 24 t001215-024 25 t001215-025 26 t001215-026 21 to01215 027 33 t0012151033 34 t001215-034 35 t0O0O1l221155-003355 36 t001215-036 37 t001215-037 38 t001215-038 39 t001215-039 40 t001215-040 41 t001215-I0O41 42 tOO1215-042 43 to01215 043 44 t001215I044 45 t001215-045 46 t001215-046 47 t001215-047 48 t001215-048 49 t001215-049 50 t001215-050 51 t001215-051 52 t001215-052 53 t001215-053 54 t001215-054 55 t001215 055 56 t0012151056 57 t001215 057 58 t0012151058 59 t001215-059 60 t001215-060 61 t001215-061 62 t001215-062 63 to01215 063 64 t0012151064 65 t001215-065 66 to01215 066 61 t001215I067 68 t001215-068 69 t001215-069 70 t001215-070 71 to01215 071 72 t001215I072 73 to01215 073 74 t001215I074 75 t001215-075 76 t001215-076 77 t001215-077 78 to01215 078 79 t0012151079 80 t001215-080 81 tO01215-081 82 t001215-082 S a q l d r r t Text MeOH Blank, TN-A-4740. Aliq. 12/04/00 M C MeOH Blank, TN-A-4740, Aliq. 12/04/00 M C 1001.7 ppb PFOS 00002-86-13 1001.7 ppb PFOS 00002-86-13 MeOH Blenk, TN-A-4740, Aliq. 12/04/00 M C MeOH Blank, TN-A-4730. Aliq. 12/04/00 CMC MeOH Blank, TN-A-4740, Aliq. 12/04/00 M C 0 ppb PI'OS 00002-86-01 2 . 5 ppb PFOS 00002-86-02 5 ppb PI'OS 00002-86-03 10 ppb PFOS 00002-86-04 25 ppb PFOS 00002-86-05 40 ppb PFOS 00002-86-06 50.1 ppb PFOS 00002-86-01 15.1 pph PFOS 00002-86-08 100.2 ppb PFOS 00002-86-09 250.4 ppb PFOS 00003-141 500.9 ppb PFOS 00002-86-12 1001.7 Fipb PFOS 00002-86-13 HeOH Blank, TN-A-4740. Aliq. 12/04/00 M C MeOH Blank, TN-A-4740, Aliq. 12/04/00 M C MeOH Blank, TN-A-4740. Aliq. 12/04/00 CMC 0 ppb PFOS 00002-86-01 2.5 ppb PFOS 00002-06-02 5 ppb PFOS 00002-86-03 10 ppb PFOS 00002-86-04 25 ppb PFOS 00002-86-05 40 ppb PFOS 00002-06-06 50.1 ppt PFOS 00002-86-07 15.1 ppt PFOS 00002-86-08 100.2 ppb PFOS 00002-86-09 250.4 ppb PFOS 00003-141 500.9 ppb PFOS 00002-86-12 1001.7 ppb PFOS 00002-86-13 MeOH Blank, TN-A-4740, Aliq. 12/04/00 CMC MeOH Blank, TN-A-4740. Aliq. 12/04/00 M C lox E00-1311-3007 lox E00-1311-3008 lox E00-1311-3009 lox 600-1311-3009ms lox EOO-1311-3010 ~. 250.4 ppb PFOS 00003-141 MeOH Blank. TN-A-4740.. Alio. 12/04/00 M C MeOH Blank; TN-A-4740, Aliq. 12/04/00 M C lox 600-1311-3011 lox EOO-1311-3012 lox 600-1311-3012m lox 600-1311-3130 lox 600-1311-3131 250.4 ppb PFOS 00003-141 MeOH Blank, TN-A-4740, Aliq. 12/04/00 M C MeOH Blank, TN-A-4740, Aliq. 12/04/00 M C lox 600-1311-3132 lox BOO-1311-3132m lox E00-1311-3133 10x 600-1311-3134 lox 600-1311-3135 250.4 ppb PFOS 00003-141 MeOH Blank, TN-A-4740. Aliq. 12/04/00 M C MeOH Blank, TN-A-4740. Aliq. 12/04/00 M C lox E00-1311-3135mr lox E00-1311-3136 lox 600-1311-3137 lox E00-1311-3138 lox E00-1311-3138ms 250.1 ppb PFOS 00003-141 MeOH Blank, TN-A-4740, Aliq. 12/04/00 QIC MeOH Blank, TN-A-4140, Aliq. 12/04/00 CMC lox E00-1311-3139 lox EOO-13114140 lox 600-1311-3141 lox 600-1311-3141ms lox E00-1311-3142 250.4 pp3 PFOS 00003-141 MeOH Blank, TN-A-4740, Aliq. 12/04/00 CMC MeOH Blank, TN-A-4140, Aliq. 12/04/00 M C lox 600-1311-3143 lox 600-1311-3144 101 BOO-1311-3144m lox E00-1311-3145 lox 600-1311-3146 250.4 ppb PFOS 00003-141 RT 6.481 6.371 6.488 6.489 6.433 6.408 6.417 6.425 6.445 6.371 6.496 6.484 6.411 6.481 6.445 6.200 6.188 6.184 6.223 6.172 6.228 6.240 6.493 6.360 6.438 6.492 6.485 6.356 6.476 6.485 6.488 6.489 6.489 6.384 6.293 6.288 6.456 6.469 6.429 6.483 6.450 6.469 6.357 6.242 6.204 6.469 6.400 6.481 6.411 6.488 6.443 6.237 6.101 6.292 6.260 6.406 6.485 6.476 6.445 6.245 6.420 6.431 6.361 6.485 6.429 6.484 6.453 6.360 6.315 6.240 6.207 6.256 6.272 6.473 6.423 6.268 6.489 6.478 6.480 6.478 6.488 6.484 Area 53206 30800 4641528 4640503 36137 35552 35344 39095 61396 77059 119454 208147 296693 386893 542145 739832 1625157 2627391 4126845 31200 28732 25271 32948 49820 64675 101190 203395 284054 345882 518826 638622 1490467 2357038 3944487 24270 23252 30587 27518 25569 1007052 26288 1311544 28127 25682 21374 25538 998865 587042 571685 1447645 21552 25476 492412 1536932 2205944 1406285 1523976 1529689 29026 26218 2204358 1996143 1996672 1935361 2548079 1536839 28963 28028 422345 583342 374356 1431728 1543781 1488024 28021 25280 1494614 1597102 2263636 2021915 1986134 1569815 Rsspanre 0.000 0.000 10770.559 10872.952 0.000 0.000 0.000 99.457 159.598 200.633 371.309 786.844 1031.971 1312.849 1854.385 2414.604 5012.082 8168.561 15693.600 0.000 0.000 0.000 107.336 165.290 217.657 349.543 720.329 939.183 1179.832 1802.378 2183.075 5091.336 8220.976 13555.334 0.000 0.000 116.821 104.562 94.837 3914.570 101.042 5035.394 0.000 0.000 78.074 97.150 3638.345 2059.048 1956.716 5035.4 61 0.000 0.000 1849.585 4835.963 6828.949 4365.327 4958.838 4997.809 0.000 0.000 7547.557 5741.427 6032.791 6022.490 7906.309 4164.796 0.000 0.000 1448.580 1737.042 1095.122 4389.666 4605.736 4509.151 0.000 0.000 4578.029 4 918.225 7136.543 6235.222 5982.209 4638.272 PPm Flags 0.00 bb 0.00 bb 729.75 bb 740.43 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 7.68 bb 29.54 bb 42.60 bb 57.71 bb 87.31 bb 118.62 bb 274.40 bb 54.5.53 bb bbI 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bbX 0.00 bbX 6.54 bbX 26.02 bb 37.64 bb 50.53 bb 84.44 bb 105.59 bb 279.56 bb 501.26 bb 1123.76 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 209.90 bb 0.00 bb 275.97 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 189.67 bb 98.66 bb 92.97 bb 275.98 bb 0.00 bb 0.00 bb 8 7 . 0 4 bb 263.27 bb 396.95 bb 233.83 bb 271.08 bb 273.57 bb 0.00 bb 0.00 bb 449.46 bb 322.07 bb 341.64 bb 340.94 bb 416.11 bb 258.78 bb 0.00 bb 0.00 bb 65.07 bb 80.84 bb 45.98 bb 235.33 bb 248.78 bb 242.75 bb 0.00 bb 0.00 bb 247.05 bb 268.50 bb 419.10 bb 355.44 bb 338.22 bb 250.82 bb %Da, od C-t -27 -26 -100 -100 -23 18 6 15 16 18 10 9 -100 -100 -35 4 -6 1 12 5 12 0 12 10 10 9 3 -3 0 Ciuantitated and Printed by (Mc on 18 Dea 00, Study E00-1311 Page 1 3M Environmental Laboratory Page 535 of 703 BACK TO MAIN Quantify Campound Suanary rlcport PFOS Msorb/Desorb Study I(:/MS I n s t - t : Tucker (IA052) Sample L i s t : Last d f i e d : hthod: Last modified: Job Code: C:~SLYNX\.Dec~tur.m(D\SamplaDB\t001215 HDll Dec 1 8 1.0:&:28 2000 C:~SLY1M\.Dacatur.m(D~tMB\001215 HDll Dec 1 8 1.0:50:01 2000 Print*: Mon m a 18 10:56:20 2000 Compound 1: PFOS(499) # NaW 8 3 t001215-083 84 t001215-084 85 to01215 085 86 t0012151086 87 t001215-087 88 t001215-088 89 t001215-089 90 t001215 090 91 t0012151091 92 t001215-092 93 to01215 093 94 t0012151094 95 t001215-095 96 t001215-096 97 t001215-097 98 t001215-098 99 to01215 099 100 t001215~100 101 tO01215-101 102 to01215 102 107 t001215I107 108 t001215-108 109 t001215-109 110 t001215-110 111 t001215-111 112 t001215-112 113 t001215-113 114 t001215-114 115 t001215-115 116 t001215-116 117 t001215-117 118 t001215-118 119 t001215-119 120 t001215-120 121 t001215-121 122 t001215-122 123 t001215-123 124 t001215-124 125 t001215 125 130 t001215-130 137 t0012151137 138 t001215-138 139 t001215-139 140 t001215-140 141 t001215-141 142 to01215 142 143 t001215I143 I44 t001215-144 145 t001215-145 146 to01215 146 151 t0012151151 152 t001215-152 153 to01215 153 159 tO01215I159 160 t001215-160 161 to01215 161 162 t0012151162 163 c0012:5-163 164 t001215_164 Sanplslist Text MeOH Blank, TN-A-4740, Aliq. HeOH Blank, TN-A-4740. Aliq. lox 800-1311-3147 lox E00-1311-3147ms lox E00-1311-3148 lox 600-1311-3149 lox EOO-1311-3150 250.4 ppb PFOS 00003-141 MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740, Aliq. lox E00-1311-3150ms lox 600-1311-3151 lox EOO-1311-3152 lox 600-1311-3153 lox EOO-1311-3153250.4 ppb PFOS 00003-141 HeOH Blank, TN-A-4740, Aliq. HeOH Blank. TN-A-4740, Aliq. MeOH Blank, TN-A-4740, Aliq. 0 ppb PEDS 00002-86-01 2.5 ppb PFOS 00002-86-02 5 ppb PFOS 00002-86-03 10 ppb PFOS 00002-86-04 25 ppb PFOS 00002-86-05 40 ppb PFOS 00002-86-06 50.1 ppb PFOS 00002-86-07 75.1 ppb PFOS 00002-86-08 100.2 pp:o PFOS 00002-86-09 250.4 p p l ~PFOS 00003-141 500.9 ppl, PFOS 00002-86-12 1001.7 ppb PFOS 00002-86-13 HeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740, Aliq. lox EOO-L311-3154 101 EOO-1311-3155 1OX E00-1311-3156 lox EOO-.L311-3156m lox EOO-:L311-3157 250.4 ppb PFOS 00003-141 MeOH Blank, TN-A-4740, Aliq. MeOH Blank, TN-A-4740, Aliq. lox E00-:1311-3158 1OX 800-1311-3159 lox E00-:.311-3159ms 10x E00-311-3160 lox E00--!.311-3161 250.4 ppb PFOS 00003-141 MeOH Blank. TN-A-4740. Alia. HeOH Blank; TN-A-4740, Alii. lox E00-1.311-3162 10x E00-1311-3162m lox EOO-1311-3163 10s EOO-1311-3161 lox E00-1311-3165 250.4 pph PFOS 00003-141 MeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740, Aliq. lox E00--1311-3165nvl lox E00-1311-3166 lox EOO-1311-3167 lox EOO-1311-3168 101 EOO--l311-31681os 250.4 pph PFOS 00003-141 MeOH Blank, TN-A-4740. Aliq. HeOH Blank, TN-A-4740. Aliq. lox E00-1311-3169 lox E00--1311-3170 lox SOO-1311-3171 lox E00-1311-3171ms lox BOO-3311-3172 250.4 pph PFOS 00003-141 MeOH Blark, TN-A-4740. Aliq. MeOH Black, TN-A-4740, Aliq. lox 600-1311-3173 lox 600-1311-3174 10x E00-1311-3174es 250.4 ppt PFOS 00003-141 HeOH Blank, TN-A-4740. Aliq. MeOH Blank, TN-A-4740, Aliq. 101 E00-1311-3184 lox E00-1311-3185 lox 6'00-1311-3186 12/04/00 M C 12/04/00 CMC 12/04/00 M C 12/01/00 M C 12/04/00 M C 12/04/00 M C 12/04/00 CMC 12/04/00 M C 12/04/00 CMC 12/04/00 M C 12/04/00 M C 12/04/00 M C 12/04/00 CMC 12/04/00 mc 12/04/00 M C 12/04/00 CMC 12/04/00 M C 12/01/00 M C 12/04/00 CMC 12/01/00 CMC 12/04/00 CMC RT 6.457 6.313 6.460 6.444 6.367 6.460 6.477 6.476 6.461 6.444 6.416 6.200 6.180 6.193 6.224 6.248 6.240 6.184 6.228 6.280 6.240 6.432 6.441 6.434 6.481 6.461 6.484 6.461 6.416 6.480 6.399 6.461 6.428 6.416 6.328 6.472 6.477 6.480 6.408 6.361 6.333 6.381 6.456 6.369 6.429 6.432 6.453 6.352 6.336 6.240 6.314 6.467 6.127 6.363 6.328 6.413 6.369 6.393 6.413 6.484 6.464 6.448 6.393 6.264 6.332 6.484 6.232 6.328 6.486 6.463 6.418 6.441 6.408 6.359 6.376 6.482 6.472 6.473 6.212 6.235 6.192 6.180 Are. 27890 25986 2160923 2795560 467443 434046 307296 1592065 27504 26941 1372094 1471355 1462737 1400633 2166117 1624666 26765 29157 28941 27909 52247 65529 99480 199217 299906 351140 531280 725423 1529458 2508341 4217609 26339 24228 1932000 1931864 1823747 2606071 589623 1486525 23881 23843 515994 398660 1391674 1313759 1336481 1630600 25232 23839 1420534 2176430 1921647 1919332 1891362 1616620 25608 25353 2518441 490459 454448 270348 1312137 1521355 23346 24500 1269778 1361053 1302570 21383 3 9 1909649 1569463 25530 25032 1924000 1823228 2505717 1551613 32065 28836 27853 27101 25663 Rsspcnse 0.000 0.000 6233.710 8625.720 1570.4 04 1307.942 917.941 4791.048 0.000 O.OO0 4498.274 4300.032 4422.156 4150.190 7015.362 4723.239 0.000 0.000 0.000 81.993 154.323 194.992 298.037 600.598 914.360 1050.562 1663.308 2262.606 5017.911 7683.917 12695.066 0.000 0.000 6231.812 5722.890 5469.763 1947.153 1792.083 4383.193 0.000 0.000 1728.388 1180.765 4215.479 3956.266 4023.424 4979.129 0.000 0.000 4680.638 6417.885 5708.008 5680.892 6470.854 5221.768 0.000 0.000 8671.869 1514.172 1362.081 804,620 3928.931 5042.004 0.000 0.000 3790.616 4423.3 67 3753.871 6326.790 5474.736 4583.933 0.000 0.000 6430.461 6107.042 7474.248 4455.908 0.000 0.000 79.638 76.961 73.164 m Flags 0.00 bb 0.00 bb 355.34 bb 533.78 bb 71.71 bb 57.44 bb 36.51 bb 260.43 bb 0.00 bb 0.00 bb 242.07 bb 229.84 bb 237.34 bb 220.60 bb 410.32 bb 256.16 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bbX 0.00 bbX 3 . 8 5 bbX 19.70 bb 36.32 bb 43.59 bb 76.79 bb 110.05 bb 274.86 bb 459.73 bb 967.50 bb 0.00 bb 0.00 bb 355.21 bb 320.83 bb 304.11 bb 479.86 bb 83.87 bb 234.93 bb 0.00 bb 0.00 bb 80.37 bb 50.58 bb 224.60 bb 208.79 bb 212.87 bb 272.38 bb 0.00 bb 0.00 bb 253.48 bb 368.04 bb 3 1 9 . 8 4 bb 318.04 bb 371.72 bb 287.97 bb 0 . 0 0 bb 0.00 bb 537.56 bb 68.64 bb 60.37 bb 3 0 . 4 8 bb 201.13 bb 276.40 bb 0.00 bb 0.00 bb 198.79 bb 237.42 bb 196.59 bb 361.74 bb 304.14 bb 247.42 bb 0.00 bb 0.00 bb 368.92 bb 346.68 bb 443.90 bb 239.44 bb 0 . 0 0 bb 0 . 0 0 bb 0.00 bb 0.00 bb 0 . 0 0 bb 8Dev 4 2 -100 -100 -61 -21 -9 -13 2 10 10 -8 -3 -6 9 15 10 -1 -4 od c-t Guantitated and Printed by CMC on 18 Dec 0 0 , Study E00-1311 Page 2 3M Environmental Laboratory Page 536 of 703 BACK TO MAIN ~~~ e W t l f y Cd- S-ry -rt PFOS Adsorbllhrorb Study LC/aas Ins-t: Tucker (LA052) SaqlO Ilst: c:Vd;*ssL~\~atur.PRO\Saql~\t001215 Last U f z e d d : ldrm OW 18 10:45:28 2000 t&thd: c:~sLnm\naaatur.PRO\M.U9B\001215 L a s t modrfied: )don DW 1 8 1 0 : 5 0 : 0 1 2000 Job C o h : PYmted: M e n tma 18 10:56:20 2000 L Corpomd 1: PFos(499) N165 t001215 165 166 tOO1215Ii66 167 t001215-167 168 to01215 168 169 t0012151169 170 to01215 170 178 t001215I178 179 t001215-179 180 t001215-180 181 t001215-181 182 t001215-182 183 t001215-183 184 t001215-184 185 t001215-185 186 t001215 186 192 t001215I192 193 tO01215-193 194 t001215 194 S.pple1i.t Text lox 800-1311-3186ms lox 800-1311-3187 250.4 p'ob PFOS 00003-141 KeOH Blank, TN-A-4740, Aliq. 12/01/00 M C HeOH B1,nnk. TN-A-4740, Aliq. 12/04/00 CKC lox 600-1311-3188 lox 800-1311-3189 lox 600~-1311-3189m 10% 800~-1311-3190 10% 600-1311-3191 250.4 ppb PFOS 00003-141 HeOH B l a n k , TN-A-4740. Aliq. 12/04/00 CKC KeOH B l m k , TN-A-4740, Aliq. 12/04/00 CKC lox 600-1311-3192 lox 800-~1311-3192ms 250.4 ppb PFOS 00003-141 HeOH B l a n k , TN-A-4740, Aliq. 12/04/00 CKC MeOH Blank, TN-A-4740. Aliq. 12/04/00 M c MeOH B l a n k , TN-A-4740. Aliq. 12/04/00 CKC 0 ppb PE'OS 00002-86-01 2 . 5 ppb PFOS 00002-86-02 5 ppb PEOS 00002-86-03 10 ppb EFOS 00002-86-04 25 ppb EFOS 00002-86-05 40 ppb EFOS 00002-06-06 50.1 ppb PEOS 00002-86-07 75.1 ppb PFOS 00002-06-08 100.2 ppb PFOS 00002-86-09 250.4 pGb PFOS 00003-141 500.9 oeb PFOS 00002~ -06-1.2~ 1001.7cipb PFOS 00002-86-13 HeOH Blank, TN-A-4740, Aliq. 12/04/00 M C KeOH B l a n k , TN-A-4740. Aliq. 12/04/00 CKC KeOH B l a n k , TN-A-4740, Aliq. 12/04/00 CKC RT 6.189 6.208 6.228 6.192 6.248 6.304 6.442 6.484 6.443 6.215 6.213 6.240 6.252 6.477 6.361 6.412 6.420 6.296 6.480 6.401 6.421 6.482 6.486 6.469 6.376 6.468 6.484 6.409 6.192 6.221 6.221 6.221 6.199 6.176 Area 1213191 28200 1709614 33076 32005 24369 24595 1090006 26337 26588 1712977 32775 29504 26709 1122264 1590409 26186 26510 27913 31358 51199 72994 106025 197302 300365 368099 547191 716285 1792194 2783510 4584416 23461 23905 25693 3646.165 84.514 4678.916 0.000 0.000 69.146 70.860 3242.894 81.389 78.975 4750.145 0.000 0.000 76.788 3604.296 5068.404 0.000 0.000 0.000 91.574 146.499 212.090 312.819 574.354 861.131 1052.172 1577.562 2213.537 4908.508 7818.634 12639.560 0.000 0.000 0.000 ppm Flags 190.14 bb 0.00 bb 253.37 bb 0.00 bb 0 . 0 0 bb 0.00 bb 0.00 bb 166.28 bb 0.00 bb 0.00 bb 257.85 bb 0.00 bb 0.00 bb 0.00 bb 187.64 bb 278.09 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bbX 0.00 bbx 4.62 bbX 18.32 bb 33.49 bb 43.60 bb 72.10 bb 107.30 bb 267.88 bb 469.98 bb 959.07 bb 0.00 bb 0.00 bb 0.00 bb 9Dev 1 3 11 -100 -100 -54 -27 -16 -13 -4 7 7 -6 -4 cd Co-t -~ Page 3 h t i t a t e d and Printed by C!&2 on 18 D o o 00, Study E00-1311 3M Environmental Laboratory BACK TO MAIN 210.10 250.40 210.40 210.40 250.10 3M Environmental Laboratory Page 538 of 703 BACK TO MAIN 3M Environmental Laboratory Page 539 of 703 E00-1311 PFOS Adsorb/Desorb BACK TO MAIN rc 0 Study# 00-131 1 Compound: PFOS Study: AdsorblDesorb s!Mww!J owo2dBo5 ow02d6D6 ow02an7 -2dB-08 WdB-09 Analyiical Inslrument: Hillaryon 12/14/00 ReprocessingWorkstation: Dioana 12/1[vM) batch H1214al.b s.m* m B r m & P B ! d t ! a a E k w e E R s P a k eEBLBI 2488 ppblHPFOY2470 ppbPFBSO 25ppbPFOSCabbnllonstd XS 28 H1214A1M HllOM8 0 5 247.0 8 57 2488 ppbTHPFOY2470 ppbPFBSO 40 mbPFOSC d h U e n std rn 2488 ppbTHPFOY2470 p i b PFBSO M 1ppbPFOSCaDbnDonsld 17 27 H l l l U IM Hluo0170 8 247.0 856 21 n1214~M1 ~iinm8D 7 247 0 8 57 2488 ppbTHPFOY2470pphPFBSU 75 1ppbPFOSCahbmbonStd ?D n1214~Mi HIIIWT) o 8 247 0 6% 2488 ppbTHPFOY2470 ppb PFBSO 1W 2ppbPFOS CalibnhOnStd #3 30 H1214A1M HillWMD 9 247 0 156 2486mbTHPFOY2470oobPFBSO CW43-141 2MiipbPFOS C.l~b~.lionStd#lO 31 H1214A1M HHIW31 D 10 247.0 8% moo28811 2488ppbTHPFOY247OppbPFBSO 4WlppbPFOSCsllbnb~St~*11 32 ~ 1 2 1 4M~ 1niitwao 11 247 0 8% 2488ppbTHPFOSl247OppbPFBSO ww2dB12 moo24613 owo3-141 ccv so0 9 ppbPFOSCallbnhonSm a12 2488 ppb THPFOY2470 ppbPFBSO 1Wl 7ppbPFOSC.lbRbon Std #13 2486ppbWFOY2470ppbPFBSO 2% 4 m h PFOS CCV 33 H1214AlM HIllOO330 12 247 0 6 57 34 H1214A1M H1lOO34 D 13 247 0 e 57 42 H1114A1M -2 D 10 247 0 6% 2486p*THPFOY2i~OppbPFBSO CCaU3-141 CCV 250 4 ppbPFOS CCV 50 ni214~M1 HUOW D 10 247.0 8% ooOo2-141 CCV 2488ppbTHPFOI247OppbPFBsO 2504 ppb PFOS CCV 56 n1214*1 M HIIIWS~ D 10 247 0 856 Ow05141 CCV 2488ppbTHPFOY247OppbPFBSO 2% 4 ppb PFOS CCV m nt214~M1 worno 10 2470 6% ow05141 CCV ow03-141 ccv ~002-86-05 oooo~as-~ 2481ppblHPFOY2470ppbPFBSO 1544 ppbPFOS CCV 2486 ppbTHPFOY2470 ppbPFBSO 250 4 ppbPFOS CCV 2486 mobTHPFOY2470 mobPFBSO 25bphPFOSCaIIbia1lonStd 1125 248 8 ppbTHPFOSJ247 0 ppb PFBSC 40 PpD PFOSCahbmbonSld ne 74 H1214A1M HlIIW740 10 2470 8 55 82 H1244AlM W1100820 10 247 0 8 53 89 H1214AlM HllOO890 5 247 0 8 53 90 H1214A1M HlOO900 B 21. 0 8 53 ow02-88-07 ww286n8 2488ppbTHPFOSJ2470pp~PFBSC 50 IppbPFOSCaIIbmtIonS I 1127 2486 ppb THPFOY2470 ppbPFBSO 75 1 ppt PFOSC.hbR11onSld #28 01 Hl214A1M H#ll0090l 7 247 0 6 53 92 H1214A1M HlllWS2D 8 247 0 8 53 ~~28609 OOW3-l4, 2486 pph THPFOSl2470 ppbPFBSC 1002 oob PFOSCahbrahonSld nS 2466 ppbTHPFOSl2410ppbPFBSO 2544 ppbPFOSC.librabon Sld #M 83 H1214A1M H1Q093D 9 247 0 8 53 04 H1214A1M H1110094 D 10 247 0 8 53 moo2.E-11 WW2.8%12 2488 ppb THPFOSJ2470 ppbPFBSO 4W 7ppbPFOS CdlbnnonStd I J I 2486 ppbTHPFOY247OppbPFBSO 5W 9 ppbPFOS CallbrehonStd U 2 05 n 1 2 i i ~Mi ntiiwssD 11 247 0 8 52 OB H1214A1M H~1100860 12 247 0 6 52 WW2-86-13 2486ppbTHPFOY241 OppbPFBSJ 1001 7ppbPFOS Callbmllan Std U3 87 H1214AlM HlllW970 13 247 0 6 52 em#B4 1.030.547.8 1.M0.2773 1.UX.578 8 1.014,~.6 1.U23.443 3 I.MI.Mo4 1,037,341.3 1.042.852.8 1.011.UX4 i.mi,wo 1.U28.888 3 1.025.828 2 1,014,181 1 BM.439 1 078,9245 958.628 4 859.545 8 864.280 1 043,308 8 955,510 1 m.758 3 055.3424 861.285 8 938,3859 248 8 246 8 248 6 248 6 248 8 248 6 248 8 248 8 248 8 248 8 248 8 248 8 248 8 248 8 248 8 246 6 248 8 248 6 246 6 248 8 248 8 248 8 248 8 248 6 QwQUQa 754 645.953 3 7.54 ~ 7 . 7m 7.56 647.800 0 7.54 642.514 9 7.54 M8.175.4 754 856,451 8 7.54 851.0132 754 8M.093 3 7.54 M4.701 0 7.54 855.563 3 754 053.181 1 7.53 855.1157 3 7.53 m.745 5 754 W5.288 6 7.52 822.280 5 7 52 599.348 4 7 52 602.015 6 7.52 813.8254 7.52 598.254 6 7 53 rn9.668 4 7 52 814.9133 7.52 M.3180 7.52 811.2124 7 52 588,8896 EQwiI 7.74 7.74 7 74 7.74 7 74 7 74 7.74 7 74 7 74 7 74 7 74 7 74 7.74 7 74 7 74 7 74 7 74 7 74 7 74 7 74 7 74 7.74 7 74 7 74 tEQ%usa 583.570 1 561.5183 707.754 0 1,M8,1604 l.YY.304 8 3,252.267.8 4,859.772 5 5,851,8855 10.1W.W90 1.~0.226 8 3,217,2125 3,228,307 5 3,122,5120 3.115.8880 3.0%.880 8 338.940 8 530,461 8 BgS,lSS 0 088.530 8 i.m5,48t 5 3.wB.623 0 4,449,8535 5.420.9n 5 9,330.6w 0 EEQaFi? 273 109% 394 I5% 49 4 773 102 1 2576 404 4 14% 30% 10% 2% 0% 498 0 02% 8804 0% 255 4 255 0 255 7 254 7 254 7 255 2 22 4 38 5 49 1 78 7 2 2% 2 1% 1 7% 17% 1 9% 10 4% 3 7% 2% 2 1% 1WB 253 8 387 5 491 5 0 4% 1 4% 0 8% 1 9% 1wB4 0 5% 00-1311 PFOS AdsorblDesortl BACK TO MAIN SwPwR Study# EM)-1311 Compound PFOS Study AdsorblDesorb Analflical InJtrumenI Hillary on 12/14/00 RepmcesslngW o ~ a t i o nDioana 12181w batch H1214bl b mp*m BUU RUMY m n h ywd w w w m ww2Ul6 o(DozdB06 oooO26607 Dmmm ww2M.m WWZ-141 ma5-11 ww2.8512 oWo2a5-13 WW2-141 CCV GXQ3-141 CCV wW3-141 CCV WWZ-141 CCV GXQ? 141 CCV WWJ-141 CCV 00002 f f i 05 O w 0 2 f f i OB oW02-Bgo7 wW2-%%08 ww2.ffin8 wDo3 141 wW2-BB11 OOWZ-BB12 2488 ppb THPFOY 247.0 ppb PFBSO 25ppbPFOS C.HbntlaStdtd.5 2486wbWFOsI2470~~bPFBSo 40Ppa PFOS 2488 ppbTnpFoSl247 0 ppb PFBSO 50 1ppb PFOS 248 8 ppb THPFOY2470 ppb PFBSO 751ppa PFOS 2488 ppbTHPFOY2470 ppbPFBSO 1W2mbPFOS 2488 ppbTHPFOW2470 ppbPFBSD 2504 ppb PFOS 2488ppbTWFOSI247 oppbPF0sD 4W 7 ppb PFOS 2488ppbTHPFOY2470ppbPFBSO 5WSppbPFOS 2488ppbTHPFOY247OppbPFB80 1W17 PpbPFDs 2488 ppbTHPFOY2470 ppbPFBSO 2504 ppb PFOS CCV 2488~PbTHPFOW247OppbPFBSO 2504 ppb PFOS CCV 2488ppblwFos1247 OppbPFBSo 2-4 ppb PFOS CCV 2488 ppbTHPFOW2470 ppbPFBSO 2504 ppb PFOS CCV 2488ppbTHPFOsI247OppbPFBSO 2504 ppb PFOS CCV 2488 ppb 1HPFOS2l 47 0 ppb PFBSO 2504 DDb PFOS CCV 2486ppbTHPFOSl247 OPPbPFBS3 25 ppb PFOS CaIIbratlonSld 125 2186ppblHPFOY2470~~IPFBS~ 40ppb PFOS Cahblallon Sld .28 2486ppbTWFOY241OppbPFBS2 50 1 ppb PFOS 2486 coblHPFOSl247 0 DDb PFBSZ 75 1 ppbPFOs Clllbrabon Sld127 Cal8braUonSld128 2488 ppbTHPFOY2470 ppb PFIS3 (00 2ppbPFOS C.libntion Sld 129 248 5 ppb THPFOSl2470 ppb PFBSO 2504 wbPFOS 2488 ppb THPFOY247 0 ppb PFBSO caml!nn std am 4W7ppbPFOS C.LbR1IOn Std8l 2486 ppbTHPFOSI2410 ppbPFBS3 Mo 8 ppb PFOS 2488 mbTHPFOS2470 PDbPFBS2 CalibmtlonSld 8 2 7 H1214B1M HIIW0I.D 5 247W 853 8 H1214B1M HllW80D 8 247M 053 0 H1214Bl M HI10391 D 7 24700 853 10 H1214B1M H11WD2 D 8 247W 853 11 Hl214B1M HIIWM)3D 8 247W 853 12 HI21481 M HlllW94 D 10 247W 853 13 H1214BlM HIIW95 D 11 247W 8.52 14 H1214BlM H111CCW D 12 247.W 8.52 15 H1214B1M Hlll0397D 13 241.00 852 24 ~ 3 2 1 4M~ 1nmmD 10 247110 851 32 H1214B1M Hill0114D 10 247.00 8.53 4a H1214B1M HIIWlPD 10 247w 8.54 48 H1214B1M HIllO1MD 10 24700 655 58 ~ 1 2 1M4H~I I~WD~ 10 24700 855 84 ~ 1 2M ~~8no1~46D 1 10 24700 854 71 n i 2 w w M nt110?530 5 267 w 8 54 72 H121481M H1110154D 8 247W 855 73 H121.81 M H1101550 7 24700 654 74 HI21401 M H8110158D 8 24700 854 75 H1214BlM Hdl0157D 9 24700 655 7U H121401 M HiMO158D 10 247W 854 77 H121481M H11101590 11 247W 854 78 H121481M H!IW1800 12 247W 654 eE&hml QsE82n 38 9 5 w 5 75 wl280 13 943308 58 956510OB sal58 31 956342 u 861285 81 oJ8xI5 88 98050 M 87Mu) 89 87Ri97u o w 19 8BoOt99.4 871858 E8 958397 w -11 58 88376 19 853208 M 88051744 88197484 95928258 859614 31 m2681 w mEE!2%& meEQsBz- 24880 248 Bo 248 80 248 Bo 248 Bo 248 Bo 248 w 248 80 148 80 248 Bo 248 Bo 248 Bo 248 eu 248 80 2 a80 248 60 248 80 248 60 248 60 248 80 248 60 248 80 24660 248 60 752 5SSM838 752 W201558 752 813825U 752 5-63 753 nW?edJ(1 752 81491325 752 %531894 752 011212U 752 -8 751 61273483 752 82528375 752 6328118s 753 6311Bo38 753 82143550 752 83151888 753 61198938 753 62282431 753 61770118 752 81689531 7 53 815541U 752 62730431 753 81799138 752 812872 13 752 81999975 EQXm 7 74 7 74 7.74 7 74 7 74 7 74 7 74 174 7 74 7.74 7 74 7.74 7 74 7 74 7 74 7 74 7 71 7 74 7 74 7 74 7 74 7 74 7 74 7.74 E!2sml 338840 84 5 3 M 1 75 ea79500 Ri8uo 81 1265481 50 XaSsnW 4449853 M 5420827 M 0350660 w m7740 75 xea70 M M78148 W so3M35 M 3045221 M 3080745 75 341318 55 53352363 08917525 876864 25 1288105 75 M55103 75 4522913 50 542403854 966958100 PEWPPh 22 65 38 84 49 59 n 47 10164 258 44 401 52 4% 38 101605 258 81 25731 255 w 251 73 257 OB 254 00 22 25 37 89 49 44 7578 101% 25534 399 54 495 35 sa9 84 8 4% 2 8% 1% 3 2% 14% 2 4% 0% 0 8% 14% 2 5% 2 8% 18% 0 5% Z7% 14% 110% 5 8% 13% 09% 2 3% 2 0% 0 3% 11% 1 2% BACK TO MAIN m 3 s5CD 3 s e b 0 3 Sample Batch H010405.b, analyzedon HillaryOCOCO1. PFOSAdrorblD.rorb SimplN. Matrix: S o i l f S l g l ~ . Standardc u m range used tor calibration ot sampler: 5-1W2 n@mL Batch method: H01040S.m Inj Dab Batch SimpTyp 416101 1253 D.ChsmWinaryWol0405.b SAMPLE 416101 13:08 D:\Chem&iWaryW10405,b CALlB-1 4(6101 1322 D:\ChemWlaryWOlW5.b CALIB-2 &WLX i;:"o ~:LPh~~.~!'3y\H01M05.CbALIB-3 4/6/01 13.51 D!ChemWiryWOlMO5.b CALIB-4 4/6/01 14.05 D ChemW1UaryWOlMO5.b SAMPLE 416101 14.20 D.ChemWllaryW010405.b CALIB-5 416101 14.34 D-ChemWillaryWolC405.b CALfB-6 416101 14.48 D-ChemWiNaryW010405.6 CAUB-7 416101 15:03 D!ChemWdlaryWOlW5 b CAUB-8 4/6/01 15.17 D.ChemW~UaryViOlMo5.b SAMPLE W 0 1 15.31 D.ChemWillaryW010405b CAUB-9 416101 1546 D:ChemWdlaryW010405.b CAUB-10 4nm14.57 D ChemWllaryWOlW05.b SAMPLE 4nm1 511 D:\ChemWilaryW010405b CAUB-11 4 n x l l 5 26 D:ChemWlaryWolMo5.b CALM-12 4 n m i 5-40D:ChemWillaryW010405b CALIB-13 4/7/01 5.55 D ChmWillaryWOlW5.b CALM-14 4/7/01 6 09 D ChemWillaryW010405.b SAMPLE 4nm16.23 D ChsmW~UaryWO1Mffi.b CALIB-15 417101 6.38 D.ChemWlaryW010405.b CALIB-I6 417/016:52D.lChemW~aryWOlMO5.b CALM-17 417m17.07 DChemWNaryWOlMO5.b CALIB-18 4/7/01 7:21 D:ChemW1llaryWOl0405b SAMPLE 417401735 DChemWdlaryWol0405.b CAUB-19 417101 7.50 DChemWllaryV1010405.b CAUB-20 File Sample Nvn8 HILLWl6.D 0 ngmL PFOSin MeOH HILLW17.D 2.5 nglmL PFOS inMeOH HILLW18.D 5 nplmL PFOS in MeOH HILLW19.D 10 nglmL PFOS in MeOH HILLW2O.U 25 w ' m i PiDSaM-*H HILLW21.D 4 0 nglmL PFOS in MaOH HILLW22.D 50.1nplmLPFOSinMeOH HILLW23.D 75.1 nglmL PFOS in MsOH HlU0024.D 1W.2 ndmL PFOS inMeOH HILLW25.D 250.5 n#mL PFOS in MeOH HILLW26.D 400.8 ng/mLPFOS in MeOH HILL0027 D 501 nglmL PFOS in MeOH HILL0028D lWZnO/mLPFOSinMeOH HlLLW83.D 0 W m L PFOSin MeOH HlLLW84.D 2.5 nglmL PFOS in MeOH H I L W 5 D 5 nplmL PFOS in MsOH HI~w088.D 10N m L PFOSinM.DH HILLWB7.D 25 W m L PFOS in MeOH HlLLW88.D 4 0 W m L PFDSVI MeOH HILLW89.D 50.1 ndmL PFOSinMeOH HILLW90.D 75.1 n d m lPFOS in MeOH HlLLW91.D 1W.2 nahnLPFOS 111 MoOH HlUW92.D 2M.5 ng/mL PFOSm MeOH HILLW93.D 4W.8 ndmLPFOSm MeOH HlLLW94.D 501 n&L PFOS VI MEOH HILL0095.D 501 nglmLPFOSin MeOH MIrc InPCompoundN a R l Ana THPFOS mwos 5.111 5.121 THPFOS 5.12 THPFOS 5107 THPFOS 5.1W THPFOS 5.121 THPFOS 5.119 THPFOS 5.121 THPFOS 5.119 THPFOS 5.112 THPFOS 5.111 THPFOS 5.112 THPFOS 5.113 THPFOS 5098 THPFOS 5.092 THPFOS 5.048 THPFOS 5.1 THPFOS 5.108 THPFOS 5.101 THPFOS 5.1 THPFOS 5.101 THPFOS 5.108 THPFOS 5.107 THPFOS 5.105 THPFOS 5.104 THPFOS 5.104 Amount 853901 254 880305 254 9W514 254 884801 254 891555 254 8- *c. L- 805109 254 9079Sg 254 902929 254 921590 254 890229 254 885051 254 soBB.uI 254 909918 254 901288 254 907830 254 893988 254 886284 2=54 8wm 254 848217 254 818488 254 824040 254 839800 254 795504 254 790146 254 798759 254 Avenae: 871828.15q w!2?!&3w.9.57909 XRSD: Compound NarRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS wos PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS wos PFOS PFOS PFOS Ana ,Amount 0 0 0 5.331 5l194 3.942931 533 1 1 w 8.364052 5 324 189988 10.48501 5 323 495541 26.37293 5 331 779774 41.22295 5 33 971274 5 0 . 8 5 3 5 331 1469171 77.71198 5 328 1921199 102.2878 5 322 4651125 255.0356 5 335 6791612 402.9106 5 322 8184382 541689 5 33 14871358 994 5332 0 0 0 5 302 53350 3326644 5 301 95517 5.429805 5 31 158439 8.752514 5 316 425595 23.3514 5 311 675739 37.43176 5 31 847857 47.35439 5311 1278693 7446758 5309 1665885 97.01042 5 31 4111457 248.754 5 308 6W4617 3980979 5 314 7263676 498.2841 5 314 13221474 1M19.264 127% 105% 105% 103% ,..n.."*,. f03% 102% 64% 101% 100% 99% 109% ea% 93% 94% 95% 99% 97% 62X 99% 99% faiw iimn +m%: 6102.W -30%: In1Date Batch 41WJ112 25 D ChemWdIaryWOlLl405b 41BR112 39 D IChemWfflaryWolMO5 b 4/6/01 76 W D !ChemWla1yWOIW5 b 4w101 16 14 D ChemW~llaryWOlW5b 4/6/011921 D ChmWiUaryWolMffi b 4 ~ 1 0 119 36 D ChemW11laryW010405b 41610122 43 D !ChemVkUaryW0104ffib w 4/6/0122 57 D \ChemWdlaiyWOIO405b 4,7101 1 D IChemW!llaryW010405 b mmi 2 M ~ChemWiIlaryWolM05b 2 4nmi 4 28 D ChemWllaryW010405b 4171014 43 D ChemWdlaryWOlW5 b 4/7m18 04 D ChemWdlaryWOlD405b S.mpTYP SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File HIUW14.D HlU0015.D HILLWZ9 D HILLWM.D HILLCiJ43.D HILLOO44.D HlLLW57.D HlU0058.D HILLW7O.D HIUW7I.D HILLW81.D HlLLW82.D HILLOWB D HILLW97.D Sanpl. Name TN-A 4802 MeOH TN-A 4802MeOH TN-A 4602 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TNA 4802MeOH TN-A 4802MeOH TN-A 4802 MeOH TN-A 4802MeOH M - A 4802MeOH TN-A 4802 MeOH Mlrc InPCompoundNaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Ana 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound NaAT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Am. 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 o a 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 00 0 BACK TO MAIN Ini Data Batch 4/6/01 1629 D ChemW~llaryW01040b5 416101 16 43 D ChemWllaryW010405b 416101 16 58 D ChemW11laryV1010405b 4/6/01 17 12 D ChemWllaryWO1MOSb 41M)l 1726 D ChemWillaryWOlM05b 4/6/01 1741 D ChemWllaryW010405b 4/6/01 17 55 0 \ChemWdlaryWOlMO5b 4Iwui 11 UY u \Lnernwtuarywuiw%D 4/6/01 18 24 D ChemWtflaryW010405b 4/6/01 18 38 D ChemWillaryWO10405b 4/6/01 18 52 D ChemW1llaryW010405b 4I6ml 1907 D \Chem~llaryWOlMO5b 4/6/01 19 50 D ChemWdllaryW010405 b 41610120 04 D ChemW~tlaryWOl04OSb 4/6/0120 19 D ChemW8UaryW010405b 416101 20 33 D iChemWllaryW010405 b 4/6/01 20 48 D ChemWtllaryW010405 b 4161(312102D ChemWiflaryW010405b 416101 21 16 D ChemW~UaryWOl0405b 4/6/01 21 31 DChemWllaryWOlMOSb 4/Bx)121 45 0 \ChemWllaryW010405b 4/6/0121 59 DChemW1llaryW01040b5 4/6/01 22 14 DChemW~llaryWOlMO5b 416101 22 28 D ChemWillaryW010405 b 4/6/01 23 11 DChemWdlaryW010405 b 4/6/01 23 26 D ChemWdlaryWO10405b 4/6/0123 40 D ChemWdlmyWOlC405b 416101 23 55 D ChemW1UaryWOl0405b 4nm10 W D ChemWllaryW010405b 4/7/010 23 D ChemWrlaryWO10405b 4/7/01 038 D ChemWollaryWOl0405b 4/7/01 0 52 D ChemWdlaryWOl0405b 4/7m1 107 D ChemWdaryWOlM05b 4 n m l 1 2 1 DChemWillaryW010405b 4/7/01 136 D ChemWdlaryW010405b 417/012 10 D C h e m W ~ ~ W O l r w obS 4/7/012 33 D ChemWllaryW010405b 4/7/012 47 D ChemW1llaryW010405b 4/7/01 3 02 D ChemWllaryW010405b 4/7/013 16 D ChemWillaryV1010405b 4/7/013 31 D ChemWllaryW010405b 4/7/01 3 45 D ChemW1llaryW010405b Wm1 3 59 D ChemWdlaryWOl0405 b 4 n m l 4 14 D ChemWiUaryW010405b SampTyp. SAMPLZ SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SMMFLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE FIIe Sample Name MISSlnfcompwnd NaRT Am HILLW3l.D 2mgiLPFOSStud~NumberEW-1311 THPFOS 5112 HILL0032 D 2m& PFOS Study Number E001311 THPFOS 5.12 HlLLW33.D 2mdL PFOS Study Number EW-1311 THPFOS 5.113 HILL0034.D 2mfl PFOS Study Number EW-1311 THPFOS 5.112 HILL0035 D l h p n PFOS Study Number EW-1311 THPFOS 5.106 HILLW38 D HlUW37.D Hia3,g ".. 10mdL PFOSSWy Number EW-1311 10mgILPFOS Study Number EW-1311 .^ -.,, "-"CC...A...a .._L__rM. ' " " ' ~ L""*C.U", I."II,MI L W I O I I THPFOS THPFOS NDFOS 5.115 5.109 "c.,+""C" HlLLW39.D 2mfl PFOSStudyNmberEW-1311 THPFOS 5.112 HILL004O.D 2mpll PFOSStudyNumber EW-1311 THPFOS 5.111 HILL0041.D 5 nglmLPFOS in MeOH THPFOS 5.113 HlLLW42.D 250.5 nglmi PFOS in MeOH THPFOS 5.118 HILL0045D 2mgL PFOS S W Number EW-1311 THPFOS 5.112 HILLW4&D 2mfl PFDSStudy NumberEW-1311 THPFOS 5.118 HILL0047 D l o a PFOSStudy Number EW-1311 THPFOS 5.108 HILL0048 D 10mplL PFOS Study Numbar EW-1311 THPFOS 5.112 HILLOM9D 1OmdLPFOSStudy Number E001311 THPFOS 5.106 H l L L ~ 5 0D lhng/L PFOSStudy Number EW-1311 THPFOS 5.112 HlU0051.D hng/L PFOS Study Number Em1311 THPFOS 5.114 HlLLW52.D O m g L PFDSStudy Number EW-1311 THPFOS 5.109 HlLL0053.D OmplL PFOS Study Number E001311 THPFOS 5.104 HILL0054 D OmglL PFDS Study Number EW-1311 THPFOS 5 098 HILLW55 D 5 @mL PFOS In MeOH THPFOS 5.112 HILLW5B.D 250 5 nglmLPFOSIn MeOH THPFOS 5.098 HILLW59.D l o m a PFOSStudy NumberEW-1311 THPFOS 5.105 H1LLW.D lompn PFOS Study NumberE001311 THPFDS 5.107 HlLLDOB1.D l~PFffiStudyNumberE001311 THPFOS 5.105 HILLW62.D 1 h d L PFOSStudy Number EW-1311 THPFDS 5.105 HILLW63.D l h # L PFOS Study Number EW-1311 HlU0064.D lhpnPFOS Study Number EW-1311 THPFOS THPFDS 5.111 5.105 HILL0065D 1 W L PFOS Study Number E001311 THPFOS 5.1 HILLWBBD 10mgtL PFOS Study Numbttr EW-1311 THPFOS 5.105 HILLDOB7D om#L PFOS Study Number Em1311 THPFOS 5.098 HILL0068.D 5 nplmL PFOS in MeOH THPFOS 5.1 HlLLW69 D 250.5 WmL PFOSin MeOH THPFOS 5 102 HILLW72.D Om& PFDS Study Number E001311 THPFOS 5.097 HILLW73D Om& PFOSStudy NumberEW-1311 THPFOS 5.091 HlLLW74 D O W PFOSStudy Number EW-1311 THPFOS 5 091 HILLW75.D OmdL PFOS Study NumberEW-1311 THPFOS 5.084 HILLOQ76.D OrnQIL PFDS Study NumberE00-1311 THPFOS 5 W2 HILLW77.D Omqll PFOSStudy NumberEW-1811 THPFOS 0 HILLW78.D ompllPFDS Study Number EW-1311 THPFOS 0 HlLLW79.D 5 ndmL PFOS in MeOH THPFOS 5.085 HILLO08O.D 250.5 n@mLPFOSin MeOH THPFOS 5.091 Amount 831638 254 645717 254 845296 254 691267 254 895152 254 904138 254 908952 254 715231 254 840577 254 843047 254 941520 254 937854 254 852429 254 688430 254 9iim7 254 919538 254 918088 254 732339 254 864599 254 844692 254 809811 254 672W 254 880662 254 872477 254 808071 254 808820 254 809437 254 648037 254 853122 254 888881 254 854113 254 700905 254 1281548 254 999732 254 916425 254 1282301 254 1283570 254 1122340 254 1275724 254 1295458 254 0 0 0 0 1122048 254 1051408 254 ISTD>130% ISTDrlM% ISTD>130% ISTD>130% ISTD>130% ISTD<70% ISTD<70% Compound N a A T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A 5.329 5 33 5 323 5 322 5 323 5 333 5 328 5 322 5 329 5 321 5 323 5328 5 329 5 328 5 318 5 322 5 323 5 323 5 324 5 319 5 322 5 315 5 322 5 315 5 322 5317 5 322 5 323 5 322 5 315 5 31 5 315 5 308 5 31 5 312 5 307 5302 5 301 5 304 5 303 5 297 5 295 5 295 5308 m Amount 1594908 91.89164 1 0 H W 5876517 1801969 1024878 4370912 326.6226 789270 41 74738 988799 51.74131 730034 38.024 ?an?dn1 2?dRsn? 1682254 96.60648 2112598 121.2132 112770 8.100833 4597708 247.11% 1619584 91.01251 4093813 305.1053 1001788 52.07933 998187 51.3553 998588 5167698 3717782 2586704 780291 40.69207 213559 12.2533 113509 7.04131 3059833 228.1126 1099W 8.465906 4451710 258.0898 W 1 2 9 437.9532 7503267 533.5302 6451764 423.3709 8372595 746.0709 1011146 5623727 1599452 8808401 1587814 87843% 4173504 305.6482 542210 20.16817 103957 5.373168 4290803 235.5874 144727 5.782359 92058 3.88763 2467820 105.8252 19188 1.282508 11715 1.007175 11778 0 2280129 0 95065 4.488151 4[182781 191.3037 122.0% 980% 129.3% 103.0% 107.5% 94.0% 89.7% 76.4% page 2 of 2 BACK TO MAIN s" Samph BatchRO10310.b, -1yz.d on Rush Stmdad c u m rangeusedlor ulibntion ol BPChmethod RO1032Om Ini Daw Batch 32Oml 1(:17 D.\ChemRushWlO320.b MM)l 1431 D:Mem\RWW010320.b MM)1 14.45 D.MunWushW010320.b YiOlOl 1459 D \Chcm\RushWOl032O.b 320101 15 14 D \ChemlFlurii~OiO:Z8.D 3120101 1528 D!Chem\RushW0103ZO.b VZOMl 15 42 DlChemIRurh\RO1032Ob SunpTyp SAMPLE CAUS-1 CUlS-2 CALIS-3 C.*L!E-4 CWB-5 CUB 8 Fila RUSHWl8 D RUSH0019.D RUSHW2O.D RUSHW21.0 RUSHW.D RUSHW23.D RUSHCQ24 D 0 WmLPFOSin MeOH 2.5 nohnL PFOS n UIOH 5 WRd. PFOS in MeCH 10WmLPFOS MIOH 25 WmLPFOS b M a 40 WlmL PFOSn YO6 5 0 W a PFOShMIOH 32Wl 1811 O\Cham'Rurh~01032Ob CALlBI8 320101 1625 D`ChemWushROlOM b CALlE 9 32Om1 1640 O:!Chcm\RurhU7010320b SAMRE Y201011654 D:\ChcmRurhWlO32O.b w e - 1 0 32010117.09 D:\Chsm~hW010320.b SAMPLE M l l O l 1620 D:\Chun~~ushW0103ZO.b SAMPLE 3/21/011635 D\ChemWuSh\ROlO320b cws-11 CALlB_l2 CUlS-13 CUB-14 3/21/01 1732 D `ChemWushWO10320b CALIB-15 wimt 1746 01~hem~ush\~o10b320CUlB-16 ~ m m18i 01 D'ChrmRurhY1010320b wus-17 32110118 15 0 \ChcmlRurh\R010320b CALM-1 8 3121I011829 D \ChcmWurhWOlOM b CALIS-19 3R11011844 D \ChemWulhWOlO320b SAMPLE 32181 18 58 D \Chcm\Rurh\ROlO320b CALlB 20 M1m11912 D\CMmWushWO10320b SAMPk RUSHWSD RUSH0027 D RUSHWZLID RUSHW23 D RUSHOOM D RUSH0127 D RUSH0128 D RUSH0129 0 RUSH01300 RUSH0131D RUSH0132D RUSH0133 D RUSH0134 D RUSH0135 D RUSH0158 D RUSH0137 D RUSH0138 D RUSHO139D lOO&LPFOSinMeOH 250 WmL PFOShMsOH 4W WmL PFOS h MaoH 500 WmL PFOS in Ulon 1WZnpllnLPFOShlMaOH 0 WmL PFOS in MeOH 2 5 w+Wd, PFOS h Id& 5 nplmL PFOS In UsOH 10WmL PFOSn UaOH 25 WmL PFOS in Ucon 40 w a PFOS in UM)H 50 r@Pa FOSn UaOH 75 WmLPFOSn MaoH 1WWmLPFOSflMsOH ZSOWmLPFOSbMeOn 4Wr@mLPFOSmMsOH 5CQWmLPFOSlnMeOH lw2ipl~rLPFOShMeOH , m L . MIUi u IInn compoundNaRT Ama THPFOS 5.517 THPFOS 5 496 MPFOS 5 A94 THPFOS 5.495 THPFOS 5.498 TYPFOS 5.494 THPFOS 5.495 THPFOS 5.496 THPFOS 5.503 THPFOS 5.49 WFOS 5.489 THPFOS 5.498 THPFOS 5 495 THPFOS 5.515 THPFOS 5 512 THPFOS 5.m wFos 5.497 mpws 5.4m THPFOS 5.4m THPFOS 5.M2 THPFOS 5.49 THPFOS 5.484 THPFOS 5.461 THPFOS 5.494 THPFOS 5 481 THPFOS 5.485 1WlW 1W171 lW8872 1Do9ua1i 1WOOM 1108159 it06726 1104875 1112297 1114997 953251 962546 p691sd 960982 9511214 951m 948455 94421 94719 9389a2 9375011 931253 925949 COmpoundwr A- &mount PFOS 0 0 0 PFOS 5.708 128796 1.792859 PFOS 5.704 203193 4.1851102 84% 2% PFOS 5705 3YIW 9.517807 os% W PFOS 5.713 85778 28.7BM 107% 2% PFOS 5.7M 1315734 43.05413 1OIx ij; PEDS 5.719 1620397 54.18483 IOlY 254 PFOS 5.72 22923S4 W.3aGi iliii 2% PFOS 5.72 2972281 105.9074 W X w PFOS 5.707 6Mo194 2B3.4ouI 106% 254 PFOS 5.708 9479889 421.7312 106% 254 PFOS 5.7W 113Cd172 524921 106% 254 PFOS 5.712 19398403 1093.974 10% 254 PFOS 0 0 0 254 PFOS 5.729 118137 1.935808 w PFOS 5.715 17683 4.131231 83% 254 PFOS 5.715 295223 8.741336 87% 254 PFOS 5.715 672893 23.-741 M% 254 PFOS 5.713 1028746 36.41873 %% 254 PFOS 5719 12592Ml 18.22542 I% 254 PFOS 5.707 1807434 12.4196 %% 254 PFOS 5.712 2314201 951839 (6% 254 PFOS 5.705 4oW995 zU.5876 83% 254 PFOS 5.711 7221977 3 6 7 M 7 91% 254 PFOS 5.890 m i i i s 8 44.2154 S I % 254 PFOS 5702 14684001 959.5687 %% 1331499 +30%: 716961 -30%. lnl Kuw Batch YPOIOI 13 46 D!ChsmWuYI\R010320b MOIO11402 DUhsmWush~OlO320b 32OIOl 1723 D Chem~urhWOlO32Ob 3ROIO11757 DIcMm~ushW010320b 31zM)120 44 D \CMm\RushH010320 b 32OlOl 20 58 D \ChemRuShWO10320b 3R1101005 D \ChemWuShWOlOUOb 3/21/010 19 D IChcm~urhWOl032Ob 321101326 0 \ChemWurhbQO10320b VlrlOr 3 "7 D_ IC~m.LQuSh~O103b20 ~ 1 / 0 1487 DU)hemW1~rh\RO1032b0 3/21/017 01 D!ChhemWuShWO10320b 3/21/011007 D IChem\RurhWOlO3ZOb 3R11011022 D uhcm~RushWOlO32b0 3/21/011300 0 \ChemWushWOl0320b YZllOl 13 14 D \ChemWushW010320 b 3/21101 1552 DChsmWYSh\R010320b _ V21m.l 16 OB 0 Mem\Rush\ROlO320b 3n1I01 19 27 D \Chun\RushWO10120b SAMPLE SAMPLE S.AMPLE ~~ SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE Fih RUSHW18.D RUSHW17.D RUSHW31.D RUSHW32.D RUSHMY5.D RUSHOM6.D RUSH(1059.D RUSHW60.D RUSHW73.D RUSH0074.D RUSHOMI7.D Rusma.o RUSHOlO1.D RUSH0102.D RUSHO113.D RUSHOll4.D RUSH0125.D RUSHO1ZB.D RUSHOl4O.D SMlPk Nm TUA4802 W O H RCA 4@Q2MeOH RCA 4802W O H TN-A 4WZ M& TKA 4 W MaM1 TKA48GZMaOH TKA 4802MsMl TN-A 4802 MeW TN-A 4602 MIOH TN-A 41102 M& TK* 1802M a TN-A 4102 M8Ml RCA 41102 MsDH TN-A 4802 MaMl TN-A 4802 MIOH TUA 4802 MIOH TN-A 4802 MIOH TNJL 4802 MMlH TN-A 4802 MoOH Mlrc In compound NaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS mpws THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS AU 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 *Rlo"nt 0 0 0 0 0 0 0 0 a o 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 C m P,undN.nT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Am, 5.7% 5.733 5.719 5.718 5.704 5.701 5714 57W 5894 5897 5715 5712 5733 5727 5733 572 5741 574 5718 Amount Mno 0 33969 0 53624 0 36113 0 y8u 0 30908 0 37789 0 33871 0 4m9 0 35794 0 41264 0 36212 0 U171 0 38719 0 soM2 0 42724 0 46381 0 42881 0 594w 0 0 -h -4 w 0 BACK TO MAIN R010320 dsta ewO.* In1 Dab Each 3R0101 1732 D:\ChemU7urh\R010120b S ~ P T Y P FN. Sample NU~Y SAMPLE RUSHW33.D 13111-506653 M O l O l 18.08 D.\Chsm\RurhW10320.b SAMPLE RVSHW34.D 13115066MSS3 3lZOlOl 1820 0 ChemWurhiRO1032O.b SAMPLE RUSHW35.D 1311dlWS3 3RDIo1 18.55 O.\Cham\RRurh\RO1032O.b SAMPLE RUSHW36D 1311~510153 yzO/O1 18.49 O.Ehem\R~hUtO10320.b SAMPLE RUSHW17D 1311-5102-S3 3ROlOl 19.03 0 \Cham\Rush\RO10320.b SAMPLE RVSr(Om8D 1311-5102ysS3 W 0 1 19.18 ~ : ~ " ~ , , ; ~.SA"MPL~E ~RU~SH~00~ 39~D .!l.J~~llS l Y- I ~-s3 ~ . ~ Mol011932 O:\Chem\RushU7010320b SAMPLE RUSHOMO.0 1311-5iSi-S3 UZ0101 W48 D:\ChemWush\R010320.b SAMPLE RUSHWI1.D 1311-5138-S3 300101 X.01 O.Mm\Rurh\R01032O.b SAMPLE RUSHOM2.D 1311-51JM16s3 32010120:15 O:Ehcm\Rwh\R010320.b SAMPLE RUSHOM3.0 5 DplmL PFOS h M6W M O l O l 2029 O:\Chem\Rurh\RO103ZOb SAMPLE RU5HW.D ZMnglmLPFOShMsOH 312010121:12 D:\Chem\Rwh\RO1OUO.b SAMPLE RUSHOM7.D 1311-5172-53 312OiU1 21:27 D:VlhemU?urh\RO1OUO.b SAMPLE RUSHO(U8.D 1311-5171.51 MOmlZl:41 O:!Ch~wh\ROlOUO.b SAMPLE RUSHOM9.D 1311-5174-53 312010121:55 D~MmWushWO10320.b SAMPLE RUSHW5O.O 1311-5174ussJ 3220101 22'10 O'\Chem\RUSh\R010320.b SAMWE RUSHW5l.D 1311-52WS3 SAM= RUSHOOU.0 1311-520453 312010122 38 0 \Chem\Rush\RO10320b SAMPLE RUSHDO53.D 1311-521053 M O I O 1 22 53 D Chsm\RurhU7010320b SAMPLE RUSHW54.D 1311-5210MS-53 312010123 07 D Chm\Rurh\RO10320b SAMPLE RUSHW55D 1311.503153 3120/012322 OEhem\Rush\R010320b SAMPLE RJSHWSBD 1311403253 uZM)123 36 D\ChemY(ushYIO1032O b SAMPLE RUSrK)IUI0 5 9 m i PFOS h USOH U2.0M12- 3 50 D\Chem\Rurh\R010320b SAMPLE RUSHWSD 250 d m PFOSn UaoH 3211010 33 D\Chem~hW01032b0 SAMPLE RUSHOOBI D 1311-&3-S3 MI101048 D:\Chem\Rurh\RO1032O.b SAMPLE RUSH00620 1311-5033MS3 M i 1 0 1 192 D:\Chm\RurhY(010320.b SAMPLE RUSHW63 D 1311--7.53 3/21/01 138 D:\Chem~urh~O1032O.b SAMPLE RUSH- D 1311-5WS-S3 3211011.31 D:\Chem\Rurh~O10320b SAMPLE RUSHW650 1311-546BS3 Ml1011:45 O.\Chem\RurhRO10320.b SAMPLE RUMOS50 ll11-508oHs-s3 31211012.00 D.\ChemlRushROl0320.b SAMPLE RUSH00870 1311-5103S3 V211012 1 4 0 \Chcm\R~urhR01032b0 SAMPLE R U S H W D 1311-51ocsJ 3/21/01 228 D\Chem\R~1h\R010320.b SAMPLE RUSHUC69D 1311-510553 3/211012:43 O:\Chsm\Rurh\RO1O320 b SAMPLE RUSHOO70.D 1311-5105M653 3/21101 2:57 D:!ChemHushbQO1032O.b SxMPLE M l l O l 311 D.\Chem\RushW10320 b SAMPLE 3/21/01354 D IChemRurhkQ010320b SAMPLE RUSH0075.D 1311~139S3 3/21/01 4.09 O.Ehem\Rush\R010320.b SAMPLE RUSHW76.D 1311-514C43 3/21/01 433 O:\ChemWurh\ROlO3ZO.b SAMPLE RUSH0077.0 13115141-S3 3/21/01 4:s D'\Chem\Ruih\R010320.b SAMPLE RUSH00780 !311-5141MSS3 3R1lOl 4 5 2 D'\Chem\Ruih\R010320.b SAMPLE RUSHOO79.D 1311-5211-53 M1101 5.08 D:!Chem\RushlR01032O.b SAbWLE RUSHOO8OD 1311-5212S3 3R11015.21 O \ C h e m ~ u r h ~ 0 1 0 3bX SAMPLE RUSHDO81D 1311-521SS3 x i m i 5.35 D:!Chsm\RuShlR010320.b SAMPLE RUSH0082D 1311-5213M-S3 3R11015:ls O:\Chem\Rush\ROlO320.b SAMPLE RUSHODLUD 1311-50%-53 31211016.04 D:\Chem\Rurh\RO10320b SAMPLE RUSH0084D 1311-503553 SAMPLE RUSHOW50 5 Wn'L PFOSin MtOH sr\MPLE SAMPLE RUSHOM6D 250 nglnk PFOSin MsOH RUSH0089 D 13~t.y1?&S~ 3 . 3 SAMPLE RUSH0090 D 131l-M16M5S1 Mirc In Canwund NaRT Am. lWiOS 5.49 5.489 MPFOS mwos 5.483 5.w THPFOS 5.482 THPFOS 5.m THPFOS 5.481 THPFOS 5.489 THPFOS 5.468 THPFOS 5.476 THPFOS 5.474 THPFOS 5.467 THPFOS 5.473 THPFOS 5.47 THPFOS 5.474 THPFOS 5404 MPFOS 5.47 MPFOS 5.474 THPFOS THPFOS 5.484 5481 MPFOS 5.494 THPFOS 5.404 THPFOS 5.484 MPFOS rnm THPFOS 5.481 5 18 5.474 WFOS 5.474 MPFOS 5 474 THPFOS THPFOS 5 472 5 472 THPFOS 5 474 THPFOS 5.489 THPFOS 5.46 THPFOS TWFOS 5.469 5.467 mpws 5.46 THPFOS mwos 5.460 5.46 THPFOS wms THPFOS 5.468 5.4e7 5.482 THPFOS 5.474 WFOS 5.476 THPFOS 5.48 MPFOS 5.507 THPFOS 5.5 THPFOS 5.498 WFOS 5.404 lUPFOS 5.487 THPFOS 5.482 1141140 972009 11W7 1149419 1150191 971562 1143798 11455oM ,I.e,".n"..7,. 963588 lll8533 11W 1129661 1115042 11MW 929428 1392W 1m5d 1290165 1042UM 1189027 1136514 1112285 109039 1119517 025302 1mw2 1103798 1103738 918M 1094801 1093215 llO8623 886016 1076701 108(1295 1114973 1101102 lW8M1 904101 1297195 1309423 1316725 1041110 1163007 1101oQo 1083524 10715d3 1075235 892740 254 PFOS 254 FFQS w PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS - %A. PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS w PFOS 254 ISTDrl3W PFOS 254 IsTD>luI% PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS PFOS 254 PFOS 254 PFOS 2% PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS w PFOS zn PFOS 2% PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS w PFOS 254 PFOS 254 PFOS 254 PFOS w PFOS 5.7 5.713 5.7 5.701 5.692 5.8W 5.698 5.706 5.696 5m 5.891 5684 5.69 5.07 5.884 5.688 5.60 5.691 5.701 5.6M 5.718 5.711 5.708 5.705 5.897 5.898 5.692 5691 5089 5889 5.691 5.8s 5.69 5.670 5.084 5.877 5.876 5.67 5678 5.677 5.879 5.868081 5.891 5.724 5.717 5.715 5.701 5.704 5.699 8 3 7 ~ 0318.52%8 11297958 62U.7308 1Od30182 467.7081 89ZOlW 371.419 11003403 485.0679 14356682 869.5144 18281734 823.9011 1-125 S1.0889 .--. 18715781 972.5325 zi<--,= .*IM . I 0-4- a", 240390 5.337948 6190150 2a.3279 11805872 532.2045 ionwi 491.843 10755750 4M.17W 13780741 873.3741 OW2U 332321 737W16 244.5963 7352450 251.8495 10536384 521.0775 284331 6.217634 83M 5.939702 197941 3.M2167 6080384 245.5533 1ini6 7871924 ~~ 4503593 210.2697 7145884 2981447 8x8381 %0505 7016805 337w2 11534808 697.0305 181WW 870.1489 15234507 841.5557 14183081 713.1438 18427112 1394.184 ZMPBO 5.m.w 5 8 5 ~ 5 1242.332i 27484446 1828.784 2631M68 1743.W ZMo1434 1676.89 2 ~ 4 0 7m2.41 12510860 400.M51 14227W1S08151 450647.783b4S70 18461602 955.5121 786091 21.65781 570479 16.95932 194667 4.0295 5756H8 236.5543 1 3 7 m 46.22885 -3642 252.5315 1038% 90.1% 792% 98.6% 10Bm 96.7% 80.5% 94.4% 4 w 0 BACK TO MAIN 3121101744 D:\ChrmbQurh\ROlOUO.b SAMPLE 51211017-56 D.~hcm\Rush\R01032O.b SAMPLE 3R1101&13 D'\Chem\Rush\R010320.b SAMPLE 3121101827 D.\ChcmV7LnhVN)lO3ZO.b W L E 3 , i i i i i 6.4: D~Gti:;~~.?nrh!.?,\P.n*MXb, SAMPLE 3Rl1018:s O:\Chem\R~sh\R010320.b SAMPLE 31211018.10 D'\ChCmWUlhRO10320b SAMPLE 31211019 24 D \ChsmWushWOl0320b SAMPLE 3R1101819D - ~ ~ u s h l Q O l O SbAMPLE Ml1019:53 D'\Chtm\R~h\RO10320.D SAMPLE MI1011036 D:\Chem\RushROlOM.b SAMPLE 31211011031 D.\ChemlRushVMl03M.b W L E 312110111:05 D:\ChamlRwh\ROl@M.b SAMPLE 3/2110111.19 D:\Chsm\Rush\R010320b SAMPLE 31211011133 D:lChnn\Rurh\R010320.b MMPLE 3121101 11:48 D:~hem\RushU701032O.b SAMPLE 3121101 1202 D:Chrm\Rush\ROlOUO.b SAMPLE M l l O l 12:18 D:Uhcm\Rush\ROl0320.b SAMPLE UZ11011231 D:\Chem\Rush\RO10320.b SAMPLE 3121101 1245 D:\CMm\Rulh\R010320.b SAMPLE 3R1101 13.28 D.~hem\RurrhVN)lO32o.b SAMPLE .3iZ-lMl 1313 D-\Chem\Rur~W01. 0.32b0 SAMPLE 5121/011357 D\Chem\Rumh\ROl0320b SAMPLE M l m l 1411 0 \Chem\Rurh\ROlOMb SNdPLE 3RtDI I 4 zb 0 lChemlQuhlRo103Mb SAMPLE 3RliVl 1440 OUChemWIPhR010320b SAMPLE 3RliUl 1454 D\Chem\RuSh\RO10320b SAMPLE VZllOl 15W D\Cham\Rush\ROlO320b SAMPLE 51211011523 D ~ h ~ \ R u S h ~ O 1 0b3 2 0SAMPLE 3/211011537 D \ChsmWurhR010320b SAMPLE RUSHWO1.D RUSHOW2.D RUSHOOB3.0 RUSH00M.D RUSHWO5.D RUYXI0QB.D RUSHWO7 D RIJSHDW8.D RUSHWS9.D RUSHO1W.D RUSHO103.D RUSH01M.D RUSHOlO5.D RUSHO10B.D RUSWl07D RWO108.D RUSHO1W.D RUSHOl1O.D RUSH0111.0 RUSHO112.D RUSH0115.D RUSHOll6.D RUSH0117.0 RUSHOll1.D WSHOll9.D RUSHO1I.D RUSHO121.D RUSH0121D RUSH0123.D RUSHO124.D 1311417CSY ' 1311-517653 1311-517763 1311.5177M553 1311407US3 ,3.,,.54.7t.s.. 1311.507263 1311-507ZMSS3 5WmL PFDSn UCOH 25OnplmLPFOSnMeOH 1311510653 1311-5107-Y 1311-510bU 1311-5108Ms53 1311-5141Y 1311-514153 1311-51U53 131141UMS-S3 5- PFOS h W 250 WmL PFOS h YSOH 1311-521-3 1311-521563 1311-52lbs3 1311-5218MSS3 1311-517bS3 1311-517ES3 1311-518oS3 1311-5180MSS3 5 WmL PFOS h MEOH 250 npmLPFOShI h O H Roll THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS ms THPFOS THPFOS THPFOS THWOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS mwos THPFOS WFOS THPFOS wws 1WFW THPFOS mwos THPFOS THPFOS THPFOS 54 n 5.48 5.401 5.474 5.46 5.482 5.467 5.46 5.411) 5.4M 5.408 5.471 5.487 5.443 5.479 5.487 5.495 5.4% 5.505 5.494 5.475 5.494 5.495 5.495 5.495 5.489 5 495 5.502 5.507 5.518 594727 ..sa5323 9389 565G 485275 1M3914 1030333 M7518 575234 5757B5 479125 562160 561713 562359 469121 lW716l 98(1753 5..979.Y)~ Mllll 602126 4939a2 980810 W5254 w isrnm% PFOS 254 i s w m % PFOS 254 I S P 7 0 K PFOS 2.5_ 4 ISnX7.0.%.~P. .FO.S. 254 ' 1 s r n < 7 ~PFOS 2% ISW70K PFOS 2~ !~lrrm*PFOS 254 1SlD<70% PFOS 2% PFOS 254 PFOS 254 1sm70% PFOS 254 ISTW7OK PFOS 254 ISlW70% PFOS 2-5.4 lS.m. r7M.L PFOS. 254 ISTLX70K PFOS 254 ISlDC70% PFOS 2% ISlW70% PFOS 254 1Sm70% PFOS 254 PFOS w PFOS 254 ISmC7OX PFOS 254 ISm70% PFOS 254 ISmC70% PFOS 254 ISm<70% PFOS 2% ISm7ML PFOS 254 ismmx PFOS 2% ISlW70% PFOS 254 1SW70% PFOS 254 PFOS 254 PFOS 5.887 5 89 5 871 5.671 5.80 5.892 5.697 5.883 5.705 5.705 5.871 5.895 5.897 5.m3 5.807 5.705 5.705 5.7w 5.729 5.704 5.678 5 e97 5.705 5.705 5.705 58s 5.705 5.712 5.732 5.733 12484311 1436.243 13594800 18720(3 12514644 1471.1i47aiuo 2m.m lBW7M 2244559 209BSBLll 3271.008 21MUMo -3i.245 224W3 5.311072 55711114 235.7W 18483579 2811.823 219w531 3511.765 22W2831 379.179 25723514 6353.82 435951U 12220.39 45427123 12Mll.l 4 0 8 8 8 1 ~10776.50 41017544 14983.72 23695132 3809 243 2431wM 5515.218 tW24.3 d22oM5 13542180 8755.161 15594555 9159.363 i .w i. 3 m.w.e 5 203wO 5030218 5141212 W . l U 1 5 UL INJECTIONVOLUME 5 UL IkECTION WLWE 5 ULINJECTIONVOLUME 5 UL INJECTIONVOcUME 5 UL INJ- ECTIO. NYOCUME 5 UL INJECTIONVOLUME 5 UL INJECTIONVOLUME 5 UL !???ECTIONVOLUME i m2% 95.3% 5 UL INJECTIONVOLUME 5 ULINJECTIONVOWYE 5 ULIMJECTIONVOWME 5 ULINJECTIONVOLUME 5 UL INJECTIONVOLUME 5 UL INJECTIONVOLIJMi 5 ULINJECTIONVOLUME 5 ULINJECTIONVOLUME 157 0% M9U 5 ULINJECTIONWWME 5 UL INJECTIONVOLUME 5 ULINJECTIONVOLUME 5 UL INJECTION VOLUME 2 UL INJECTION VOLUME 2 ULINJECTIONVOLUME 2 UL INJECTION VOLUME 2 UL INJECTIONVOLUME lWI% 93 5% Page3 013 BACK TO MAIN Sample BatchHO1DW.b. anaiyuQ on Hillary C+OW1. PFOSAdswbmson umplrr. Matrix SoivSidSesl. Sundard CUM nngs used iorulibntionol samples: 10-1002ndmL Batchmethod: H010405.m (axt.nul SlandardQuad) 14 Dab mlch - m p m FU. SamphNum Misc 4 m l 12 53 0 @hemWdh#yWOlW5b SAMPLE HILLW16.D 0nMmLPFOSinMaOH 416l01 1308 0 EhamW~Ua#y\HolMob5 CWB-1 HiLLOOl7.D 2.5n#mL PFOSInMeOH 4'clCr *I21 83 LClumWlliaryWOlMO5b CUB-2 HILL0018D 5 r@mL PFOSin MsDH U6M113 36 D EhemVidIaryVIOlM05b CALIB-3 riLL%iS D :C a#m- PFOSmUsOH 1/6/0113 51 DUhemWiliaryWOlMO5b CALIE-4 HILLW20.D 25 WmL PFOS inMLOH 4iBm114 05 DIChemWdaryWOlM05b SAMPLE HILLW21.D 40n#mLPF0SinM10H 4Ki01 14 20 D UhemWdW!HOlMosa CALlE-5 HILLWZ.0 50.1 nphnLPFOSinMeOH 4l6M114 34 D UhcmWlsryWOlMOs b CALIB-6 HILL0023.D 75 1ngmL PFOSinMeOH 4 m l 14 48 DUhemWdlaryWOlMOSb W B - 7 HiLLW24.D 1032n#mL PFOSlnMsOH 4iBml 15 03 OEhemWtUaryVIOlMOSb CUB-8 HILLW25.D 250.5 ndmL PFOSin McOH 446m115 17 D U l n m W d l a ~ O l M 0 5 b SAMPLE HILLW26.D 4w.8 nofmL PFOSfflMsOH 4 I o I 1531 D EhemWtUa#y\HOlM05b CALlB-9 HlLLW27.D 501ngmlPFOSinMsOH 4 0 1 1546 DIChemWdlaryWOlMOSb CALIB-10 HILLW28.D 1W2ngmL PFOSmMsOH 4I7ml4 57 DIChsmWdary!HOlMO5b SAMPLE HILLW83.0 0n#"d. PFOSinUsOH 4nm15 11 DChemWlaryWOlMO5b CALlB-11 HlLUXlMO ZSng/mLPFOSinM&H 417101 5 26 D IChemW~llsryWOlMOSb CALIB-12 HILLW85.D 5 nglmLPFOSinHsOH 417101 5 40 DUhcmWllrryWOlMO5 b CUB-13 HiLL0DBg.D tOn&LPFOShMsOH 4nmi 5 55 D UhemWillaflOlMOs b CALIB-14 HlLLW87.D 25 ngmLPFOSin MoOH 4I7ml6 W 0 EhemWvKiflOlMOs b SAMPLE HlLLOO88.D 40 ndml PFOSinMsOH 4I7lal6 23 D UhemWdlnryVI010405b CAUB-15 HlLLW89.D 50.1 ngrmL PFOSmMeOH 4/7/016 38 D !ChsmWlllaryWOlMOSb CALlE-18 HILLOMM.0 75.1ngmL PFoSmMcOH Mi01652 D!GWmWlUBlyWOlM05b CAlIE-17 HILLW91.D 1W.Z n#mL PFOSinMeOH 4nl01 7 07 DUhemWllaIyW0lM05 b CUB-18 HILLW92.D 250.5 WmLPFOSinMeOH 4nmi 7 21 D \chemWilla#yWOlMo5b SAMPLE HILLOW3.0 400.8 nplmL PFOSinMeOH 401017 35 D EhcmWllsryWOlMo5 b CUB-19 HILLCV94.D M1nprmlPFOSIn MsOH 4n1017 M 0 EhemWcil~ryVIOlMo5b CALIB-20 HlLLOO95.D M1 n#mL PFOSinMoOH Inj Dah Salch -mpTn ). 4WOl 1225 D.UhemW#tlsMlMQ5.b SAMPLE 4 m 1 12.39 D.lChsmW#llrMlMO5.b SAMPLE 4Kml 16.W O.UhemWiaryVIOlMo5.b SAMPLE 41610116.14 O:UhemWlls~W010405b SAMPLE 4m01 1921 D.IChamWillsryVIOlMO5b SAMPLE 4 m 1 1938 D:IChamWillsryWOlMO5.b SAMPLE 44616101 2243 WUhemWilla#yWOlMo5.b SAMPLE 4 0 1 2257 D.UhemWilla#yWOlMO5.b SAMPLE 4nmi 1.50 D.UhemWitlls~OlMob5 SAMPLE 4i7m12M D\ChemUlluyV(010405.b SAMPLE 4nm1428 D.\UMmWlaryWOlMOSb SAMPLE 4Umi 4:43 D:\CChmWUBryWOlMO5.b SAMPLE Wml 8.M O:UhsmWillsryWOlMO5.b SAMPLE 4 m O l 818 D:UhemW~ilaryWOlMo5.b SAMPLE File HILLO014.0 HILLWl5.0 HlLLW29.D HlLL0030.D HlLLWU.0 H1LLWU.D HILLrn7.D HlLLW58.D HiLLW70.D HILLW7l.D HiLLOOII1.D HILL0082.D HILLW%.D HtLLW97.D %mph Nam TN-A 4802 MeOH TN-A4MIZ MsOH TN-A 4802 MsOH TN-A4802 Mdw TN-A 4602 W TN-A4802 MsOH TN-A4802 MsOH TN-AWZ MuJH TN-A4802 MuJH TN-AUIOZ MsOH TN-Am2 MaOH TN-A 4802 MoOH TN-A 4802 MUJH TN-A48CQ MuJH C'. CompovndNlRT Am. THPFOS 5.111 THPFOS 5.121 THPFOS 5.12 THPFOS 5.107 ,nrrOS 5.105 THPFOS 5.121 THPFOS 5119 THPFOS 5.121 THPFOS 5.119 THPFOS 5.112 THPFOS 5.111 THPFOS 5.112 THPFOS 5.113 THPFOS 5.098 THPFOS 5.092 THPFOS 5.098 THPFOS 51 THPFOS 5.106 THPFOS 5.101 THPFOS 5.1 THPFOS 5.101 THPFOS 5.1ffi THPFOS 5.107 THPFOS 5.105 THPFOS 5.104 THPFOS 5.lM Amount 853901 254 880305 254 9W514 254 aueui 2% ai555 zn wsm 2% 905309 254 901966 254 902928 254 921590 254 890229 254 885051 254 sa46 254 909918 2% 9012m 254 907830 254 893968 254 866284 254 854070 254 848217 254 818488 254 BZ4MO 254 839800 254 7955041 254 790146 254 796759 254 CwnpoundNafiT PFOS PFOS PFOS PFOS PFOS pros PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 5.331 5.33 5.324 5.323 5.331 5.33 5.331 5.329 5322 5335 5.322 5.33 0 5.302 5.301 5.31 5.318 5.311 5.31 5.311 5.- 531 5.508 5.314 5.314 Aru Amount 0 0 4194 0 1 1 m 2.152886 189968 8.660505 495541 Z4.6wg2 779774 11.55324 971274 U.01579 1469171 83.12445 1921199 110.8424 4651125 285.888 6791612 432.6167 8184382 532.4149 1467135E 1059.765 0 0 53650 0 95517 1 . 1 W 158439 4.812732 425595 20.52568 875739 35.35248 847857 45.620% 1276693 71.55369 1665685 95.12872 4111457 250.3098 6oM617 377.7554 7263676 466.0545 1 ~ 1 4 7 4m . 2 3 n 1133377 +30%: 610280 -30%: 43% 67% 99% 104% 106% 111% 111% 114% 108% 106% 106% 23% 48% 82% 88% 91% 95% 95% 100% 94% 93% 52x Compound w.RT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS AN 0 0 0 0 0 0 0 0 0 0 0 0 0 0 AWnt 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compovnd NaaT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Ana 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amounl ' 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 BACK TO MAIN I"j Dala Batch SmPTYp. 4/6/01 16:29 D:ChemW~llsrv\HOlMO5.b SAMPLE 4151011643 D:ChamWdnryW01M405.b SAMPLE 4/6/01 1658 D ChemW1Uarv\HolMo5.b SAMPLE y6H)l 17:12 DChsmWilla~WOlMO5.b SAMPLE 4&91 17.26 D !ChemWillarvWO1MO5.b SAMPLE 416m1 17.41 uu;n~m'~;I~-"~"~Ob1a?SoAsMPLE 416101 17.55 D.ChcmWtUaryWolMO5.b SAMPLE 416101 18 W D.ChamWiUaryWOlMO5.b SAMPLE uM)1 18.24 D:~hsmWillaryWO1MiJ5,b SAMPLE 41610118.1 D.ChemWdl~OlMiJ5.b SAMPLE .wemi ia:52 D.ChsmwUaryWOlMOlb SAMPLE 4I66x)I 19:07 D:ChcmWtllarv\HolMD5.b SAMPLE 4,616101 1950 D:ChemWiUaryWOlMW.b SAMPLE 416101 20.M D C h e m W # w W O l ~ . b SAMPLE 41610120:19 D:ChcmWdla~Wo1MW.b SAMPLE 4161012033 O : C h e m ~ U a r y W o l ~ . bSAMPLE 4K1012048 O:ChemWiUsryW01Ma5.b SAMPLE 41610121:02 DChemW~llsrv\HOlMO5.b SAMPLE 416101 21:16 DChemWill~~WOlMOb5 SAMPLE 416101 21.31 D.ChsmWillaryWO1MO5.b SAMPLE 416101 21:45 D.ChamWillawWOlMO5.b SAMPLE 416101 2159 D.ChsmWdswWOlMO5.b SAMPLE UMH 2214 D ChemWillawWOlMa5.b SAMPLE m o i 22.28 D:CbmWdla~WOlW5.b SAMPLE UMIl 23.11 D:\Ch~mWillaryWOlMO5.b SAMPLE vM)l 23:26 WChemWillwWOlMO5.b SAMPLE UFJOl 2340 D.ChcmWillawUiOlMO5.b SAMPLE 41610123'55 D:ChsmWillawWOlMO5.b SAMPLE 4/7/010:09 DChsm~dlarv\HOlMO5.b SAMPLE 4nmi 0.23 D.ChsmWillaryWOlMO5.b SAMPLE tffm10:1 D.ChemWillaryWOlMO5.b SAMPLE 4nm1 0.52 D:ChsmW~llarv\HOlMO5.b SAMPLE 4ffm1 1.07 DChemWillarv\HOlMO5.b SAMPLE m m 1 121 D:ChemWillarv\HOlMO5b SAJJPLE 4nmi 1:s D:ChamWdIarv\HOlMOSb SAMPLE m m i 2:ig D:ChemW~llarv\HolMo5b SAMPLE 4/7/012'33 D:lChemUiillaryWOlMO5b SAMPLE 4nmi 2:47 D:\ChemWillaryWOlMO5.b SAMPLE m m i 3.02 D:ChemUiillaryUrOlMO5.b SAMPLE 4nlol 3.16 D:\ChemWill~OlMO5.b SAMPLE 4nmi 3:31 D:\ChsmWiUuv\nolMO5.b SAMPLE 4nmi 3;45 D.ChsmUiiUaWHOlMO5.b SAMPLE 4nml 359 D:\ChemWiUawYK)lMO5.b SAMPLE 4nml4:14 D:ChemW1U~W01M05.b SAMPLE Fila S.mpkNamm Mac Info HILL0031D 2mgllPFOSSludyNumbarEW-1311 1311-5M?-Sl HILL0032D 2r& PFOSStudyNumber001311 1311-5M+Sl H I L m 3D ZmplLPFOSStudyNumbar EW-1311 1311-504551 HILL0031.D 2r& PFOSStudy Numbar EW-1311 1311-5045MSSl HILL0035.D lomplLPFOSStudy Numbar EM1311 1311-504951 HiUW1.D 1OmprLPFOSSiudiNumLw Em1311 1311-505asl HILLoO37.D 1- HlUW38.D lo& F i G S i U . + j k 7 k r E-I311 1311-505151 PFOS Stvdy Numbar EW-1311 1311-5IHIMSSl HILL0039 D 2w PFOS Sludy Elumbar EW-1311 1311-5079.S1 HILWM0.D 2n@PFOSS~NUmbaEWl311 1311-5080Sl HILLOM1.D 5n#mLPFOSinMEOH HILLOM2.D 250.5 n@nL PFOSfflMeOH HlL~W45.0 2mpn PFOSSbrdyNumberEW-1311 i 3 i i . ~ a i - s i HlLLW46.D 2mWL PFOS S(udyNhlNumbsrEW-1311 1311-5MIlMSSl HILLW47.D 1hQJLPFOSSbrdyWrEW-1311 1311-M85-S1 lw HILL0048.D lDm~PFOSSlUdyNvmberELW1311 1311-5086Sl HILLCC49.D PFOS Sludy Number Em1311 1311-%8731 HILLW5O.D lOmqLPFOSSludyNumberEMl311 1311-5M17MSSl HILLW5l.D OqJLPFOSStudyNurnbar EW-1311 1311-509131 HlLLW52.D OnWPFOS StudyNumbsrEW-1311 1311-5Os251 HILLOO53.D OmfiPFDs Study Numkr EM1311 131l-Mg3-Sl HlLLOo54.D CnqRPFOSStudy Number EW-1311 1311-5093MSS1 HILLOo55.D 5 nprrnL PFOS In MeOH HIUWM.0 250.5 n#mL PFOSin MeOH HIUW59 D 1OmplLPFOSSW Number EW-1311 1311412151 HILLCWJD 10~PFOSSWNumberEW-1311 1311412251 HILL006l.D lhnonPFOSShdyNumbsrEM1311 1311412351 HILLW62.D l O ~ P F O S S ~ d y N u m t u E M 1 3 1113114123MSSl HILLW63D lL%n@lPFOSSbdy Numbar EW-1311 1311415751 H1LLWM.D I W L P F O SSudy NumbsrEM1311 1311-515651 HILL0065.D I h w l P F O S Study NvmMr EM1311 1311-515p51 HILL0066.D lL%n@lPFOS Sbdy NumWr EM1311 1311-5159MSS1 HILL0067.D PFOSStudy NumbsrEW-I311 i ~ i i - s i a i - s i HiLLW6a.D 5 n # PF~OSin MaOH HILL0069.D 250.5 nprmLPFOSin MeOH HILL0072.D ~ L P F O W S NumbaEW-1311 131i-5iaz-si HILL0373D W L P F O S W Numbar EOC-1311 1311.5ia~si HILwo74.D ~ P F O s S h dNyumbarEW-1311 1311-5183MSS1 HILLW75D cm#l PFOSSudy NumberEM1311 1311-5199.51 HILLW76.D CmglPFOSSudy Numhsr EW-1311 1311-5200Sl nlLL0077.D ~PFOsS~dy NumkrEW-1311 1311-520151 HlLL007a.D Om& PFOSSWy Nwnb.rEW-1311 1311-5201MS-S HILL0079.D 5 ngImlPFOSnMeDH H1LLWWI.D 250.5nplmLPfOSin MeOH compound Ndl THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFUS THPFOS MPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.112 5.12 5.113 5.112 5.106 5.115 5.1W ac ., "=I 5.112 5.111 5 113 5 116 5.112 5.118 5.1W 5.112 5.1ffi 5 112 5.114 5.109 5.104 5.wa 5.112 5.098 5.105 5.107 5.105 5.105 5.111 5.105 5.1 5.105 5.098 5.1 5.102 5.097 5Wl 5.091 5.w4 5.092 0 0 5.W5 5.Wl 6452% 691267 a95iu 904138 908952 745233 uosn 643447 941520 937852429 686430 911967 91951 gisffia 732339 864599 BUS92 a9811 672064 860662 872477 W71 808820 a09437 646037 853122 8WI 854113 700905 i2aiyB 999732 918425 12a23ni i2awo 1122340 1275724 12954% 0 0 1122048 i0514oa lunt compound h e r Am Amt 254 PFOS 5.329 1594W4 8079793 254 PFOS 5.33 1011663 5544188 254 PFOS 5.323 1801969 1034959 254 PFOS 5.322 4370912 267.3979 254 PFOS 5.323 789270 42.1201 254 PFOS 5.333 986788 53.91793 254 PFOS 5.326 73w34 38.58667 254 PFOS 5.322 s a s i 2w.44~ 254 WUS 5.32? 1692254 96.75814 254 PFOS 5.321 2112598 122.6887 254 PFOS 5.323 11~7702.13wa 254 PFOS 5.328 459noa 282.43s 254 PFOS 5.329 16195U 92.30717 254 PFOS 5.328 409113 249.139 254 PFOS 5.3ia iwi7ffi ~ ~ a i a 254 PFOS 5.322 998187 5451181 254 PFOS 5323 254 PFOS 5.323 254 PFOS 5.324 254 PFOS 5319 254 PFOS 5.322 254 PFOS 5315 254 PFOS 5.322 254 PFOS 5.315 254 PFOS 5.322 2% PFOS 5.317 254 PFOS 5.322 254 PFOS 5.323 254 PFOS 5.322 254 PFOS 5.315 254 PFOS 5.31 254 PFOS 5.315 254 ISTc1130% PFOS 2% PFOS 5.308 5.31 . . .. 254 PFOS 5.312 4298803 2526356 254 ISTD>13w( PFOS 5.307 144727 4.W- 254 ISTD,130% PFOS 0 254 PFOS 5.301 254 lSTD>l3M( PFOS 0 254 ISTD>lMX PFOS 0 0 IST[h70% PFOS 0 0 ISTB7W PFDS 52% 254 PFOS 5.295 254 PFOS 5.m w 0 . . BACK TO MAIN s" n v c d n Sampk Batch H010402.b. analyzed on Hillary 044241. PFOSAdrorb/DaroIb samples Matrix: SOiUSlplS~. 5.0 fac i&&ro, Standad C U N ~nnae used forCallbmtlonof samnbs: ~ m 0 0 2dni~ Bdsh method Ho10402.m Inj Dab Batch SampType File SBmplS Nuno 4N01 12.30 D.\ChemWillatyW010402.b SAMPLE HlLLW16.D 0 ng'mL PFOS in MeOH 412101 12 51 D.\ChemWiIdawW010402.b CALI6 1 HlLLW17.D 2.5 ndmL PFOSin MeOH 41.0~71305 D Cka,~*<Ih-,?UClMn2 b CAUB-2 rllLLOO10 D 5 ngmL PFOS In MeOH mol 1320 D \ChemWdlaryW01M02b CALIB-3 HILLW19D 10ngImL F F S (13 4/2/01 1334 D \ChemWdIaryWO10402b CALIB-4 HlLLW20D 25 ng"PFOS ln MeOH 4/2/01 1340 D \ChemWdliuyW010402b SAMPLE HlLLW21D 4 0 nglmL PFOSin MeOH 4 / m l 14 03 D \ChemWaryW010402b CALIB-5 HlLLWZZ D 50 InWmLPFOSIn MeOH 4/2/01 14 17 D \ChemWillaryW010402 b CAUB-6 HILL0023D 75 1n W L PFOS m MeOH 4N01 14 32 D ChemWillaryWOlM02b CAUB-7 HILL0024D 1W2 nglmLPFOS in MeOH 4/2/01 1446 D \ChemWdlaryWOlMOZb CAUB-8 HILL0025D 250 5 nglmtPFOSm MeOH 4/2/01 15W D \WemVldaryW010402b SAMPLE HILLW26 D 400 0 nglmL PFOSinMBOH 4/2/01 15 15 D \ChemWllaryW010402b CAUB-9 HILLW27 D 501n@mLPFOSin MeOH 4/2/01 1529 D \ChemW1llaryW010402b CALIB-10 HILL0020D iW2 nglnltPFOS inMeOH 4131013 14 D\ulemWflaryWOlO4W b SAMPLE H I U 7 7 D 0 n@mLPFOSin MeOH 4131013 20 D \ChamW1aaryWOIMO2b CALIB-11 HlLLW78D 2 5 nglmLPFOS in MeOH 4/31013 43 D \ChemWBaryW010402b CALIB-12 HILLW79 D 5 ngmL PFOS m MeOH 413m13 57 D \ChemWdlaryWOlMO2 b CALIB-13 HILL0080 D 10n g h L F'FOS m MeOH 4/3/014 I1D ChemWWaryW010402b CALIB-14 HILLW81D 25 nglmLPFOS in MeOH 413m14 26 D \ChemWdlaryW0104D2b SAMPLE HILLWE2D 40 ngmL PFOS in MeOH 4/31014 40 D \ChemWdlaIydiO10402b CALIB-15 HILL0083 D Y) 1 nglmL PFOS In MeOH 419314 54 D \ChemWillaryW010402b CALIB-16 HILL0084 D 75 1nQ/mL PFOSVI MeOH 4131015 09 D \ChemWllaryW010402b CALIB-17 HILL0085D 1W2 nglmLPFOS In MeDH 4/yo15 23 D \ChemWluaryul010402 b CALIB-18 HILLCUE8D 250 5 nglmLPFOS m MeOH 4/3/01 5 38 D ChemU.(lIaryWO10402b SAMPLE HILL0087D 4028 nUmLPFOS in MeOH 413101 5 52 D \ChemWllalyW010402 b CALIB-19 HILL0088 D 501 n@mt PFOS in MeOH 4131010 06 D \ChemWdlaryW010402b CAUB-20 HILL0089 D 1032 nglmt PFOSin MeOH Misc InfCompound THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS MPFOS THPFOS THPFOS THPFOS NaRT Ana Amount 5104 884438 254 5099 891647 254 5105 073155 254 5099 914977 254 5105 941733 i54 5107 960037 254 5104 936141 254 5115 916274 254 5114 94oMu 254 5 107 893340 254 5112 922772 254 5 111 980724 254 5105 893327 254 5108 1211076 254 5105 1169631 254 5100 1115864 254 5097 1128520 254 5105 1132730 254 5104 1144180 254 5112 1008719 254 5105 1050910 254 5107 1034815 254 5105 989240 254 5105 988215 254 5106 1060023 254 5107 928330 254 Avenae 999239.808 Std BY1:02082.113 W S D : 10.2% InJDate Fhtch 41210112 00 D ChemWdlaryW010402b 412101 12 22 D \ChemUi~lla~O1040b2 m o l 1543 D \ChemwlIarywO10402 b 412101 I 5 58 D\ChemW1llaryW010402b 412m1 10 12 D \ChemWllaryWO10402 b 412101 19 19 D IChemWdiary\H010402b 4 m 1 1933 D Chem!4iilwW010402 b 4N0121 14 D ChemWillaryW010402b 4 m 1 21 28 D \ChemWlIaryW010402b 4121012157 0 ChamHdIaryWlM02 b 4 m 1 2 2 20 D iGhem!HiIlaryW010402 b 4/2/0122 54 D\ChemWdlaryWOlMO2b 412101 23 23 D \ChemUidlaryW010402 b 4 1 2 ~ 123 52 D ChemW~llaryW01040b2 4/3/01021 D \ChemWllaryWOIMOZ b 413m1 0 50 0 \ChemWhyWO10402b 4/33 119 D \ChemWdlaryWOlM02b 4 m 1 1 47 D ChemW1IlaryW010402b 4 m 1 2 45 D EhemWlaryWO1MOZb 4/3/01 2 59 D \ChemWdlaryW010402b 413101 6 21 D ChemWiUaryW010402 b 413J01035 D \ChemWllaryW010402b SampTyps SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE Fib HlLLWl4 D HILLW15 D HILLW29 D HlLLOO3O.D HILLW31 D HILLW44 D HlLLW45.D HILLW52.D HILLW53.D HILL0055.D HlLLW57.D HILL0059.D HILLW3l.D HILLWB3.D HILLW65.D HILLW67.D HlLLW69.D HILLW71.D HlLLW75.D HILLW76.D HlLLO09Q.D HILLW9I.D Sampk Name TN-A 4802 MeDH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MnOH TN-A 48M MeOH TN-A 4802 MeOH TN-A 4802 MeOH TT-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4tA2 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Miso InfCompoundNaRl THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS rnPF0S THPFOS THPFOS THPFOS THPFOS THPFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 C o m w u n o 1NJ31AT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS An. Amount 0 0 0 5323 76123 2937764 5322 112527 4927384 5323 219535 I002044 5329 564068 2 7 W 3 9 5 331 90- 42 62353 5335 1124594 54-8 5 332 1641678 83 18952 5331 2175779 108093 5 331 4790973 286 3wB 5338 7485094 4198087 5328 9634440 5170107 5.329 15519974 1025.7 0 0 0 5.322 76339 2019f59 5325 108809 3492407 5 321 209068 7 510677 5322 565907 22W294 5 329 929330 30 56921 5330 1114120 4049134 5 322 1638985 71 91555 5331 2152910 972404 5329 4767507 2420323 5329 7513403 3905142 533 9712588 4815275 5 331 15404980 975 7589 1299012 +30%: ggs4ga -30%: 99% 100% 110% 107% 110% 111% 103% 102% 70% 75% 88% 91% 93% a96% 99~77%..u_ 4'74, 96% 97% Compound N a A T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5405 0 5.406 542 0 0 0 0 C 0 0 0 0 0 0 0 0 0 0 0 5.425 0 Ama Amount 18449 0 0 0 33972 0 11581 0 0 0 0 0 0 0 0 0 O O 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 38059 0 0 0 page 1of 2 BACK TO MAIN In1 Data Blkh 4/2/011626 D ChEmW!UaryMlO4a2b 4/2/011641 D ChemW~1UaryWO1M0b2 4/2/01 1655 D ChemWaryV1010402b 4No1 17 09 D ChemWillalyWOlMO2b 4/2/011724 D ChemUillaryW010402b 41W1 1738 D ChsmWdaryWO10402b 4/2/01 17 53 D IChsmWllaryW010402 b 412101 18 07 DChemWdlaryW010402 b 4/2/01 1821 D ChemWoUaryW01M02b 4No1 I 8 36 D ChemWilIaryW010402b 4/2/0118 50 D ChernwtaaryWOimb 4m01 1904 D ChemUi1llaryWO10402b 412101 1948 D ChemWllaryW010402b 4/2/0120 02 D ChemWlaryW010402 b 4n/0120 16 D iChemWlaryWOlM02 b 4/2/0120 31 D ChemWdlaryW010402b 4No120 45 D \ChemWlla~W010402b 41210120 59 D \ChemW1llaryWOl04OZb 4 m 1 21 43 D ChemWdlaryWOIMOZb 4/2/0122 11 D ChemUillaryW010402b 4/2/0122 40 D ChemUillaryWO104OZ b 4No123 09 D ChemWdlaryWOl0402b 4/2/01 23 38 D ChemUilllaryWOlMOZ b 4TJxH 0 06 DChemWdlaW10402 b 413/01035 D \ChemWdlaryW010402b 4/3/01 104 D ChemWdlaryWO1C402b 4No1 133 D ChemWllaryWO10402b 4/3R12 02 D ChemWdlaryW010402b 413/012 16 D ChemUillaryW010402b 4/5/012 31 D ChernW!~la~Oro4obz SampTyp SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE Fb HILLD032D HlLLW33D HIUW34.D HILLW35.D HILL0036.D HILLW37.D HlLW038.D HILLW39.D HlUW40.D HIUW4I.D HILLW42.D HILLW43.D H1110046.D HlLLW47.D HlLLW48.D HILLW49.D HlU0050.D HILLW51.D HILLW54.D HILLWSB.0 HILL0058.D H1LLWMI.D HlLLCC62.D HlUW64.D HILL006B.D HlLLW68.D HILLW7O.D HILLW72.D HILLW73.D HILLW74.D Sample Name 2mglL PFOS Sludy Num~cE001311 ZmUL PFOS Study Number E001311 5mplL PFOS Study Number E00131f %I&PFOSSLudy NumberECC-1311 Sm#l PFOS Study Number E001311 5mg.k PFOS Study NumberE001311 1CmgAPFOS StudyNumberE001311 n@or.l PFOS Stwly Nomber E001311 I h g A PFOS Study Number E001311 1OmplLPFOS Shdy Number E001311 5 nglmL PFOS in MeOH 250 5 ndmL PFOS in MmH SOmplL PFOS Study Number E001311 MrnplLPFOS Study Number E001311 SOmplL PFOS Study Number E001311 5CmdLPFOSStudyNumberE001311 5 ndmL PFOS m MeOH 250 5 nUmL PFOSin MeOH ompnPFDSStudyNumberE001311 O W L PFOS StudyNumberE00131I Om& PFOS Study Number E00-1311 Cm& PFOS Study Number E001311 om& PFOS Study Number E001311 Cm& PFOS Shldy Numixr E001311 OmplL PFOS Study Number E001311 CmgL PFOS Study Number E001311 5mplLPFOS Study Number 00-1311 5- PFOS Study Number E001331 5 WmL PFOS111 MeOH 250 5 WmL PFOSn M a O H Misc InfCompoundNaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.115 5.112 5.119 5.134 5.121 5.119 5.120 5.127 5.12 5.125 5.127 5.127 5.133 5.133 5.127 5 128 5.128 5 119 5 112 5.111 5.107 5039 5.108 5.098 5.097 5.098 5.098 5 105 5.105 5.088 Area Amount 1089043 254 840525 254 1140615 254 1121827 254 1105% 254 914972 254 1092485 254 1128533 254 1141778 254 912742 254 929W4 254 875517 254 1181781 254 1078087 254 1116896 254 951406 254 924450 254 875538 254 1559964 254 1545380 254 1539293 254 1521208 254 I584873 254 1594416 254 1612740 254 1582196 254 1615581 254 1590591 254 1403089 254 1313803 254 ISTD>IM% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>IM% ISTD>130% ISTD>l3O% ISTD>1M% lSTD1130% ISTD>130% ISTD>I30% Compuna ku#T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS .i=z &mcwi 5.339 91788 2852832 5336 3307825 1904263 5338 250070 9070036 5358 255801 9465038 5 345 202135 7 399684 5343 3416478 1800553 535 415060 164674 5351 524864 2040436 5351 516752 1982583 5 349 3833223 204 1541 5 351 115805 4 724463 94 5% 5 344 4809365 272 8592 1089% 535 2608914 1053019 5 35 2143323 92 71704 5351 1984759 824808 5353 4992173 2595911 5345 121763 505741 101 1% 5 343 4808081 272 7724 108 9% 0 0 0 0 0 0 0 0 0 5324 3196100 982237 0 0 0 0 0 0 0 0 0 5 329 3075504 90 56478 0 0 0 0 0 0 532s l o o a n 2 3 2 1 9 ~ 1 46 4% 5 322 4689812 1716327 68.5% page20f2 BACK TO MAIN Sample Batch R010329b.b. analyzed on Rush 03-2941. PFOS Adiorbl[)esofb Samples. Matrix: SoiVSlglSed. Standard cuwe range used for calibration of samples: 5-501 ng/mL (2.5 ng/mL std not included due to the hlgher sample concentration range), Batch m e t h o d R010329.m lnj Date Batch SampType File Sample Name Misc Info Compound N a S T Area Amount Compound N3T Area Amount - 3130101 1444 D:\ChemViush\ROl0329.b SAMPLE RUSHOIM.D 0 ndmL PFOS in MeOH THPFOS 5.574 E45852 254 PFOS 0 0 D h 3/30/01 1458 D:\Chem\Rush\Rolo320.b CALIE-7 RUSHCllnS 0 2.5 h m L PFOS in MeOH THPFOS 5.561 650507 254 PFOS 5.771 234324 2.803619 3130/01 1 5 13 O:\Chem\Rush~Ol0329.b CALiE-2 RUSHO1OG.D 5 ng1mL PFOS in MeOH rhrrvu 5.v 805498 254 PFOS 5.78 259067 4.511131 90.2% 3/30/01 1527 D\ChemViush\R010329.b CALIE-3 RUSH0107.D 1 0 ng/mL PFOS in MeOH THPFOS 5.574 844287 254 PFOS 5 . i i 8 2?2K!4 %%E22 89.8% 3/30/01 1541 O;\Chem\Rush\R010329.b CALIE-4 RUSHOlO8.0 25 ng/mL PFOS in MeOH THPFOS 5.574 874761 254 PFOS 5.777 7506t7 25.05443 100.2% 3130101 15% D:\Chem\Rush\R010329.b CALIB-5 RUSHOID9.0 4 0 ng1mL PFOS in MeOH THPFOS 5.575 874280 254 PFOS 5.778 1074369 39.99818 99.7% 3/30/01 16:lO D:\ChemlRush\R010329.b CALIB-6 RUSH0110.0 50.1 n g h L PFOS in MeOH THPFOS 5.575 856450 254 PFOS 5.778 1261642 50.16737 100.1% 3130101 16:25 D:\ChemViush\RO10329.b CALIB-7 RUSHO111.0 75.1 ng1mL PFOS in MeOH THPFOS 5.562 857550 254 PFOS 5.765 1770429 75.8725 101.0% 3/30/01 1639 D:\ChemWush\R010329.b CALIB-8 RUSH0112.0 100.2 n#mL PFOS in MeOH THPFOS 5.568 863358 254 PFOS 5.771 2201517 96.11491 97.9% 3/30/01 16.53 O:\Chem~ush~O10329.b CALIB-9 RUSHO113.0 250.5 ng/mL PFOS in MeOH THPFOS 5.576 806157 254 PFOS 5.789 4379739 251.4603 100.4% 3/30101 I T 0 8 O:Ghem\Rush\R010329.b SAMPLE RUSH0114.0 400.8 n g h L PFOS in MeOH THPFOS 5.574 858200 254 PFOS 5.777 6738788 406.2194 3/30/01 17:22 D:\Chem\Rush\RDl0329.b CALIE-IO RUSH0115.0 501 n g h L PFOS in MeOH THPFOS 5.57 909424 254 PFOS 5.773 8394525 508.9853 101.6% 3130101 17% D:\Chem\Rush\R010329.b SAMPLE RUSH0116.0 1002 ng/mL PFOS in MeOH THPFOS 5.568 813760 254 PFOS 5.778 12942478 1114.479 3/31/01 10:24 O:\Chem\Rush\RO10329.b SAMPLE RUSH0188.0 0 ng/mL PFOS in MeOH THPFOS 5.52 760278 254 PFOS 0 0 0 3/31/01 1038 D:\Chem\Rush\R010329.b CALIB-I1 ~ U s ~ o 1 8 7 .2D.5 right PFOS in MeOH THPFOS 5.534 761291 254 PFOS 5.744 222040 3.400639 3/31/01 1053 D:\Chem\Rush\RD10329.b CALIE-12 RUSH0188.0 5 ng/mL PFOS in MeOH THPFOS 5.517 731965 254 PFOS 5.727 254163 5.463481 109.3% 3/31/01 11:07 D;\Chem\Rush\R010329.b CALIB-13 RUSH0189.D 10ng/mL PFOS inMeDH THPFOS 5.515 771260 254 PFOS 5.725 358164 9.856814 98.6% 3/31/01 H:21 D\Chem\Rush\RO10329.b CALIB-14 RUSHO190.0 25 nglrnL PFOS in MeOH THPFOS 5.511 764462 254 PFOS 5.721 666714 25.61491 102.5% 3/31/01 1136 D:\ChemRush\R010329.b CALlB-I5 RUSH0191.D 40 na/mL PFOS in MeOH THPFOS 5.517 769541 254 PFOS 5.727 980488 40.53221 101.1% 3/31/01 1150 D:\Chem\Rush\R010329.b CALlE-I6 RUSH0192.D 50.1 n g h L PFOS in MeOH THPFOS 5.524 769770 254 PFOS 5.734 1138148 50.39724 100.8% 3/31/01 12:W D:\Chem\Rush\ROl0329.b CALIB-17 RUSH0193.0 75.1 n@mLPFOS in MeOH THPFOS 5.517 764856 254 PFOS 5.727 1583158 76.11235 101 3% 3/31/01 1219 D:\Chem\Rush\R010329.b CALIE-18 RUSH0194.0 100.2 ndmL PFOS in MeOH THPFOS 5.526 787147 254 PFOS 5.729 2037660 99.93338 59.7% 3/31/01 I 2 3 3 D:\Chem\Rush\R010329.b CALlB-I9 RUSHD195.D 250.5 ng/mL PFOS In MeOH THPFOS 5.519 733588 254 PFOS 5.729 3963988 249.7285 W.7% 3/31/01 12:48 D:\Chem\Rush\R010329.b SAMPLE RUSH0196.D 400.8 nQ/mLPFOS in MeOH THPFOS 5.522 775073 254 PFOS 5.733 6072032 406.9537 3/31/01 1302 D:\Chem\Rush\R010329.b CALIE-20 RUSH0197.D 501 n#mL PFOS in MeOH THPFOS 5.525 827129 254 PFOS 5.728 7615022 507.1578 101.2% 3/31/01 1316 D.\Chem\Rush\R010329.b SAMPLE RUSHOl98.D 1002 ng/mL PFOS in MeOH THPFOS 5.525 744097 254 PFOS 5.728 11828629 1113.673 Averaoe: 809251.5 Std Dev: 50097.37 HRSD: 6.2% 1052027 +3D%. 568478 -30%: 73 Iu M (D VI VI page 1 of 4 BACK TO MAIN Sample Batch R010329b.b. analyzed on Rush 03-20-01. PFOS AdsorbfDesorb samples. Matrix: SoiVSlg/Sed. Standard curve range used for calibration of samples: 5-501 nghL (2.5 nglmL std not included due t o the higher sample concentration range). Balch m e t h o d R01032S.m lni Data Batch SampType 1nj Data Batch SampTyp. 3%&! !A15 ~-\Chem'~ushiRO10329.bSAMPLE 3/30/01 1429 D:\ChemRush\R010329.b SAMPLE 3/30/01 1751 D:\Chem\Rush\R010329.b SAMPLE 3130101 l8:05 O:\Chem\Rush\R010329.b SAMPLE 3/30/01 1820 D:\Chem\Rush\R010329.b SAMPLE 3130/01 21 27 0 \Chem\Rush\R010329 D SAMPLE 313M)l 21 41 D \Chem\Rurh\R010329b SAMPLE 3/31/01 0 4 8 D:\Chem\Rush\R010329.b SAMPLE 3i31/01 1:03 D:\Chem\RushW010329.b SAMPLE 3/31/014 1 0 D:\ChemU7ush\R010329.b SAMPLE 3/31/01 4 2 4 D:\ChemWush\R010329.b SAMPLE 3/31/017 3 1 D:\Chem\Rush\R010329.b SAMPLE 3/31/017 4 6 D:\Chem\Rush\R010329.b SAMPLE 3/31/019:41 D:\ChemWush\R010329.b SAMPLE 3/31H)1955 D:\Chem\Rush\RO10329.b SAMPLE 3/31/01 1009 O:\Chem\RushlR010329.b M M P L E 3/31/01 1 3 3 1 O\Chem\Rush\RO10329.b SAMPLE File Sample Name File Sample Name RUSHOIOZ.D TN-A 4802 MeOH KLISHC8iGS.D :?!-A 4BC2 MPOH RUSH0117.D TN-A 4802 MeOH RUSH0118.D TbA480.2 MeOH RUSH0119.D TN-A 4802 MeOH RUSH0132 D TN.A 4802 MeOH RUSH01330 TN-A4802 MeOH RUSH0146.D TN-A 4802 MeOH RUSH0147.D TN-A 4802 MeOH RUSH0160.D TN-A4802 MeOH RUSHO181.D TN-A4802 MeOH RUSH0174.D TN-A 4802 MeOH RUSH0175.D TN-A 4802 MeOH RUSHO183.D TNA4802 MeOH RUSH0164D TNA4802 MeOH RUSHO185.D TN-A 4802 MeOH RUSH0199.D TN-A 4802 MeOH Misc Info Compound N a A T M i c info Compound N a A T THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amwnt Amount 0 0 0 0 0 " 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 CompoundNIT Compound ERT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area Amount Ana Amount 5.792 144070 0 5.789 136863 0 5.798 170024 0 5.793 144025 lj 5.797 138657 0 5.758 145074 0 5.769 139112 0 5.781 142482 0 5.788 134617 0 5.764 139821 0 5.765 133049 0 5.749 142142 0 5.738 136409 0 5.749 147797 0 5.749 139494 0 5.737 140062 0 5.756 174751 0 0 -h page 2 of 4 BACK TO MAIN Sample Batch R010329b.b. analyzed on Rush 01-29-01. PFOS AdsorblDesorbsamples. Matrix: SoiUSlgiSed. Standard cutve range used for calibration of samples: 5-501 nglmL (2.5 nglmL s l d n o t included due to the higher r a m p i e concentration range). Batch method: R010329.m inj Date Batch S a wT y p lnj Date Batch SampTyp 3/30/01 18-34 D:\Chem\Rush\R010329.b SAMPLE 3/30/01 18:48 D:!CnemuiushU?OiD3229.C S.A%PLE 3/30/01 1903 D:\Chem\Rush\R010329.b SAMPLE 3/30/01 19:17 D:\Chem\Rush\R010329.b SAMPLE 3/30/01 1932 D\ChemRush\R010329.b SAMPLE 3/30/01 19:46 O:\Chem\Rush~010329.b SAMPLE 3?i.Ob31 2000 D:\ChemViush\R010329.b SAMPLE W 0 1 2015 D:\ChemRush\R010329.b SAMPLE 3/30/01 20:29 D:\Chem\RushRO10329.b SAMPLE 3/30/01 2043 D:\ChemRush\R010329.b SAMPLE 3/30/0120:58 O:\Chem\Rush\R010329.b SAMPLE 3i3OX)l 21:12 O:\Chem\Rush\ROlO329.b SAMPLE 3/3wD121:55 D\Chem\RushW010329.b SAMPLE 3/30/01 2210 O:\Chem\Rush\R010329.b SAMPLE 3/30/01 2224 D \ C h e m ~ u s h ~ O l 0 3 2 9 . bSAMPLE 3/30/01 2239 O:\Chem\Rush\R010329.b SAMPLE W M 1 2253 O:\ChemIRush\R010329.b SAMPLE 3/30/01 2307 D:\Chem\RushW010329.b SAMPLE 3L30/01 23:22 D:\Chem\Rush\R010329.b SAMPLE 3/30/01 2336 O:\Chern\Rush\R010329.b SAMPLE 3/30/01 2351 D:\ChemRush\R010329.b SAMPLE 3131101 0:05 D:\ChemRush\R010329.b SAMPLE 3/31/01020 O:\Chem\Rush\R010329.b SAMPLE 3/31/01 0 3 4 O:\Chem\RushW10329.b SAMPLE File Sample Name File Sample Name RUSH0120.D Study Number E001311 RLISHO121.D Study Number E001311 RUSH0122.D Study Number E001311 RUSH0123.D Study Number E001311 RUSH0124 D StudyNumberE001311 RUSH0125.0 Sludy NumberE001311 RUSH0126.D Study Number E001311 RUSH0127.D Study Number E001311 RUSH0128.D Study Number E001311 RUSH0129.0 Sludy Number E001311 RUSH0130.D 5 ng/mL PFOS in MeOH RUSH0131.D 250.5 ng/mL PFOS in MeOH RUSH0134.0 Study NumberEOO-1311 RUSH0135.D Study NumberEW-1311 RUSHO136.D Study Number EOO-1311 RUSH0137.D Study Number EOC-1311 RUSHO138.D Study Number EBO-1311 RUSH0139.0 Study Number E001311 RUSH0140.D Study Number E001311 RUSHO141.D Study Number E001311 RUSH0142.D Study Number E001311 RUSH0143.D Study Number E001311 RUSHO144.D 5 ng/mL PFOS in MeOH RUSH0145.D 250.5 ng/mL PFOS in MBOH Misc Info Misc Info Compound NalRT Compound NarAT THPFOS -.THPFOS 4 nrrva THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Amount Area Amount 5.574 700662 254 5.565 880404 254 5.569 El20419 254 5.57 821252 254 5.579 673700 254 5.573 843531 254 5.568 821307 254 5.56 824221 254 5.554 655636 254 5.551 814171 254 5.547 794288 254 5.553 791691 254 5.562 835122 254 5.571 804691 254 5.57 644452 254 5.567 873023 254 5.567 887648 254 5.58 926167 254 5.561 758299 254 5.568 824449 254 5.574 804828 254 5.567 789160 254 5.57 774516 254 5.568 788822 254 c= Compound tRT Compound t R T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area Amount Area Amount 5.777 3839014 254.22 5.769 2916166 135.13 5.779 2814668 141.11 5.161 iei623 :42.97 6.789 5475251 427.65 5.776 1878094 83.18 5.779 1731214 77.82 5.763 1739800 77.95 5.75 4384199 329.52 5.755 3390903 179.53 5.757 258302 4.64 5.7% 4310524 252.17 5.765 3594706 187.10 5.774 3233585 171.68 5.773 5569928 465.00 5.77 2263901 101.23 5.77 2361032 103.30 5.763 2579566 109.27 5.764 5414508 359 43 0 0 0.00 5.784 203794 I.98 0 0 0.00 5.78 250673 4.59 5.771 4205216 253.74 92.9% 100.7% 91.7% 101.3% 0 -h -4 w 0 page 3 of 4 BACK TO MAIN Sample Batch R010329b.b. analyzed on Rush 03-29-01. PFOSAdsorbKksOrbSamplES. Matrix: SoivSlglSad. Standard c u w e range usedfor calibration of samples: 5-501 ng/mL (2.5 ng/mL rtd not included dueto the higher sample conceptration range). Batch m e t h o d R010329.m Inj Date Batch 3/31/01 1:17 D:\Chem\Rush\R010329.b 3/31/01 1 3 2 D:\ChefN?ush\nU10528.b 3/31/01 1:46 D:\Chem\Rush\R010329.b 3/31/01 2:W D:\Chem\RushLQO10329.b 3/31/01 2:15 D:\Chem\Rush\R010329.b 3/31/012 2 9 D:\Chem\Rush\R010329.b 3/31/01 2:43 D:\Chem\Rush\R010329.b 3/31/012 5 8 D:\Chem\Rush\R010329.b 3/31/01 3:12 D:\ChemRushLRO10329.b 3/31/01 3127 D:\Chem\Rush\R010329.b 3/31/01 3:41 D:\Chem\Rush\R010329.b 3/31/01 3 5 5 D:\Chem\Rush\R010329b 3/31/01 4:39 D:\Chem\Rush\R010329.b 3/31/01 4 5 3 D:\ChemWush\R010329.b 3/31/01 5 9 7 D:\Chem\Rush\R010329.b 3/31/01 5 2 2 D:\Chem\Rush\RO10329.b 3/31/01 5:36 D:\Chem\RushlR010329.b 3/31/01 5 5 0 D:\Chem\Rush\R010329.b 3/31/01 6:05 D:\Chem\Rush\R010329.b 3/31/016:19 D:\ChemWush\R010329.b 3/31/016:34 D:V;hem\Rush\R010329.b 3/31/01 6:48 O:\Chem\Rush\R010329.b 3/31/017:02 D:\Chem\RushV7010329.b 3/31/017:17 D:\Chem\Rush\RO10329.b 3/31/01 8:W D:\Chem\RushlR010329.b 3/31/01 8:14 D:\Chem\Rush\R010329.b 3/31M18:29 D:\ChemWush\R010329.b 3/31/018:43 D:\Chem\Rush\R010329.b 3/31/018.57 D:\Chem\Rush\R010329 b 3/31/01 9:12 O:\Chem\RushW010329.b 3/31/019:26 D:\Chem\Rush\ROlO329.b SamuTvpe SAMPLE SA::PLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File Sample Name RUSH0148.D StudyNumber E001311 P.FSH0149.D StudyNumber E001311 RUSHO15O.D SludyNumber E00-131I RUSH0151.O StudyNumber E00-1311 RUSH0152.D StudyNumber E M 1 3 1 1 RUSH0153.0 Study Number E00-1311 RUSH0154.D StudyNumber 00-1311 RUSH0155.D StudyNumberEOO-1311 RUSH0156.D StodyNumber E00-1311 RUSHOI57.D StudyNumber 00-1311 RUSH0158.0 5 n@mLPFOS in MeOH RUSH0159.D 250.5 n g h L PFOS in MeOH RUSHO162.D StudyNumber E00-1311 RUSH0163.D StudyNumber E001311 RUSH0164.0 StudyNumber E001311 RUSH0165.0 StudyNumber 00-1311 RUSH0166.0 Study Number E M 1 3 1 1 RUSH0167.D Study Number 00-1311 RUSHO168.D StudyNumber E001311 RUSH0169.D StudyNumber 00-1311 RUSH0170.D StudyNumber 00-1311 RUSH0171.D Study NumberEOO-1311 RUSH0172.D 5 nghnL PFOS in MeOH RUSH0173.0 250.5 nglmL PFOS in MeOH RUSH0176.0 Study Number E00-1311 RUSH0177.0 Study Number E00-1311 RUSH0178.D StudyNumber E M 1 3 1 1 RUSH0179.0 StudyNumber E001311 RUSH0180.D Study NumberE00-1311 RUSHO181.0 5 nglmL PFOS in MeOH RUSH018Z.0 250.5 ng/mL PFOS in MeOH Mlrc info Compound NarRT THPFOS THPFOS T::"FOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Amount 5.568 648571 254 5.571 777614 254 5.56 773093 254 5.57 765364 254 5.56 699682 254 5.554 752148 254 5.553 740653 254 5.552 760503 254 5.547 630350 254 5.54 726008 254 5.543 737132 254 5.541 729955 254 5.54 758508 254 5.541 757756 254 5.547 615598 254 5.537 734440 254 5.533 771181 254 5.529 754378 254 5.518 599700 254 5.533 860517 254 5.529 908478 254 5.532 746279 254 5.532 742286 254 5.532 728504 254 5.528 615539 254 5.524 771909 254 5.528 694870 254 5.525 717026 254 5.525 618466 254 5.524 706770 254 5.526 709256 254 Compound WT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Ana Amount 5.778 3031707 207.59 5.774 1604497 75.82 5.763 1592359 75.66 5.771 1911308 95.65 5.763 4619176 324.00 5.757 6721579 486.79 5.756 7944853 627.78 > 501 u g h 5.749 7336093 541.01 501 u g h 5.75 8586480 885.44 > 501 ugR 5.743 3782037 238.27 5.753 251147 5.22 104.4% 5.744 4087493 261.45 104.4% 5.743 3926573 236.36 5.751 3793091 226.44 5.75 5938887 541.09 > 501 u g h 5.74 6989609 530.96 > 501 ugh 5.736 7352037 532.24 > 501 uglL 5.739 7301746 543.57 > 501 ugh 5.728 9140058 1045.56 w 501 ugR 5.736 5403042 303.36 5.739 5358582 279.64 5.743 4454098 283.95 5.742 253008 5.23 104.5% 5.735 3903435 247.03 98.6% 5.738 6430648 604.83 > 501 UgiL 5.727 740559 29.08 5.738 238023 5.29 5.735 210945 3.49 5.728 3041758 221.42 5.741 249768 5.69 113.9% 5.736 3915802 256.72 102.5% page4of4 BACK TO MAIN Sample Batch R010329a.b. analyzed on Rush 033941. PFOS AdsorblDesorb samples. Matrix: SoiIISlglSed. Standard curve range used for calibration of samples: 5-501 ng/mL (2.5 nglmL std not includeddue to the higher sample concentration range). h Batch method: R010329.m Ini Date Batch SamDTVDeFile SamDle Name 3/29/01 19:W D:\Chem\RSAMPli' RUSH00220n g h L PFOSin MeOH 3/29/01 19:19 D:\Chem\RCALIB-l RUSH00232.5 ng/mL PFOS in MeOH 3/29/01 19:33 D:\Chem\RCALIB-2 RUSH00245 ng/mL PFOS in MeOH 3/29/01 19:47 D:\Chem\RCALIB-3 RUSH002510 nglmL PFOS in MeOH 3/29/01 20:02 D:\Chem\RCALIB-4 RUSH002625 ng/mL PFOS in MeOH 3/29/01 20:16 D:\Chem\RCALIB-5 RUSH002740 ng/mL PFOS in MeOH 3/29/01 20:30 D:\Chern\RCALIB-G RUSH002850.1 ng/mL PFOS in MeOH 3/29/01 20:45 D:\Chem\RCALIB-7 RUSH002975.1 ng/mL PFOS in MeOH 3/29/01 20:59 D:\Chem\RCALIB-8 RUSH0030100.2 ng/mL PFOS in MeOH 3/29/01 21:13 D:\Chem\RCALIB-9 RUSH0031250.5 ng/mL PFOS in MeOH 3/29/01 21:28 D:\Chem\RSAMPLE RUSH0032400.8 ng/mLPFOS in MeOH 3/29/01 21:42 D:\Chem\RCALIB-lO RUSH0033501 ng/mL PFOS in MeOH 3/29/01 21:57 D:\Chem\RSAMPLE RUSH00341002 nglmL PFOS in MeOH 3/30/01 14:44 D:\Chem\RSAMPLE RUSH01040ng/mL PFOS in MeOH 3/30/01 14:58 D:\Chem\RCALIB-11 RUSH01052.5 ng/mL PFOS in MeOH 3/30/01 15:13 D:\Chem\RCALIB-l2 RUSH01065 ng/mL PFOS in MeOH 3/30/01 15:27 D:\Chem\RCALIB-13 RUSH010710 nglrnL PFOS in MeOH 3/30/01 15:41 D:\Chem\RCALIB-14 RUSH010825 ng/mL PFOS in MeOH 3/30/01 15:56 D:\Chem\RCALIB-15 RUSH010940 ng/mL PFOS in MeOH 3/30/01 16:lO D:\Chem\RCALIB-lG RUSHOl 1050.1 ng/mL PFOS in MeOH 3/30/01 16:25 D:\Chem\RCALIB-l7 RUSHOl1175.1 ng/mL PFOS in MeOH 3/30/01 16:39 D:\Chem\RCALIB-18 RUSHOl12100.2 ng/mL PFOS in MeOH 3/30/01 1653 D:\Chem\RCALIB-19 RUSH0113250.5 ng/mL PFOS in MeOH 3/30/01 17:08 D:\Chem\RSAMPLE RUSHOl14400.8 ng/mL PFOS in MeOH 3/30/01 17:22 D:\Chem\RCALIB-PO RUSH0115601 ng/mL PFOS in MeOH 3/30/01 17:36 D:\Chem\RSAMPLE RUSHOl161002ng/mL PFOS in &OH Misc InComoouncRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Amount 5.581 937536 254 5.587 932041 254 5.582 892607 254 5.59 941200 254 5.586 952213 254 5.581 964296 254 5.588 940694 254 5.582 913845 254 5.584 931382 254 5.581 882940 254 5.577 925627 254 5.582 989407 254 5.585 884676 254 5.574 845419 254 5.561 850637 254 5.57 805498 254 5.574 844287 254 5.574 874781 254 5.575 874280 254 5.575 856450 254 5.562 857550 254 5.568 863358 254 5.578 806157 254 5.574 858200 254 5.57 909424 254 5.568 813760 254 ComDouncRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 5.797 5.793 5.793 5.789 5.784 5.798 5.792 5.787 5.791 5.787 5.785 5.788 0 5.771 5.78 5.778 5.777 5.778 5.778 5.765 5.771 5.789 5.777 5.773 5.778 Area 0 233998 265016 397179 812531 1183051 1389031 1906080 2452896 4875108 7451045 9377197 14614178 0 234682 259067 372504 750517 1074369 1261642 1770429 2201517 4379739 6738768 8394525 12942478 Amount 0 2.84 4.50 9.07 25.37 40.13 50.34 76.36 101.14 253.12 415.73 519.76 1161.45 0.00 3.73 5.40 9.78 25.55 40.21 50.20 75.43 97.27 247.92 402.04 501.13 1096.91 89.9% 90.7% 101.5% 100.1% 100.5% 101.7% 100.9% 101.0% 103.7% 107.9% 97.8% 102.2% 100.3% 100.2% 100.4% 97.1% 99.0% 100.0% -- Average: 890317.9 Std Dev: 49995.31 %RSD: 5.6% 1157413 +30%: 623223 -30%: Page 1 of 4 BACK TO MAIN s" Sample Batch R010329a.b, analyzed on Rush 03-29-01. PFOSAdsorblDesorb samples. Matrix: SoiUSlglSed. Standard curve range used for calibration of samples: 5-501 nglmL(2.5 ng/mL std not included due to the higher sample concentration range). Batch method: R010329.m lnj Date Batch SampTypeFlle Sample Name 3/29/01 18:35 D:\Chem\RSAMPLE RUSH0020TN-A 4802 MeOH 3/29/01 18:50 D:\Chem\RSAMPLE RUSH0021TN-A 4802 MeOH 3/29/01 22:ll D:\Chem\RSAMPLE RUSHOO35iN-A4802 MeOH 3/29/01 2225 D:\Chem\RSAMPLE RUSH0036TN-A 4802 MeOH 3/30/01 0:49 D:\Chem\RSAMPLE 3/30/01 1:03 D:\Chem\RSAMPLE 3/30/01 4 : l l D:\Chem\RSAMPLE 3/30/01 4:25 D:\Chem\RSAMPLE 3/30/01 7 3 2 D:\Chem\RSAMPLE 3/30/01 7:46 D:\Chem\RSAMPLE RUSH0046TN-A 4802 MeOH RUSH0047TN-A 4802 MeOH RUSH0060TN-A 4802 MeOH RUSH0061TN-A 4802 MeOH RUSH0074TN-A 4802 MeOH RUSH007-N-A 4802 MeOH 3/30/01 1 0 9 D:\Chem\RSAMPLE RUSH0086fN-A4802 MeOH 3/30/01 11:08 D:\Chem\RSAMPLE RUSH0089TN-A 4802 MeOH 3/30/01 14:15 D:\Chem\RSAMPLE RUSH0102TN-A 4802 MeOH 3/30/01 14:29 D:\Chem\RSAMPLE RUSHOIOJTN-A4802 MeOH 3/30/01 1751 D:\Chern\RSAMPLE RUSHOl17TN-A 4802 MeOH 3/30/01 18:05 D:\Chem\RSAMPLE RUSHOl18TN-A4802 MeOH 3/30/01 1820 D:\Chem\RSAMPLE RUSH0119TN-A4802 MeOH Mise InCompouncRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 CompounrRT Area Amount PFOS 5.806 157757 0 PFOS 5.809 137641 0 PFOS 5.804 167176 0 PFOS 5.798 141973 0 PFOS 5.809 145679 0 PFOS 5.803 135609 0 PFOS 5.803 138237 0 PFOS 5.803 134040 0 PFOS 5.807 144692 0 PFOS 5.808 137246 0 PFOS 5.796 142382 0 PFOS 5.794 138943 0 PFOS 5.792 144070 0 PFOS 5.789 134518 0 PFOS 5.798 170024 0 PFOS 5.793 144025 0 PFOS 5.797 138657 0 BACK TO MAIN Sample Batch RGiiXZSa.b, aii~!'yz$d$5 Rmh 03-29-07. PFOSAdsorblhsorb samples. Matrix: SoiIIslg/s8d. Standard curve range used for calibration of samples: 5-501 flg/mL (2.5 ng/mL sta not inciuded d i e :a tks !?!gharsample concentration range). Batch method: R010329.m Inj Date Batch SampTypeFile Sample Name Mise InCompouncRT Area Amount CompouncRT 3/29/01 22:40 D:\Chem\RSAMPLE RUSH0037Study Number EOO-1311 THPFOS 5.588 074070 254 PFOS 3/29/01 22% D:\ChemRSAMPLE RUSHOO38Study Number E00-1311 THPFOS 5.502 901936 254 PFOS 3/29/01 23:08 D:\Chem\RSAMPLE RUSHOO3btudy Number E00-1311 THPFOS 5.508 905901 254 PFOS 3/29/01 23:23 D:\Chem\RSAMPLE RUSH0040Study Number EOC-1311 THPFOS 5.586 727872 254 PFOS 3/29/01 23:37 D:\Chem\RSAMPLE RUSH0041StudyNumber E00-1311 THPFOS 5.581 801852 254 PFOS 3/29/01 23:52 U:\Chem\RSAMPLE RUSH0042Study Number 00-1311 THPFOS 5.502 084596 254 PFOS 3/30/01 0:06 D:\Chem\RSAMPLE RUSH0043Study Number E00-131I THPFOS 5.583 880085 254 PFOS 3/30/01 0:20 D:\Chem\RSAMPLE RUSH00445 ng/mL PFOSin MeOH THPFOS 5.502 090865 254 PFOS 3/30/01 0:35 D:\Chem\RSAMPLE RUSH0045250.5 ng/mL PFOS in MeOH THPFOS 5.50 877456 254 PFOS 3/30/01 1:10 D:\Chem\RSAMPLE RUSH0048Study Number EOO-I311 THPFOS 5.508 694334 254 PFOS 3/30/01 1:32 D:\Chem\RSAMPLE RUSH0049Study NumberEOO-1311 THPFOS 5.503 970838 254 PFOS 3/30/01 1:47 D:\Chem\RSAMPLE RUSH0050Study NumberE00-1311 THPFOS 5.582 911997 254 PFOS 3/30/01 3/30/01 3/30/01 3/30/01 3/30/01 2:Ol 235 2:30 2:44 259 -- D:\Chem\RSAMPLE D:\Chem\RSAMPLE D:\ChemRSAMPLE D:\Chem\RSAMPLE D:\Chem\RSAMPLE RUSH0051Study RUSH0052Study RUSH0053Study RUSHOO54Study RUSH0055Study Number E00-1311 Number E00-1311 Number E00-1311 Number E00-1311 Number E00-1311 THPFOS THPFOS THPFOS THPFOS THPFOS Yuwas 5.575 084072 5.575 711307 5.571 895011 5.569 093422 5.568 900655 &.56.7746683 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254-eWs 3/30/01 3:27 D:\Chem\RSAMPLE RUSHOO57Study Number E00-1311 THPFOS 5.575 868476 254 PFOS 3/30/01 3:42 D:\Chem\RSAMPLE RUSH00585 n g h L PFOSin MeOH THPFOS 5.501 060307 254 PFOS 3/30/01 3:56 D:\Chem\RSAMPLE RUSH005a50.5 ng/mL PFOS in MeOH THPFOS 5.581 045346 254 PFOS 3/30/01 4:39 D:\Chem\RSAMPLE RUSH0062Study Number EOO-1311 THPFOS 5.581 879621 254 PFOS 3/30/01 4 : s D:\Chem\RSAMPLE RUSHOO63Study Number 00-1311 THPFOS 5.578 865113 254 PFOS 3/30/01508 D:\Chem\RSAMPLE RUSHOO64StudyNumber E00-1311 THPFOS 5.573 713593 254 PFOS 3/30/01 5 2 2 D:\Chem\RSAMPLE RUSH0065Study Number00-1311 THPFOS 5.581 056465 254 PFOS 3/30/015:37 D:\Chem\RSAMPLE RUSHOO66Study Number00-1311 THPFOS 5.501 844166 254 PFOS 3/30/015 5 1 D:\Chem\RSAMPLE RUSHOO67Study NumberE00-1311 THPFOS 5.502 840621 254 PFOS 3/30/01 6:06 D:\Chem\RSAMPLE RUSH0068Study Number00-1311 THPFOS 5.579 669997 254 PFOS 3/30/01 6:20 D:\Chem\RSAMPLE RUSH0069Study Number00-1311 THPFOS 5.577 810557 254 PFOS 3/30/01 6:34 D:\Chem\RSAMPLE RUSH0070Study Number EOO-1311 THPFOS 5.502 015811 254 PFOS 3/30/01 6:49 D:\Chem\RSAMPLE RUSH0071Study Number 00-1311 THPFOS 5.574 023985 254 PFOS 3/30/01 7:03 D:\Chem\RSAMPLE RUSH00725 ng/mL PFOS in MeOH THPFOS 5.571 023981 254 PFOS 3/30/01 7:17 D:\Chem\RSAMPLE RUSH0073250.5 nglmL PFOS in MeOH THPFOS 5.570 821611 254 PFOS Area 5.791 3351053 5.705 3334462 5.791 3176252 5.79 5058869 5.791 6707348 5.785 4533069 5.787 6721663 5.799 279066 5.791 4055798 5.792 0002466 5.793 2166125 5.792 2001596 5.770 1925950 5.785 4007082 5.701 7066726 5.779 7171691 5.771 7403683 5.zua4d.65u 5.785 471637 5.798 272404 5.792 4664476 5.791 207413 5.708 175106 5.703 3349107 5.705 2228059 5.784 2133042 5.785 1411558 5.702 4285006 5.70 7109748 5.705 5211026 5.777 0017544 5.788 275231 5.781 4574902 Amount 159.93 152.92 143.26 415.70 391.37 230.09 387.34 5.09 253.86 795.21 02.81 85.1 1 80.38 329.29 404.55 414.16 433.90 @a56 13.57 5.11 252.91 2.29 1.09 205.86 99.69 96.20 58.15 306.23 460.98 305.78 539.08 > 5.85 255.08 101.0% 101.3% 5DluglL 102.1% 101.0% 501ug/L 117.0% 102.136 0 -h Page 3 O f 4 BACK TO MAIN Sample Batch R010329a.b. analyzed on Rush 03-29-01. PFOS AdsorblDesorb samples. Matrix: SoillSlg/Sed. Standard curve range used for calibration of samples: 5-501ng/mL (2.5 nglmL std not included due to the higher sample concentration range). Batch method: ROlO329.m 3130101 8:Ol D:\Chem\RSAMPLE RUSH0076Study Number E00-1311 THPFOS 5.568 690116 254 PFOS 3/30/01 8:15 O:\Chem\RSAMPLE RUSH0077Study Number E00-1311 THPFOS 5.579 956969 254 PFOS 3/30/01 8:29 D:\Chem\RSAMPLE RUSH0078Study Number E00-1311 THPFOS 5.574 870548 254 PFOS 3/30/01 8:44 D:\Chem\RSAMPLE RUSH0079Study Number EOO-1311 THPFOS 5.581 845769 254 PFOS 3/30/01 8:58 D:\Chem\RSAMPLE RUSH0080Study Number E00-1311 THPFOS 5.574 710436 254 PFOS 3/30/01 9:13 D:\Chem\RSAMPLE RUSH0081Study Number E00-1311 THPFOS 5.576 852256 254 PFOS 3/30/01 9:27 D:\Chem\RSAMPLE RUSH0082Study Number 00-1311 THPFOS 5.576 913113 254 PFOS 3/30/01 9:42 D:\Chem\RSAMPLE RUSH0083Study Number E00-1311 THPFOS 5.585 834426 254 PFOS 3/30/01 9:56 D:\Chem\RSAMPLE RUSHOOWtudy Number E00-1311 THPFOS 5.578 702989 254 PFOS 3/30/01 1O:lO D:\Chem\RSAMPLE RUSHOO85SStudyNumber E001311 THPFOS 5.581 919415 254 PFOS 3/30/01 10:25 D:\Chem\RSAMPLE RUSH00865 nglmL PFOS in MeOH 3/30/01 10:39 D:\Chem\RSAMPLE RUSH0087250.5 ng/mL PFOS in MeOH THPFOS 5.579 828884 254 THPFOS 5.573 820925 254 PFOS PFOS 3/30/01 11:37 D:\Chem\RSAMPLE RUSHOOSlStudy Number E00-1311 THPFOS 5.575 851126 254 PFOS 3/30/01 11:51 D:\Chem\RSAMPLE RUSH0092Study Number EOO-1311 THPFOS 5.577 699580 254 PFOS 3/30/01 12:06 D:\Chem\RSAMPLE RUSHOO93StudyNumber 00-1311 THPFOS 5.581 833674 254 PFOS 3/30/01 12:20 D:\Chem\RSAMPLE RUSH0094Study Number E00-1311 THPFOS 5.575 827651 254 PFOS 3/30/01 12:34 D:\Chem\RSAMPLE RUSHOO95StudyNumberE00-1311 MPFOS 5.579 833417 254 PFOS 3/30/01 12:49 D:\Chem\RSAMPLE RUSHOO96Study Number 00-1311 THPFOS 5.573 660626 254 PFOS 3/30/01 1303 D:\Chem\RSAMPLE RUSHOO97StudyNumber E00-1311 THPFOS 5.575 831428 254 PFOS 3/30/01 13:17 D:\Chem\RSAMPLE RUSHOO9Study Number 00-1311 THPFOS 5.572 822165 254 PFOS 3/30/01 13:32 D:\Chem\RSAMPLE RUSHOO99Study Number 00-1311 THPFOS 5.576 815744 254 PFOS 3/30/01 13:46 D:\Chem\RSAMPLE RUSH01005 ng/mL PFOSin MeOH THPFOS 5.569 788928 254 PFOS 3/30/01 14:Ol D:\Chem\RSAMPLE RUSH0101250.5nglmLPFOS in MeOH THPFOS 5.574 788989 254 PFOS 5.778 5.782 5.778 5.784 5.777 5.779 5.779 5.788 5.781 5.785 5.789 5.783 5.785 5.78 5.784 5.785 5.789 5.783 5.785 5.775 5.779 5.779 5.777 10151474 4102214 3443662 3186935 5795265 6155804 8769331 5927478 8168548 4411967 270806 4516252 4018521 6442026 1056562 376593 275264 3353185 846945 885719 850807 261893 4409485 976.13 > 5Olug/L 183.73 166.25 156.55 423.27 359.52 529.37 > 501uglL 351.66 692.32 > 501ug/L 211.71 5.58 111.6% 251.94 100.6% 207.41 499.47 41.77 10.29 5.71 227.32 31.83 34.15 32.79 5.77 115.5% 257.10 102.6% D M [1) ID VI VI 03 Page4 of 4 BACK TO MAIN n ltdh oKmI 5w 5m WOS 5w PFOP 58 PFOI 58 Ros 58 PFOS SW PFOS sn PFOt 5a PFOS 521 Pfos 5m FfM 5P PFDS 5P wC M Km PFOS 521 wC M .W PFOS 5 21 wC M PFOS 5 24 ROS L,D PFOS sn Ros 522 *OS Om a0 ff m 5.2, 20 PFOP 521 6.4 Ros 5n PFOS sn ROS 522 ROS 522 ROB 121 PFOS LP ROS sn PFos 58 PFOS 5 21 -0 a, 0 ID ul CD 0 0 -h 0 0 MPLE UPLE WE UPLE *LE WLE BACK TO MAIN WFOS TNPFOS WFOS nwos THPFOI MPFOS THPFOS WFOI mPFDs wos WFOS sm WPFOS sd3 MPFOS SOD WFOS SOD WOS MPFDS MPFOS mwos WFW Twpfos MPFOI WFOS THPFm mPPm THPFOS WOS WFOS mpm mww mpfm mwoa WOS MPFDP mwos WFOS mwos WfDs mffos WFOS WfOS WFOS mwos MPFDS mwos MPFOS niwm WFOS mms mPFOs MPFOS THPFDI WDS MPFOS mwos WFOS MPFOS mwos MPFOS THPFOS 3PFC-S MPFOS THPFOS WFOS mwos THPFOI m PFOS om m PFOS om m PFOS om m PFOS PFW PFOS PFOI ms PFOS m PFOS sa m PFOS om m wOS 5n 54 PFOS om m PTOS om m PFOS om m PFOS 522 m WO8 522 m PfOS am m PFOS 522 m PFOS mm PFOS PFOS m Pros m PfOS m PFOS m PFOS m PPO* m PFOS W ffos W PFOS m ROS 521 m Pros 532 zy PFOI m PFOIl m PFOI W ffO* m W PFOS SFOS W cos m pros m PFOS m PFOS m PFOS m PFOI m PFOS m PFOS m PFOS m PFOS m PFW m Pros m PFOI m PFOS 254 PPOS m PFOS m Pros m PFOS m PFOS m PFOS W PFOS W PFOS mIy PfOI PFOS W PFOS zy PFOS zw PFOS zw PFOS m PFOS W PFOS Iy PFOS 2y PFOS W PFOS W PFO6 W PFOS 2y Pfos W PFOS 5n W PFOS sn 2y PFOS 5n BACK TO MAIN 00 on 00 00 00 00 00 BACK TO MAIN s h b0- 0 3. ) BACK TO MAIN D Iu M n, 0 -k w 0 0 BACK TO MAIN | | BACK TO MAIN r nJ b 0 3 $ D D (P ID 0 -h HO10404external standardquantxlr Q 3 r Sample B i t c h H01WX.b, analyzedon Hlllay OUKOI. PFOSAdsotiwUesoe samples Matrix: SolUSlplSed. Standard CuNe range used for calibration d samples: 10400.8 n d m L Batch method HO1MM.m (ExternalStandard Ouant) In] ate Batch SmpTyp. 414101 1617 D-ChemWillaryWO10404.b SAMPLE ii4;Gi 1?3:5:~ : ` P ~ ~ m ? H i l l a l y u ( O l 0 .CbALIB-1 4/4/01 18.46 D:ChemWillarywOl0404b CAUB-2 4/4101 19.00 D:ChemWdiaryW010404.b CALlB-3 4/4nlf 19:14 D:\ChemWiuaF/WOl0404b CAUB-4 414101 19 29 D.!ChemW~llwyW0104M4.b CALIB-5 414101 19 43 DChemWiNaryWOIOI1(Y.b CALIB-6 414101 19.57 WChemWiNaryWOlD404.b CALIB-7 41410120.12 D:ChemWParyW010404.b CALIB-8 414m1 20 26 D.\chemwiUalvwO10404b CAUE-9 414101 2041 DChemWllaryWOl0404b CAUB-10 4/41012055D:ChemWillaryWOlW04.b SAMPLE 414M121.09 D:\Chem~illaryW0104M.b SAMPLE ml ~l.f9D:\ChemWillalyutol0404.b SAMPLE 415101 11:33 O.\themWla.rNO104M.b CALIB_lI 415101 1147 D ChemWdlsryWO10404b CALIB~12 415101 12 02 D ChemWdlaryWO10404b CAUB-13 41510112 16 D ChemWdIqWOlO4M b CAUB-14 4l5101 12 31 D C h e m W t l l a ~ O 1 M 0b4 CALIB-15 41Y01 12 45 D \ChamWiltaryW010404b CAUB-16 415101 I 2 59 D ChemWillaryWO10404b CAUB-17 415101 13 14 D ChemWIaryWO10404 b CALIB-18 4No1 13 29 D \ChemWKawWO<M04b CALI6 19 415~0113 42 D memV11a ~ W 0 1 0 4 Mb CAUB120 4,501 13 57 D Q2hernu(H.~sryV10104b04 SAMPLE 415101 14 11 D Cnamu(lrryH010404 b SAMPLE File HILLOO16.D HlLL0017.D HILLCC~B D HILLWISD HILLOO2O.D HlLLoO21.D HILL0022D HlLLW23.D HlLL0024.D HILL0025.D HILL0026.D HlUW27.D HIUW28.D HlUOO87D HILLW66.0 HlUW89.D HlLLOO9O.D HILL0091D HlLL0092.D HlLLW93.D HlLLMM4.D HlLLW95.D HILL009B.D HlU0097 D HlLLW96 D dLL0099 D Sample Nuns 0 nVmCPFOS m MeOH 2.5 nglmL PFOS in MeOn 5 >&?L PCflS m MaOH IOnglmLPFOSin MeOH 25 W L PFOS il MeOH 40nVmLPFOSin MeOH 50.1 nght PFOSinMeOH 75.1 n&LPFOS in MBOH 103.2 ng/mLPFOS in MeOH 250.5 n W L PFOS in MeOH 4W.8 WmLPFOSinMSOH 501 ngllnLPFOS in MeOH 1W2 nglmLPFOS in MeOH OnglinLPFOSmMsoH 2.5WmLPFOS in MeOH 5 W m L PFOSin MBOH 10nWmLPFOSm MBOH 25 n m L PFOSin MeOH 40 nWmL PFOS in M e O n 50.1 nghnLPFOSinM& 75.1 WmL PFOS in MeOH 100.2 WmL PFOS in M.OH 250.5 rWmL PFOS h MeoW 400 8 G m L PFOS m M e n 501 nwm- PFOS m MaOH 1002 ngmL PFOS m MeOH Mlsc InfCompaund NaRT THPFOS THPFOS -,THPFOS h^r-rewC THPWS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Am4 5.113 5.112 5 112 5 112 5 113 5 I11 5 112 5 113 5 114 5 113 5 112 5 113 5 114 5 092 5 091 5 093 5 09 5 092 5 W1 5098 5 098 5 093 5 092 5 092 5093 5 099 Amount 806065 254 889526 254 877571 254 402873 254 680573 2% 931996 254 803398 254 684697 254 699168 254 657703 254 891222 254 907981 254 840757 254 1261932 254 1203313 254 1167470 254 I191649 254 1181183 254 1183642 254 I129902 254 1099744 254 11M)820 254 1030899 254 1039403 254 1052373 254 862330 254 Averroe: 5Std Dav: 85107.0294 HRSD 7.6% c Compound N a R T PFOS PFOS PFOS PFOS PFCS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS ms ffos PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Ana Amount 0 0 0 5.329 72734 1.190813 5.329 110448 3.153981 5.329 204980 6.062458 5.51 54~l4712568227 5.329 683638 43.iSBi.i 5329 1056705 53.09021 5.33 1555069 79.67175 5.331 2075718 107.8776 5.323 4653038 252.4225 5.329 7377624 414 1189 5.33 9097217 520.6761 5 331 15189218 928379 0 0 0 5.301 62293 0647625 5.31 90724 2543506 5.307 166223 7200022 53 w 494122 23 22532 5.301 813449 4 0 0 6 w 5 315 975991 4869034 5.315 1451614 74 11635 5.31 1962240 1017013 5 309 4432636 2397418 5.309 6951500 3882267 5 31 6649086 4927043 5.309 14944991 911 1632 14M)4BB +30%: 768405 30%: 63% 61% 103% r,"nZn,"w IC%% 1cB% 108% 101% 103% 104% 93% 51% 72% 93% 100% 97% B4.h 101% 86% 97% 98% 91% In) D M Batch 4/4/0114 41 D Chemw!llaryWol0404b 414101 14 56 D \ChemWdlary\HOI0404 b 414101 15 39 D ChemVldlary\H010404WOl0404 b 414~11553 D ChemWisarywolWM b 414101 1746 D IChemWaawO10404 b 4141011603 D ChemWdIaryW0104Mb 41410121 24 D ChemWtUaar/W010404b 4l4l012138 D \ChemWllaryWD10404 b 415/010 45 D ChemWdlaryWO10404 b 4/5/01 1 0 0 DChemWdl&H0104W b 415101407 D ChemWlaryWol0404b 415/01421 DChemW1llaryW010404b 4/5/01 7 26 D ChemWllaryW010404b 4/51017 43 DChemWdlaryW010404b 415m1 1050 D \ChsmWllaryW010404b 4R101 1104 D \ChemWillaryWOlOdMb 415101 14 26 D ~ m W d l a r y W 0 1 0 4 0b4 415101 14 40 D \ChemWltaryY1010404 b SmpTypa SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE FIO HILL0001D HILL0002D HILL0005D HILLMX)~ D HILL0014 D HlLLW15 D HILL0029 0 HlLLW30 D HILL0043 D HILL0044 D HILL0057 D HILLW58 D HILLW71 D HILL0072 D HlLLW65 D HILLWE6 D HlLLOIOO D HILW101 D Sampb Name TN-A 4802 MeOH TN A 48112 MeOH TN-A 48112 MeOH rN-A 48112 M ~ O H TN-A 4802 MeOH T U 8 4802MeOH TN-A 4802MeOH TN A4802 MeOH TN-A4802 MeOH TNA4602MeOH TN-A 4802 MeDH TN-AQOZMeOH TN-A 4802 MeOH TN-A 4602 MeOH TN A 1002 MeOH TN-A 4802 MeOH TN-A 4002 MeOH T K A4602 MeOH Mire InfCompoundNaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Am 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound N a A T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Am 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amoun( 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 page 1 Of 2 BACK TO MAIN HO104Me a m a l standardquanLxls lnj Date htch SampTyp 4/4/012152 DChemW~llaryW010404.b SAMPLE 4/4/01 22 07 D ChemWBaryW01M04b SAMPLE 4/4/01 22 21 D ChemWdlarvWO10404b SAMPLE 414/012236 D CnemHlaryWO10404D SAMPLE 41410122 M D ChemW.llaryr1010404b SAMPLE 41410123 04 D CnemWlllaryW010404b SAMPLE 44'01 23 19 D CaemU~,llaryUIOIQ104b SAMPLE 414mi 23 33 D ChemWiilaryHOlM04 a SAMPLE 4/4/0123 48 D ChernHLaryWO10404b SAMPLE 4/5/010 02 D ChsmW~llaryW01040b4 SAMPLE 415101 0 16 D CnemW llary~O10404b SAMPLE 4151010 31 D CnemWillaFl\k010404b SAMPLE 415101 1 14 D Chemvl~.IaryW010404b SAMPLE 415101 128 D ChemWdlaryW010404b SAMPLE 4/5/01 1 43 D CnemWllaryW010104b SAMPLE 4.Y01 157 DCnemWdIaryviO10404b SAMPLE 41M12 11 D CnemH~llary~OlM0b4 SAMPLE 415101 2 26 D ChemW~llaryh010404b SAMPLE 41M12 40 D CnemW!llaryh010404b SAMPLE 4,5101 2 55 DChemW~llaryHOlMMb SAMPLE 415101 3 09 D ChemW#llaryW010404a SAMPLE 4.501 3 23 D ChemWl.aryHO10404b SAMPLE 41501 3 38 D ChamWIIaryH01MC-l b SAMPLE 415013 52 D ChemWllaryWO1C404b SAMPLE 41M14 35 O C h e m W ~ l l ~ W O l 0 4b0 4 SAMPLE 415014 50 D Chemih!llaryW010404b SAMPLE 46/01 5 04 D Chem~~lmryH01040b4 SAMPLE 415IOl 5 19 DChemW1~iaryHO1040b4 SAMPLE 4151015 33 D ChemW#haryW0104Mb SAMPLE 4,501 5 47 D ChemW~I~sryW0104bM SAMPLE 41501 602 DChemWtllaryd010404b SAMPLE 415,Ol 6 16 D Cnemih.llaryh010404b SAMPLE 4/5/016 31 D ChemW.laryY1010404 b SAMPLE 41M16 45 D Chamdo laryH010404 b SAMPLE 41M16 59 D ChemWdlaryH0104Mb SAMPLE 4,5/01 7 14 DChemWdaryHOl0404 b SAMPLE 415017 57 D ChemHidaryHOlCM04b SAMPLE 415101 8 11 DChemW#laryVIO1040b4 SAMPLE 4/5/018 28 D !&hem* llaryh010404b SAMPLE 4,51018 40 D Cnemw ilaryyto10404b SAMPLE 415101 8 55 D ChemWdlaryHO10404b SAMPLE 41M1 9 09 D ChemWdlmyJiO10404D SAMPLE 4/5/019 23 D ChemW IhryWO10404 b SAMPLE 4,Ml 9 38 D Chemih llary\k010404 b SAMPLE 415101 9 52 D Chem~#llaryWOl040b4 SAMPLE 41501 1007 D ChemWllaryH010404b SAMPLE 4/5/01 1021DChemWlaryWO10404b SAMPLE 4 l M 1 1036 DChemWra~yho1040b4 SAMPLE File HILL0031.D HlLL0032.D HILL0033 D HILL0034 D HlLLw35 D HILL0036 D HILL0037 D HILL0038 D HILL0039 D HILL0040 D HILL0041 D HlLLW42 D HlLLW45 D HILLOM6 D HlLLW47 D HlLLW48 D HlLLW49 D HILL0050 D HILL0051 D HILL0052 D HILL0053 D HILL0054 D HILL0055 D HILL0056 D HILL0059 D HILLMXK) D HILL0061 D HILLOM2 D HILL0063 D HIWD HlLLwB5 D HlLLW30 D HILL0007 D HILL0068 D HILUX169 D HILL0070 D HlLlW73D HILLCO74 D HILL0075 D HILL0076 D HILL0077 D HILL0078 D HILL0079 D HILLOOBO D HILL0081 D HILL0082 D HILL0083 D HILL0084 D S a m P Name W P F O S Study Numb.rEW-1311 DmQiLPFOSStudy Number E00-1311 Om@ PFOS Study Number EW-1311 Om@ PFOSStudy Number E001311 OmflPFOS Study Number EW-1311 Om& PFOS Study Number EW-1311 OmfiPFOS Study NumtmEM1.1311 hnplLPFOSStudy NumberEW-1311 5mgLPFOS Study Numb.rEW-1311 SmgLPFOSStudy Number EW-1311 5 ng/mL PFOS in MeOH 250 5 nUmL PFOS m MeOH 5m#t PFOSStudyNumberEW-1311 SmaPFOS Study Number E001311 5mWPFOS Study Number EW-1311 srnWPFOSStudyNumberE00-1311 SmWPFOS ShldyNumberE001311 SmQiLPFOS StudyNumber E001311 SmaPFOS Study NumberEM1.1311 5mgllPFOSS M y Number E001311 5mgLPFOS Study Number EW-1311 Sman PFOS S U y Number E001311 5 nphnt PFOS m MeOH 250 5 n#mL PFOS in MeOH SmWPFOSStudy Number E001311 5mWPFOS Study Number E00-1311 SmOnPFOS Study NumbMEW-1311 SmgLPFOSStudy Number EW-1311 5mgRPFOS Study NumberEW-1311 5mdtPFOSStudyNumberEW-1311 5mPnPFOS Study Number E001311 5mW PFOS Study Number EW-1311 5mWPFOS Study Number E001311 5mpllPFOSStudy NumberEW-1311 5 wmt PFOS tn MeOH 250 5 n@mLPFOS m MeOH SmgLPFOS Study NumberEW-1311 5mgllPFOS Study Number E001311 5mplLPFOS Study Number E001311 5m@PFOs Study Number EW-1311 5mgLPFOSSludyNumberEW-1311 SmgAPFOS Study Number EW-1311 SmpiLPFOSStudy Numtmr EW-1311 5mgLPFOS Study Nwnber EW-1311 5m@APFOSStudy Number Em1311 SmglLPFOSStudy Number EW-1311 5 nplmt PFOS m MeOH 250 SnplmL PFOS m M e O n Mlsc InfCompoundNaRT Ana THPFOS 5.108 THPFOS 5.111 THPFOS 5 107 THPFOS 5 108 THPFOS 5 098 THPFOS 51 THPFOS 5094 THPFOS 5099 THPFOS 5 099 THPFOS 5 098 THPFOS 5 105 THPFOS THPFOS 5 108 5 ma THPFOS 5 098 THPFOS 5 105 THPFOS 5 099 THPFOS 5094 THPFOS 5 098 THPFOS THPFOS 5 097 5 mi THPFOS 5 091 THPFOS 5 099 THPFOS 5 104 THPFOS 5 098 THPFOS 5 048 THPFOS 51 THPFOS 5 099 THPFOS 5 099 THPFOS 5 098 THPFOS 5 099 THPFOS 5048 THPFOS 5 092 THPFOS 5 091 THPFOS 5 09 THPFOS 5092 THPFOS 5 098 THPFOS 5 091 THPFOS 5 098 THPFOS 5 097 THPFOS 5 099 THPFOS 5 092 THPFOS 0 THPFOS 0 MPFOS 5085 THPFOS 5 085 THPFOS 5 084 THPFOS 5 087 THPFOS 5 086 hOMI CompoundN a A T Ana Amount 1582301 254 I S T D l M % PFOS 0 0 0 1575594 254 ISTD>lM% PFOS 0 0 0 1560082 254 ISTD>130% PFOS 0 0 0 1537278 254 ISTD>130% PFOS 5.316 31709% 186.3053 1599896 254 ISTD>130%PFOS 0 0 0 1613917 254 ISTD>130% PFOS 0 0 0 1644862 254 ISTD,130% PFOS 0 o n 1578150 254 ISTD>130% PFOS 5.309 2970771 157.1483 158738s 254 ISTD>130%PFOS 0 0 0 1587309 254 ISTD>lM% PFOS 0 0 0 1307817 254 PFOS 5.315 101216 2873254 11- 254 PFOS 5.318 4807627 249.8049 1569404 254 ISTD>130% PFOS 5.315 2027% 7.956382 15211W 254 ISTD>130% PFOS 5.315 3255972 173.0552 1583690 254 ISTD>lM% PFOS 5.315 80242 1581493 1535494 254 ISTD>130% PFOS 0 0 0 1528194 254 ISTD>130% PFOS 0 0 0 1514404 254 ISTDrl30% PFOS 5.315 3115242 185 1936 1537503 254 ISTD>130% PFOS 5.314 76776 1401129 1529992 254 ISTD>lM% PFOS 5.308 m528 2429182 1541462 254 ISTD>130%PFOS 5.308 168651 8082828 1500713 254 ISTD>13O% PFOS 5.309 3133475 1862108 1341697 254 PFOS 5.314 103787 2 80712 1246317 254 PFOS 5.308 4550667 2485252 1687410 254 ISTD>130% PFOS 5.3w 183857 6980244 1546322 254 ISTD>130%PFOS 5.31 148784 5151322 1570952 254 ISTD>lM% PFOS 5.316 80452 1582421 1511291 254 ISTD>130%PFOS 5.316 3105298 164639 1520307 254 ISTDr13O%PFOS 5.315 81053 1623698 1536595 254 ISTD>130% PFOS 5.316 74150 1264487 1504984 254 ISTD>130% PFOS 5.308 119473 3 624028 1472241 254 ISTDI130% PFOS 5.302 3098377 164 2531 1543912 254 ISTDr130% PFOS 5.308 134114 4386787 1511129 254 ISTD>l30% PFOS 5.301 178554 6 7 5 5 m 1329935 254 PFOS 5.309 99459 2581778 1283173 254 PFOS 5.308 4490291 2430532 1537210 254 iSTD>130%PFOS 5.W 181284 684802 1489558 254 ISTDrl30% PFOS 5.308 3114794 165 1 6 s 1509221 254 ISTD>130% PFOS 5.307 7 W 3 1384206 1509704 254 ISTD>13O% PFOS 5.309 138272 4803457 1492328 254 ISTD>13O% PFOS 5.309 231419 9462838 0 0 ISTD<7O% PFOS 5.302 3083518 162 3102 0 0 ISTDc70% PFOS 5.295 191090 7357805 1474995 254 ISTD>130% PFOS 5.302 170928 6 305786 1468047 254 ISTD>130%PFOS 5.302 88BBo 2030021 1443304 254 PFOS 5.301 2902477 153 3541 1338208 254 PFOS 5.304 100507 2.63634 1274099 254 PFOS 5 2% 4412461 238.5841 53 5% 99 7% 58 1% gs 4% 51 6% 87 0% 52 7% 952% page 2 of 2 BACK TO MAIN 3 b b 0 3 D aa, (D H010412.xlr Sample Batch HO10412.b, analyzedon HlllatycCl201. PFOSA&oridDewrb UmpleS. Mltrlr: Solk'SI~d Standard curve range usedfor calibration ofsamples: 10400.8 n@mL Ratch method H010412.m In] Date Batch SampType 4/12/01 1751 D\ChemWllIaryW010412Ab SAMPLE 4/12/01 18 05 O ChemW1lla1yWO10412Ab CALlB-1 4,1201 18 19 D\ChemWillaryWOlMlZAb CALK-2 4/12/0118 34 D\ChemWillaryW010412Ab CALIB-3 4/12/01 1848 0 V)hemWdlaryW010412Ab CALiB-4 4/12/01 19 03 D \ChemWillatyW010412A b CALlB-5 4/12/01 19 17 D!ChemWiIlaryW10412Ab CALL-6 4/12/01 1931 D!ChemWiUaryWOl0412A b CALIB-7 4/12/01 1946 D\ChemWillaryW010412Ab CALIB-8 4/12/01 20 00 D\ChemWillaryW010412Ab CALK-9 4/12/0120 15 D\ChemWillaryW010412Ab CALiB-10 4/12/01 2029 D\ChemWillaryWOl0412Ab SAMPLE 4/12/01 20 43 D \ChemWillary\H01041ZA b SAMPLE 4/13/01 7 02 D \ChemWiIlaryWO10412Ab SAMPLE 4/13/01 7 17 D\ChemWillaryWOl0412Ab WlB-11 4113101 7 31 D \ChemWillary\H010412A b CALIB-12 4/13/017 45 D ChemWillaryW010412Ab CALIB-13 4/13/01 8 W D ChemWdfaryW010412A b C4LlB-14 4/13/018 14 ~\ChemWiIIary~OlO4lZbA CALlB-15 4/13/01829 ~\ChemWillaryW010412Ab CALIB-16 4/13/018 43 D \ChemWillaryW010412A b CALIB-17 4/13/01 8 58 D\ChemWillaryW010412Ab CALIB-18 4/13/019 12 D~hemWiIIaryWOlO4lZAb CALlB-19 4/13101926 D ~ h e m W l l I a ~ W O l ~ l ? ACAbLlB-20 4/13/019 41 ~\ChemWilla1yW010412b~ SAMPLE 4113101 9 55 D \ChemWillaryW010412A b SAMPLE Ale HILL00160 HILLW17D HILL0016 D HILLWIO D HILLODZOD HILL0021D HILL0022D HILL0023 D HiLL0024D HILL0025 D HILL0026 D HILL0027 0 HILL0026 0 HILL0071 D HILL0072 D HILL0073 D HILL0074 D HIUW75 D HILL0076 D HILL0077 0 HILL0078 D HILL0079 D HILL0080 D HILLWBl D HILL0082 D HILL0083 D Sample N8me M uInfCompoundNa RT 0 nglmL PFOS in MeDH THPFOS 2 5 n$mL PFOS in MeOH THPFOS 5 nglmL PFOS in MeOH THPFOS In _ _ I lYfiYlllL .d&H r"C,n"EI l,l"l , THPFOS 25 n&L PFOS in MeOH THPFOS 40 n$mL PFOS in MeOH THPFOS 50 1 nglmL PFOS in MeO THPFOS 75 1 n$mL PFOS in MeO THPFOS 1W 2 n$mL PFOS in Me THPFOS 250 5 n$mL PFOS H)Me THPFOS 400 8 n$mL PFOS in Me THPFOS 501 n$mL PFOS in MeOH THPFOS 1002nwinL PFOSin Me0 THPFOS O n g G PFOS in M ~ O H THPFOS 2 5 ng/mL PFOS in MeOH THPFOS 5ngImL PFOS in MeOH THPFOS 10ngmL PFOS in MeOH THPFOS 25 ng/mL PFOS in MeOH THPFOS 40 n$mL PFOS in MeOH THPFOS M 1 n$mL PFOS In Me0 THPFOS 75 1 n$mL PFOS in MeO THPFOS 1W2 nglmLPFOS in Me THPFOS 250 5 nglmL PFOS in Me THPFOS 400 8 ng/mL PFOS in Me THPFOS 501 n$mL PFOS In MeOH THPFOS 1002n$mL PFOS In Me0 THPFOS Area 5 106 5 105 5 097 5 105 5.098 5.093 5 098 5.105 5.105 5.104 5.106 5.106 5.104 5 099 5 099 5096 5 098 5 099 5 092 5 092 5 098 5 085 5 09 5 099 5 097 5 084 Amount 101ffi80 254 1014600 254 1026197 254 1049688 254 1021353 254 1028355 254 1027805 254 1029130 254 1037720 254 1024280 254 1016328 254 1009794 254 lwD8lO 254 882895 254 892938 254 895922 254 899640 254 884732 254 9-30766 254 891237 254 894208 254 891115 254 885221 254 886337 254 884329 254 859618 254 Compound N i m l Area Amount PFOS 0 0 0 PFOS 5 323 55595 1292822 PFOS 5314 99110 344801 PFOS 5315 177299 7180735 PFOS 5308 488699 L J U U W PFOS 5303 ma2 3759613 PFOS 5308 980853 4789974 PFOS 5315 1465942 7243472 PFOS 5 315 1929805 95 25518 PFOS 5314 4613300 2361376 PFOS 5509 7015531 3672555 PFOS 5316 8452648 4490379 PFOS 5314 15272484 848646 PFOS 0 0 0 PFOS 5 309 53548 1559602 PFOS 5 307 98474 4135939 PFOS 53W 180965 8847021 PFOS was 5316 5302 474368 2617914 771667 4281933 PFOS 5302 9 6 W 5447431 PFOS 5308 1455847 8309964 PFOS 5296 1905711 1099345 PFOS 5308 4583269 2726371 PFOS 5309 6974946 4209773 PFOS 53 8448498 5156745 PFOS 5294 14868206 971 933 a AVeRGe: 888368.5077 10482.05486 %RSD: 1.2% 1154879 +30%: 621858 30%: 69% 72% 52% 84% 96% 96% 96% 84% ~2% 93% 85% 83% 88% 105% 107% 109% Ill% iim 109% 105% 103% 97% Inj Date Batch SampTypc 4/12/01 1722 OKhemWfllaryWO10412Ab SAMPLE 4/12/011735 D\ChemWiUaryWOl04lZ4b SAMPLE 4/12Xll20 58 D \ChemWiIlatyWOlC412A b SAMPLE 4/12/0121 12 D~hemWiIIaryW010412Ab SAMPLE 4/13/01 o 19 D\ChemWiIIaryW010412Ab SAMPLE 4/13/01 0 33 D \ChemWillaryWOlO412A b SAMPLE 4/13/01341 D\ChemW1IIary\H010412Ab SAMPLE 4/13/01 3 55 0!ChemWillaryWO10412Ab SAMPLE 4/13/016 33 D ChemWillaryWO1041ZA b SAMPLE 4/13/01648 D\ChemWllla~WOlMl2Ab SAMPLE 4/13/01 10 10 D\ChemWilla~OlC412Ab SAMPLE 4/13/01 1024 D\ChemWlllaryWO10412Ab SAMPLE Flle HILLW14.D HILL0015.D HILL0029 D HILL0030 D HILL0043.D HILL0044.D HILL0057.D HlLLW58.0 HILLW69.D HILL0070.D HILLO384.0 HILLW85.D Sample Name TNA 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN.A 4802 MeoH TN-A 4602 MeOH TNd4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Misc InlCompoundNa RT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound N a m l PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Am. 0 0 0 0 0 0 0 0 0 0 0 0 Amoum 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page 1 of 2 BACK TO MAIN H010412.xk e-- In1Dale Batch -4/12/01 21 26 D\ChemWillaryW010412Ab 4/12/01 21 41 D\ChemWillaryW010412Ab " , . . ln.* -"I&I I C L "" nlr*^-~U,I^-,Yn.n,.*.L "~"*","'.,,P',","'Y~'L~Y 4/12/01 22 10 D \ChemWillaryW0104124b 4/12/01 22 24 DChemWillafyW010412A b 4/12/0122 38 O\ChemW1IIaryWO10412Ab 4/12/0122 53 D\ChemWillaryWOl0412Ab 4/12/0123 07 D \ChemW~llaryW010412bA 4/12/01 2321 D\ChemWilIaryWO10412Ab 4/12/01 23 36 D \ChemWilIwWO104124 b 4/12/0123 50 D \ChemWillaryW010412Ab 4/13/01 005 DChemWillaly\HOl0412A b 4/13/01048 D\ChemWilIaryWOlC412Ab 4/13/01 1 02 D \ChemWilIaryWO10412Ab 4/13/01 1 17 o\ChemWillaryW010412Ab 4/13/01 1 3 1 DChemWinaryWOl0412A b 4/13/01 145 D\ChemWillaryWO10412Ab 4/13/01200 DChemWdIaryW010412Ab 4/13/01 2 14 D \ChemWdlaryW0104124b 4/13/01 229 DEhemW1llaryW010412Ab 4/13101 2 43 D\ChemWiIIaryWO10412Ab 4/13/012 57 D !ChemWillaryWOl04lZAb 4/13/01 3 12 DChemWillaryW010412A b 4/13/01 3 26 DChemWillaryW010412A b 4/13/014 09 D \ChemWillaryW010412b 4/13/01 4 24 D \ChemWillaryW010412Ab 4/13/01 4 38 D \ChemWilIaryWO10412Ab 4/13/01453 D\ChemWiII~O10412Ab 4/13/01 5 07 DChemWillaryW010412A b 4/13/01 521 DChemWillaryW010412A b 4/13/015 36 D\ChemWillaryW010412Ab 4/13/015 50 D ChemWdlaryW010412Ab 4/13/016 05 D \ChemWillaryW010412Ab 4/13/01 6 19 D\ChemWillaryW010412Ab SampTw SAMPLE SAMPLE E:".% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File HILL0031.D HILL0032.D I111 I ""** n ! IILL"Wa.Y HILL0034.0 HILL0035.D HILLW36.D HILLW37.D HILLW38.0 HILLW39.D HILL0040.D HlLLw41.D HlLLW42.D HILLW45.D HILL0046.D HILLOC47.D HILLW48 0 HILL0049 D HILL0050.D HILL0051.D HILLW52.D HILL0053 D HILL0054.D HILLW55.D HILL005S.D HILL0059.D HiLL0ffiO.D HILL0061 D HlLLW62.D HILLW63.0 HILLW64.D HILLW65.D HILL0066.D HILL0067.D HILLW68.D Sample Name MISSInfCompundNa RT Area 1311518441 THPFOS 5098 13115185s1 1 1 . 4 C."P -1 I* I l Y l u w t THPFOS -, .^?^^ I nrrVD 5 098 5 G92 1311-5186MS41 THPFOS 5086 1311-518741 THPFOS 0 1311-518841 THPFOS 5 085 1311518941 THPFOS 5 084 13115189MS41 THPFOS 51 131151soS1 THPFOS 5 091 1311-5191-S1 THPFOS 5 105 5 ng/mL PFOS in MeOH THPFOS 5 09 250 5 nglmL PFOSin Me THPFOS 5 093 1311 5 19 2 4 1 THPFOS 5 OW 13115192MS41 THPFOS 5 111 1311-520241 THPFOS 5 092 1311-5203-Sl THPFOS 5 084 1311520441 THPFOS 5 084 13IlS2MMS41 THPFOS 5084 13115205-SI THPFOS 5084 1311-52oaS1 THPFOS 5 092 1311-520741 THPFOS 5 083 13115207MS-S1 THPFOS 5084 5 nglmL PFOS in MeOH THPFOS 5 085 250 5 nghnL PFOS in Me THPFOS 5 092 1311520gS1 THPFOS 5084 1311-520941 THPFOS 5 083 1311521oS1 THPFOS 5 096 1311-5210MS41 THPFOS 5 084 1311-521141 THPFOS 5 091 1311-5212S1 THPFOS 5 091 1311-521341 THPFOS 5 09 13115213MSSl THPFOS 5 097 5 n@mL PFOS in MeOH THPFOS 5 099 250.5 ngmL PFOSin Me THPFOS 5 098 Amounl Compound NanUT 1421318 --_- . .^ 1386650 lJJJwLI 254 STD>130%PFOS 254 STD,130%PFOS 2- STD>,WhPFOS 1167677 254 STD>130%PFOS 0 0 ISTDc70% PFOS 1378613 254 STD,130%PFOS 1378731 254 STD>130%PFOS 1203962 254 STD>l30%PFOS 1027068 254 PFOS 843460 254 PFOS 933401 254 PFOS 809322 254 PFOS 1068135 254 PFOS 819845 254 PFOS 1481313 254 STD>lWhPFOS 1430325 254 STD>130%PFOS 1442269 254 STDrl30%PFOS 1273255 254 STD,130%PFOS 1406869 254 STD>130%PFOS 1404007 254 STD>130%PFOS 1398417 254 STD>IBO%PFOS 1228700 254 STD>l30%PFOS 1163680 254 STD>130%PFOS 1059764 254 PFOS 1078804 254 PFOS 1062929 254 PFOS I137098 254 PFOS 868940 254 PFOS 1076613 254 PFOS 1079410 254 PFOS 1083530 254 PFOS 872902 254 PFOS 882171 254 PFOS 851213 254 PFOS Ana 5.308 5308 5309 5 303 5 293 5 302 5 301 5318 5 301 5 315 53 5 303 5 316 5 322 5302 5 302 5 301 5 294 5 301 5 309 5 301 5 301 5 302 5 302 5 301 5 293 5 306 5 301 5 308 5 301 5 307 5 307 5 309 5 315 AlllOvnt 121664 2.881555 244130 7549882 154787 4341296 2811652 1241501 290916 0 303230 981694 261759 8262414 2936973 1258164 255948 1132774 265286 1470451 955% 3752122 4533055 2621838 142453 5346159 3212267 2045971 111849 2360961 91312 1759256 81813 1392345 2746281 1109w6 242229 7349539 188695 5399388 183603 5239191 2820818 1182271 95332 267728 4415425 2179421 327252 14 12675 266793 114209 193712 7255599 3239017 194376 342271 14 87953 531168 2389509 545049 2446187 3604117 2159226 101365 4393428 4585830 2840595 75 0% 104.7% 53 5% 87.0% 87 9% 1134% BACK TO MAIN RoI0412.xiS Sample Batch R0104012.b, analyzedon Rush 04-1241. PFOS AdsorbDecorb samples. Matrix: SolUSlglSed. Standard curve rang0 used for calibration of samples: 10-1002 nglmL (2.5,5 nglmL std not Included due to the hqher slmpia concentration range). Batch method: R010412.m Inj Date Batch 4/12/01 17:41 U:CneriiG~ijhL90!!%!2 b 4/12/01 1756 O:\ChemlRush\ROl041Z.b 4/12/01 1 8 : l O D:\ChemWush\R010412.b 4/12/01 18:24 D:\Chem\Rush\R010412.b 4/12/01 1639 D\Chem\Rush\R010412.b 4/12/01 1653 D:\Chem\Rush\R010412.b 4/12/01 1908 D:\Chem\Rush\RO10412.b 4/12/01 1922 O:\Chem\RushWOIM12.b 4/12/01 1936 O:\Chem\Rush\R010412.b 4/12/01 1951 D:Xhem\Rush\R010412.b 4/12/01 2005 D\ChemlRushlRO10412.b 4/12/01 20:19 D:\Chem\Rush\RO10412.b 4/12/01 20:34 D\Chem\Rush\ROIM12.b 4/13/01 1253 D\ChemWush\ROlWIZ.b 4/13/01 1397 O:\Chem\Rush\ROI0412.b 4/13/01 1322 D\Chem\Rush\ROI0412.b 4113iU1 1336 D:\Chem\Rush\R010412.b 4/13/01 1350 D:\Chem\RushWO10412.b 4/13/01 14.05 D\Chem\Rush\R010412.b 4/13/01 14:19 D:\Chem\RushR010412.b 4/13/01 1433 D:\Chem~ushWOl0412.b 4/I3/01 14:46 O:\Chem\Rush\RO1041Z.b 4/13/01 1502 D\Chem\Rush\R010412.b 4/13/01 1517 D:\Chem\RushWO10412.b 4/13/01 1531 D\Chem\Rush\R010412.b 4/13/01 1545 D:\Chem\Rush\RO10412.b SampWp. SAMPLE CALlE-I CALIB-2 CALlE-3 CALIE-4 SAMPLE CALlE-5 CALlB-8 CALlE-7 CALlB-8 SAMPLE CALIE-9 CALIE-10 SAMPLE CALlE-11 CALIE-12 CALiE-I3 CALlE-14 SAMPLE CALIE-15 CALIE-16 CALl8-17 CALlE-18 SAMPLE CALlB-19 CALlE-20 File RUSHDO17.D RUSHWi8.D RUSH0019.D RUSH00ZL.D RUSH0021.D RUSHW2Z.0 RUSH0023.D RUSHWZ4.0 RUSH0025.D RUSH00ZB.D RUSHW27.D RUSH00ZB.D RUSH0UZB.D RUSH0097.D RUSHOOS8.D RUSHW.D RUSH01OO.D RUSHOIO1.D RUSH0102.0 RUSH0103.D RUSH0104.D RUSHO105.D RUSHO1ffi.D RUSH0107.D RUSHOlO8.D RUSHOlM).O Sample Name 0 n&L PFOS in MeOH 2.5 ag.JmLPFOS in MeOH 5 nalml PFOSin MeOH 1 0 ng/mL PFOSin MeOH 25 ng/mL PFOS in MeOH 4 0 nglmLPFOSin MeOH 50.1 n g h L PFOSin MeOH 75.1 ng/mL PFOS in MeOH 100.2 ng/mL PFOS in MeOH 250.5 nglmL PFOS in MeOH 400.8 n g h L PFOSin MeOH 501 n@mLPFOSin MeOH 1002 ng/mL PFOSin MeOH 0 ng/mLPFOS in MeOH 2.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 10 ng/mL PFOSin MeOH 25 ng/mL PFOS in MeOH 4 0 nglmL PFOSin MeOH 50.1 ng/mL PFOS in MeOH 75.1 ng/mL PFOS in MeOH 100.2 n@mLPFOSin MeOH 250.5 ng/mL PFOS in MeOH 400.8 ng/mL PFOS in MeOH 501 ng/mL PFOS in MeOH 1W2 ng/mLPFOS in MeOH Misc InfCompounaT THPFOS THPFOS THPFOI THPFOS THPFOS THPFOS THPFOS THPFDS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Amount 5.583 598645 254 5.585 600613 254 5.5es m w s 254 5.593 600915 254 5.574 597942 254 5.58 601700 254 5.588 602030 254 5.577 604353 254 5.579 599001 254 5.587 592421 254 5.58 598537 254 5.581 586806 254 5.585 566i718 254 5.543 576686 254 5.554 579447 254 5.559 564774 254 5.551 585534 254 5.549 579681 254 5.551 577089 254 5.545 576872 254 5.555 579170 254 5.551 582102 254 5.558 578231 254 5.551 570124 254 5.553 566337 254 5.545 571690 254 CompoundlT PFOS PFOS PFOS PiOI PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area Amount 0 0 0 5.795 124534 0 5.788 162745 2.292686 57E9 2.16433 7.373546 5.777 479447 24.5.5608 5.783 712400 41.060268 5.784 860733 51.933337 5.774 1214934 78.281691 5.782 1517772 102.89232 5.79 3189495 251.02982 5.783 4665182 395.00116 5.785 5465982 494.621 5.788 9329369 1006.4382 0 0 0 5.784 108654 0 5.762 146886 1.502829 5.754 222698 6.829581 5.752 463425 24.442741 5.754 683988 41.135446 5.748 631833 52.479175 5.758 I172849 78.947857 5.755 1462631 103.52283 5.761 3120176 251.71766 5.754 4477040 398.70415 5.756 5297025 497.2204 5.746 9058485 999.91911 45.9% 73.7% 98.2% 102.4% 103.7% 104.2% 102.7% 100.2% 98.7% 30.1% 88 3% 97.8% 102.6% 104.7% 105.1% 103.3% 100.5% 99.2% Av0raqe: 587644.7 Std Dev: 11704.42 %RSD: 2.0% 763938 +30% 411351 -30%: IniD m Batch 4/12/01 17:13 D\Chem\Rush\ROlM12.b 4/12/01 1737 D:\ChemWushWOlMlZ.b 4/12/0120:M D:\ChemWush\R010412.b 4/12/0121:03 D:\Chem\Rush\R010412.b 4/13/01 a09 D:\Chem\Rush\R010412.b 4/13/01 024 D:\Chem\RushWO10412.b 4/13/01 3:31 D\Chem\Rush\R010412.b 4/13M1 345 D:\Chem~ush\RO10412.b 4/13/01 652 D:\Chem\Rush\R010412.b 4/13/01 7:06 D:\ChemRush\RO10412.b 4/13/01 916 D\Chem\RushW010412.b 4113/01 9:31 D\Chem\Rush\ROl0412.b 4/13/01 1209 D\Chem\RushR010412.b 4/13/01 1224 O:\Chem\Rush\R010412.b 4/13/01 1236 D\ChemRush\RO10412.b 4/131O1 16:W D:\Chem\RushROl0412.b 4/13/01 1614 D:\Chem\Rush\R010412.b SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File RUSH0015.D RUSH0018.D RUSH0030.D RUSHOO31.D RUSHW44.D RUSHOO45.D RUSHOO58.D RUSHOO59.D RUSHW72.D RUSHW73.0 RUSHWB2.D RUSHW83.D RUSHOOM.0 RUSHWO5.D RUSHOLW5.D RUSHO1IO.O RUSHO111.0 Sample Name TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4602 MeDH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Misc InfCornpounBT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFDS THPFOS THPFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compourib(T P\rea Amount PFOS 5.8 92075 0 PFOS 5.799 71408 0 PFOS 5.797 88361 0 PFOS 5.795 74724 0 PFOS 5.785 70265 0 PFOS 5.782 66840 0 PFOS 5.793 69743 0 PFOS 5.776 66261 0 PFOS 5.792 67260 0 PFOS 5.769 63670 0 PFOS 5.763 66988 0 PFOS 5.762 62760 0 PFOS 5.764 67549 0 PFOS 5.777 60061 0 PFOS 5.775 596W 0 PFOS 5.79 76873 0 PFOS 5.768 61967 0 Page 1of 2 n-0l (P (D u1 -4 0 0 -k -4 0 0 BACK TO MAIN R010412As Inj Date Batch SampType 4/12/01 21:17 D.\Chem\Rush\R010412.b SAMPLE 4/12/01 21:31 D\Chem\Rush\R010412.b SAMPLE ^ * . ~ 4/12/01 21:46 D:\Chem\Rush\R010412.b SAMPLE 4/12101 22:W D:\Chem\RushWOlM12.b SAMPLE 4,I L W I LL. D:',~.h.P~~\a~~Ph\ROlOl2.bSAMPLE 4/12/01 22:29 D:\ChemWush\RO10412.b SAMPLE 4/12/01 2243 D:\Chem\RushW010412.b SAMPLE 4112/01 2257 D:\Chem\RushWO10412.b SAMPLE 4/12/01 2312 D\Chem\Rush\R010412.b SAMPLE 4112M1 2326 D:\Chem\Rush\R010412.b SAMPLE 4/12/01 2340 D:\Chem\Rush\RO10412.b SAMPLE 4/12/01 23:55 D\Chem\Rush~O10412.b SAMPLE 4/13/01036 D:\Chem\Rush\ROl0412.b SAMPLE 4113/01052 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01 1:07 D:\Chem\RushROl0412.b SAMPLE 4/13/01121 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01 1:36 D:\Chem\RushW010412.b SAMPLE 4/13/01 150 D\Chem\Rush\R010412.b SAMPLE 4/13/01 2:04 D:\Chem\Rush\ROl0412.b SAMPLE 4/13/012:19 D\Chem\Rush\ROI0412.b SAMPLE 4/13/01 233 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 2:47 D\Chem\Rush\R010412.b SAMPLE 4/13/01 3 0 2 D:\Chem~ushWD1L?412.b SAMPLE 4/13/013:16 D:\Chem\Rush\R010412.b SAMPLE 4/13/01359 D:\ChemWush\R01041Z.b SAMPLE 4/13/01 4:14 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01428 D:\Chem\Rush\ROlMl2.b SAMPLE 4/13/01 4:43 D\Chem\RushWO10412.b SAMPLE 4/13/01 457 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 5:11 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01526 D:\Chem\Rush\ROl0412.b SAMPLE 4/13/01 5:40 D:\ChernWush\RO10412.b SAMPLE 4/13/01 5 5 5 D:\Chem\Rush\ROl0412.b SAMPLE 4/13/016:09 D:\ChemWush\ROl0412.b SAMPLE 4/13/01623 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 6:38 D:\ChernWush\RO10412.b SAMPLE 4/13/01 7:21 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01 735 D:\Chem\Rush\R010412.b SAMPLE 4113K)I 750 D:Fhem\RushU?010412.b SAMPLE 4/13/01 8:04 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 8:18 D\Chem\Rush\RO10412.b SAMPLE 4/13/01 8:33 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01 8:47 D:\ChemWushtR010412.b SAMPLE 4/13/01 9:02 D\Chem\Rush\R010412.b SAMPLE 4/13/01 9:45 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 l0:W D:\Chem\RushWO10412.b SAMPLE 4/13/01 10:14 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 1028 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01 10:43 D:\Chem\Rush\RO10412.b SAMPLE 4/13/01 1057 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 11:12 D:\Chem\RushWO10412.b SAMPLE 4/13/01 11:26 D:\Chem\RushW010412.b SAMPLE 4/13/01 11:41 D:\Chem\Rush\R010412.b SAMPLE 4/13/01 1155 D:\ChemWush\R010412.b SAMPLE File RUSH0032.0 RUSH0033.D RUSH0034D RUSH0035.D RUSHOO36.0 iiUSHGC37.D RUSH0038.D RUSHOO39.D RUSHOC4.D RUSHOOP1.D RUSH0042.D RUSHOOP3.0 RUSH0046.D RUSHWII7.D RUSHW(8.D RUSHOM9.D RUSHOO59.D RUSH0051.D RUSHOO5Z.D RUSHW53.D RUSHW54.D RUSH0055.D RUSHWS.D RUSHW57.D RUSHW60.D RUSH0061.D RUSM2.D RUSHo63.D RUSHW64.D RUSHW65.D RUSHOC66.D RUSHM167.D RUSHN68.D RUSW9.D RUSHO070.D RUSHW71.D RUSH0074.D RUSH0075.D RUSHW76.D RUSHW77.D RUSHW78.D RUSHW79.D RUSHW80.D RUSH0081.D RUSHOOB4.D RUSHCO85.D RUSHW66.D RUSH0087.D RUSHO088.D RUSHOOB9.D RUSHOO9O.D RUSHO091.D RUSHOO92.D RUSHm3.D Sampio Name 1311-5124-51 1311-512551 1311-512651 1311-5126MSS1 1311-5127-51 !?1-512&SI 1311-5129-51 1311-5129MSS1 1311-51X)-Sl 131I-5131-SI 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 1311-5132-SI 1311-5132MS-SI 1311-5133-SI 1311-513441 1311-513551 1311-5135MS-SI 1311-5136-S1 1311-5137-S1 1311-5138S1 1311-5138MSS1 5 ng/mL PFOS in MeDH 250.5 ng/mL PFOS in MeOH 1311-5139-S1 1311-514081 1311-5141-S1 1311-5141MSS1 1311-5142-SI 1311-514581 1311-5144-S1 1311-5144MS-S1 1311-514551 1311-514651 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 1311-5147-S1 13115147MS-S1 1311-5l45S1 1311-5149-S1 1311-5150S1 1311-5150MS-S1 5 nghL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 1311-5151-S1 1311-515241 1311-5153Sl 1311-5153MSSl 1311-5154-S1 1311-515551 1311-5156-51 1311-5156MSSl 5 ngmL PFOS in MeOH 250.5 n g h L PFOSIn MeOH Misc InfCompounMl THPFOS THPFOS THPFOS THPFOS THPFOS T-H.P_FOS InrF03 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFDS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Amount 5.58 677530 254 5.571 656863 254 5.557 633889 254 5.551 650748 254 5.568 615903 254 5.572 613221 254 5.5ES W 5 5 254 5.585 485715 254 5.567 594618 254 5.565 575974 254 5.572 592560 254 5.553 m 7 7 0 254 5.565 614288 254 5.557 483260 254 5.565 587357 254 5.565 585569 254 5.572 585514 254 5.565 477977 254 5.566 565186 254 5.567 580244 254 5.564 577866 254 5.562 480568 254 5.559 577392 254 5.572 578945 254 5.551 595025 254 5.55 639476 254 5.557 616815 254 5.559 496627 254 5.558 608824 254 5.551 600876 254 5.565 607245 254 5.559 554564 254 5.572 W380 254 5.545 588635 254 5.562 584267 254 5.561 584334 254 5.565 602683 254 5.556 481237 254 5.572 584694 254 5.571 579440 254 5.554 560769 254 5.565 464515 254 5.559 571261 254 5.551 577867 254 5.572 579739 254 5.561 567623 254 5.565 566068 254 5.549 451967 254 5.553 560862 254 5.568 547161 254 5.557 562481 254 5.554 446367 254 5.547 570884 254 5.558 584635 254 CompounRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.77 5.774 5.753 5.747 5.769 5.782 0 5,775 5.777 5.769 5.775 5.756 5.768 5.76 5.775 5.768 5.775 5.768 5.769 5.77 5.767 5.772 5.769 5.775 5.754 5.754 5.761 5.769 5.768 5.754 5.775 5.762 5.775 0 5.772 5.764 0 5.761 5.782 5.775 5.757 5.775 5.769 5.754 5.775 5.757 5.768 5.752 5.75 5.769 5.768 5.757 5.757 5.761 e-- A n a Amount 3454739 235.14955 3355208 235.64253 3182334 230.60435 6054164 493.84798 444477 21.144501 168978 2.504388 0 '0 235335 221.25701 480775 24.842763 373656 18.057138 158302 2.158669 3218501 256.73464 502482 25.246348 2628517 254.1411 1602422 112.23406 1852365 133.55448 1678850 135.81745 3662482 386.66394 1220182 a5.185002 1144435 76.528101 I130123 75.760492 3167549 321.0065 157432 2.385234 3179184 257.08626 2160001 157.04195 2298555 155.2245 2208338 154.50156 4097578 424.19511 1622807 109.20753 1479479 99.477125 1456259 96.43578 3859865 343.24391 214358 5.865127 0 0 152719 1.92182 3226476 258.79876 0 0 2325043 220.44504 1727840 123.26243 1311565 90.083398 1 9 m 7 5 152.50789 3830754 423.93446 155989 2.401694 3239422 263.57325 5190205 470.27597 5181003 481.76818 4993539 461.55284 6454778 867.49401 3101765 259.20449 3159998 273.24465 3121769 260.40515 4577579 559.64233 157988 2.553111 3184410 265.50363 43.2% 102.5% 47.7% 102.6% 38.4% 103.3% 48.0% 105.2% 51.1% 106.0% Page 2 of 2 BACK TO MAIN -0 Iu (cl tD SampleBatch HOlO3W.b, analyzed on Hlllay 010941. PFOSAdsorbitesorb sampl-. Standard curve range usad for calibration of samples: 5 4 0 . 8 nOlmLIN1n@mLctd not Includeddue to the low Sample conmntntionnnO.1. Batch mathod H010309.m gDab Balch SampType 3/9/01 19 38 D \ChemWllaryW010309b SAMPLE 3/9/01 19 49 D \ChemWllaryW010309b CALIB-1 3i9/0120 01 D \ChemW1llaryWOIO309b CALIB-2 3/9/0120 12 D \ChemWllaryW010309b CALIB-3 3I9m12024 D \ c h e m W r ~ W O l l w o sb CALIB-4 319/012035 D ChemWdlaryW010309b CAUB-5 3/8/0120 46 D ChemW1llaryW010309b CALIB-8 3/9/0120 58 D iChemWdiaryW010309b CALlB-7 3/9/0121 09 D \ChemWllary\H010309b CALIB-8 3/9/01 21 20 D iChemWllsryWOlO309b CALIB-9 3/9/0121 32 D IChernW1llaryW01030b9 CALIB-10 mrni21 43 D \ c h e m ~ ~ i i s r y ~ 0 1 0b3 rSnAMPLE 3 l W O 1 19 09 D iChemWilaryW0103O8b SAMPLE 3/10/01 1920 D \chemW1IlaryWO10309b CAUB-11 3H0101 1931 D \chemWdlaryWOlOJosb CAUB-12 310101 1943 DiChemW~llaryW01030b9 CALiB-13 310101 19 54 D !ChemWdlaryW010309b CAUB-I4 3/1010120 05 D \ChemWllaryW010309b CALIB-15 3lOlOl20 17 D \ChemWllaryW010309b CALIB-18 31WO120 28 D \ChemW1llaryWOlO309b CALK-17 31W012040 D\ChemW1llaryW010309b CAUB-18 311WO120 51 D \ChsmWilarvW010309b CCAUB 1 i l l w o l 2 1 o 2 D Ichemwll&W010309 b CAuB_i;D 3110101 21 14 D\Chem~~llaryW01030b9 SAMPLE 3101010 22 D \cr+emWdlaryUiOlO309b CCALIB-1 3101010 33 D \ChemWllaryWOIOM9b CCALIB-1 3101013 01 D \Cmn~111aryW0103b09CCALlB-1 3/10!013 13 D I C M m W d l a ~ l O M B bCCALIB-1 310,Ol 5 41 D \cr+emW8 oaryWO10309 b CCAUB-1 3110,Ol 5 52 D ChemW~iIaryWOlOJobs CCALlB-1 3110101 8 20 D ChemWIltaryWOIOJos b CCALIB-1 3 l O l O l 8 31 D ChemW#amryW0103Wb CCAUB-1 311W01 1059 D C h e m haryUiOlO309 b CCALIB-1 31WO1 11 11DCnem\h~laryW010309bCCAUB-1 3 l W O l 1339 D ChemklllaryW010309b CCALIB-1 31WO1 1333D\ChemW1laryW010309b CCAUB-1 3 1 0 I O 1 1607 D Chemw I a ~ O l bOCC~ALIB-1 310101 16 18 D iChemUidlaryW010%3 b CCAUB-1 3/1WO11823 D Ch.mWllsryWO10309b CCALIB-1 Fils HILLW21 D HlLLM22 D HlLLW23.D HlLLW24.D HlUW25.D HILLW2B.D HILL0027.D HILL0028.D HILLO029.D H1LLM)M.D HILLW31.D HILL0032.D HlLL0145.D HILLO148.D HiLL0147.D HlLL0148.D HILL0149.D HlLL0150.D HlLLO15l.D HILL0152.D HlLLO153.D HlLL0154.D HILL0155 D HILL0158 D Sample Nanm 0 nplmLPFOSInMeOH 2 5 ndmL PFOSIn MeOH 5 n@mLPFOS in MeOH r o i p l m L PFOSm M ~ O H 25 ndmL PFOS in MeOH 4 0 nplmL PFOSin MeOH 50 1nplmL PFOSIn MeOH 75 1n@mLPFOSin MeOH 1002 nplmL PFOSin MeOH 2 5 0 5 ndmL PFOSm MeOH 400 8 nplmLPFOSIn MeOH 501 nvmL PFOSin MeOH 0 nplmL PFOS in MeOH 2 5 nplmL PFOS in MeOH 5 nplmL PFOS in MaOH 1 0 n m L PFOS m MeOH 25 nplmL PFOSin MeOH 4 0 nplmL PFOS in MeOH 5 0 In@mLPFOS In MeOH 75 1n#mL PFOSIn MeOH 1002 nplrnLPFOSin MeOH 250 5 ndmL PFOSVI MeOH 4W 8 n&L PFOSin MeOH 501 nglmL PFOS in MeOH Misc Info Compound Name RT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area A w n 1 C-nd 5049 1.. 07.. 32_ 8.1 . 2-5~4 PFOS 5 041 1072804 254 PFOS 5.05 1108750 254 PFOS 5 042 1078385 254 PFOS 5 035 1076706 254 PFOS 5 039 1100085 254 PFOS 5 043 1076389 254 PFOS 5 038 1055026 254 PFOS 5 045 1081297 254 PFOS 5 044 1069673 254 PFOS 5 038 1034737 254 PFOS 5 036 1060528 254 PFOS 5 023 888821 254 PFOS 5015 870619 254 PFOS 5MK) 912239 254 PFOS 5 013 888038 254 PFOS 5 018 880755 254 PFOS 5 008 920893 254 PFOS 5 017 899188 254 PFOS 5 015 876702 254 PFOS 5 014 901682 254 PFOS 5W8 899022 254 PFOS 5W9 898706 254 PFOS 5014 899348 254 PFOS Name RT Ares 0 5 285 5 274 5.273 5.259 5.271 5.274 5.267 5.269 5.288 5.287 5.28 0 5.2u) 5.232 5.237 5.247 5.232 5.241 5.246 5.238 5.232 5233 5238 Amount 0 0 e 4 5 1 2.270782 143418 4.248778 231999 7.730027 622428 2254388 1029087 3723449 1260789 4890954 1838015 7078131 2464526 6343521 5867511 2338441 0794548 3733181 10677107 449 019 0 0 79381 2700768 150012 5873501 233970 9723374 607127 2710542 998520 4338523 1226451 5499273 1767880 8231103 2372952 108 4295 5738392 274 4434 8481603 417304 10729909 541 808 HILLCC46.D HlLLOM7.D HILL0080.D MLLWg1.D HlLLW74.D HlLLW75.D HILLW88.D HlLLW89.D HILL0102.D HlLLO103.D HILLOi1B.D HILLOll7.D HILWl29.D HILLOl3O.D HlLLO14l.D YII I"<AD n 5 nplmL PFOS in MeOH 250 5 nplmLPFOSIn MeOH 5 nglmL PFOSin MeOH 2 5 0 5 W m L PFOSII) MeOH 5 nplmL PFOSin MeOH 250 5 nplrnLPFOSin MeOH 5 W m L PFOSin MeOH 250 5 n m L PFOSinMeOH 5 nplmL PFOS in MeOH 250 5 ndmL PFDS m MeOH 5 nplmLPFOSin MeOH 250 5 nplmL PFOS in MeOH 5 nplmLPFOS m MeOH 250 5 nplmL PFOSm MeOH 5 nplmL PFOS in MeOH Amnaa: Std Dw: Wlk THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPEnS S83395.417 94153.7839 9.6% 5.029 5.031 5.028 5.029 5.027 5.023 5.028 5.021 5.033 5.035 5.017 5.021 5.02 5.017 5.014 s nia +30% 1278414 4% 608377 1094159 254 PFOS 1070122 254PFOS ' 1Mu793 254 PFOS 1-55 254 PFOS 968230 254 PFOS 978188 254 PFOS 922690 254 PFOS 806571 254 PFOS 909132 254 PFOS 908551 254 PFOS e89545 254 PFOS 872093 254 PFOS 888500 254 PFOS 870533 254 PFOS 888391 nnnn 254 PFOS Dcnc 5.253 5.262 5.252 5.253 5.259 5.247 5.253 5.245 5.257 5.288 5.241 5.245 5.244 5.241 5.238 5 Y,' 133354 3.9456 5758785 228.8809 143353 4.362347 5711018 228.462 137467 4856142 5853787 246.9623 138789 5.015913 5622338 258.1543 140178 5.256988 5838922 2883707 135055 5302078 5547134 273.4258 137470 5.423749 5593808 278.4058 141405 5.473911 .WA?I1A?Cd716 31- I 85% 77% m% 93% 94% 94% 92% 93% 93% 113% 97% 108% 108% 110% 109% 106% 110% 1M% 1W% 106% 105% 106% 106% 109% 108% 110% BACK TO MAIN Inj Date Batch SampType 39/01 1915 D:ChemWillaryW010304.b SAMPLE 3/9/01 1927 WChemWiUaryWOlO3.b SAMPLE 3/9/01 2155 D.ChemWiilaryW0103.b SAMPLE 319m122.0g D:ChemWlaryWOlO3.b SAMPLE 3/9/0122:17 DChemWiUaryW010309.b SAMPLE UlWOl 0:45 D:ChemWUIaryWOlO309.b SAMPLE UlWOlO.58 D:ChemWiUaryWOlO309.b SAMPLE UlW013:24 D:ChemWillaryWOlO30.b SAMPLE 3llWO1 3:M D:ChemWiliaryWol030.b SAMPLE 3110101 8:03 D:ChemWiUaryW01030.b SAMPLE U1M)l 6:15 D:ChemWillaryWOlO3W.b SAMPLE UlW018:43 DChernWUlaryW0103W.b SAMPLE U1M)l E54 DChemWdlaryWOlO3W.b SAMPLE 3 l l M l l 11'22 DChemW~laryWOlO3o9.bSAMPLE Uloml H:34 D : C h e m W i I l a ~ O l O ~ . SbAMPLE 3llMll l4:02 DChsmWillaryWOlo9.b SAMPLE UlOR11413 D:\wemWdlaryWOlo3oS.b SAMPLE U1M)l 16:30 D.ChemWtUaryWOlO3.b SAMPLE UlOm116:41 D:WemWillsryW010309.b SAMPLE Uloml 18:46 D:ChemWillaryWO10309.b SAMPLE Uloml 18.57DChamWillaryWOlo309.bSAMPLE UlOm121:25 DChemWillaryWO1030.b SAMPLE Re Sample Name HlUOO19.D HlLLO02D.D HlLLW33.D HlLLW34.D HlLLW35.D HILLM8.D HlLLW49.D HILLW82.D HlLW3.D HlLLW7E.D HILLW77.D HlLLW90.D HILLWIH.0 HIU104.D HlLLO105.D HlLLO118.D HlLLO119.D HlLLO131.D HlU0132.D HlUO143.D HIU0144.D HlU0157.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 M a O n TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Mi% l n b CompoundName RT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount CompoimdName RT Area 0 0 PFOS 0 0 PFOS 0 OPFOS 0 0 PFOS 0 0 PFOS 0 OPFOS 0 0 PFOS 0 0 PFOS 0 OPFOS 0 0 PFOS 0 OPFOS 0 OPFOS 0 OPFOS 0 OPFOS 0 OPFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 OPFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 5.33 0 5.315 0 0 5.315 0 5.301 0 5.294 0 0 0 5.303 0 0 0 0 0 0 0 5.28 Amount 20788 0 0 0 19572 0 0 0 0 0 9584 0 0 0 9498 0 0 0 9444 0 0 0 0 0 0 0 8875 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 17138 0 BACK TO MAIN InlDale Batch SampTp W 0 1 22.29 D:ChemWillarvui01030S.b SAMPLE 319101 22 40 DChsmWilla&\n010309b SAMPLE L9101 22 51 D ChomWllaryW010309 b SAMPLE M,01 23 03 D Chem%HdlaryW010309b SAMPLE u9101 23 14 D CnsmW.llaryW010309 b SAMPLE m o l 2 3 25 D CnemW1llaryW010309D SAMPLE Y9m1 23 37 D ChemHlaryw010309 b SAMPLE 39/0123 48 D ChemHi arvWo10309 b SAMPLE 31910123 59 D Chem\nllaryW010309b SAMPLE 510101 0 11 D ChemW.llsryW010309 b SAMPLE 3110,ol 108 D CnemWdlaryW010309b SAMPLE 3110101 1 19 D CnemVlll~yW010309S~AMPLE YlOlOl 130 D Chem~llaryV1010309b SAMPLE 3110101 1 42 D ChemMllaryW310309b SAMPLE 311OD1 1 53 D YlhemWI am010309 b SAMPLE 3110101 2 M D ChsmWo.aryWOlO309 b SAMPLE 3110101 2 16 D Chemhd ary\n010309 b SAMPLE 3110101 2 27 D IChemWdlaryW010309b SAMPLE 3110101 2 39 D CnemW llaryw010.309b SAMPLE 311Om12 50 D Ch.mw~llaryW010309b SAMPLE 310101347 D ChemHdlaryW010309b SAMPLE 3110,Ol 3 58 D ChomWdlaryWO10309b SAMPLE 3110101 4 10 D ~hembi~llaryWOlO30b9 SAMPLE 3110101 421 DYlhemWllaryW010309b SAMPLE 310101 4 32 D ChemWJlaryiHOlO309b SAMPLE 410101 444 DChsmiHllaryV1010309b SAMPLE JllOD1 4 55 D ChemHdla~010309b SAMPLE YlOlOl 5 06 D ChemWdlaryW010309b SAMPLE 311W15 18 DCbmW1IlaryWOlO309b SAMPLE Y l W 1 5 29 D ChemW,lla~OlO309b SAMPLE 311(u010 28 D ChemWI aryW010309 b SAMPLE Y101010 38 D Chsmui IlaryWO1Oy)Bb ?AMPLE 3110101 6 49 D Ch~mV(lla~W0103b09SAMPLE 31101017 W D Chernui.llaryW010~b SAMPLE 3110101 7 12 D CnemWillaryW010308 b SAMPLE YlOD17 23 D CnemW~llaryWO1Oy)Bb SAMPLE 3110101734 D CnemWllaryW010308b SAMPLE Y l W l 7 46 D CMmW#llaryHOlOMg b SAMPLE Flle Sample Nsme HILLW36.D HILLW37.D HILLW38.D HlLLW3S.D HlLLW4O.D HILLW41.D HlLLW42.D HILLOM3.D HILL0044.D HlLLW45.D HlLL0050.D HILLW51.D HlU0052.D H1LLWm.D HlLLW54.D HILLW55.D HILLWSB.D HlLLW57.D HILL0058 D HILL0059.D HILLWB4.D HlLLOCS5.D H1LLWBg.D HlUCC67.D HILLW68.D HILLCC69.D HlLLW70.D HILLW71.D HILLW72.D HILLW73.D HlLLW78.D HILLW79.D HILUKIE0.D HILLw8l.D HILLO082.D HlLLWC3.D H1LLW.D HlLLW85.0 EO013114109Sl E001311-4104-S1 E001311-4105-51 E00131141O~Sl-MS E00131141OgSl ECC-13114107S1 E0013114105S1 E0013114108SI-MS E0013114lO9-S1 E0013114110Sl E0013114111Sl E0013114111-S1-MS EW-1311-4112-S1 E0013114116Sl E001311411CS1 E001311411CS1-MS E0013114115S1 E0013114115S1 E001311-4117-Sl E0013114117-S1-MS E0013114115Sl E001311411aSl E00131141MS1 EW-1311412OSl-MS E001311403+S2 EO013114W5SZ E0013114OC6S2 E001311-402552 E001311403052 E m 1 3 11-4wcS2 E0013114035-52 E0013114l%-S2 E001311~S2 E001311-4059-52 E0013114060S2 EO01311 m S 2 E001311-4085S2 EW-1311- Mirclnfo CompoundNama RT Area Amount CwnpoundNsma RT Area Amount THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5034 5.03 5.042 5.029 5.038 5.035 5.028 5 029 5.027 5.031 5.028 5.029 5.035 5.029 5.032 5 028 5.028 5.028 5.029 5.023 5 028 5.m 5.022 5.023 5.027 5.028 5.028 5.029 5.031 5.029 5.028 5.03 5.028 5.022 5.027 5.029 5.021 5.027 1058178 1221819 1028589 074849 1488017 1055707 1050237 865Mo 1073533 1045079 1036444 869342 1043258 1053741 1654927 836338 1048939 1038327 1024948 865270 998797 1004358 1012808 843094 941893 914587 aiono 951757 912591 919151 924250 $24751 879571 869204 80&u? 870882 814404 889708 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 5.288 5.289 5.268 5.28 5.28 5.288 5 25 5.26 5.250 5.282 5.259 5.28 5.288 5.26 5.203 5 252 5.252 5.259 5.253 5.247 5.254 5.248 5.252 5.254 0 0 0 5.253 5.255 5 253 0 0 5.259 5 248 5.258 0 0 0 234470 215844 237536 3983142 452939 325164 304848 4611498 173898 178135 165195 3920789 170915 178264 330413 3890653 177753 181171 164575 3867704 leoBl8 178877 176413 3760328 0 8.012285 8.1698 8.375534 190.9872 11.53411 11.51244 10.78999 195.2088 5.573715 5.956354 5.488121 190.0809 5.646499 5788485 7.103971 196.3718 5.890369 6.081278 5.516164 188.3050 8.353969 6.139234 6068331 187.8729 0 0 270433 2641% 58201 0 2302809 0 10.5408 10.7588 1.571008 0 9.8320704 260133 290040 0 0 0 10.88282 13.58092 0 0 0 4 0 w BACK TO MAIN ... (Dale Bald? SarnpTypn 310101 7 57 D ChemWll~W010309b SAMPLE 310101 808 D\ChemWilla~W010309b SAMPLE 31M)19 06 D !ChemWdlaryWOl0308 b SAMPLE 31ox)19 17 D `ChemWdlaryWOlO308b SAMPLE 3/10101928D\ChernW~IhyWOl0308b SAMPLE 3101019 40 D ChernWdaryW010308b SAMPLE 310101 9 51 D ChemWlllaryW010309b SAMPLE 3110101 1003 D ChemWillaryWOlM09b SAMPLE 3/10/01 10 14 D ~hem~1llaryw0103b0eSAMPLE 3110101 1025 D \ChemWillaryWOI0309b SAMPLE 3110101 10 37 D ChemW~llaryW01030b9 SAMPLE 3lOIO1 1048 D V)hemWillaryW010309b SAMPLE 3110101 1145D\ChemWdlaryW010309b SAMPLE 3/1M)1 1156 D \ChernWillary\HO10308b SAMPLE 310101 1208 D \ChemWillaryW010329b SAMPLE 3110101 12 19 D ~hernW~llaryWOlcMOb9SAMPLE 3110101 12 30 D \ChemWllaryWOl[UO9b SAMPLE 3110101 1242 D \ChemWdlaryW010309b SAMPLE 311010112 53 D \ChemWllaryW010309b SAMPLE 31010113 05 D ChemWalaryWO10308b SAMPLE 31010113 16 D \ChemWtllaryWO10309b SAMPLE 3110101 13 27 D \Ch:hsmWdlaryW010308 b SAMPLE 310101 14 24 D \ChernWdlaryW010309b SAMPLE I 310101 14 38 D \ChernWillaryW0103Wb SAMPLE 3110101 1447 D ChemW1llaryW010308b SAMPLE 310101 14 59 D \ChemWlllaryW010309 b SAMPLE 3110101 15 10 DChernWdlaryWO1M09b SAMPLE 3101011521 D \ChemWllaryW010309b SAMPLE 310101 15 33 D\ChemWdIan/WafO309b SAMPLE 310/01 1544 D \ChemWdlaryW010308b SAMPLE 3110101 15 56 D \ChemW~llaryW01030b9 SAMPLE 310101 18 52 D \ChemWllsryW010309b SAMPLE 31m117 04 D \ChemWdIaryW010309b SAMPLE 311M)l 17 15 D \ChemWillaryW0103Wb SAMPLE Y1m1 1726D ChemWiUalyW010309b SAMPLE 310101 17 38 D ChemW1larvW010309b SAMPLE 3110101 17 49 D ChemWiUaryW010309 b SAMPLE 311m1 1601 D \ChernWillaryW010309 b SAMPLE 310101 18 12 D ChernWdlaryW0103Wb SAMPLE File HILL0086 D HILLMKI7.D HILLWO2.D HlLLW93.D HlLLWg4.D HlLLW95.D H1LLWW.D HILLW97.D HlLLW9B.D HILLOW9.D HILLO1W.D HILLO101.D HILLO1W.D HILLO107.D HlU0108.D HILL0109.D HILLO11D.D HILL0111.D HILL0112.D HILLO113.D HlLL0114.D HlLL0115.D HlLLO120.D HlLLO121.D HILL0122.D HILL0123.D HILL0124.D HlU0125.D HILL012B.D HlLLOl27.D HILLO128.D HlLL0133.D HILL0134.D HILL0135.D HILLO136.D HILL0137.D HILL0138.D HILL0139.D HILL0140 D Sample Name E00-1311-408BS2 EW-1311aSS2 EW-1311-4WOS2 EO0-1311-4094s2 E00.1311-408542 EW-1311-4WS2 EW-1311-411BS2 E00.1311-4119-S2 EO0-1311-4120-52 E00-1311-4W4-S3 EO0-1311-4W5S3 E001311-4W6-S3 EW-1311-402aS3 EW-1311430S3 EW-1311-4035S3 EW-1311-403e43 Em131 1-405aS3 EOC-1311-405943 E00-1311dOBOS3 E001311-4064S3 E001311-408553 EW-1311-4WS3 E m 1311-4088-53 EW-1311-408943 E m 1 3 11-4090.S3 E m 1311-4094S3 EW-1311-4085S3 EW-1311-408gS3 E m 1 3 114116S3 EW-1311-4119-S3 EW-1311-412C-S3 EW-1311-4w4s4 E00131145S4 E001311-400SS4 E00-1311-402BS4 E001311d030S4 EW-1311-403444 E001311435S4 EOC-1311-403SS4 IIII MircInfo Compound Name RT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Am 5028 5.028 5.03 5 043 5.046 5.035 5.042 Amount ComparndName RT Area 883099 871382 917602 858298 897083 8mw 874070 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 5252 5.250 5 254 0 0 0 5288 Amount 541521 495693 547710 0 0 0 357854 2456545 22.1668 23.31443 0 0 0 1564721 THPFOS 5.038 899818 254 PFOS 5 267 357623 1515864 THPFOS 5.038 802577 254 PFOS 5 267 411380 1754001 THPFOS 5.041 877509 254 PFOS 5 265 646257 2904183 THPFOS 5.034 849226 254 PFOS 0 0 0 THPFOS 5 028 898143 254 PFOS 0 0 0 THPFOS 5.029 871502 254 PFOS 5 253 244415 1039048 THPFOS 5.029 887421 254 PFOS 528 242159 1008219 THPFOS 5 028 878559 254 PFOS 0 0 0 THPFOS 5.029 762849 254 PKlS 0 0 0 THPFOS 5.029 889217 254 PFOS 5 253 101283 3720289 THPFOS 5.028 83Xl81 254 PFOS 5 252 130273 5345841 THPFOS 5.029 851383 254 PFOS 5 253 260840 1145682 THPFOS 5.028 e85697 254 PFOS 0 0 0 THPFOS 5.023 837808 254 PFOS 0 0 0 THPFOS 5.023 814470 254 PFOS 0 0 0 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPKlS THPFOS THPFOS THPFOS THPFOS THPFOS 5.018 5.014 5.022 5.02 5.021 5.013 5.023 5.013 5.021 5.014 5.008 5 014 838311 e81294 BMBo8 810228 819327 728839 8742W 878280 825208 640817 883425 893529 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 5 242 373687 17 14026 5 238 497521 2252588 5 248 491884 23.11219 I 0 0 0 0 0 0 0 0 0 II 5 247 5 245 199280 8.254569 118886 4.49281 5 245 928893 45.09718 0 00 0 0 I 0 0 0 0 THPFOS 5.015 824687 254 PFOS 5 248 27wO1 12.30281 THPFOS 5.014 976257 254 PFOS 5 238 223858 8.300946 THPFOS 5.013 823949 254 PFOS 0 0 0 THPFOS THPFOS 5.018 5016 8842w 823859 254 PFOS 254 PFOS I 0 0 0 0 0 0 BACK TO MAIN R010405 internalslacdard.ala Simple Batch ROlMOl.b, analyzedon HillaryMOB.01. PFOSAdsorblOerorb sampler. Matrix: SoiUSIgEed. Standard CYNO range used for calibnllona( sampler: 25-1002 ndmL Batch method: ROlMO5.d lnj D a b Batch 416101 13:07 D.ChemWurhWO1MOS.b 416101 1322 O.ChemWurhW010405.b 46/01 13 38 D:ChernWurhW010405.b 4WO1 13.50 D'Chem\RushW010405.b 4W01 14.05 D:ChemWurhW010405.b 4161011419 D'ChemWurhW010405.b 4W01 14% D.ChsmWushW010405.b 4/6x)1 14:48 D:\Chem\RurhW010405.b 46/01 1502 D:ChemWurhWO1MOS.b 4/6/01 15.17 D:ChemWushW0104OS.b 41BM11531 O:\ChemWushW010405.b 4,5101 15.45 D:ChemWurhW010405.b 4/6/01 16.00 D:\ChemWurhW010405 b 4/7/01623 DChemWurhWO1MOS.b 4/7/01 6.37 D.ChemWurhW010405.b 4/7/016 5 2 D:ChemWushW010405.b 4/7/017:06 D.ChemWurhW010405.b 4/7/01 7:20 D.ChemWushWo10405.b 4/7/01735 D:ChemWushW010405.b 4mU1 7.49 D:ChemWurhW010405.b 4/7/01 8.04 D.ChemWushWO10405.b 4/7/01 8.18 D.ChsmWurhW010405.b 4/7/018:32 D:ChemWurhU7010405.b 4l71018.47 D.ChemWurhW010405b 4/7/01 9:01 D:ChemWurhW010405.b W / 0 1 9.15 DChemWurhW010405.b SarnpTyp SAMPLE CAUB-1 CALlB-2 CALiB-3 CAUB-4 SAMPLE CAUB-5 CALIB-8 CALIB-7 CALIB-8 SAMPLE CAUB-9 CAUB-10 SAMPLE CALlB-11 CALK-I2 CALIB-13 CALIB-14 SAMPLE CAUB-15 CAUB-18 CALIB-17 CALlB-18 SAMPLE CALlB-IS CALIB-20 File SamplcName RUSHW17.D 0 ndmLPFOSin MeOH RUSH0018 D 2.5 WmL PFOS in MeOH RUSH0019.D5 ndmLPFOSin MeOH RUSHW2O.D10 na/mLPFOS in MeOH RUSHW21.D25 ngmLPF0S in MeOH RUSHW22.D40 ndmLPFOSin MeOH RUSHW23.0 50.1 WImL PFOS in MeOH RUSHW24.D 75.1 ndmL PFOS in MeOH RUSHW25.D100.2 WmL PFOS m MeOH RUSH0026.D250.5 n#mL PFOSin MeOH RUSHW27.D 400.8 ndmLPFOSin MeOH RUSHOO28.DW1 nphnL PFOSin MeOH RUSHW29.D1002 n#mL PFOSin MeOH RUSHW89.00 nglmLPFOSin MeOH RUSHW0.D 2.5 nglmLPFOS inMeOH RUSH0091.D5 W m L PFOSin MeOH RUSHW92.D 10 ndmL PFOS in MeOH RUSHW93.0 25 ndmL PFOS in MeOH RUSHW94.D4 0 ndmLPFOSinMeOH RUSH0095.D 50.1 nmL PFOS in MeOH RUSHW9B.D 75.1 WmL PFOS in MeOH RUSHW97.D 100.2 ndmL PFOS in MsOH RUSHW88.D 250.5 ndmL PFOS in MeOH RUSHW9S.D400.8 W L PFOS in MeOH RUSHO1W.D 501 ndmL PFCS in MeOH RUSHOIO1.D 1002 WmL PFOS in MeOH Miss InfCompound NiRT ARI THPFOS 5.573 THPFOS 5.572 THPFOS 5.563 THPFOS 5 577 THPFOS 5.571 THPFOS 5.573 THPFOS 5.568 THPFOS 5.563 THPFOS 5.557 THPFOS 5.573 THPFOS 5.504 THPFOS 5.561 THPFOS 5.588 THPFOS 5.573 THPFOS 5.568 THPFOS 5.553 THPFOS 5.57 THPFOS 5.561 THPFOS 5 559 THPFOS 5.557 THPFOS 5554 THPFOS 5.561 THPFOS 5.558 THPFOS 5.56 THPFOS 5.545 THPFOS 5.551 Amount 539235 254 541201 254 530210 254 544175 254 556935 254 575120 254 555475 254 580525 254 564583 254 554331 254 56uBB 254 5m7 254 551338 254 559057 254 550680 254 533382 254 556117 254 553124 254 576802 254 550084 254 548419 254 553360 254 5-97 254 544285 254 580621 254 525351 254 Compamd PFOS PFOS. PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS NaAT 0 5.775 5.767 5787 5.774 5.778 5.769 5.788 5.78 5.778 5767 5.764 5.771 0 5.785 5.783 5.773 5.771 5.762 5.787 5.784 5.764 5.768 5.764 5.755 5.754 Area Amount 0 0 1456~ o 177598 0 255188 4252916 520711 26.14883 778358 46.19528 8mxa Y).~I.so~ 1254456 897- 1593523 119.474 3289063 289.5214 4814176 446.0827 5878253 542.0292 9480515 1071.163 0 0 llSW)2 0 142789 0 210206 o.031512 430360 18.72559 643226 34.73718 755748 47.18652 1044359 73.14746 I341441 99,1613 2714138 242.7803 4031839 377.1597 4912948 461.7658 7877904 9030327 -__ Awanaa: 552630.6823 Std Day: 14747.09534 XRSD: 27% 718420 *30%: 388841 -30% ox 43% 105% 115% 117% 120% 119% 116% 111% 108% 107% ox ox 75% 87% 94% 97% 99% 97% 84% 82% 90% In1 Dab Batch 4W01 12 39 D ChemWurhW010405b 4/6/01 12 53 D ChemWushW010405b 416l01 16 14 D \ChemWurhW010405b 4/6/01 1629 0 ChemWurhW010405b 4/6/01 19 35 DChemWushW010405b 416101 19 50 D ChemWurhW010405b c, 4/13/01 22 57 D \ChemWurhW010405b 41610123 11 DChemWushW010405b 3 $ 4/7/01 2 I 8 D ChemWushW010405b 4/7/01 2 33 D ChemWushW010405b 4/7/01 5 40 D ChemWurhW010405b 4/7/01 5 54 DChemWurhW010405b 4/71016 W D ChemWurhWO104OSb 4/7/01 9 30 D ChemWushW010405b 3- 4/7/01 9 44 0 ChemWushW010405b S.mpTyw SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File Sample Name RUSHWIS D TN-A 4802 MeOH RUSHWl6 D TN-A 4802 MeOH RUSHW3O D TN-A 4802 MeOH RUSH0031 D TN-A 4802 MeOH RUSH0044D T K A 4802 MeOH RUSH0045 D TN-A 4802MeOH RUSH0058 D TN-A 4002 MeOH RUSH0059 OTN-A 4802 MeOH RUSHW72D TN-A 4802 MeOH RUSH0073D TN-A 4802MeOH RUSH0088 D TN-A 4802 MsOH RUSHW87D TN-A 4802 MeOH RUSHW88D T K A 4802 MeOH RUSH0102D TN-A 4802 MeOH RUSH0103D TN-A 4802 MeOH a -- MISCInfCompound NaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Am. 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Compound NIAT PFO.S~ PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Ana 5.78.5. 5.781 5 79 5.774 5.781 5.798 5.776 5 775 5 763 5.788 5.778 5.784 5.775 5.782 5.765 Anl0"nt 1oB775 0 91018 0 103874 0 84825 0 82678 0 78114 0 82141 0 76802 0 76352 0 71081 0 74008 0 89593 0 87762 0 83254 0 64445 0 page 1 Of 2 BACK TO MAIN Inj D a b Batch 416101 16:43 D.ChemWurhW010405.b 4/6/01 1857 O.Chem\RushWO10405.b 416101 17:12 DChemWurhWO1MOS.b 4/6/011726 D:ChemWushWOlM05.b 416101 17:40 D ChemWurhW010405.b 4/6/01 1755 DChernWurhV7010405.b 4iM)l l a 09 D.Chern'b?urhW010405.b 4/6/01 1823 D ChamWushW010405.b 4/6/01 1 8 : s D ChemWurhW010405.b 4/6/01 1852 D.ChemWurhW010405.b 4/6/01 1907 O:ChemWurhW010405.b 4/6/01 19.21 D.ChemWurhW010405.b 4/6/01 2O:M D.ChemWurhW010405.b m m l 20.18 O:~emWurhW010405.b 4/6/01 20:33 D\ChemWurhWOl0405.b 4161012047 O:ChemWushW010405.b 4/6/0121:02 DChemWurhW010405.b 4m121:16 D.Chem\RushW010405.b 4/6/0121:30 D.ChemWurhW010405.b 416101 21'45 D.ChernWurhW010405.b 4/6/0121:59 D:ChemWurhW010405.b 4/6/01 2213 O:\ChernWurhW010405.b 416101 22:28 D:ChernWushW010405.b 4/6/0122:42 D:bChernWurhWO10405.b 416101 23:25 D:ChernWurhW010405.b 4/6/01 2340 DChemWurhW010405.b 4/6/01 23% DChemWurhW010405.b 4/1/01 009 D:ChemWurhLQ010405.b 4/7/01 023 DChemWurhW010405.b 4!7/01 0'37 D:ChemWurh!R010405.6 4/7/01 052 VChemWurhW010405.b 417101 1.mO:ChemWushW010405b 4l7101 1 2 1 D:ChemWurhW010405.b 4nm1 1'35 DChemWurhWO10405.b 4I7/01 1:49 DChemWurhWO104OS.b 4/7/01 2:04 O:\ChemWushW010405.b 4,7101 247 D:\ChernWurhW010405.b 4/7/01 301 D:ChernWurhW010405.b 4/7/01 316 D:\ChsmWushW010405.b 4/7/01 3:30 DChernWurhW010405.b 4mo1 3 4 5 D:ChemWurhW010405b 4/7/013.59 D:ChernWushW010405.b 4!7/01 4:13 D:ChemWurhW010405.b 4/7/014128 D:ChemWushWOl0405.b 4/7/01 4:42 D:ChemRurhW010405.b 4/7/01457 D:ChemWurhW010405.b 417101 511 D.ChemWurhW010405.b 47/01 5.25 O.ChemWushW0>0405.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE ...-RUSHW32.D Study Number E001311 RUSHW33.D Study Number Em1311 RUSHW34.D Study Number Em1311 RUSHW35.D Study Number Em1311 RUSHW3f.D Study Nvnber EoO-1311 RUSHW37.D Study Nvmber Em1311 RUSHW38.D Study Number E001311 RUSHOO39.D Study Numbsr EM)-1311 RUSH0040.DSludy Nwnber Em1311 RUSHW41.D Study Number Em1311 RUSHW42.D 5 ndmL PFOS in MeOH RUSH0043.D250.5 WmL PFOSin MeOH RUSHW46.D Study Number Em1311 RUSHW47.D Study Number Em1311 RUSHW48.D Study Number E001311 RUSHW49.D Study Number Em1311 RUSHW50.D Study Number Em1311 RUSHW51.D Study Number Em1311 RUSHW52.D Study N h r Em1311 RUSHW53.D Study NumberE00-1311 RUSHW54.D Study Number Em1311 RUSHW55.D Study Number Em1311 RUSHW56.D 5np/mLPFOSin MeOH RUSHW57.D 250.5 ndmL PFOSin MeOH RUSHW3J.D Study Number E001311 RUSHWB1.DSludy Number Em1311 RUSHWB2.DSludy Number EW-1311 RUSHWB3.DStudy Number Em1311 RUSHWg4.D Study Number Em1311 RUSHWB5.0 Study Number Em1311 RUSHWBBDStudy Number Em1311 RUSHWB7.D Study Number EOQ1311 RUSHW@a.D Sludy Number Em1311 RUSHWB9.D Study Number EW.1311 RUSHW7O.D 5 n@mLPFOS in MeOH RUSHW71.D 250.5 n W L PFOS in MeOH RUSHW74.D Sludy NumbsrEW.1311 RUSHW75.D Study Number E001311 RUSHW78.D Study Number EW-1311 RUSHW77.D Sludy Nvmber Em1311 RUSHW78.0 Study Number Em1311 RUSHW79.0 Study Number Em1311 RUSHW60.D Study NumberEmlSll RUSHW81.D Sludy Number E001311 RUSHW82.D Study Number EMJ-1311 RUSHW83.D Sludy Number E001311 RUSHW04.D 5 n@mLPFOS in MeOH RUSHWS D 250.5 n$mL PFOS in MeOH M i s s InfCompound NaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area 5.567 5.569 5.565 5.567 5 559 5.584 5.583 5.571 5.572 5.571 5.559 5.582 5.568 5.558 5.565 5.554 5.548 5.559 5 551 5.561 5.568 5.589 5.564 5.572 5.561 5.57 5.585 5.561 5.568 5.581 5.551 5.565 5.567 5.561 5.547 5.558 5.58 5.561 5.549 5.557 5.552 5.544 5.562 5.546 5.549 5.547 5.552 5.556 Amount 549855 254 546340 254 551952 254 543988 254 556241 254 556138 254 557637 254 467615 254 560192 254 553257 254 577885 254 567895 254 558163 254 546057 254 558505 254 554244 254 550460 254 539432 254 547053 254 559047 254 549045 254 543576 254 563324 254 586595 254 551418 254 563119 254 551121 254 533687 254 559718 254 53ao81 254 549935 254 538497 254 548482 254 552442 254 544700 254 549811 254 539554 254 530879 254 538799 254 550408 254 540857 254 518943 254 538710 254 544277 254 552811 254 537904 254 544157 254 535679 254 Compaund N a A T PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Ana 5.77 . 5.765 5.768 5.777 5.762 5.774 0 5.762 5.775 5.781 0 5.765 5.776 5.761 5.775 5.757 5.749 5.769 5.762 5.784 5.769 5.792 0 5.775 0 0 0 5.771 5.778 5.771 5.761 5.768 0 0 0 5.759 0 5.764 0 0 5.762 5.747 5.773 5.756 5.752 5.757 0 5.759 Amount 692574 41.69038 614092 35.16084 997270 68.33123 3033445 268.9711 266CQ8 4884134 512785 2553805 0 0 2253516 226.2934 358332 12.22107 341742 11.19223 0 0 3181790 270.4896 MBBMl 8.188777 2580190 221.0756 800286 50.04657 921208 61.22001 965W3 65.68839 2988304 286.8858 219943s 182.5878 2324379 190.9588 2803069 242.2878 4426533 422.8252 0 0 3078172 280.7912 0 0 0 0 0 0 2297114 197.9487 305322 7.818031 269990 5.7797 280197 6.14042 2329314 199.9928 0 0 0 0 0 0 2913840 253.3329 0 0 2181139 187.322 0 0 0 0 218149 1.206327 2172754 191.5886 736133 47.25497 855021 57.65922 981309 66.77087 2761164 243 8076 0 0 2787890 247.8607 0 0% 108.wC 0.0% 104.1% 0 0% 101.1% 0 0% 98 9% page 2 Of 2 BACK TO MAIN -u a, M (D Sample Batch ROlM02b.b. analyzed on Rush 04-02-01. PFOS Adso~WDesorbsamples. Patrlx: SoiNSiglSed. Standard curve nnoe used For calibntion of samples: 101002 n g h l (25 and 5 nglmL std not Included due to the higher sample concentration range). Batch method: R010002b.m c. f h Inj Date Batch 4/3/01 8 10 D \Chem\Rush\RO10402b 4/3/01 8 24 D \Chem\Rush\RO10402b 4/3/01 8 38 D \Chem\Rush\R010402 b 4/3/01 8 53 D \Chem\Rush\ROlM02 b 4/3/01 9 07 D \Chem\Rush\R010402 b 4/3/01 9 21 D \Chem\Rush\R010402 b 4/3/01 9 36 D lCChemIRushlQO10402b 4/3/01 9 50 D \Chem\Rush\R010402 b 4/3/01 10 04 D \Chem\Rush\R010402 b 4/3/01 10 19 D \Chem\RushU7010402b 4/3/01 1033 D\Chem\Rush\RO10402b 4/3/01 10 48 D \Chem\Rush\R010402 b 4/3/01 11 02 D\ChemUiush\R010402b 4/3/01 22 19 D\Chem\Rush\RO1040Zb 4/3/01 22 33 D \Chem\Rush\R010402 b 4/3/01 22 47 D \Chem\RushR010402 b 4/4/0123 02 D \Chem\Rurh~0104Mb 4/4/01 23 16 D \Chem\Rush\R010402 b 4/4/01 23 30 D \Chem\Rush\R010402 b 4/4/01 23 45 D \Chem\Rush\R010402 b 4/4/01 10 08 D \Chem\Rush\R010402 b 4/4/01 10 22 O\Chem\Rush\RO10402b 4/4/01 10 37 D \Chem\Rush\R010402 b 4/4/01 10 51 D\Chem\Rush\R010402b 4/4/01 11 05 D \Chem\Rush\R010402 b 4/4/01 11 20 D\ChemWush\RO10402 b SampType SAMPLE CALlB-1 CALlB-2 CALlB-3 CALIB-4 SAMPLE CAM-5 CALlB-6 CALl8-7 CALl8-8 SAMPLE CALIB-9 CALlB-10 SAMPLE CALlB-11 CALIB-12 CALlB-13 CALIB-14 SAMPLE CALF-15 CALIB-16 CALlB-I7 CALlB-18 SAMPLE CALIB-19 CALlB-20 File RUSH0104 D RUSH0105 D RUSH0106 D RUSH0107 D RUSH0108 D RUSH0109 D RUSH0110 D RUSH0111 D RUSH0112 D RUSH0113 D RUSH0114 D RUSH0115 D RUSH0116 D RUSH0163 D RUSH0164 D RUSH0165 D RUSH0166 D RUSH0167 D RUSH0168 D RUSH0169 D RUSH0170 D RUSH0171 D RUSH0172 D RUSH0173 D RUSH0174 D RUSH0175 D Sample Name 0 ndmL PFOS in MeOH 2 5 & n L PFOS in MeOH 5 ng/mL PFOS in MeOH 1 0 ng/mL PFOS in MeOH 25 ng/mL PFOS in MeOH 4 0 n@mLPFOS m MeOH 50 1 ndmL PFOS K) MeOH 75 Ing/mL PFOS m MeOH 1W 2 ng/mL PFOS in MeOH 250 5 nglmL PFOS in MeOH 4W 8 n@mLPFOS in MeOH 501 n@mLPFOS in MeOH 1002 ng/mL PFOS in MeOH 0 n@mLPFOS in MeOH 2 5 ng/rnL PFOS in MeOH 5 ng/mL PFOS in MeOH 1 0 ng/mL PFOS in MeOH 25 nglmL PFOS 111 MeOH 40 n@mLPFOS m MeOH 5 0 1 ng/mL PFOS in MeOH 75 1 n@mLPFOS in MeOH 1W 2 n@mLPFOS in MeOH 250 5 n@mLPFOS in MeOH 400 8 ng/mL PFOS in MeOH 501 ng/mL PFOS in MeOH 1002 n@mLPFOS in MeOH Yisc InCompoun RT Area THPFOS 5.545 THPFOS 5546 THPFOS 5 558 THPFOS 5 553 THPFOS 5 553 THPFOS 5 543 THPFOS 5 553 THPFOS 5 55 THPFOS 5 541 THPFOS 5544 THPFOS 5546 THPFOS 554 THPFOS 5 542 THPFOS 5 537 THPFOS 5544 THPFOS 5 548 THPFOS 5 551 THPFOS 5 53 THPFOS 5 551 THPFOS 5 559 THPFOS 5 625 THPFOS 5 609 THPFOS 5 599 THPFOS 5 595 THPFOS 5 594 THPFOS 5 593 Amount 691265 254 707691 254 726641 254 702679 254 71 1476 254 695068 254 697300 254 709991 254 709014 254 744829 254 710505 254 719310 254 745057 254 619245 254 643440 254 655629 254 629187 254 639165 254 649746 254 65031 1 254 717155 254 86050 254 714495 254 69513 254 683159 254 707430 254 CompounRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area Amount 0 0 0 5.756 192592 0 5.768 249725 1.588495 5.757 339511 7.167098 5.756 641983 24.24615 5.739 905841 41.026119 5.749 1085138 51.837004 5.753 1535613 78.469104 5.744 1912604 102.76639 5.747 4147318 246.4199 5.749 5754500 391.55477 5.743 6939227 488.84633 5.745 12088828 974.5569 0 0 0 5.747 181340 0 5.75% 238783 2.406374 5.754 311745 7.661761 5.733 614103 26.666053 5747 872886 42.7321109 5.762 1054849 54.680469 5 828 1572840 79.825492 5.819 1906689 106.54576 581 4102314 255.81083 5.805 5711729 418.05536 5.797 6776340 506.61571 5.795 11937411 1028.811 31 8% 71 7% 97 0% 102 3% 103 5% 104 5% 102 6% 98 4% 97 6% 48 I % 76 6% 1067% 1066% 109 1% 106 3% 106 3% 102 1% 101 1% Avenqe: 689821.2108 - _ Std Dev: 34866.78097 YRSD: 5.1% 895768 +30% 482075 -30%: Page 1 of 3 BACK TO MAIN Sample Batch R010402b.b. analyzedon Rush 04-0201. PFOS A d s o M e r o r b samples. Matrix: SoiWSlglSed. StandardC U N ~ranne used for calibrationof samDIes: 10-1002n d m L 125 and 5 nglmLstd not includeddue to the higher sample concentrationrange). Batch method ROib40Zb.m Inj Date Batch SampType File Sample N u m Miac InCompoun RT Area Amount 4/3/01 7 41 D \Chem\Rush\R010402b SAMPLE RUSH0102 D TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 7 55 D \Chem\Rush\R010402b SAMPLE RUSH0103 D TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 11 16 D \Chern\Rush\RO10402 b SAMPLE RUSH0117 D TN-A 4802 MeOH THPFOS 0 0 0 413101 11 31 D \Chem\Rush\R010402b SAMPLE RUSH0118 D TN-A 4802 MeOH THPFOS 0 0 0 4/3/011145 D\Chem\Rush\R010402b SAMPLE RUSH0119 D TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 14 52 D\Chem\Rush\R0104M b SAMPLE RUSH0132 D TN-A 4802MeOH THPFOS 0 0 0 413/01 1507 O\Chem\Rush\R010402b SAMPLE RUSH0133 D TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 18 14 D \Chem\Rush\R010402b SAMPLE RUSH0146 D TN-A 4802 MeOH THPFOS 0 0 0 40101 18 28 D\Chern\Rush\R010402b SAMPLE RUSH0147 0 TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 21 35 D \Chem\Rush\ROlM02 b SAMPLE RUSH0160 D TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 21 50 D \Chem\Rush\RO10402 b SAMPLE RUSH0161 0 TN-A 4802 MeOH THPFOS 0 0 0 4/3/01 22 04 D \Chern\Rush\RO1MOZ b SAMPLE RUSH0162 D TN-A 4802 MeOH THPFOS 0 0 0 4/4/01 11 34 D\Chem\Rush\ROlMOZb SAMPLE RUSH0176 D M A 4802 MeOH THPFOS 0 0 0 4/4/01 1149 D \Chem\Rush!RO10402 b SAMPLE RUSH0177 D M-A4802 MeOH THPFOS 0 0 0 CompwnRT Area Amount PFOS 5.772 131207 0 PFOS 5.764 128138 0 PFOS 5.768 153626 0 PFOS 5.771 130584 0 PFOS 5.764 126241 0 PFOS 5.764 130330 0 PFOS 5.765 119843 0 PFOS 5.763 122906 0 PFOS 5.77 120557 0 PFOS 5.761 145239 0 PFOS 5.764 143817 0 PFOS 5.768 144439 0 PFOS 5.818 154900 0 PFOS 5.824 133822 0 Page 2 of 3 BACK TO MAIN Sample Batch ROlWZb.b, analyzed on Rush 0 4 0 2 0 1 . PFOS AdsorbiDesorb samples. Mab'ix: SoiUSlglSed. Standard curve range used for calibration of samples: 10-1002nglmL(2.5 and 5 ng/mL s l d not included due to the higher sample concentration range). Batch method R010402b.m Inj Dale hlch Samplype File Sample N a m Misc In Compoun RT Area Amount Compoun RT Area Amount 4/3/01 1159 D:\Chem\Rush\R010402.b SAMPLE RUSH0120D Study Number EW-1311 THPFOS 5 554 725886 254 PFOS 5757 978597 42932438 4/3/01 12:14 D:\Chem\Rush\ROIO402b. 4/3/01 12:28 D:\Chem\Rush\R010402.b SAMPLE SAMPLE RUSH0121 D Study Number EW-1311 RUSH0122 D Study Number EW-1311 THPFOS THPFOS 5 547 5 558 690051 254 701604 254 PFOS PFOS 5 7 5 933343 43 120798 5761 940734 42621787 4/3/01 12.43 D:\Chem\Rush\R010402b SAMPLE RUSH0123 D Study Number EW-1311 THPFOS 555 577118 254 PFOS 576 3533131 27670087 4/3/01 1257 D:\Chem\Rush\RO10402.b 4/3/01 13:Il D:\Chem\Rush\RO10402.b 4/3/01 1326 D:\Chem\Rush\R010402b 4/3/01 13:40 D:\Chern\Rush\R010402.b 4/3/01 13.55 D:\Chern\Rush\R010402b 4/3/01 14.09 D.\Chem\Rush\R010402.b 4/3/01 14:23 D:\Chem\RushW010402.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0124 D RUSH0125 D RUSH0126 D RUSH0127 D RUSH0128 D RUSH0129 D RUSH0130 D Study Number EW-1311 Study Number EW-1311 Study Number EW-1311 Study Number EW-1311 Study Number EW1311 Study Number EW-1311 5 ng/mL PFOS in MeOH MPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5 558 5 554 5 552 5546 5 553 5 552 5 549 667527 254 674789 254 668248 254 550211 254 652849 254 655706 254 680355 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5754 5 757 5755 5749 5749 5 755 5759 2610383 2478325 2680467 4917918 5170053 5129723 253055 16075044 149 07W8 1657409 44349026 38056422 374 88948 2715008 4/3/01 1438 D:\Chem\Rush\R010402.b 4/3/01 1521 D:\Chem\Rush\R010402b 4/3/01 1535 D:\Chem\Rush\R010402b 4/3/01 1550 D:\Chem\Rush\R010402.b 4/3/01 16.04 D:\Chem\Rush\R010402.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0131 D RUSH0134 D RUSH0135 D RUSH0136 D RUSH0137 D 250 5 n g h L PFOS in MeOH Study Number EW-1311 Study Number EW-1311 Study Number EW-1311 Study Number EW-1311 THPFOS THPFOS THPFOS THPFOS THPFOS 554 5544 5 547 5 552 556 693668 254 680330 254 570439 254 656434 254 674502 254 PFOS PFOS PFOS PFOS PFOS 5751 5747 575 5755 5 763 4099082 5372136 7416165 2754639 2672733 26497215 37928766 721 85686 17499347 163 32509 4/3/01 16:19 D:\Chem\Rush\RO10402 b SAMPLE RUSH0138D Study Number EW-1311 THPFOS 554 679000 254 PFOS 5743 2840570 17434555 4/3/01 16:33 D:\Chem\Rush\R010402.b 4/3/01 16:47 D:\Chem\R~sh\R010402.b SAMPLE SAMPLE RUSH0139D Study Number EW-1311 RUSH0140D Study Number EW-1311 THPFOS THPFOS 5 548 5 554 660801 254 684382 254 PFOS PFOS 5751 5013884 36082333 5757 1412950 74086291 4/3/01 17:02 D:\Chem\Rush\R010402b SAMPLE RUSH0141D Study Number EW-1311 THPFOS 5 547 688891 254 PFOS 575 1505023 79446466 4/3/01 17:16 D:\Chem\Rush\ROIM02b. 4/3/01 1731 D:\Chem\Rush\ROI0402.b 4/3/01 17:45 D:\Chem\Rush\R010402.b SAMPLE SAMPLE SAMPLE RUSH0142 D RUSH0143 D RUSH0144 D Study Number EW-1311 Study Number EW-1311 5 nglmL PFOS in MeOH THPFOS THPFOS THPFOS 554 5 549 5 551 667236 254 669472 254 711232 254 PFOS PFOS PFOS 5744 1329804 7091215 5752 3830875 25476073 5754 247651 1768823 4/3/01 1759 D:\Chem\Rush\RO10402 b 4/3/01 18:43 D:\Chem\Rush\R010402.b 4/3/01 18.57 D:\Chem\Rush\R010402.b SAMPLE SAMPLE SAMPLE RUSH0145 D RUSH0148 D RUSH0149 D 250 5 ne/mL PFOS in MeOH Study Number EW-1311 Study Number EW-1311 THPFOS THPFOS THPFOS 5 553 5 555 554 711428 918872 885106 254 PFOS 254 STD~130WFOS 254 PFOS 5756 4044257 25272329 0 0 0 0 0 0 4/3/01 19.11 D.\Chem\Rush\R010402.b SAMPLE RUSH0150 D Study Number EW-1311 THPFOS 5546 945311 254 STD>I3OI(PFOS 0 0 0 4/3/01 1926 0 \Chem\Rush\RO10402.b SAMPLE RUSH0151D Study Number EW-1311 THPFOS 554 703724 254 PFOS 5743 2896965 17099756 4/3/01 19:40 D.\Chem\Rush\R010402.b SAMPLE RUSH0152D Study Number EW-I 311 THPFOS 5544 856144 254 PFDS 0 0 0 4/3/01 19.55 D \Chern\Rush\R010402.b SAMPLE RUSH0153D Study Number EW-1311 THPFOS 5534 834838 254 PFOS 0 0 0 4/3/01 20.09 D \Chem\Rush\R010402.b SAMPLE RUSH0154 D Study Number EW-1311 THPFOS 5 539 816843 254 PFOS 0 0 0 4/3/01 2023 D.\Chern\Rush\ROl0402.b 4/3/01 20 38 D.\Chem\Rush\RO10402.b SAMPLE SAMPLE RUSH0155 D Sludy Number EW-1311 RUSH0156D Sludy Number 00-1311 THPFOS THPFOS 5 539 5 55 623341 254 851433 254 PFOS PFOS 5 742 2925075 2W 24318 0 0 0 4/3/01 20 52 D \Chem\Rush\R010402b 4/3/01 21:07 D-\Chem\Rush\RO10402.b 4/3/01 21.21 D.\Chem\Rush\ROlMOZb SAMPLE SAMPLE SAMPLE RUSH0157 D RUSH0158 D RUSH0159 D Study Number EW-1311 5 ng/mL PFOS in MeOH 250 5 n g h L PFOS in MeOH THPFOS THPFOS THPFOS 5 543 5 55 5 554 837861 254 641250 254 631991 254 PFOS PFOS PFOS 0 0 0 5753 234427 2461139 5757 3979419 28641899 54.3% 1058% 1588 9% 28.3% 35 4% 1W.9% 49 2% 1143% Page 3 of 3 BACK TO MAIN Q 5 r Sample Batch R010402a.b. analyzed o n Rush 040201. PFDSAdsorbmesorb samples. Matrix: SoiVSlglSed. Standard curve range used for calibratlon of samples: 5 4 + H nglmL (2.5 ng/mL otd not included due to the higher sample concentration range). Batch method: R010402a.m 51 (3-fd Inj Date 4/2/01 1230 4/2/011244 4/2/01 1259 4/2/01 13:13 4/2/01 13:27 4/2/01 13:42 4/2/01 1356 4/2/01 14:11 4/2/01 14:25 4/2/01 14:39 4/2/01 1454 4/2/01 1508 4 N o 1 15:22 4/3/01 8:lO 4/3/01 8:24 4/3/01 8:38 4/3/01 853 4/3/01 907 4/3/01 9:zi 4/3/01 9 : s 4/3/019:50 4/3/01 IO:M 4/3/01 1019 4/3/01 10:33 4/3/01 10:48 m m i I:OZ Batch D:\Chem\Rush\R010402.b O:\Chem\Rush\RO10402.b D:\Chem\Rush\ROl 0402.b D\Chem\Rush\RO10402.b O:\Chem\RushROl0402.b D:\Chem\Rush\RO10402.b D\Chern\Rush\ROI0402.b O:\Chern~ush\RO10402.b O:\Chem\Rush\RO10402.b D:\Chem\Rush\RO10402.b D:\Chem\Rush\RO10402.b O:\Chern\Rush\ROl0402.b D:\Chern\Rush\RO10402.b D.\ChemWush\R010402.b O:\Chem\Rush\RO10402.b D\Chem\Rush\RO10402.b D:\Chern\Rurh\RO10402.b O:\Chern\Rush\RO10402.b D:\Chem\Rush\RO10402.b D:\Chem\Rush\R010402.b O:\Chem\Rush\RO10402.b O:\Chern\Rush\ROl0402.b O:\Chem\Rush\RO10402.b D:\Chem\Rush\R010402.b O:\Chern\Rush\RO10402.b 0 .\ChernRush\R010402.b SampType SAMPLE CALIB-1 CALIB-2 CALIB-3 CALIB-4 SAMPLE CALlB-5 CALIB-6 CALlB-7 CALlB-8 SAMPLE CALK-9 CALIB-IO SAMPLE CALIB-11 CALIB-12 CALlB-13 CALIB-14 SAMPLE CALlB-15 CALIB-16 CALiB-I7 CALIB-18 SAMPLE CALIB-I9 CALIB-20 File RUSHW22.D RUSHW23.D RUSHW24.D RUSHW25.D RUSHW26.0 RUSHW27.D RUSHW28.0 RUSHW29.D RUSHW30.0 RUSH0031.0 RUSHW32.D RUSHW33.0 RUSHW34.D RUSH0104.D RUSHOIO5.D RUSH0106.D RUSH0107.D RUSH0108.0 RUSHOI09.D RUSHO11O.O RUSHO111.D RUSHO1IP.D RUSH0113.D RUSH0114 D RUSHO115.D RUSH0116.0 - Sample Name 0 na/mL PFO~ S in.MeOH 2.5 n g h L PFOSin MeOH 5 nglmL PFOS in MeOH 1 0 ng/mL PFOS in MeOH 25 ng/mL PFOS in MeOH 4 0 ng/mL PFOS in MeOH 50.1 ng/mL PFOS in MeOH 75.1 ng/mL PFOS in MeOH 100.2 n g h L PFOSin MeOH 250.5 ng/mLPFOSin MeOH 4W.8 ng/mL PFOSin MeOH 501 ng/mL PFOS in MeOH 1002 nglmL PFOSin MeOH 0 nglmLPFOSin MeOH 2.5 ng/mL PFOSin MeOH 5 ng/mL PFOS in MeOH 1 0 ng/mLPFOS in MeOH 25 ng/mL PFOS in MeOH 4 0 nglmL PFOS in MeOH 50.1 ng/rnL PFOSin MeOH 75.1 n g h L PFOS in MeOH 100.2 ng/mL PFOS in MeOH 250.5 ng/mLPFOSinMeOH 400.8 n g h L PFOSin MeOH 501 nglrnL PFOSin MeOH 1002n g h L PFOS in MeOH Misc InfCompouncRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Area Amount 5.549 673482 254 5.55 687494 254 5.559 717007 254 5.553 692713 254 5.559 698171 254 5.553 694018 254 5.557 699817 254 5.558 708280 254 5.559 701188 254 5.567 732842 254 5.561 711160 254 5.564 714631 254 5.567 739760 254 5.545 691238 254 5.546 707818 254 5.558 726841 254 5.553 702679 254 5.553 711476 254 5.543 695068 254 5.553 697300 254 5.55 709991 254 5.541 709014 254 5.544 744829 254 5.546 710505 254 5.54 719310 254 5.542 745057 254 CompoundU PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 5.76 5.769 5.763 5.769 5.763 5.767 5.768 5.769 5.77 5.764 5.774 5.77 0 5.756 5.768 5.757 5.756 5.739 5.749 5.753 5.744 5.747 5.749 5.743 5.745 Area Amount 0 0 201953 1.38861 259654 3.944702 339488 8.769619 641564 25.343497 908997 40.988941 1106262 52.140717 1545079 77.738587 1912602 102.07183 4155372 250.46887 5685914 406.28894 6981587 505.86859 12248403 1053.3589 0 0 193236 0.616118 249725 3.252923 339511 8.507324 641983 24.690572 905841 40.723752 1085138 51.118799 1535613 76.928129 1912604 100.70449 4147316 244.83253 5754500 394.96094 6939227 497.41946 12088828 1022.9766 78.9% 87.7% 101.4% 102.2% 104.1% 103.5% 101.9% 100.0% 101.0% 65.1% 85 1% 98.8% 101.6% 102.0% 102.4% 100.5% 97.7% 99.3% Average: 709288.4 Std Dev: 17649.55 - %RSD- 2.5% 922075 +30% 496502 -30%: Page 1 of 4 BACK TO MAIN Sample Batch RO104OZa.b. analyzedon Rush 040241. PFOSAdsorblDesorb samples. Matrix: SoivSlgiSed. Standard cuwe range used for calibration of sampler: S-reePnglmL (2.5 nglmL std not included due to the higher sample concentration range). Batch method: R010402a.m 50 U%<S I f S / O \ Inj Date Batch SampType File Sample Name Mise InfCompouncRT Area 4/2/01 1201 D:\Chem\RushR010402.b SAMPLE RUSHW20.D TN-A 4802 MeOH THPFOS 0 4/2/01 12313 D:\Chem\Rush\R010402.b SAMPLE RUSHW21.D TN-A4802 MeOH THPFOS 0 4/2/01 1537 D:\Chem\Rush\R010402.b SAMPLE RUSH0035.D TNA4802 MeOH THPFOS 0 4/2/01 1551 D:\ChemiRush\R010402.b SAMPLE RUSH0036.D TKA4802 MeOH THPFOS 0 4/2/01 18:15 D:\Chem\Rush\R010402.b SAMPLE RUSHOC46.D TNA4802 MeOH THPFOS 0 4/2/01 1829 D:\Chem\Rush\R010402.b SAMPLE RUSHW47.D TN-A4802 MeOH THPFOS 0 4/2/01 21:36 D:\Chem\Rush\R010402.b SAMPLE RUSH0060.D TN-A4802 MeOH THPFOS 0 4No1 21:51 D:\Chem\Rush\R010402.b SAMPLE RUSHW61.D TN-A 4802 MeOH THPFOS 0 4/3/01 0:58 D:\Chem\Rush\R010402.b SAMPLE RUSH0074.D TN-A 4802 MeOH THPFOS 0 4/3/01 132 D:\Chem\Rush\R010402.b SAMPLE RUSH0075.D TN-A 4602 MeOH THPFOS 0 4/3/014 3 9 D:\ChemU?ush\R010402.b SAMPLE RUSHW88.D TN-A 4802 MeOH THPFOS 0 4/3/01 4:34 D:\ChemRushR010402.b SAMPLE RUSHW89.D TN-A 4802 MeOH THPFOS 0 4/3/01 7:41 D:\Chem\Rush\R010402.b SAMPLE RUSH0102.D TN-A 4802 MeOH THPFOS 0 4/3/01 755 D:\Chem\Rush\R010402.b SAMPLE RUSH0103.D TN-A 4802 MeOH THPFOS 0 4/3/01 1136 D:\ChemRush\R010402.b SAMPLE RUSHO117.D TNA4802 MeOH THPFOS 0 4/3/01 11:31 D:\Chem\Rush\R010402.b SAMPLE RUSH0118.D TNA4802 MeOH THPFOS 0 4/3/01 11:45 D:\Chem\RushW010402.b SAMPLE RUSHO119.D TN-A4802 MeOh THPFOS 0 Amount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 CompouncRT Area Amount PFOS 5.764 155059 0 PFOS 5.771 133949 0 PFOS 5.792 160821 0 PFOS 5.78 138099 0 PFOS 5.77 138330 0 PFOS 5.761 134138 0 PFOS 5.792 136128 0 PFOS 5.771 130679 0 PFOS 5.754 139503 0 PFOS 5.754 127186 0 PFOS 5.778 129477 0 PFOS 5.774 126456 0 PFOS 5.772 131523 0 PFOS 5.764 125537 0 PFOS 5.768 153626 0 PFOS 5.771 130584 0 PFOS 5.764 126241 0 Page 2 of4 BACK TO MAIN Sample Balch R010402a.b, analyzed on Rush 04-02-01. PFOSAdsoWLbsorb samples. Matrlx: SolUSlglSed. Standard curve range used for calibration of samples: 5 - W n g l m L (2.5 nglmL std not included due to the higher sample wncenbation range). Batch method R010402a.m Inj Date 4/2/01 16:06 Batch D:\Chem\RushRO10402.b SamPTYw SAMPLE File RUSHW37.D Samole Name Stud; Number E001311 Mirc InfComwundlT Area Amount THPFOS 5.56 720158 254 4/2/01 1620 D:\Chem\Rush\ROl0402.b SAMPLE RUSHW 38.D Study NumberE001311 THPFOS 5.546 709660 254 4/2/01 1 6 : ~ D:\ChemWush\R010402.b SAMPLE RUSHW39.D Study NumberE001311 THPFOS 5.558 722650 254 4/2/01 16:49 D.5ChemWushW010402.b SAMPLE RUSH0040.D Study NumberE001311 THPFOS 5.548 707567 254 4/2/01 1703 D:\Chem\Rush\ROl0402.b SAMPLE RUSHW41.D Study Number E001311 THPFOS 5.548 713572 254 4/2/01 17:17 D.\ChemWushW010402.b SAMPLE RUSHW42.D Study Number EO01311 THPFOS 5.546 724968 254 4/2/01 1732 D:\Chem\RushWO10402.b SAMPLE RUSHW43.D Study NumberE001311 THPFOS 5.554 721402 254 4/2/01 17:46 D:\Chem\Rush\RO10402.b SAMPLE RUSHW44.D 5 nglmL PFOSin MeOH THPFOS 5.548 753692 254 4No1 18:Ol D\Chem\Rush\R010402.b SAMPLE RUSHW45.D 250.5 ng/mLPFOSin MeOH THPFOS 5.551 746193 254 4/2/0118:44 D:\Chem\Rush\ROl0402.b SAMPLE RUSHW48.D Shldy Number EW-1311 THPFOS 5.554 710136 254 4/2/01 1 8 : s D:\Chem\Rush\ROlWZ.b SAMPLE RUSHW49.D Study Number EW-1311 THPFOS 5.551 709407 254 4/2/01 19:13 D:\Chem\Rush\RO10402.b SAMPLE RUSHW50.D Study Number~ 0 0 1 3 1 1 THPFOS 5.56 687539 254 4/2/01 1927 D:\Chem\RushUi010402.b SAMPLE RUSHW51.D Study Number E001311 THPFOS 5.563 693912 254 4/2/01 i9:4i D:\Chern\RushWO10402.b SAMPLE RUSHW52.D Study NumberEW-1311 THPFOS 5.557 573314 254 4/2/01 1956 D:\Chem\RushWO10402.b SAMPLE RUSHW53.D Study Number E001311 THPFOS 5.558 689156 254 4/2/01 2030 D\ChemWush\RO10402.b SAMPLE RUSH0054.0 Study Number E001311 THPFOS 5.555 698632 254 4/2/01 20:a O:\Chem\Rush\RO10402.b SAMPLE RUSHOO55.D Study Number EOC-1311 THPFOS 5.558 701032 254 4/2/01 20:39 D:\ChemWush\ROl0402.b SAMPLE RUSHW56.D Study Number EW-1311 THPFOS 5.564 697975 254 4/2/01 2053 D:\ChemRushU7010402.b SAMPLE RUSHW57.D Study Number EW-1311 THPFOS 5.566 722953 254 4 N o 1 21:08 O:\Chem\Rush\R010402.b SAMPLE RUSW58.D 5 nglmLPFOS in MeOH THPFOS 5.575 742818 254 4/2/01 21:22 D\ChemWushWO10402.b SAMPLE RUSHW59.D 250.5 ng/mL PFOSin MeOH THPFOS 5.56 738144 254 4/2/01 22:05 D:\ChemWush\RO10402.b SAMPLE RUSHW62.D Study Number EW-1311 THPFOS 5.561 724679 254 4/2/01 2220 D:\Chem\Rush\R010402.b SAMPLE RUSHW63.D Study Number EW-1311 THPFOS 5.56 732716 254 4NOl22:34 D\Chem\Rush\ROIW2.b SAMPLE RUSHWB4.D Study Number EW-1311 THPFOS 5.551 709950 254 4No12248 D:\Chem\Rush\ROWl 2 . b SAMPLE RUSHW65.D Study Number E001311 THPFOS 5.541 717003 254 4/3/01 2303 O:\Chem\Rush\R010402.b SAMPLE RUSHW66.D Study NumberE001311 THPFOS 5.546 703450 254 4/3/01 2337 D:\Chem\Rush\RO10402.b SAMPLE RUSHWB7.D Study Number EO01311 THPFOS 5.541 699666 254 4/3/01 2331 D:\Chem\Rush\RO10402.b SAMPLE RUSHW68.D Study Number EW-1311 THPFOS 5.533 585285 254 4/3/01 2346 D\Chem\RushW010402.b SAMPLE RUSH0069.D Study Number E001311 THPFOS 5.539 675221 254 4/3/01 0:OO O:\ChemWushWO10402.b SAMPLE RUSHW70.D Study Number E001311 THPFOS 5.532 679762 254 4/3/01 0 3 5 D:\ChemWush\RO10402.b SAMPLE RUSHW71.D Shldy NumberEOO-1311 THPFOS 5.533 576140 254 4/3/010 2 9 D.\Chem\RushWO10402.b SAMPLE RUSH0072.D 5 ng/mL PFOSin MeOH THPFOS 5.535 704091 254 4/3/01 0:43 D:\ChemWush\ROWl 2 . b SAMPLE RUSHW 73.D 250.5 ng/mL PFOS in MeOH THPFOS 5.543 709848 254 CompoundlT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.764 5.749 5.759 5.751 5.758 5.756 5.757 5.756 5.754 5.757 5.761 5.77 5.768 5.76 5.768 5.765 5.761 5.767 5.769 5.792 5.77 5.764 5.763 5.747 0 0 0 5.736 5.742 5.735 5.736 5.745 5 739 Area Amount 1429691 69.243301 1319817 63.879261 1351379 64.31529 3835296 236.73617 6391949 450.7897 4812925 305.70323 5198125 339.49098 266077 3.60348 4140558 243.77425 7163224 528,02219 2197087 119,09938 926960 42.675468 697046 28.725867 3024950 229.85155 2174774 121.84417 2284600 127.2331 2386809 133.63027 4749637 315.49117 1411113 67.811262 262089 3.595994 4133826 246.60414 1328107 62.727361 1708104 64.309464 4317226 273.50922 0 0 0 0 0 0 2892741 211.04908 643295 26676048 647862 26.69003 3230023 246.93617 259690 4196199 4132026 258 85952 72.1% 97.3% 71.9% 98.4% 83 9% 103 3% Page3of4 BACK TO MAIN Sample Batch R010402a.b, analyzed on Rush 040241. PFDSAdsorUDcsorb samples. Matrix: SoiVslgSed. Standard curve range used for calibration of samples: 5-1682ngflL (2.5 nglmL std not included due to the higher sample concentration range). Batch method: R010402a.m >%I & ? & p - C b-1 l J - 7 d l 4/3/01 127 D:\Chem\Rush\RO10402.b SAMPLE RUSHW76.D Studv NumberE001311 THPFOS 5.565 7W501 254 4/3/01 1:41 mrni 1:55 D:\Chem\Rush\RO10402.b O:\Chem\Rush\RO10402.b SAMPLE SAMPLE RUSH0077.D Stud; Number E001311 RUSH0078.D Study Number E001311 THPFOS 5.552 679568 254 THPFOS 5.56 670087 254 4/3/01 2 1 0 O:\Chem\RushWOCl 402.b SAMPLE RUSHW79.D Study NumberE00.1311 THPFOS 5.544 568572 254 4/3/01 2:24 D:\ChemWushWO10402.b SAMPLE RUSHW80.D Sludy Number E001311 THPFOS 5.54 650461 254 4/3/01 2:38 D:\Chem\Rush\RO10402.b SAMPLE RUSHW81.D Study Number E001311 THPFOS 5.533 w e 0 5 254 4/3/01 2 5 3 D:\Chem\Rush\RO10402.b SAMPLE RUSHOO8Z.D Study NumberE001311 THPFOS 5.539 648526 254 4 ~ m3i:07 O:\ChemWush\RO10402.b SAMPLE RUSHW 83.D Study NumberE00-1311 THPFOS 5.534 560495 254 4/3/01 3 : ~ O:\Chem\Rush\R010402.b SAMPLE RUSHW 84.D Study Number E001311 THPFOS 5.54 660562 254 4/3/01 3:36 D:\Chem\RushWO10402.b SAMPLE RUSHW85.D Study Number E001311 THPFOS 5.531 672433 254 4/3/01 3:50 D:\Chem\RushWOI0402.b SAMPLE RUSHW86.D 5 ng/mL PFOS in MeOH THPFOS 5.543 700545 254 4/3/01 4:05 O:\Chem\Rush\RO10402.b SAMPLE RUSH0087.D 250.5 ng/mL PFOS in MeOH THPFOS 5.554 709410 254 4/3/01 502 D\Chem\Rush\RO10402.b SAMPLE RUSHO091.D Study Number E001311 THPFOS 5.551 669389 254 4 n m i 517 O:\Chem\Rush\R010402.b SAMPLE RUSHW92.D Study Number E001311 THPFOS 5.546 683096 254 4/3/01 5:31 O:\Chem\Rush\ROlC402.b SAMPLE RUSHO093.D Study Number E001311 THPFOS 5.543 683769 254 4/3/01 5:45 D:\Chem\Rush\RO10402.b SAMPLE RUSHW94.D Study NumberE001311 THPFOS 5.54 702574 254 4/3/01 6:W O~\Chem\RushROCI402.b SAMPLE RUSHo95.D Study Number E00-1311 THPFOS 5.553 672540 254 4/3/01 6 1 4 D:\Chem\Rush\R010402.b SAMPLE RUSHW96.D Study NumberE00-1311 THPFOS 5.544 690375 254 413101 6:29 O:\Chem\Rush\RO104M.b SAMPLE RUSHW97.0 Study NumberE001311 THPFOS 5.544 677814 254 4/3/01 6:43 D:\Chem\Rush\RO10402.b SAMPLE RUSHW98.D Study Number EW-1311 THPFOS 5.544 674569 254 4/3/01 657 D:\Chem\Rush\RO10402.b SAMPLE RUSHW99.D Study Number E001311 THPFOS 5.539 565914 254 4/3/01 7:12 D:\Chem\RushWO10402.b SAMPLE RUSH01W.D 5 nglmLPFOSin MeOH THPFOS 5.545 710818 254 4/3/01 7:26 O:\Chem\Rush\RO10402.b SAMPLE RUSHO1OI.D 250.5 ng/mL PFOSin MeOH THPFOS 5.547 699529 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.761 5.755 5.763 5.741 5.743 5.736 5.735 5.737 5.743 5.734 5.753 5.757 5.754 5.75 5.746 5.743 5.749 0 0 0 5 742 5.755 5.75 1988079 1990346 1686695 4300957 4141363 3611282 3972287 6061330 1849680 2010670 254899 4162725 4302522 6535234 6711588 6936083 84794205 0 0 2730205 259422 4064532 107.11332 111.28762 106.22388 361A4666 289.87301 249.67287 276.01481 580.02025 105.37736 114.12314 4.03926 261.46317 293.38551 491.9271 509.06131 513.00765 715.92273 0 0 0 20482416 4.0507 258.26619 80.2% 104.4% 81.0% 103.1% Page 4 of 4 EW-1311 PFOS AdslDes BACK TO MAIN . . Samole Batch R010314.b. analvzedon Hillarv 03-14-01. PFOSAdsorblDerorbsamoles. Matdx: Sediment Standardcurve range used for calibration oiumple.~: 2.5-250.5 n g h L (4M.8 and501 nglmL std not includeddue to the lower sample e o n ~ n t n t l o rnange). Batch method R010314t.m In1D a b w4m121 05 3/14/0121 19 3/14/0121 33 3/14/01 21 48 3/14/01 22 02 3/14/01 22 16 3/14/0122 31 3/14/0122 45 3/14/01 23 00 3/14/0123 14 3/14/0123 28 3/14/0123 43 3/15/01 2 4 9 3115/013 03 3/15/016 10 3/15/01 6 24 3/15/01 9 31 3/15/01 9 45 3/15/01 1252 3/15/01 1306 3/15/01 1350 3/15/01 1404 3/15/01 14 18 3/15/01 1433 3/15/01 1447 3/15/01 1501 3/15/01 15 16 3/15/01 1530 3/15/01 1544 3/15/01 1559 3/15/01 16 13 3/15/01 16 28 Batch D Wlem\RushE3010314b D WlemWush E3010314b D WlemWushE3010314b D WlemWush iW010314b D \chemWush hR010314 b DWlemWush E3010314b D Wlem\Rush hR010314 b D Wem\Rush E3010314b D WlemWush E3010314b D hem\Rush 1W010314b D Wlem\Rush iUt010314b D Wlem\Rush1W010314b D WlemWush hR010314 b D MemWRushhR010314b D khem\Rush1W010314b D Wlem\Rush hR010314 b DMem\Rush E3010314b D \chem\Rush E3010314b DWlem\RUshE3010314b D Wlem\Rush E3010314b D WlemWush hR010314b D WlemWush 1W010314 b D WlemWush iUt010314b D WlemWush kR010314b D Wlem\RushE3010314b D MemWush E3010314b D khemWushtWO10314 b DWem\Rush iW010314 b D \chem\Rush 1W010314b D Wem\Rush tWO10314 b D WemWush 1W010314b DWlem\RushE3010314b SampTyp. SAMPLE CALlB-I CALlB-2 CALIB-3 CALlB-4 CALIB-5 CALlB-6 CALIB-7 CALlB-8 CALIB-9 CALlB-IO SAMPLE CCALIB-1 CCALIB-1 CCALIB-I CCPLlB-I CCALIB-1 CCALIB-I CCALIB-1 CCALIB-I SAMPLE CALK-1 1 CALM-I2 CALIB-13 CAM-14 CALIB-15 CALIB-16 CALlB-I7 CALlB-18 CALlB-IS CALlB-20 SAMPLE File RUSH0017 D RUSHWIBD RUSH0019 D RUSH0020 D RUSH0021 D RUSH002 D RUSH0023 D RUSHW24 D RUSHOO25D RUSH0026 D RUSH00270 RUSH00280 RUSHWI D RUSH0042 D RUSHOOSS D RUSH0056 D RUSH0069D RUSHW70D RUSHOO83D RUSH0084 D RUSHW87D RUSHOOBB D RUSH0089 D RUSHOWO D RUSHW91 D RUSHW9ZD RUSHW93D RUSHW94 D RUSHW95 D RUSHWID RUSH0097 D RUSH00980 Sample Name 01W307-01 010030742 010030703 010030704 01W 3 0 7 0 5 010030706 010030747 010030708 010030749 0100307-10 01wJ-07-11 01WW7-12 01w307-03 01003.07-IO 010030703 0100307-10 0:0030703 01003-07-10 010030743 OlW3-07-10 01W307-01 01W307-02 010030703 010030704 010030705 010030706 OlW30707 D lW30708 010030709 01W307-10 0100307-11 0100307-12 Mlsc Info Compound Name THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFDS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT 5 48 5.47 5.46 5.45 5.46 5.46 5.46 5.47 5 47 5.46 5.46 5.46 5.47 5.47 5.47 5.48 5.47 5.46 5.47 5.46 5.47 5.47 5.46 5.47 5.47 5.47 5.46 5.46 5.46 5.46 5.46 5.47 Ana 1W9005 1002399 1offiuB 1013743 1002095 1014289 998269 1016405 1001184 1022553 1019780 1018171 1050373 1036120 I050495 1042671 1051910 1047495 1051525 1042848 I053861 1050989 1056424 1041839 1040134 1051034 1043368 1052178 1038121 1028679 1035833 1034919 _ _ _ Averaae: 1032038.969 Std Dev: 18725 XRSD: 1.8% Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Compound Nune PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS ' PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS RT ow 568 568 567 567 568 568 568 569 568 567 568 569 569 569 569 569 568 569 568 ow 569 568 569 569 568 568 568 568 568 568 568 Area 0 129429 209405 330471 783497 1209876 1458055 2128988 2648411 5889029 8711721 I0307257 194784 5934195 196061 5869851 188546 5823836 187794 5774991 0 121720 183452 317434 756712 1162752 1426057 2081314 2616038 5630191 8331328 9922517 Amount 00 27 55 99 26 3 41 9 52 5 78 5 102 3 257 9 427 4 536 5 47 256 1 47 251 8 45 246 9 44 245 7 00 22 43 89 24 3 38 6 487 73 6 967 242 1 394 9 498 5 QC IS range (+I-30% average): +30%: 1341651 -30%: 722427 108 0% 109 3% 99 3% 105 1% 104 8% 104 7% 104 3% 102 1% 1030% xx xx. 93 4% 102 3% 94 3% 1005% 89 1% 98 6% 88 6% 98 1% 89 4% 85 2% 88 9% 97 0% 96 5% 97 3% 97 8% 96 6% 96 7% xx xx Page 1 of 3 BACK TO MAIN LG, 9(D (D VI (XJ VI 4 w 0 E00-1311 PFOS AddDes Sample Batch ROlO314.b, analyzed on Hillaty 03.l4-01. PFDS AdsottJDaorb Sample% Matrix: Sediment StandardCUNB range usedfor calibrationof samples: 2.5-250.5 nglmL (400.8 and 501 ng/mL Std not includeddue to the lower sample concentrationrange). Batch method R010314t.m lnj Date 3/15/010 26 3/15/01 0 40 3/15/01 054 3/15/01 109 3/15/01 123 3/15/01 137 3/15/01 1 5 2 3/15/01 2 06 3/15/01 2 20 3/15/01 2 25 3/15/01 347 3/15/01 4 01 3/15/014 15 3/15/01 4 30 3/15/01 4 44 3/15/01 4 58 3/15/01 5 13 3/15/015 27 3/15/01 5 41 3/15/015 56 3iwaU.w 3/15/01 7 22 3/15/01 7 38 3/15/01 7 50 3/15/01 805 3/15/018 19 3/15/018 34 3/15/01 6 48 3/15/019 0 2 3/15/019 17 3/15/01 1029 3/15/01 1043 3/15/01 1057 3/15/01 11 12 3/15/01 11 26 3/15/01 11 40 3/15/01 11 55 3/15/01 1209 3/15/0i 12 23 3/15/01 12 38 Batch D Wem\Rush hR010314b D WemWush hR010314 b D WemRush hR010314 b DWemWush hR010314 b D \chemRush iW010314b D MemWurh hR010314 b D WemWush AR010314 b D WemRush hR010314 b D Wem\Rush iW010314b D \chem\RushiWOIO314 b D \chem\Rurh N1010314 b D WemWuoh tWO10314 b D Wem\Rush hR010314b D Wem\Rush hR010314 b D \chemRush hR010314 b D WemWush hR010314 b D MemRush N1010314 b D WemWush hROl0314b D WemRush hR010314 b D Mem\Rush iW010314b P D Mem\Rush hR010314 b D Mem\Rush iW010314b D Wem\Rush iW010314 b D Wem\Rush iW010314 b D Wem\Rush hR010314b D WlemWush 1W010314b DWem\Rush hR010314b D WemRush hR010314 b D \chern\Rush hR010314 b D WemRush W.010314 b D WemWush iW010314b D WemWush iW010314 b D WemWush tW010314b D WemWurh 1W010314b D \chemWushiW010314b D Wem\Rush iW010314b D WlernRush hR010314 b D\chemWush hR010314 b D WemWush 1W010314b SampType File Sample Name SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE fppJpLs SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSHW31 D RUSH0032 D RUSH0033 D RUSHW34 D RUSHW35 D RUSHWID RUSH0037 D RUSHWID RUSH0039 D RUSHLWO D RUSHW45 D RUSH0048 D RUSHLW7 D RUSH0048 D RUSH0049 D RUSHWSO D RUSHWSI D RUSH0052 D RUSHWSS D RUSHWD auswswa RUSHWGO D RUSHOOG1 D RUSH0062 D RUSH0063 D RUSH0064 D RUSH0065 D RUSHW6S D RUSH0057D RUSH0058 D RUSH0073 D RUSH0074 D RUSH0075 D RUSHW76 D RUSHW77 D RUSHW78 D RUSHW79 D RUSHWBO D RUSHWBI D RUSHWBZ D 1311 ~ 1 2 1 5 1 13114122S1 13114123-S1 131l4123MS-S1 13114124-S1 13114125Sl 13114126Sl 13114126MS-SI 13114127-S1 1311412Bs1 13114129Sl 13114129MS-Sl 13114130-SI 13114131S1 13114132-SI 131j4132MS-SI 13114133-SI 1311 4 13451 1311413551 13114135MS-S1 su4U64s 13114137-SI 13114138-SI 13114138MS-S1 1311413951 1311 4 1 4 0 5 1 13114141-SI 131I4141MS-SI 13114142-SI 1311 4 143-SI 13114144-51 13114144MS51 13114145-S1 13114146-SI 13114147-SI 13114147MSS1 13114 1 4 8 S 1 13114149-S1 1311415OS1 1311415OMSSl Misc Info Compound N w THPFOS THPFOS THPFOS THPFOS MPFOS MPFOS THPFOS THPFOS THPFDS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS WPFCs THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS MPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT 5 47 5 47 5 47 5 47 5 48 548 546 5 48 5 48 5 48 5 48 5 48 5 48 5 49 548 5 49 548 5 51 5 48 5 48 aca 5 48 5 47 5 47 5 47 5 47 5 48 5 47 5 48 5 47 5 48 546 5 47 546 5 47 546 5 47 5 47 5 47 5 47 Area 1425324 1078944 1090803 931360 1093465 I057249 1038845 903745 1084923 1074853 1660202 947684 1095965 1091572 1101888 919194 I073078 10812M I077793 921307 a I099389 1083504 947454 1086262 1087521 1075484 915669 1079679 llLX514 1091080 895662 1070260 1090781 IM)B406 898964 10-5 1052012 1055409 887792 Averane: 1062023 Std Dev: 137692 XRSO: 13.0% Amount CompoundName RT Area Amount 254 PFOS OW 0 00 254 PFOS OW 0 00 254 PFOS ow 0 00 254 PFOS 568 4322756 1979 254 PFOS ow 0 00 254 PFOS ow 0 00 254 PFOS 254 PFOS 569 4220111 1994 254 PFOS 569 1155260 370 254 PFDS 569 4106846 1568 254 PFOS 570 1343718 273 254 PFOS 569 5004132 2316 254 PFOS 569 799984 243 254 PFOS 570 725496 21 9 254 PFOS 569 822873 250 254 PFOS 571 4874564 2329 254 PFOS 569 729534 225 254 PFOS 573 759438 233 254 PFOS 569 769202 237 254 PFOS 570 4762247 2257 a @64s waaE%$ M 254 PFOS 569 757619 228 254 PFOS 569 757822 232 254 PFOS 569 4939810 2281 254 PFOS 569 684895 207 254 PFOS 569 677314 204 254 PFOS 569 687097 21 0 254 PFOS 568 4776931 2282 254 PFOS 570 673507 204 254 PFOS 569 716747 21 3 254 PFDS 570 688862 207 254 PFOS 569 4609795 2245 254 PFOS 569 640428 195 254 PFOS 568 644391 192 254 PFOS 569 636594 190 254 PFOS 5 6 8 4605162 2232 254 PFDS 5 6 8 649889 201 254 PFDS 568 645335 200 254 PFOS 569 651186 202 254 PFOS 569 4565770 2243 Page 2 of 3 EM)-1311PFOS AUslDes BACK TO MAIN Sample Batch R010314.b. analyzed on Hillary 03-14Oi. PFOS AdsoMOesorbsamplea Matrix: Sediment Standardcurve range used for calibration of samples: 2.5-250.5 nglmL (4W.8 and SO1 n@mLrtdnot Included due to the lower sampleconcentration range). Batch mathod R010314t.m In1 Date 3/14/01 20 36 3/14/01 20 M 3/14/01 23 57 3/15/01011 3/15/01 3 18 3/15/01 3 32 3/15/016 39 3/15/016 53 3/15/01 1000 3/15/01 10 14 3/15/01 1321 3/15/01 1335 3/15/01 16 43 3/15/01 1657 Batch D \chem\RuJh RR010314b D WemWush iW010314 b DWem\Rush hR010314b D Wern\RushAR010314 b D Wem\Rush hR010314b DWemWush i\R010314b D \chem\Rush 1W010314b DWemWush 1W010314b 0 WemWush AR010314 b D \them\Rush bR010314b D H e m m u s h iWOlO314b DichemWushARO10314 b D WernWush AR010314 b D Wlern\RushhR010314b SamPTyp. SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File Sample Name RUSH0015D RUSHWIG D RUSH0029 D RUSHWJO D RUSHW3 D RUSH0044 D RUSH0057 D RUSHW5ID RUSH0071 0 RUSHLX72 D RUSHWE5 D RUSH0086 D RUSH0099 D RUSHOIW D TN-A 4802 MeOH TN-A 480'2 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802MeOH TN-A4602 MeOH Mlrc Info Compound Name RT THPFOS ow THPFOS ow THPFOS ow THPFOS 000 THPFOS OM) THPFOS ow TNPFOS ow THPFOS ow THPFOS ow THPFOS OM) THPFOS 000 THPFOS ow THPFOS ow THPFOS ow Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount C:ompoundNanm RT 0 PFOS 5 70 0 PFOS 5 63 0 PFOS 5 69 0 PFOS 5 63 0 PFOS 564 0 PFOS 564 0 PFOS 5 69 0 PFOS 5 70 0 PFOS 5 69 0 PFOS 568 0 PFOS 5 68 0 PFOS 5 70 0 PFOS 568 0 PFOS 568 Area 40923 29136 40534 30463 33501 7- . 57454 51654 57753 53172 57830 45965 56083 47554 Amount 0.0 00 0.0 0.0 00 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 4 0 w BACK TO MAIN Sample Batch R010309.b. analyzed on Rush 030901. PFOSAdsohlDesorb samples. Matrix: Cntrl and Soils 1.2, h 3. Standard curve range used for calibration of sampler: 10.501 ng/mL (2.5. and Ing/mL std not included due to the higher sample concentration range). Batch method R010314t.m In) Date Batch 3/9/01 20 26 D \chem\Rush1W010309b 3/9/01 20 37 D \chem\Rush AR010309 b 3/9/01 20 48 0 khem\Rush hR010309 b d l Y N l L1 W U Wemwush Iu1010309b 3/9/01 21 11 D WemRush 1W010309b 3/9/01 21 22 D WemRush hRO103W b 3/9/01 21 33 D Wem\Rush hR010309 b 3/9/01 21 44 D WemRush 1R0103Wb 3/9/01 21 56 D \chemRush ARO10309 b 3/9/01 22 07 D \chemRush WO103W b 3/9/01 22 18 O\chem\Rush hR010309 b 3/9/01 22 29 0 \chem\Rush 1R010309b 3/10/01 0 54 D khem\Rush iR0103W b 3ll0/01 1 06 D Wem\Rush hR010309 b 3110101 3 31 DWem\Rush hR010309b 3/10/01 342 0 Wem\Rush AR010309 b 3/10/01 6 07 D MemRush hR0103W b 3/10/01 6 19 OWem\Rush 1\R010309b 3/10101 8 44 D Wem\Rush hR010309 b 3/10/01 8 55 D \chem\Rush1W010309b 3/10/01 11 21 D \chem\Rush t\R0103W b 3/10/01 11 32 D\chem\RushhR010309b 3/10/01 13 58 D\chem\RushW010309 b 3/10/01 14 09 D \chem\Rush1W010309b 3/10101 16 34 0 \chemRush 1W010309b 3/10/01 16 46 0 \chemRush 1W010309b 3/10/01 I 8 38 D Wem\Rurh 1W010309b 3/10/01 1849 D \chem\RushhR010309b 3/10/01 1922 DWem\Rush hR010309b 3/10/01 1933 DWem!RushhR010309b 3/101011945 DWemRushi\R010309 b 3/10/01 19 56 D \chemRush 1W010309b 3/10/01 20 07 D WemRush hR010309 b 3/10/0120 18 DWemu1ush ARO103W b 3/10/0120 29 D Wem\Rush hR010309 b 3/10/012040 D \chemWush ARO10309 b 3/10/0120 52 D \chem\Rush1W010309b 3/10/01 21 03 0 WemRush hR010309b 3/1wO121 14 DWem\Rush hR010309 b 3/101012125 DWem\Rush hR0103W b SamPVp. SAMPLE SAMPLE CALlB-I CALIB-2 CALIB-3 CALIB-4 CALlB-5 CALlB-6 CALIB-7 CALl8-8 CALIB-9 CALlB-I 0 CCALIB-I CCALlB-I CCALIB-I CCALlB-I CCALIB-I CCALIB-I CCALIB-1 CCALIB-1 CCALIB-1 CCALIB-1 CCALIB-1 CCALlB-I CCALIB-I CCALIB-I CCALIB-I CCALIB-1 SAMPLE SAMPLE CALlB-I 1 CALK-12 CALlB-13 CALIB-14 CALlB-I5 CALlB-16 CALlB-17 CALM-18 CALlB-19 CALIB-20 File Sample Name RUSH0022D 0100307-01 RUSH0023 D 010034742 RUSHW24D 010034743 RUSH0025D 010034744 RUSH0026D 010034745 RUSH0027 D 010030706 RUSH0028 D 010030747 RUSH0029D 010030748 RUSHWBOD 01003-0749 RUSH0031D 0100347-10 RUSHW32 D 0100367-11 RUSH0033D 0100307-12 RUSH0046D 5 ng/mL PFOS RUSH0347 D 250 5 nglmL PFOS RUSHWGO D 010034743 RUSHWGI D 0100347-10 RUSH0074 D 010030703 RUSH0075 D 0100307-10 RUSHW88D 010034743 RUSH0089 D 01003-07-10 RUSH0102D 010034703 RUSH0103 D 01003-07-10 RUSHO116D 010030743 RUSH0117 D 0100347-10 RUSH0130D 010030743 RUSH0131 D 0100367-10 RUSH0141 D 010034703 RUSH0142D 0100307-10 RUSH0145D 01W307-01 RUSH0146D 01W3-0742 RUSH0147 D 01003-0703 RUSH0148 D 010034744 RUSH0149 D 010036745 RUSH0150 D 010034706 RUSH0151 D 01W 3 0 7 4 7 RUSH0152D 010034708 RUSH0153 D 010034749 RUSH0154 D 01W347-10 RUSH0155 D OlwJ07-11 RUSH0156 D 0100307-12 Ylsc Info 2.5 nglmL PFOS 5.0 nglmL PFOS 10nglrnLPFOS 25 ngiML PFOS 40 n@mLPFOS 50 nglmL PFOS 75.1 nglmL PFOS 1W.2 nglmL PFOS 250 5 r@mL PFOS 400.8 ngmL PFOS 501 nglmL PFOS 2 5 n g h L PFOS 5 0 nglmL PFOS 10 ngmL PFOS 25 ngiML PFOS 40 nglmL PFOS 50 n@mL PFOS 75.1 ng/mL PFOS 100.2 nglrnL PFOS 250 5 ngmL PFOS 400 8 nglmL PFOS 501 nglmL PFOS o m p o u n d N m RT THPFOS 5 571 THPFOS 5 569 THPFOS 5566 THPFOS 5 579 THPFOS 5 579 THPFOS 5 577 THPFOS 5566 THPFOS 5 572 THPFOS 5 563 THPFOS 5 557 THPFOS 5 553 THPFOS 5566 THPFOS 5 55 THPFOS 5 55 THPFOS 5538 THPFOS 5 547 THPFOS 5 536 THPFOS 5548 THPFOS 5 539 THPFOS 5 543 THPFOS 5565 THPFOS 5 552 THPFOS 5546 THPFOS 5544 THPFOS 5 5 4 THPFOS 5 53 THPFOS 5 537 THPFOS 5 543 THPFOS 5 547 THPFOS 5 551 THPFOS 5 53 THPFOS 5 5 4 THPFOS 5 53 THPFOS 5 543 THPFOS 5 537 THPFOS 5 543 THPFOS 5 547 THPFDS 5 55 THPFOS 5 5 4 THPFOS 5 543 Area 1468051 1464363 1466531 1454968 1451878 1446455 1446507 1431459 1426618 1421352 1446399 1409274 1275681 1266963 1199867 1189673 1186907 1174775 I189770 1195540 1228262 1192842 1191068 1162130 I 174278 1176312 1186618 1178574 1190379 1197508 1190786 1193614 1189879 1188319 1207047 1206309 1201824 1192316 1277981 1207619 Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 OmpoundNanw RT PFOS 5711 PFOS 5779 PFOS 5783 PFOS 5789 PFOS 5796 PFOS 5794 PFOS 5783 PFOS 5782 PFOS 5773 PFOS 5767 PFOS 5764 PFOS 5776 PFOS 576 PFOS 576 PFOS 5748 PFOS 5764 PFOS 5753 PFOS 5758 PFOS 5756 PFOS 576 PFOS 5775 PFOS 5769 PFOS 5763 PFOS 5761 PFOS 5757 PFOS 574 PFOS 5747 PFOS 5753 PFOS 5687 PFOS 5761 PFOS 5747 PFOS 5757 PFOS 5747 PFOS 576 PFOS 5755 PFOS 5753 PFOS 5757 PFOS 5767 PFOS 575 PFOS 5753 Area 467665 400427 226905 408798 1016639 1557482 1933591 2767322 3545665 7811414 11707065 13729087 213475 7409689 207290 7301061 209110 7206080 211149 7439383 216178 7363242 215488 7166019 205428 7213554 213374 7252833 417527 375240 209130 379300 918545 1439357 1778172 2591174 3298534 7225944 11337407 12852853 Amount 90 66 29 76 23 6 38 3 48 6 73 0 963 236 5 375 1 471 6 34 254 4 36 269 2 37 269 1 37 273 7 37 271 1 39 270 7 36 269 0 38 270 1 102 81 37 90 264 43 6 541 82 0 107 5 265 3 419 8 527 1 X 76% 94% 96% 97% 97% 96% 94% 94% 94% below LOP 102% b l o w LOO 107% below LOQ 107% beiow LOO 109% below LOP 108% below LOQ 107% X 90% 105% 109% 108% 1W% 107% 106% 105% 105% Page 1 of 4 BACK TO MAIN 3/9mi 23 03 3/9/01 23 14 39/01 23 25 3/9/01 23 36 m m i 23 47 3/9/01 23 58 3/10/010 10 $,lasl 021 310/01 032 3/1wO1 0 4 3 3/10/01 1 3 9 3/10101 1 5 0 3/10mi 2 01 3104012 13 3/104012 24 3/10/01 2 35 3/104012 46 3/10/01 2 57 3/10/01 3 08 3/10/01 3 20 3/10/01 4 16 3 101014 27 3/10/01 4 38 u101014 49 3/10/01 5 W 3/10/01 5 11 3110/01 5 23 3/10/01 5 34 3/10/01 5 45 3/10/01 5 56 310/01 6 52 3/10/017 03 3/10mi 7 15 3110401 7 26 3/10401 7 37 3/io/oi 7 48 31om1 7 59 3/10/01 0 11 3101018 22 3/10401 8 33 3/10401 9 29 3/10/01 940 3/10/01 951 3loM1 1003 D Wlem\Rush iW010309 b D \chem\Rush 1W010309b D \chem\Rush 1W010309b D \chem\Rusn 1W010309b D \chem\RLsh AR010309 b D Wlem\Rush 1W010309b D\chem\RJsh N1010309 b D bcnemiRusn ~ , h u i a uDr D Wem\RbSh AR010309 b D \chem\Rdsh hR010309 b D \ChemVlusha@010309 b D Wlem\Rdsh t\ROlOJD9 b D \chemlRJsh AR010309 b D Wlem\Rusn 1W010309b D \cnem\Rush 1W010309b D \mm\Rush tW010309 b D \cnem\Rush 1WOlO309b D \chem\RJsh i\R010309 b D \chem\Rush aAR010309 b D \Chem\RUsh Ni010309 b D \chem\Rush 1W010309b D \cnem\RLsn .W010309 b D \cnem\Rbsh W010309 b D WlemVldsh I\Ro10309 o D WlemVlush 1W010309b D Wem\Rurh 1W010309a D \cnem\Rush 1W010309b D \chem\Rush 1W010309b D Wem\RLsh tW010M9 b D Wlsm\Rush 1AR010309b D Wlem\Rdsh AR010309 b D \chem\Rrsh ,AROIOM9 b D WlemiRdsh ~ARO103090 D \mem\Rdsh hROIoJ09D D \cnemARush 1WO10309a D Wlem!Rt.sh tW010309 b D Wiem\Rdsh W010M9 b D Wlem\Rush W010309 b D \chem!Rdsh 1\R010309b D Wern\Rush RROlOM9 b D \chem\Rdsh i\ROlWW b D \cnem\Rusn 1\R010309b D \chem\Rush ~W010309b D \Chem\Rush 1W010309b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSHW36 D RUSH0037 D RUSH0038 D RUSHW39 D RUSHW D RUSHW41 D RUSHW42 D KUbHWJ D RUSHW D RUSHW45 D RUSHWSO D RUSHW51 D RUSHW52 D RUSHW53 D RUSH0054 D RUSHW55 D RUSHWD RUSHW57 D RUSH0058 D RUSH0059 D RUSH- D RUSHW65 D RUSH0066 D RUSHW67 D RUSHW68 D RUSH0069 D RUSHW7O D RUSH0071 D RUSH0072 D RUSH0073 D RUSH0078 D RUSH0079 D RUSH0080 D RUSHWI D RUSHWB2 D RUSHW83 D RUSH0084 D RUSH0085 D RUSH0086 D RUSHWB7 D RUSH0092 0 RUSHW93 D RUSH0094 D RUSHW95 D 1311-4058-54 1311 4 0 5 9 4 4 13114064-S4 1311-4065-54 13114066-54 13114088-S4 1311 4 0 8 9 6 4 13114~S4 13114094-S4 1311-409554 1311 4 w 6 - S 4 1311411BS4 1311 4 119-54 13114120-S4 13114W4-S5 1311-4W5-S5 13114W6-S5 1311 4 0 2 B S 5 1311-40M-S5 13114034-55 13114035-S5 1311-4036-S5 13114058-55 I311-4059-55 13114060-S5 1311-4064-S5 13114065-S 1311 4 0 6 6 S 5 1311 4 0 8 B S 5 13114089-S5 13114090S5 13114O94-S5 i3114w5-s5 1311-45 1311-4118-S5 13114119-S5 1311412&S5 131l-iOOeS6 13114W5-S6 1311400546 13114006MS-S6 13114028-S6 13114030-56 13114030MS-S6 Soill SOlll Soil2 Soil2 Soil2 Soil2 Soil2 SOIL2 Soil3 Soil3 Soil3 sod3 Soil3 Soil3 CnVl Cntrl Cnvl Cntd Cntrl SOlll sodl Soill Soill Soill Soill Soil2 Soil2 SOC? Soil2 Soia so112 Soil3 Soil3 Soil3 Soil3 Sot13 Soil3 Cntrl Cntrl Cntrl Cntrl Cntrl cntr1 Cnlrl THPFOS 5546 1463951 254 THPFOS 5 545 1400690 254 THPFOS 5 547 1086434 254 THPFOS 5 55 1289185 254 THPFOS 5 556 1063982 254 THPFOS 5 55 1351089 254 THPFOS 0 0 0 THPFOS 5544 1366635 254 THPFOS 5 549 1099645 254 THPFOS 5 537 1234304 254 THPFOS 5 557 62815 254 THPFOS 5 554 1038219 254 THPFOS 5 551 II72073 254 THPFOS 5 547 1188995 254 THPFOS 5 551 1269801 254 THPFOS 5 543 1239213 254 THPFOS 5 541 1295229 254 THPFOS 5 548 1187969 254 THPFOS 5 55 1957411 254 THPFOS 5 547 1453881 254 THPFOS 5 539 1153414 254 THPFOS 5 537 I099339 254 THPFOS 5544 1282394 254 THPFOS 5 536 1246108 254 THPFOS 5 535 1223354 254 THPFOS 554 1264548 254 THPFOS 5544 1228663 254 THPFOS 5544 1263001 254 THPFOS 5 552 1235655 254 THPFOS 5 542 1193060 254 THPFOS 5 547 1318378 254 THPFOS 5 55 I180237 254 THPFOS 5 551 1226490 254 THPFOS 5 542 1308839 254 THPFOS 5536 1290456 254 THPFOS 5 537 1336554 254 THPFOS 5 539 1245142 254 THPFOS 5 539 1304860 254 THPFOS 5 539 1261162 254 THPFOS 5 533 1247359 254 THPFOS 5 57 1071760 254 THPFOS 5565 1300949 254 THPFOS 5 569 1303672 254 THPFOS 5 57 1032466 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5756 5762 0 0 0 5788 5706 5761 0 5684 5704 5764 5768 5757 0 0 0 5758 5767 0 0 0 5754 5753 5753 0 O 0 5769 5759 5764 0 0 0 5753 5754 5757 0 0 0 578 5775 5786 578 408283 469387 0 0 0 2735601 12191 863841 0 2999325 11924 420566 644551 595758 0 0 0 419771 476453 0 0 0 1014587 985016 1148377 0 D 0 1393130 1451794 1656632 0 0 0 747647 955425 958092 0 0 0 5486963 444872 428399 5773407 96 96 00 00 00 768 00 21 0 00 940 42 123 178 159 00 00 00 103 62 00 00 00 271 271 329 00 00 00 403 438 454 00 00 00 189 241 263 00 00 00 2170 99 94 241 4 Page 2 of 4 BACK TO MAIN 3110101 10 14 D \chem\RLsn ARO10309 b 31iomi 10 25 D\chem\RdshhR010309D 3110101 10 36 D WrnlRdsh i\R010309b 3110101 1047 D knem!RLsn hR010309b 3110101 10 59 D \chemlRusn hR010309b 31lOtO1 11 10 DkhemlRdsh tW010309b J l l O l O l 12 06 D m \ R d s h iW010309b 3110101 12 17 D Wlem\Rush t\R010309 D 71lnl~1l 2 ?R n \rh?mlQnsh S & O Q * Q ~cQ ~ 3110101 12 39 D hemlRush hR010309b 3110101 12 51 D knem\Rbsh1U7010309b 3110101 13 02 D WlemRush tW010309 D 3110101 13 13 D ichem\RdshW.O10309o 3110101 13 24 D \chemRush ARO10309 b 311D101 13 35 D \cnem\Rush1WOlOx19b 311010113 46 D knemWushI ~ o i 0 3 0 9b 3110101 14 43 D \chemLQush iW010309 b ~ 1 0 1 0114 54 O\chem\Rush~ ~ 0 1 0 3 0b9 311010115 05 D \cnem\RbshiAJ3010309b 311010115 16 D!chem\RJsh.\R010309b 3110101 1527 O!chem\RushNi010309b 3110101 15 39 D WmlRusn 1u1010309b 311010115 50 D \cnem\Rush<W010309b 311010116 01 D WlemWurh1W010309b 3110101 16 12 0 Wem\Rusn 1U7010309b 3110101 16 23 D \cnem\RLsh AR010309 0 311010117 19 D \chemW.sh 1AR010309o 311010117 30 D \chern\RushiAR010309b 3110101 17 42 D \chem\Rush N1010309 b 3110101 17 53 D \cnern\Rusn iWO10309 b 3110101 1804 D Mem\Rusn 1hR010309o 3110101 18 15 D WlemVLsh tAfZ010309 b 3llO101 18 26 D\chem\Rush 1\R010309b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0096 D RUSH0097 D RUSHW96 b RUSH0099 D RUSHOlW D RUSH0101 D RUSHOICG D RUSH0107 D DL'SUO'OB E RUSH0109 D RUSH0110 D RUSH0111 D RUSH0112 0 RUSH0113 D RUSH0114 D RUSH0115 0 RUSH0120 D RUSH0121 D RUSH0122 D RUSH0123 D RUSH0124 0 RUSH0125 D RUSH0126 D RUSH0127 D RUSH0128 D RUSH0129 D RUSH0134 D RUSH0135 D RUSH01360 RUSH0137 0 RUSH0138 0 RUSH0139 D RUSH0140 D 13114034-S6 13114035-S6 13114036-S6 13114036MS-S6 1311405866 1311-4O59-S6 13114WJS6 1311406OMS-S6 13114c63 s5 1311406566 13114WS6 13114066MS-S6 1311408&s6 1311-4089-S6 1311409OS6 13114090MS-S6 13114O94-S6 1311 4 0 9 5 3 6 13114096-S6 13114096MS-S6 1311 4 11866 13114119s6 13114120-S6 13114120MS66 13114004S7 13114W5-S7 13114006-S7 13114028-57 13114030-S7 1311-4034-S7 13114035S7 1311 4 0 M S 7 13114058-S7 sol11 Soill soill Soill Soill Soill Snill Soill e-:- YVlY Soin Soil2 Soil2 Soil2 sol12 Soil2 Soil2 Soil3 Soil3 Soil3 Soil3 Soil3 SOB3 Soil3 Soil3 Cntrl Cnlrl Cnlrl Cnlrl Cnlrl Soitl Soill Soill Soill THPFOS 5565 1333744 254 THPFOS 5 572 1338340 254 THPFOS 5 572 1245746 254 THPFOS 5 565 1068189 254 THPFOS 5 565 1280942 254 THPFOS 5 559 1242425 254 THPFOS 5 556 1262511 254 -..,.-.^^ THPFOS TI wnrn.. IrlrrV- 5 565 5s 1213422 ILJJIaV 254 2% THPFOS 5 557 1250558 254 THPFOS 5 559 1239303 254 THPFOS 5 551 1034913 254 THPFOS 5 565 1253690 254 THPFOS 5 553 1250794 254 THPFOS 5 557 1285551 254 THPFOS 5 543 1080374 254 THPFOS 5 561 1242888 254 THPFOS 5 551 1231504 254 THPFOS 5543 1217872 254 THPFOS 5 538 1050039 254 THPFOS 5 543 1289869 254 THPFOS 5544 1232248 254 THPFOS 5 545 1307515 254 THPFOS 5 537 1053782 254 THPFOS 553 1230338 254 THPFOS 5544 1250384 254 THPFOS 5 543 1221946 254 THPFOS 5 538 1266595 254 THPFOS 5 537 1 192244 254 THPFOS 5 535 1218042 254 THPFOS 5 53 1194839 254 THPFOS 5 539 1252105 254 THPFOS 5 532 1194656 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 0 0 5775 5775 5776 5766 5775 u 0 0 5768 5775 577 5775 576 0 0 0 5755 576 5754 5755 5747 0 0 0 5748 5748 0 574 0 5742 0 0 0 5657330 1095297 1011012 1003621 5974975 o 0 0 5360487 1362179 1415860 1334234 6447671 0 0 0 5229681 1101877 1018381 993087 6331963 0 0 0 432393 423701 0 375306 0 962584 00 00 00 226 5 29 6 28 0 27 2 208 2 00 00 00 220 8 385 405 367 260 5 00 00 00 211 0 29 6 28 5 25 9 262 6 00 00 00 99 10 4 00 89 00 27 7 Page 3 of 4 BACK TO MAIN 3/9/01 20 04 3/9/01 20 15 39/01 22 40 3/9/01 22 51 3410101 1 17 3/10101 1 28 31101013 53 3110101 4 W 34101016 30 3110101641 3/10/01 9 07 3410/01 9 18 3/10101 11 43 3110/01 11 54 3/10101 14 20 3/10/01 14 31 3/10/01 16 57 3l10101 17 08 3410101 19 W 3/10/0119 11 3110101 21 36 3/10101 21 48 D khwmwush RR010309b D WemWush W010309 b D Wem\Rush 1W.010309b D Wwm\RushRR010309b D Wsm\Rush 1W.010309b 0 \chem\Rush W010309 b D WwmWush WO10309b D Wem\Rush W010309 b D Wem\Rush 1W010309b DMe1n\RushiWO10309b 0 WernWush 1W.010309b 0 \chwm\Rush i ! R O I O J w b 0 WemWush W010309 b 0 Wem\Rush W0103W b DWem\Rush RR010309b 0 MemRuSh 1W.010309b D Wwm\Rush1W.010309b 0 Wem\Rush RR010309b D Mem\RushRR0103W b OWwm\Rush 1W0103W b D\chem\RushRR010309b 0 WemWush W010309 b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RAMPI F SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0020 D RUSH0021 D RUSHW2-I D RUSH0035 D RUSH0248 D RUSHW49 D RUSH0052 D RIISHMW n RUSH0076 0 RUSH0077 D RUSH0090 D RUSH0091 D RUSH0104 D RUSH0105 D RUSH0118 D RUSH0119 D RUSH0132 D RUSH0133 D RUSH0143 D RUSH0144 D RUSH0157 D RUSH0158 0 TNA 4802 MWOH TNA 4802 MWOH TN-A 4802 MeOH TNd4802 MWOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 M ~ O H TN-A4802 MeOH TN-A 4802 MaOH TNA 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TKA4802 MeOH TN-A 4802 MeOH TN-A4802 MWOH TN-A 4802 MWOH TN-A 4802 MeOH TN.A4802 MeOH TN-A 4802 MeOH TN-A 4802 MWOH THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 TUPFOS n THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 THPFOS 0 0 0 PFOS 5802 49447 00 0 PFOS 5809 24769 00 0 PFOS 5799 34422 00 0 PFOS 5792 20717 00 0 PFOS 5785 21865 00 0 PFOS 575 15324 00 0 PFOS 5783 18986 00 PFG8 5685 i5i24 00 0 PFOS 5697 18689 00 0 PFOS 5707 15833 00 0 PFOS 5788 23180 00 0 PFOS 5718 16806 00 0 PFOS 5782 23713 00 0 PFOS 5712 le643 00 0 PFOS 5701 22854 00 0 PFOS 5698 20038 00 0 PFOS 5682 25164 00 0 PFOS 569 20930 00 0 PFOS 5696 24815 00 0 PFOS 5698 22446 00 0 PFOS 5783 38306 00 0 PFOS 5705 27663 00 Page 4 of 4 EW-1311 PFOSAdslOes BACK TO MAIN Samole Batch H010313.b. analned on HlllaN 034301. PFDS AdsorbIDesorb8ampIu. M8Wx: SolUSlglSed. StandardcuNe range u&d for~callbntlonotsamplu: 5501 ngmL (2.5 ngmLstd-not included due tolhe hlgher sampleconcentration nnge). Batch method HOlO3lld.m Inj Date Batch SampType File Sample Name MISCInfo CompoundName RT Area Amount CompoundNams RT A n a Amount 3/13/01 12:M D WemWiilary iW010313b 3/13/01 IS07 D M e m W i l l w iW010313 b 3/13/01 1338 D WwmWillary iW010313b 3/13/01 1330 D WemWillary AH010313 b 3/13/011341 D MemWillary iW010313b 3/13/01 1352 0WemWillary iW010313b 3/13/0114:04 DMemWilla~yiW010313b 3/13/01 14:15 D MemWillary iW010313 b 3/13/01 1426 D MemWiliary tW010313 b 3/13/011438 D WemWillary iW010313b 3/13/01 14:49 DWemWillary iW010313b 3/13/01 15:Ol DWemWiilary iW010313b 3/13/0117:40 DWemWillary iW010313b 3/13/011751 DMemWillary iW010313 b 3/14/01 9:37 DMemWillary iW010313 b 3 m m 1 9-48 D\chemWilIa~yiW010313 b wi4mi i z : i 6 D WemWiliary iW010313 b 3/14/01 12.28 D WemWiliary tW010313 b 3/14rnii4:44 D MemWillary iW010313b 3/14/01 14:s DMwmWiliary iW010313 b 31141011530 0WlemMllary iWO10313 b 3/14/01 15.41 D WemWillary iWO10313 b 3/14/01 1553 DWemWillary iW010313b 3/14/01 1 6 : ~D WemWiliary iW010313b 3/14/01 1635 D MemWillary iW010313 b 3/14mi16:27 0 MemWillary iW010313 b 3/14/01 16-38 D WemWillary iW010313 b 3/+4/01i6:49 D WemWiliafy tWO10313 b 3/14/01w o i D WemWllary iW010313b 3/14/01 1 7 : ~ D MemWiilaty iW010313 b 3/14/01 17:24 D WemWillary iW010313 b 3/14/01 1 7 s DWemWillary tW010313 b SAMPLE SAMPLE CALlB-I CALIB-2 CALIB-3 CALIB-4 CALIE-5 CALIE-6 CALIE-7 CALlB-8 CALIB-9 CALlB-10 CCALIB-1 CCALlE-1 CCALiE-1 CCALIB-1 CCALIB-1 CCALIB-1 CCALiB-I CCALIB-1 SAMPLE SAMPLE CALlE-11 CALIE-12 CALIB-13 CALIB-14 CALM-15 CALlE-16 CALIE-17 CALIB-18 CALIE-19 CALlB-20 HILLW16.D 0 nglmL PFOS in MeOH HILLW17.D 2.5 nglmL PFOS in MeOH HILL0018.D 5 W L PFOS in MeOH HlLL0019.D 10WnL PFOS in MeOH HILL0020.D 25 W L PFOS in MeOH HILLW21.D 40 nglmL PFOS in MeOH HILL0022 D 50.1 nglmL PFOS in MeOH HILLW23.D 75.1 nglrnL PFOS in MeOH HILL0024 D 100.2 n#mL PFOS in MeOH HILL0025.D 250.5 nghnL PFOS In MeOH HILL0026.D 400.8 nglmL PFOS in MeOH HILL0027.D 501 nglmL PFOS in MeOH HILLW41.D 5 nglmL PFOS in MEOH HILLW42.D 250.5nglmL PFCSin MeOH HILLW55.D 5 n#mL PFOS in MeOH HILLW56.0 250 5 nghnL PFOS in MeOH HILL0069.D 5 n@L PFOS in MeOH HILL0070.D 250.5 nglmL PFOS in MeOH HILL0082.D 5 ngmL PFOS in MeOH HILLW83 D 250.5nglmL PFOS in MeOH HILL0086 D 0 npknc PFOS in MeOH HILL0087.D 2.5 nphnL PFOS in MeOH HILLW88.D 5 nghnL PFOS in MeOH HlLLW89.D 10cghnL PFOS in MeOH H1LLWSO.D 25 n#mL PFOS in MeOH HILL0091.D 40 nghnL PFOS in MeOH HILL0092.D 50.1 ngmL PFOS in MeOH HILLOO93.D 75.1 nphnL PFOS in MeOH HiLLW94 D 1 W 2 M L PFOS in MeOH HILLWO5.D 250.5 nghlL PFOS in MeOH H1LLWM.D 400.8nglmL PFOS in MeOH HILL0097.D 501 nglmL PFOS in MeOH THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 499 986728 499 1004472 499 1053980 499 969429 499 1025198 499 1022879 499 1010348 499 998418 499 1010291 499 1043378 498 975369 498 10401w 498 973042 498 965534 501 1293233 499 1084981 498 953043 498 928765 498 916687 497 906152 497 884570 497 895265 498 62083 498 913122 488 9 2 2 w 498 836408 498 925210 498 908053 498 925726 498 987131 498 893733 498 968040 -- Avenae: 977950 Std Dev: 77747.7 %RSD: 0.0% 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 OC IS range (+3I-2% average): 1271335 +30%. 684565 -30%: PFOS PFDS PFOS PFOS PFOS PFOS PFDS PFDS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFOS PFOS PFDS PFOS PFOS PFDS PFOS 0.00 521 5.21 5.21 5.21 5.21 5.21 5.21 5.21 5.21 5.20 5.20 5.20 521 5.24 5.21 5.20 5.20 5.22 50.2000 5.20 5.20 5.20 5.21 5.20 5.20 5.21 5.21 5.21 5.20 5.20 0 81205 141737 225923 598942 MU44 1166397 1754434 2316691 5628366 8318503 lOJg0908 154385 5687791 160636 6108094 155058 5707416 273109 56620486 83400 153877 221204 589951 936043 I160241 1701449 2264695 5613136 8216BM) 10392100 0.0 2.9 5.1 8.9 23.8 38.2 47.9 73.7 97.1 239.1 394.6 469 7 61 263 0 53 250 4 63 275.3 11.9 280.3 0.0 34 62 96 261 41 3 52 1 78 a 1038 258 8 429 2 511 3 yDev 102 6% 89 1% 95 3% 95 6% 95 7% 98 1% 98 9% 95 5% 98 5% 93 8% 122 5% 105 0% 106 9% 1000% 125 9% 109 9% 238 4% 111 9% 123.6% 95.8% 104.5% 103.2% 104 0% 104.9% 103.6% 103.3% 107.1% 102 1% Page 1 of3 EW-1311 PFOSAdslDes BACK TO MAIN 73 Lu (D m Sample Batch H010313.b. analyzed on Hlllary 03-13.01. PFOSAdsorblDUorb SImpleS. Matrlx: SolVSlplSed. Standard cuwe rangeused For calibration ofsampies: 6-501 n@mL(2.1 n@mLstd not Included due to the hlgf Batch method H010315d.m Inj Date Batch SampType File Sample Name Miss Info 3/13/01 1546 3/13/01 1557 3/13/01 16:M) 3/13/01 16:20 3/13/01 1631 3/13/01 16:43 3/13/01 1654 3/13/01 17:ffi 3/13/01 17:17 3/13/01 17:28 3/13/01 19.22 3/13/01 1933 3113101 19:45 3/i3mi 20.08 3/14/01 10:23 3/14/01 1034 3/14/01 io:45 3/14/01 10:57 3/14/01 ii:o8 ~ i 4 mi i : i g 3/14/01 1131 wi4mi ii:4z 3/14/01 11% 3/14/01 12:05 DWlernWillary.iW010313.b SAMPLE HILLW31.D D:WlemWillary.iW010313b SAMPLE HILLW32.D D:WemWillary.i\H010313.b SAMPLE HILL0033.D DMemWillary.iW010313.b SAMPLE HILLW34.D DWemWillary.iV(O10313.b SAMPLE HILLW35.D D\chemWillary.iWO10313.b SAMPLE HiLLOO36 D D:WemWillaryRH010313.b SAMPLE HILLW37.D D:WemWillary.RH010313.b SAMPLE HILLW38.D D.WlemWillary.iW010313.b SAMPLE HILLW39.D D WlemWillary.iW010313.b SAMPLE HILL0040 D SP*LPLEU"'M"C"fPUPLEU"'M"P"fPUPLEnum4za- v-w- D.WernWillary.iW010313.b SAMPLE HILLW50.D D:WlmWillary.iWO10313.b SAMPLE HILLW51.D DWernWillaN.lW01W13.b SAMPLE HlLLW52.D --w+wlw SAUaEu"'ML.1" DWlemWillary ih010313 b SAMPLE H.LLW54 D D WlemWlllary Mol0313 b SAMPLE HILLW59D D Wemhillary !W010313 b SAMPLE HILLWBOD D\chemW.llaryiW010313 b SAMPLE HILL0061 D D\chemWillaryiW010313 b SAMPLE hlLL0062D D \chernWillary1h010313 b SAMPLE HILL0063 D D WemWl.lary RHO10313b SAMPLE H I L L W D D~emWllary1W010313b SAMPLE HILL0065 D 0 \damWdlary iW010313 b SAMPLE HLL0066D D WernWiI ary iW010313 b SAMPLE HILL0067 D D\chernWillary1W010313b SAMPLE HILL0068 D vsAAIeLsl=uumun vsAAwLaU"'M7"" vsAlAaLSU."M7C." vfP*LeLSY'1M7C" sAAwLaMucw?.o EW-13115062S2 E0013115063SZ E00.1311-5063MSS2 EW-1311-5064S2 E00-13115065S2 EN1311-506BS2 E00.13115066MSS2 EW-13115087SZ EW-13115068SZ EW-1311-5069S2 - EW1311-509142 EN1311JWZS2 EOC~13115093S2 EN1311-509442 EW-13115095S2 Em1311 - 5 0 9 M 2 E00-13115096YSS2 E00-1311509752 EWl311-509BSZ EW-1311-5099-SZ E0013115099YSS2 E001311 5 1W S 2 EW.1311-5101S2 - - - -E00-13115102S2 Soil2 Soilz Sol12 Soil2 soil2 Soil2 So112 Soil2 Soil2 Soil2 foro solla solla foro soil3 Soil3 S.oi~ l3. &#a SO113 SOID Soil3 Soil3 SOB3 Soil3 Soil3 Soil3 Soil3 Soil3 soil3 rioiu foro foiu &#a fciu THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFDS THPFOS SblPFof SblPFof XnBCas XnBCas XnBCas THPFOS THPFOS THPFOS UlPEof THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS xuEos xn!aEas TWKs SblPFof XnBCas xn!aEas WeFnS XnBCas SblPFof 4.99 4.98 4.99 4.99 4.99 4.99 4 99 4.99 4.99 4.09 498 49s 488 eo0 488 4.98 4.99 4.90 499 4 99 4.99 4.98 4.90 4 98 4.98 4.99 4.99 4.98 499 4.98 e98 488 498 498 488 488 499 49s poz -Amount ISTD ucrfomance commentt 909345 254 895204 254 758109 254 865275 254 860270 254 048747 254 733500 254 826114 254 835017 254 833819 254 xu34 a54 a5823 a54 a34522 a54 ZM401 142 6wau a54 824186 254 786360 254 815722 254 6eI.Ga a54 814408 254 878131 254 874013 254 723198 254 652831 254 841962 254 822198 254 709765 254 827302 254 824224 254 830977 254 u6a.u a54 8260.?4 a54 843dal3 834.736 a54 6lx3E4 a54 395312 a54 ZLDDU 142 ZE52%2 a54 67xuis a54 Compound Name RT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS WclS PCQf PEOf nwas PEOf PFOS PFOS PFOS psoc PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PEOf pcoc PEOf P.$as pcoc WclS psof PEOf 5.22 5.20 5.21 5.20 5.20 5.21 5.21 5.21 5.21 5.20 510 510 510 w 510 5.20 5.21 5.21 w 5.21 5.22 5.21 5.21 5.20 5.20 5.21 520 5.20 5.20 5 20 .a$ 510 511 ha0 510 510 518 519 519 Ana 1448358 1150879 4304297 2329091 2422898 3659129 6555441 7740434 7494802 6105464 a5aEaZB azu6.7a aa535Ea zl?axuS 14219500 2640517 945552 670677 362Sa35 822587 7N5W 736105 4068910 2533547 2481828 2597099 -5483252 6079541 5936738 6228226 8966(p1 4-wYW6 4w44.76 15*90681 v 34a53u azE65s6 36a3aa3 Avenue: 802682.15 Std Lkv: 61470.3 XRSD: 7.m Amount 666 53 4 252 7 1147 120 2 lea2 415 8 438 9 4178 -333 4 66aa aous a4Su 4662.0 1376 49 9 33 8 235A 41 7 35 2 346 250 2 127 1 126 1 135 5 353 6 334 7 327 4 -342 0 6191 638.6 WLO zokl lODe0 3u.u 3aZQ.a 4ca5.9 Comments Page 2 of 3 EW-1311 PFOSAddDes BACK TO MAIN Sample BatchHOIOS13.b, analyzedon HMIay 034591. PFOS AdroIWWSOrb samples. Matrix. S o l U S l ~ t d . Standad cuwe range usedfor callbratlonofsamples: 6-601 nplmL(2.5 ng/mLrtd not Includeddueto the hlghersample COncentRUOn range). Batch method H010313d.m In1 Date Batch SmpTypyp. File Sample Name Mlrc Info CompoundName RT A n a 3/13/01 1233 3/13/01 1244 3/13/01 i5:iz 3/13/01 i s m 3/13/01 15.35 3/13/01 1802 3/13/01 18:14 3114~1110:w 3/14/0iio:11 3/14/01 1239 3114101 i2:51 3/14/01 15:07 3/i4mi i5:ig 3/14/01 17:46 3114101 1758 D khernWillaryiUi010313b D WernWillary1W010313b DkhernWillaryiUi010313b DWernWtllaryiUi010313b D WlemWillary 1W010313b DWernWlllary1W010313b D WernWlllary iW010313 b D khernWtllaiyiUi010313b DkhernWillary 1W010313b D WernWillary iW010313 b DWmWtllary Ni010313b D WernWlllary iW010313 b DWemWlllaryiWOl0313 b D WernWillary iW010313 b DWernWtllaryRH010313b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0014.D HILLW15.D HILLW28.D HILL0029.D HILL0030.D HILL0043.D HlLLW44.D HILLW57.D HILLW58.D HILLW71.D HILLW72.D HILL0084.D HlLL0085.D HILLOOO8.D HILLW99.D TN-A4802 MeOH TN44802 MeOH TN-A4802 MeOH TN-A 4802 MeOH TN-A4802 MeOH TN44802 MeOH TN44802 MeOH TN44802 MeOH TN44802 MeOH TN-A4802 MeOH TN-A4&02 MeOH TN-A4802 MeOH TN4 4802 MeOH TN-A 4802 MeOH TN44802 MeOH THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 000 0 ow 0 ow 0 000 0 ow 0 OW 0 ow 0 ow 0 ow 0 ow 0 ow 0 000 0 ow 0 ow 0 ow 0 Amount Compound Name UT Area 0 PFOS 5.25 23051 0 PFOS 0.00 0 0 PFOS 5.25 18799 0 PFOS 0.w 0 0 PFOS 0.w 0 0 PFOS 5.25 0263 0 PFOS 0.00 0 0 PFOS 0.03 0 0 PFOS 0.00 0 0 PFOS 5.25 10516 0 PFOS 0.00 0 0 PFOS 5.25 23204 0 PFOS 5.25 1m1 0 PFOS 5.25 16777 0 PFOS 0.00 0 Amount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Page3013 BACK TO MAIN Appendix I: Traceability Information This appendix includes traceability information on the test substances and standards used in this study. 3M Environmental Laboratory Page 594 of 703 -or reference # Substance/chemit:al name: LotJbatch #: TCR Substance # Purified PFOS, Perfluorooctanesulfonate (Primary Suntdk)nown Received from: TCR-00017-046 George Moore BACK TO MAIN Expiration date: 08/31/2001 IInitials: 7 7 containers: I / 20 mL Nalgene bottle g o o d white powder IRetain 0.3480 g Amount received (wt. or vol): Date: 05/31/2000 Shipper: unknown MSDS Wn) Date of Retain mYUN 05/31/2000 IPurity: 97.9% LAC 09/19/00 IRecords received: NIA Recrystallized by George Moore, Bldg 236 fabrication, or derivation i records: Std Location/Storage: FI9, Frozen /Molecular Formula: ~ C8Fl7S03-K+ Standard has been moved to Freezer 19 in room 347 KJD 6/7/00 Empty container weight approximatelly 11.869. LCG 8/16/00 tandard weighed on 9\28/00was stored frozen at -2OC+/- 10C untilshippment on 10/3/00 LAC 10/3/00 Standard was stored at room temperature prior to 6/7/00 LAC 12/21/00 tcr99030-46msds.pdf COA(PF0S Primary Std).pdf 3M Environmental Laboratory Page 595 of 703 BACK TO MAIN Centre Analytical Laboratorks, Inc. 3048 Research Drive State College, PA 16801 Phone: (814)231-8032 Fax: (814)231-1253or (814)231-1580 INTElUM CERTIFICATE OF ANALYSIS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-021 3M Product: PFOS, Primary Standard Test ControlReference # TCR00017-46 Purity: 97.9% Metals I. `calcium' 2. Magnesium 3. Sodium 4. Potassium' 5. Nickel 6. Iron - Residual SolGents (TGA) Purity by DSC Inorganic Anions (IC) 1. 0.006 wt./wt.% 2. 0.002 wt./wt.% 3. 1.216 wt./wt.% 4. 6.685 wt./wt.% 5. <0.001 wt./wt.% 6. 0.002 wt./wt.% None Detected 97.5 Mol. %. 2. Hydrogen 3. Nitrogen 4. Sulfur 5 Fluorine COA023-02 1 3M Environmental Laboratory 2. TheoreticalValue =0% 3I Theoretical Value =0% 4. Theoretical Value = 5.95% 5. Theoretical Value = 60% 2. 0.456 wt./wt.% 3. 1.51 wt./wt.% 4. 7.80 wt./wt.% 5. 58.0 wt./wt.% Page 1 of 3 ___--. - -~ Page 596 of 703 BACK TO MAIN - 3048 Research Drive State College, PA 16801- Phone: (814)231-8032 Fax: (814)231-1253or (814)231-1580 INTERIM CERTIFICATE OF ANALYSIS Centre Analytical Laboratories COA Reference #: 023-021 . Date o f Last Analysis: 08/31/00 Expiration Date: 08/31/01 StorageConditions: Frozen 5-10C Re-assessmentDate: 08131/01 `Purity= 100% - (sum of metal impurities, 1.226% +LC/MS impurities, 0.14%+Inorganic Fluoride, 0.60%+NMR Xmpurity, 0.13%). Total impurity from all tests = 2.09% Purity = 100% - 2.09% i= 97.9% 2Pota+ssiumis expected in this salt form and is thereforenot considered animpurity. 3Sulfilrin the sample appearsto be converted to SO4 and hence detectedusing the inorganicanion methodconditions. The anion result agrees well with the s u l h determinationin the elemental analysis,lending confidenceto this interpretation. Based ,P- on the results, the SO4 is not consideredan impurity. 9FA HFElA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoicacid Pentafluoropropanoicacid STheoreticalvalue calculationsbased on the empiricalformula, C&7SO3X+ ( M W 4 3 8). Tbis *workwas conductedunder EPA Good LaboratoryPractice Standards(40 CFR 160). COA023-021 3M Environmenfal Laboratory Page 2 of3 - - . - ___ - Page 597 of 703 BACK TO MAIN Ctsntrti Analytical Laboratorigs, Inc. 3048 Research Drive State College, PA 16801 f- MP&&pm%JB~ ~ - ~ ~ ~ (81~4) 23$1-15f80 j ~ O r i CentreAnalyticalLaboratoriesCOA Reference# 023-021 LCMS Purity Profile: Total Note: The C7 value was calculatedusing the averageresponse factors from the C6 and C8 standard curves. Prep:wed By: 9/ohm Date Date Laboratory Manager, Centre Analytical Laboratories . COAO23-021 3M Environmental Laboratory Page 3 of 3 Page 598 of 703 BACK TO MAIN I withdrawal 19.90999 I (massor vol) 10.5069 g Gross wt/vol aRer I withdrawal 19.4030 g Purpose (enter standard number) I(Adsorb/Desorb Study Balance I D Initials Date I1914 IILCG I~10/17/2000 1I 3M Environmetiltal Laboratory Page 599 of 703 BACK TO MAIN lLot/batch #: \Initials: containers: -1[Retain "Don Uglem" 00-2404 12/31/2015 LCG dried and sieved Received from: Agvise Amount received (wt. or 900 grams, Bulk vol): Date: 10/23/2000 Shipper: Fed Express MSDS (v/n) Date of Retain 3YWN Ifabrication, or derivation I I I I Irecords: I Std Location/Storage: Container stored ambient in TCR-CO2. LCG 12/26/00 . ..-. Molecular Formula: I-f.,.nrn, mon,.t,c II T.C-R.- -st-i.c-.ker a-d-d--ed- t-o- bottle after original weight LCG 10/25/00 I I"1 I I1 Don Uglem loam-0-6.pdf 3M Environmental Laboratory Page 600 of 703 BACK TO MAIN Highway I5 P.O. Box 510 Northwood ND 58267 (701) 587-6010 FAX 000 587-6013 email: agvise@pIarcomm.com Homepage agvklabscom AGVISE S o i l Characterization Report Submi.tting firm = 3M Protocol or Study No = NA Sample ID. = DON UGLEM-LOAM 0-6 Trial. ID. = NA Date Received = 10-23-00 Date Reported = 10-31-2000 AGVISE L a b NO 00- 2404 Percent Sand 39 Percent Silt 50 Percent Clay 11 USDA Textural Class (hydrometer method) Loam Cation Exchange Capacity (meq/100 g) 23.9 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total. Nitrogen (%) 4.9 8.4 7.4 0.358 Base Saturation Data Cation Calcium Magnesium Sodium Pot as sium Hydrogen eercent 52.2 20.9 0.7 3 -5 22.7 QQm 2500 600 38 324 54 These! tests were completed in compliance of 40 CFR Part 160. io-31- 00 Date 3M Environmeni!alLaboratory Agricultural Testing Page 601 of 703 BACK TO MAIN A m K L A B O R A T O ER I E S 1 Highway 15 P.O. BOX 510 Northwood ND 58267 (701) 587-6010 FAX (701) 587-6013 email: agvise(Ppolarcommcom Homepage agviselabs.com The following personnel have been duly trained to perform Plant Analysis, Soil and Water Characterizationmethods under 40 CFR Part 160 Good Lahratory Practice Standards. Technical Support Staff Aaderson, LindaM. - TechnicianIII - Deutsch, Robert L. President Hart,Linda M. - TechnicianIII - Hime, SherryL. TechnicianI Johnson,Julie M. - Nutrient LaboratoryManager - McNeil, Vigo (Art) TechnicianI Moen, Lucinda S.- TechnicianIII - Polled, Garis Nutrient LaboratoryAnalyst - Pollock, John TechnicianI - Wall,Mary J. TechnicianII Wyant, Linda L. - TechnicianI Office Support Staff - Berg, Eileen A. SecretaryIII - Ducioame, Gail M. Quality Control Specialist Fuglestad, Teresa S.- SecretaryII - Hagen, Shelly J. Administrative Assistant Qualitv Assurance Thingelstad, Mary L. - Quality Assurance Manager COPY OF ORGINAL oratories, Inc. lniti DateJ9-2J'-- 05/00 3M Environmental Laboratory Agricultural Testing Page 602 of 703 BACK TO MAIN - Bulk De& Disturbedbulk density is determined by weighing a known volume of dried and ground S ; O (~NUT.02.10). Core or nondisturbed bulk density is determined by weighing a known t volume of an intact,dried soil core (NUT.02.02). Water Holdine CaDacitv and Water Relations M o i s t u n a - Determined by gravimetricloss upon drying (NUT.02.36). Saturatql'zkvdrauicConductivity- Determind byusingthe ccmtant head method and measuring the rate of flow of water through a saturated soil column (NUT.02.34). - Water InfiltrationRate Determined by using the constant head method and measuring the length of time fiom water applicationto production of a leachate from a soil column (NUT.02.35)- .., Water Holdine Capacity- Determined by measuringthe moisture remaining when saturatedsoilis placed under 1/3 or 0.10 bar pressure ("l'.02.08). Water Holdine Cauacity - Determined by measuring the moisture remaining when saturated soil is I placed under 15 bar pressure (NUT.02.13). All of the above methods are detailed in the current analyticalSOPSused by AGVISE Laboratories' Characterizationtesting laboratory. NUT.05.01. Low Term Storaee of Soil and Water Characterization Specimens: According to this SOP, soil characterizationsamples will be retained by AGVISE Laboratoriesfor at least twoyears before dqosal and water characterization samples will be retained for a period of 60 days before disposal. ADM.05.01. Archivist Duties and Archivine Procedures: This SOP states that copies of soil and water characterizationreports, original COC's and original raw data will be archivedwithin 60 days after the signatureby the analytical investigator. Hard copies generated by computer will be archived weekly, and supplemental data will be archived annually. OAU.08.01. Oualitv Assurance InsDections of Facilities. Studies. and Processes for GLP ComDliance: Method inspectionswill be performed on a regular basis at AGVISE Laboratories, Inc. Far soil characterization, two methodswill be inspected per month and one water charactlsrization inspection will be conducted per month. An annual facility audit will be perfomled by AGVISE Laboratories, Inc. Quality Assurance Unit. All of the above methods are detailed in the current analytical SOP'S used in AGVISE Laboratones' characterization laboratorv. . APPROVEDBY ANALYTICAL INVESTIGATOR -Robert L. Deutsch, Soil Scientist ate 3M Environmenl'al Laboratory Page 603 of 703 BACK TO MAIN Collection Information - 'i SiteIdentification 7)- hl*, % & ! I Sample ID AGVl SE kb+t d o 0 ~ 1 0 4 GeographicalReference h . h j J L/7 * l/f/' Lonq~&.:-ql . 48I Date ofSampling /0-19-00 PA, Use Elattern (e.g. agricultural,forest, etc.) N o m I . 1- - Depth of Sampling 0 L, " Collectedby &-k P&k ........................................................ .K. e& SiteIdentification fin- ,!.oa/m, Sample ID A h Y / l s F Lah # (JOY ac105 GeographicalReference h & t d ~~ ./ 7 * J a ' Lon*;l2p/r,." 4 97 "r/b' - - Date of Sampling 10 19 00 Use Pattern (e.g. agricdtud, forest, etc.) A , DepthofSampling Collectedby O-L " Pn&k ........................................................ ,80- .A SiteIdentification 12uu/l> Adc/n, Sample ID OO-A'+ob 46visE Labe GeographicalReference Lnt;;tud, : 4 7 45' Lona&d,, ~ 97037' Date of Sampling 10 - I9 - 00 Use 'attern(e.g. a g r i m forest, etc.) ,MA - Depthof Sampling 6 I1 m Collectedby A r t C N Q d . 0 h8attm-A ........................................................ K SiteI d e ~ ~ t i o nd h c n - , to. f - SampleID A 6 V i s F h b e 60aaI/07 GeographicalReference LL&.!L& $f * h a ' I_oh&:-96 'VI' Date of Sampling i o - a i - 00 . . use I'attern (e.g. agricultural,forest, etc.) Depth of Sampling - I( L\wuu.&wd, $yb 3M Environmental Laboratory Page 604 of 703 BACK TO MAIN GLP Ll Non-GLP Characterization Chain of Custody SEND RESULTSTO 7& jl/// BILL TO: Phone: AGVISE Use Only Date received 7 0 A 06' n v Comments Purchase Order # Protocol/study # Test Substance stuuy Director Sponsor Initiation Date Specimen I.D. ~GVISE Laboratories, Inc. P.O. Box 5WHighway15 Northwood, ND58267 - Telephone (701) 587-6010 FAX (701)587-6013 Series 1. Soil Chara&rization 500 g sample minimum pH, %Mganicmatter,cationexchangecapacity.water hddillg ca& (1Band 15 bat),%sand-siltday,texture, bulk - density,X totalnitrogen,phosphorus, andsdublesans. Series 2 Soil Charadertetion 500 g sampie minimum pH, X organicmatter, c a h exchange capedty,m e r holding - capacity (1Bbar), %sand-sillday, texture, and bulkdensity. Series3.Water Characteritetion 500mi sample minimum pH. W m , magnesium,endim,hardnas,cardudivity. - d i m ebsorptifflmtio, tdaldissolved solids,and Wdty. Series4. Water Characterimton 500 misampleminimum pH, caldum, magnesium,sodium,hardness,d u m absop tion ratio, and conducthrity. SWy Directof$Management Natured Study TeslSNem:SoilI Water .- cirdeC.h.3 RequestedT e s t ( ~ ) I I A c m of this COC will be mailed fo mi when soedmensare receivedbv Lab. I ,,m BACK TO MAIN I USE LOG Gross wt/vol Purpose (enter standard number) Balance I D Initials Date I withdrawal 1954.79 I I after (mass or vol) withdrawal 160.1 g 1894.6 g I~E00-1311SuitableAn Study I1904 IILCG I110/25/2000 II 3M EnvironmentalLaboratory Page 606 of 703 BACK TO MAIN Before 834.69 Amnt. withdrawn (mass or vol) 610.2g Gross Wvol after withdrawal rr4.4g Purpose (enter standard number) E00-1311 Sorption Study Balance ID Initials Date 904 LCG 11/13/2000 3M Environmental Laboratory Page 607 of 703 BACK TO MAIN Test Control and Reference Substance Log 7 or reference # soil name: ILot/batch #: Kittson Co. NA 12/31/2015 00-2407 Inihals: containers IRetain LCG 1L Nalgene dried and sieved 'TCR Substance # T P <<J mb5-017 Lmc >I.;L-~/o( Received from: Agvise Amount received (wt. or Bulk vol): Date: 10/25/2000 Shipper: FedEx MSDS Wn) - aYWN Date of Retain I kocation of svnthesis. fabrication, or derivation records: Std Location/Storage: 1 NA Container stored ambient in TCR-COZ. LCG 12/26/00 L 1 kittson co clay-0-6.pdf 3M Environmental Laboratory Page 608 of 703 BACK TO MAIN L AEoRATO R IEs i i .AGVISE Soil Characterization Report Highway 15 P.0. Box 510 Northwood ND 58267 (701) 587-6010 FAX (701)587M113 ernail: agvise@polarcornmmm Homepage agviselakcom Submitting firm = 3M Protocol or Study No = NA Sample ID. = KITTSON CO CLAY 0-6 Trial ID. = NA Date Received = 10-23-00 Date Reported = 11-02-2000 AGVISE Lab No 00- 2407 Percent Sand 16 Percent Silt 22 Percent Clay 62 USDA Textural Class (hydrometer method) Clay Cation Exchange Capacity (meq/lOO g) 54.5 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen (%) 2.6 4 -5 7.2 0.223 Base Saturation Data Percent opm Calcium Magnesium Sodium Potassium Hydrogen 54.2 34.6 0.9 3.6 6.8 5900 2260 110 771 37 Thesg! tests were cpnpleted in com-pliance of 40 CFR Part 160. //-J Robert Deutsch Date Soil Scientist/Analytical Investigator - 00 Agricultural Testing 3M Environmenita/ Laboratory Page 609 of 703 BACK TO MAIN LAEORATORIIZS Highway 15 P.O. Box 510 Northwood. ND 50267 (700587410 FAX (701)5874l13 emall: agvise@polarcommcom Homepage agviselabscom The following personnel have been duly trained to perform Plant Analysis, Soil and Water Characterizationmethods under40 CFR Part 160 Good LaboratoryPractice Standards. TechnicalSupwrt Staff - Anderson, Linda M. TechnicianIII - Deutsch, Robert L. President Hart,Linda M. - Technician111 - Hime, SherryL. TechnicianI - Johnson,Julie M. Nutrient LaboratoryManager - McNeil, Vigo (Art) TechnicianI Moen, Lucinda S.- TechnicianIII - Pollert, Garis Nutrient LaboratoryAnalyst - Pollock, John TechnicianI - Wall,Mary J. TechnicianII Wyant, Linda L. - TechnicianI - Berg, Eileen A. - SecretaryIII Ducioame, Gail M. - Quality Control Specialist Fuglestad, Teresa S. - Secretary 11 Hagen, ShellyJ. AdministrativeAssistant Oualitv Assurance Thingelstad, Mary L. - QualityAssurance Manager COPY OF ORtGlNAL oratories, Inc. DateA9.U- 05/00 3M EnvironmeniLal Laboratory Agricultural Testing Page 610 of 703 BACK TO MAIN - Bulk Density Disturbedbulk density is determinedby weighing a knownvolume of dried and ground soil (NUT.02.10). Core or non-disturbed bulk density is determined by weighing a known 1 volume of an intact, dried soil core (NUT.02.02). Water `AoldineCaDacitv and Water Relations Moisture % - Determinedby gravimetricloss upon drying (NUT.02.36). Saturated Hvdraulic Conductivitv - Determined by using the constant head method and measuring the rate of flow of water through a saturated soil column (NUT.02.34). - Water InfiltrationRate Determined by using the constanthead methodand measuring the length of time from water applicationto prcduction of a leachatefiom a soil column (NUT.02.35). . ., - Water Holdhe CaDacity Determinedby measuringthe moisture remainingwh& saturated soil is placed under 1/3 or 0.10 bar pressure (NUT.02.08). Water Holdinn Capacity - Determined by measuring the moisture remaining when saturated soil is placed under 15 bar pressure (NUT.02.13). All of the above methods are detailed in the current analytical SOPSused by AGVISE Laboratories' Characterizationtesting laboratory. NUT.05.01. Lone Term Storage of Soil and Water Characterization Soecimens: According to this SOP, soil characterizationsamples will be retained by AGVISE Laboratoriesfor at least two years before disposal and water characterization samples will be retained for a period of 60 days before disposal. ADM.05.01. Archivist Duties and Archivine Procedures: This SOP statesthat copies of soil and water characterizationreports, original COC's and original raw data will be archived withi 60 days.after the signature by the analytical investigator. Hard copies generated by computer will be archivedweekly, and supplemental data will be archived annually. OAU.08.01. Oualitv Assurance Insuectionsof Facilities. Studies. and Processes for GLP Compliance: Method inspections will be performed on a regular basis at AGVISE Laboratories, Inc. Fcir soilcharacterization,two methods will be inspectedper month and one water characterizationinspection willbe conductedper month. An annual facilityauditwill be perfomied by AGVISE Laboratories,Inc. Quality Assurance Unit. All of the above methods are detailed in the current analytical SOP'Sused in AGVISE Laboratories' characterization laboratory. A APPROVED BY ANALYTICAL INVESTIGATOR Robert L. Deutsch, Soil Scientist 3M Environmental Laboratory Page 611 of 703 BACK TO MAIN Colllection Information : ? I a c k Site Ideacation Uah - S q l e I D A G V l S F L he dfio 2404 . GeographicalReferencelati&& J 4 7 ' p / ' Lona&,-'? . 7'1/8' I Date of use att Sampling l D - 1 9 - 0 0 tern (e.g. agricuItural, forest, etc.) Nn;twc PA-. . . Depth of sampling 0- 0 " COUelCtedby &A& PdQOAk ........................................................ SiteIdentifimtion K. R A W SampleID A ~ V I S E Loh Jt &. Loa-,, 0fiLlaq05 - GeographicalReferenceJ&&L& y7'qa' Date QfSampbg 10- 19 - 60 use Pattern (e.g. agricdturaI, forest, etc.) &&I, Depth of sampling 0 (b II Lorla;&&,- Collectedby .&AiA P O W "d 97 "40' JAI site Icientiiication -An- R/MJ PA SampleID O O - a u o b A ~ Y EK Lub* GeographicalRefaenceLn;t;;tudr.:4 7 '4 5' Lona&&. z - Date of Sampling 10 - 19 - 00 0 use Pattern (e.g. agricultural,forest, etc.) .MA I RiLuG &&ow3 Depth of sampling 0- 6 I' Collectedby A r t M c I\JJJ. 97" 37' ........................................................... site bientification K[ f t i j b - . t o . PJL - Sample ID A b V i 5 F L h 600 2407 GeographicalRekence L U :4g' 6 9 ' Lor\&.. - 9 b = VI' Date ofSampling I O -2/- 00 Use Pattern (e.g. agricuIturaI,forest, etc.) - Depth of Sampling O 6" u Collectedby Il-1, * . 3M Environmental Laboratory Page 612 of 703 BACK TO MAIN r$ GLP c3 Non-GLP Characterization Chain of Custody SEND RESULTS TO: 3/r BILL T O Phone: AGVISE Use Only Date received 2 0 'ad U Comments Purchase Order # Protocd/ Study # Test Substance Study Director Sponsor initiation Date AGWSE Lab # _ _ _ _ _ _ _ ~ _~_____ Specimen I.D. Laboratories, Inc. P.O. BoxSlWighway15 Northwood,ND5826?' - Telephone(701) 567-6010 FAX (701) 5876013 Series 1. Sail Charactaimtion 500 g sample minimum W, X Mganic maner,cationsxchangecapady, water noiciing capacily (lnand 15 bar), 56 Mnd-siltclay. texture. bulk densw, %total nibogen. phosphorus, and solublesalts. . - serles2Soilcharactwrzatr'on 500 g sampleminimum pH,96 o m matter, cation exchange capadty.water hdd4t-g Capacity(Inbar), X sand-siltclayt,exture, and bulkdensity. - Series3.Water Characterization 500 misample minimum pH. caldum. magnesium. sodium. hardness,conduclivity, - sodium absorption ratio, totaldissolved sdi, and lufbidw. Series 4. Water Charecterlzation 500 ml sampk minimum PH.cakjum, maqnesium, sodium,hardness,d u m & s o p tion ratio, and conductivity. Study Dirstoi's Management Natureof Sudy TestSysfemSolIsdllWater ci&lCkw, RequestedT M s ) I I METHOD OF SHIPMENT Shipment I.D. #(s) Fed Express I I A corw ofthisCOC will be maledto VOLI when soecimensare receivedbv Lab. Wrdn BACK TO MAIN I USE LOG Before 1243.7 g Amnt. withdrawn (mass or vol) 160.1 g Gross Wvol after withdrawal 1183.6 g Purpose (enter standard number) E00-1311 Sorption BalanceI D Initials Date 904 LCG 11/13/2000 Page 614 of 703 BACK TO MAIN I--- t USE LOG Before 696.0 g Amnt. withdrawn (mass or vol) 255.769 Gross wt/vol after withdrawal 440.24g Purpose (enter standard number) E00-1311 Sorption Study Balance I D Initials Date 904/916 LCG 11/28/2000 3M Envimnmental Laboratory Page 615 of 703 BACK TO MAIN Before 390.82 g withdrawn 122.44 g after 368.38 g Purpose (enter standard number) Balance ID Initials Date E00-1311PFOS AdsorbIDesorb 9041916 CMC 01/22/2001 3M Environmental Laboratory Page 616 of 703 BACK TO MAIN I USE LOG I withdrawal 1368.37 g Gross wt/vol 1 1 after (mass or vol) withdrawal 175.27 g 1293.1 g Purpose (enter standard number) 1IE00-1311PFOS AdslDes Balance ID I1904/914 Initials IICMC Date I~01/25/2001 1I 3M Environment,alLaboratory Page 617 of 703 BACK TO MAIN 7 USE LOG t CR-00065-077 Before 293.01 g Amnt. withdrawn (mass or vol) 197.54 g Gross wt/vol aRer withdrawal 195.47 g Purpose (enter standard number) E00-1311 PFOS Ads/Des ~~~ Balance I D Initials Date 9041916 CMC 01/29/2001 3M Environmental Laboratory Page 618 of 703 BACK TO MAIN I------ USE LOG Before 1363.9 g withdrawn after 16Q.2 g 1303.7 g Purpose (enter standard number) Balance ID Initials Date E00-1311 Suitable Analytical 904 LCG 10/25/2000 3M Environmental Laboratory Page 619 of 703 BACK TO MAIN Test Control and Reference Substance Log ILot/batch #: K. Broeren 00-2405 'F (Initials: NA 12/31/2015 LCG [Retain Dried and Sieved "TR Substance # T C P % l&-J C.C,C?I. 5 -,>("c\ cvqc Sl-lC\ I o\ 1 I Received from: Agvise Amount received(wt. or Bulk vol): Date: Shipper: MSDS Wn) 10/23/2000 Fed Ex - dY@N Date of Retain Ipunty: IRecords received: fabricabon, or derivabon records: Std Locahon/Stor<ige: Molecular Formula: Comments NA Agvise Soil Characterization Report 00-2405 NA Container stored ambient in TCR-COZ. LCG 12/26/00 TCR sticker added after original weight taken. LCG 10/25/00 K Broeren clay loam-0-6.pdf 3M Environmental Laboratory Page 620 of 703 BACK TO MAIN L A B o R A T O-R I E s 1. Highway 15 P.O.Box 510 Northwood ND a 6 7 (701) 587-6010 FAX (701) 587-6013 email: agvse@pIarcomm.com Homepage: agviselabs.com AGVISE Soil Characterization Report Submi.tting firm = 3M Protocol or Study No = NA Sample ID. = K BROEREN-CLAY LOAM 0-6 Trial. ID. = NA Date Received E 10-23-00 Date Reported = 10-31-2000 AGVIGE L a b NO 00- 2405 Percent Sand 21 Percent: Silt 46 Percent Clay 33 USDA Textural Class (hydrometer method) Clay Loam Cation Exchange Capacity (meq/lOO g) 24.7 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen ( % I 2.6 4.4 6.0 0.216 Base Saturation Data Cation Calcium Magnesium Sodium Potassium Hydrogen Percent 52.7 24.3 0.7 5.8 16.5 =. 2600 720 39 557 41 These tests were completed in compliance of 40 CFR Part 160. A a lytical Givestigator - / D 3/-00 Date 3M Environmental Laboratory Agricultural Testing Page 621 of 703 BACK TO MAIN Highway 15 P.O. Box 510 Northwood, ND 58267 (701) 587-6010 FAX (701)587-6013 t email: agvise@plarcommcom Homepage agviselabscom The following personnel have been duiy trained to perform Plant Analysis, Soil and Water Characterizationmethodsunder 40 CFRPart 160 GoodLaboratoryPractice Standards. Technical Support StafF Anderson, Linda M. - TechnicianIII - Deutsch, Robert L. President Hart,Linda M.- Techni~ian111 - Hime, SherryL. TechuicianI - Johnson, Julie M. Nutrient LaboratoryManager McNeil, Vigo (Art) - TechnicianI - Moen, Lucinda S. TechnicianIII Pollert, Garis - Nutrient LaboratoryAnalyst - Pollock, John Te~hnicianI Wall,Mary J. - Technician11 - Wyant, Lmda L. TechnicianI office suuuort Staff Berg, Eileen A. - SecretaryIII Ducioame, Gail M. - Quality Control Specialist - Fuglestad, Teresa S. SecretaryI1 - Hagen, Shelly J. AdministrativeAssistant OUalitvAssurance Thingelstad, Mary L. - Quality Assurance Manager COPY OF ORGINAL oratories, Inc. lniti DateA942'y~ 05/00 3M Environmental Laboratory Agricultural Testing Page 622 of 703 BACK TO MAIN Bulk De& - Disturbed bulk dens-ityis determined by weighing a known volume of dried and ground soil (NUT.02.10). Core or non-disturbed bulk density is determined by weighing a known i volume of an intact,dried soil core (NW.02.02). Water Holdinv CaDacitv and Water Relations - Moisture % Determined by gravimetric loss upon dryins (NUT.02.36). Saturated Hvdraulic Conductivity - Determined by usmg the constant head method and measuring the rate of flow ofwater through a saturated soil colunm ("T.02.34). Water Infiltration Rate - Determined by using the constant head method and measuring the la& of time h m water application to production of a leachate from a soil column (NUT.02.35). - ,. .; Water Holdinp CaDacity- Determined by measuringthe moisture remaining when saturated soil is placed under 1/3 or 0.10bar pressure (NUT.02.08). Water Holdinn Caoacity- Determined by measuringthe moisture remainingwhen saturated soil is placed under 15 bar pressure (NUT.02.13). i All of the above methods are detailed inthe current analytical SOPSused by AGVISE Laboratories' Characterization testing laboratory. NUT.05.01. Long Term Storage of Soil and Water Characterization Snecimens: A c c o r k g to this SOP, soil characterization samples willbe retained by AGVISE Laboratories for at least two years before disposal and water characterization samples will be retained for a period of 60 days before disposal. ADM.05.01. Archivist Duties and Archivine Procedures: This SOP states that copies of soil and water characterkition reports, original COC's and original raw data will be archived within 60 days after the signature by the analytical investigator. Hard copies generated by computer will be archived weekly, and supplemental data will be archived annually. OAU.08.01. Oualitv Assurance Insoeetions of Facilities. Studies. and Processes for GLP Cornuli- Method inspectionswill be performed on a regular basis at AGVISE Laboratories, Inc. For soil characterization, twomethodswill be inspected per month and one water charactcxization inspectionwill be conductedper month. An annual facility audit will be perfonnied by AGVISE Laboratories, hc. Quality Assurance unit. All of the above methods are detailed in the current analytical SOP'S used in AGVISE Laboratories' characterization laboratory. /I APPROVED BY ANAL'YTICAL INVESTIGATOR: Robert L. Deutsch, Soil Scientist ate 3M Environmental Laboratory Page 623 of 703 BACK TO MAIN Collection Information - 1 Site[dentitication UR& La/rvL Sample ID A 6 V l S Lab# dno a404 GeographicalReference L&J.. J q7 e , Lon a (f-8 . . . Date of Sampling l o -1 9 -00 Use Pattern (e.g. agricultural, forest, etc.) No;tluc, P u - Depth of Sampling 0 b I' c0llt:ctedby A& PdAAk ........................................................ K. Siteldentification fin-. & Loam,, Sample ID A b V I S F L a b 9 ooy aq05 . GeographicalReference -L.&hbk 4 7 ' q a ' Lona&&, ' Date of Sampling 10-14 - 00 <'97'(/()' - usePattern(e.g. agricultural forest, etc.) &&c&J!u Depth of Sampling O 6 " Collectedby ~dQk AA, ........................................................ - *- Site ldentiiication d o - RUNAJ h h w ,PA, SampleID 00- a4o b cI6Y1sE Lab* GeographicalReference Ln;t;;tudc~ :4 7 ' 4 5 ' L O t W ,z- 9737' Date of Sampling 10 I 9 - 00 use ]'attern (e.g. agricultural,forest, etc.) ,MA I b ! i i ~ U ~ Depth of Sampling 0- ,& " Collectedby A r t . Mc A/Jl#. ......................................................... K Site Jdentification t k b n - . to. f &M - u Sample ID A 6 V l s E @ 600 a407 GeographicalReference L d h d t a :$8' b 9 ' Date of Sampling m a l - oo LDr\ak&&~ -9 b * 89' Use Pattern (e.g. agricultural, forest, etc.) Depthof Sampling O-Gn 3 IJ-a-00 3M Environmental Laboratory Page 624 of 703 BACK TO MAIN 76 GLP I3 Non-GLP Characterization Chain of Custody SEND RESULTSTO: BILL TO: Phone: AGVISE Use Only Date received /&2 0 * od " ' Comments Purchase Order # Protocollstudy # Test Substance Study Director Sponsor initiation Date ~GVISE Laboratories; Inc. - ' P.O.BoxSl(YHighway15 Northwood,ND58267 Telephone (701)5874010 FAX pol)587-6013 Series1. SoilCharacterization 500 gsample minimum pH, %organicmatter,cationexchange capacity,water holding Capacity (Inand 15 bar),%sand-siltday,texture, bulk - den*ty, %tdal nitrogen,phosphorus,andsolublesalts. Series 2 Soil Characterization 500 g sample minimum PH.% ~ganicmatler, cationexchangecapadty, waterholding - capadty(1Bbar).%sand-sillcby, texhrre,andbulkdenslty. series 3. Water Chaacteriratlon 5M)mlsample minlmum pH, caldum, magnesium. sodium, hardness,mdudiviiy, - sodiumSbSorptiMl ratio, totaldissdved solids. and IUhidily. S e t i e s 4 . W a t e' r io~n 500 ml sample minimum pH. calcium, magnesium, sodium. hardness, sodium absolp tion ratio, and mnductlvity. Sludy Diredds Management Natured Study Test System: SoilI Water Wohe I I I I BACK TO MAIN Before withdrawn after 1188.0 g 17!3.2 g 1108.8 g Purpose (enter standard number or reason for removal) 00-1311 PFOS AdsorblDesorb Balance Balance ID ID 1 2 Initials Date 9041914 CMC 01/20/2001 3M Environmental Laboratory Page 626 of 703 BACK TO MAIN I------ USE LOG I Before 1055.79 Amnt. withdrawn (mass or vol) Balance ID 2 16t0.2~ Gross W v o l after withdrawal Balance ID 1 995.59 Purpose (enter standard number or reason for removal) E00-1311 Sorption Balance Balance ID ID 1 2 Initials Date 904 LCG 1I/I3/2000 3M Environmental Laboratory Page 627 of 703 BACK TO MAIN lay Loam USE LOG Before 1108.8 g Arnnt. withdrawn (mass or vol) Balance ID 2 1917.3 g Gross Wvvol after withdrawal Balance ID 1 1011.5 g Purpose (enter standard number or reason for removal) E001311 PFOS AdslDesorb Balance Balance ID ID 1 2 Initials Date 904/916 CMC 01/30/2001 3M Environmental Laboratory Page 628 of 703 BACK TO MAIN 1175.7g Amnt. withdrawn (mass or vol) 60.0 g Gross wt/vOl after withdrawal 1715.7 g Purpose (enter standard number) E~~~~iy Balance ID Initials - 904S t ~ LCG Date 10/25/2000 3M Environmental Laboratory Page 629 of 703 BACK TO MAIN I USE LOG CR-00065-064 Before 1055.7g withdrawn after 995.59 Purpose (enter standard number) Balance I D Initials Date E00-1311 Sorption 904 LCG 11/13/2000 3M EnvironmentiJ Laboratory Page 630 of 703 BACK TO MAIN or reference # r a ILot/batch #: t "K. Broeren" `k IInibals: NA 12/3112015 LCG 00-2405 containers: ICondlhon:. IRetain Dried and Sieved TCR Substance # Received from: Amount received (wt. vol): Date: Shipper: MSDS Wn) Date of Retain . -RCT r i7A o \- c h ( o C - elmC s/+1 0\ Agvise or bulk 10/23/2000 FedEx - c ) Y - N IRecords received: Agvise Soil Characterization Report 00-2405 NA I I fabrication, or derjvation Irecords: Std Locabon/Storage: Container stored ambient in TCR-COZ. LCG 12/26/00 Molecular Formula: Comments I K Broeren clay loam-0-6.pdf 3M Environmental Laboratory Page 631 of 703 BACK TO MAIN lay Loam USE LOG Before 1188.0 g Amnt. withdrawn mass or vol) 17!).2 g Gross Wvol afer withdrawal 1108.8 g Purpose (enter standard number) E00-1311PFOS Adsorb/Desorb Balance ID Initials Date 9041914 CMC 0112012001 3M Environmental Laboratory Page 632 of 703 BACK TO MAIN 7 USE LOG Before 1108.8 g withdrawn after 197.3 g 1011.5 g Purpose (enter standard number) Balance ID Inibals Date 00-1311 PFOS AdslDesorb 9041916 CMC 01/30/2001 3M Environmental Laboratory Page 633 of 703 BACK TO MAIN Test Control and Reference Substance Log ILoVbatch #: IInibals: containers (Condltlon: IRetain 12/31/2015 LCG Dried and Sieved Received from: Agvise Amount received (wt. or Bulk vol): Date: 10123/2000 Shipper: FedEx MSDS Wn) -- c)Y-N Date of Retain 1Purit-y: Records received: fabrication, or derivation Std Location/Storage: Molecular Formulii: Comments Attachment(s) NA Agvise Soil Characterization Report 00-2406 NA Container stored ambient in TCR-CO2. LCG 12/26/00 TCR sticker added after original weight was taken. LCG 10/25/00 3M Environmental Laboratory Page 634 of 703 BACK TO MAIN LABORATORIES Highway 15 P.O.Box 510 Northwood, ND 58267 (701) 587-6010 FAX (701)587-6013 email: agvise@polarcommcom Homepage agviseIabs.com AGVISE Soil Characterization Report Submitting firm = 3M Protocol or Study No = NA Samp1,eID. = GOOSE RIVER-SEDIMENT 0-6 Trial ID. = NA Date Received = 10-23-00 Date Reported = 10-31-2000 AGVISE Lab No. 00- 2406 Percent Sand 39 Percent Silt 42 Percent Clay 19 USDA Textural Class (hydrometer method) Loam Cation Exchange Capacity (meq/lOO g) 17.5 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen ( % ) 1.3 2.3 7.7 0.101 Base Saturation Data Cation Calcium Magnesium Sodium Potassium Hydrogen Percent 57.2 28.6 4.8 3.4 6 .O u2In 2000 600 193 232 10 These! tests were completed in compliance of 40 CFR Part 160. Analytical Investigator / o -J/-OO Date 3M Environmental Laboratory Agricultural Testing Page 635 of 703 BACK TO MAIN L A B 0 R A T 0 R IE S r: t Highway 15 P.O. Box 510 Northwood NU 58267 (701)587-6010 FAX (701)587-6013 email: agvise@polarcommcom Homepage agviselabscom The following personnel have been duly trained to perform Plant Analysis, Soil and Water Characte*ation methods under 40 CFR Part 160Good LaboratoryPractice Staudards. Technical SuDDort StafF - Anderson, Linda M. - Technician111 Deutsch, Robert L. President Hart,Linda M. - Technician111 Hime, SherryL. - TechnicianI Johnson, Julie M. - Nutrient Laboratory Manager McNeil, Vigo (Art) - TechnicianI Moen, Lucinda S.- TechnicianIII - Pollert, Garis Nutrient LaboratoryAnalyst - Technician1 - i Pollock, John Wall, Mary J. Technician 11 Wyant, Linda L. - TechnicianI Office Support Staff - Berg, Eileen A. SecretaryIII - Ducioame, Gail M. Quality ControlSpecialist - Fuglestad, Teresa S. Secretary11 , - Hagen, Shelly J. AdministrativeAssistant Ouality Assurance Thingelstad, Mary L. - Quality Assurance Manager COPY OF ORGINAL oratories, Inc. Date/02Yye 05/00 3M Environmental Laboratory Agriculturfll Testing Page 636 of 703 BACK TO MAIN Bulk Den:& - Disturbed bulk densityis determined by weighing a known volume of dried and ground soil (NUT.02.10). Core or non-disturbedbulk density is determined by weighing a known volume ofan intact, dried soil core (NUT.02.02). i1.. Water Holding Caoacitv and Water Relations Moisture `g- Determinedby gravimetricloss upon drying (NUT.02.36). Saturated Hvdraulic Conduaivi& - Determined by using the constant head method and measuring the rate offlow ofwater through a saturated soil column ("'-02.34). Water Infiltration Rate - Determined by using the constant head method and measuring the length of time from water application to production of a leachatefrom a soil column (NUT.02.35). ... .:, Water H ~ ~ l dCi anD~acity - Determined by measuringthe moisture remaining when saturated soil is placed under 1/3 or 0.10 bar pressure (NUT.02.08). . Water Hclldine CaDacity - Determined by measuringthe moisture remaining when saturatedsoil is placed under 15 bar pressure (NUT.02.13). All of the above methods are detailedin the current analyticalSOPSused by AGVISE Laboratories' Characterizationtesting laboratory. NUT.05.01. Lone Term Storage of Soil and Water Characterization Soecimens: According to this SOP, soil characterizationsampleswill be retained by AGVISE Laboratoriesfor at least two years before disposal and water characterizationsamples will be retainedfor a period of 60 days before disposal. ADM.05.01. Archivist Duties and ArchivinPProcedures: This SOP states that copies of soil and water characterizationreports, original COC's and original raw data will be archived within 60 days after the signatureby the analyticalinvestigator. Hard copiesgenerated by computerwill be archived weekly, and supplementaldata willbe archived annually. OAU.OS.01. Ouality Assurance InsDections of Facilities. Studies, and Processes for GLP C o m o l i m s Method inspectionswill be performed on a regularbasis at AGVISE Laboratories, Inc. For soil characterization, two methodswill be inspectedper month and one water characterizationinspection willbe conducted per month. An annual ficility audit will be performed by AGVISE Laboratories,hc. Qualay Assurance Unit. All of the above methods are detailed in the current analytical SOP'Sused in AGVISE Laboratories' characterization laboratory. APPROVED BY ANALYTICAL INVESTIGATOR: Robert L.Deutsch, SoilScientist COPY QF QRtilGINAL 3M Environrnent(a1Laboratory Page 637 of 703 BACK TO MAIN Collection Information Site Identification Drn F SampleID AbVlSF L b i . GeographicalReference Ldt&,L, J q7 L a n a b . . -.q 7' 48' Date of Sampling / o - r s -00 .. Use Pattern (e.g. a g r i c m forest, etc.) N w . P?h- Depth of Sampling 0- L I' CoUectedby ~% Po&& ,-,,l, ........................................................ c4au Site Identification K. R n tvuu- Loa, 1 ofiu SampleID A A V I S E L~a#h a405 .- GeographicalReference LQ?&.&~. q 7 . w LonL l U , ' . 9 7 "40' Date of Sampling 10- 14 - 00 use Pattern (e.g. agricdtud, forest, etc.) Depth of Sampling 0 - L 'I Collectedby A& PohLd &&d#.wiJ, ........................................................ SiteIdentscation doSam, LJ ~ d c / m a ~ Sample ID 00- 2404 A 6 Y / s Lab* Geographical Refaence L - : r17 '45' :-97"37' - . Date of Sampling 10 1 9-00 Use Pattern (e.g. agricdtura~,forest, etc.) ,MR - Depth of Sampling 6 II % Betta3, CoUectedby A r t M c M R J . ........................................................ r SiteIldentification K &'b,0-. .thu- SampleID A 6 V i s F L b boQa(/o7 GeographicalReference L&&u!L :48 ' b 2 ' Isn&:-9b 'S'I' Date of Sampling m-ai- 00 Use F'attern (e.g. agricultural, forest, etc.) a .e. J , Depth of Sampling 0-6 " CoUected by J .OI- 3M EnvironmentalLaboratory Page 638 of 703 % GLP 0 Non-GLP 2 m CharacterizationChain of Custody 55 . SEND RESULTS TO: BILL TO: 3 2 2 2 Ime 0 3 $ 'hone: Purchase Order # AGVISE Use Only I Protocol/ Study # BACK TO MAIN Laboratories, Inc. P.O. Box 51O/Highway15 Northwood,ND 58267 - Telephone(701) 587-6010 FAX (701) 5876013 Series 1. Soil Characterization 500 g sample minimum pH. %organic malter.cation exchange capacity,water W i n g capacity (Inand15 bar), %sand-siltday.texture,bulk density, %total nilrogen,phosphorus. andsolublesalts. - Series2. SoilCharacterization 500g sampleminimum pH, %organic matter. cationexchangecapacity.Water holding capacity(Inbar), %sand-siltday, texture, and bulk density. - Series3. Water Characterization 500mi sampleminimum pH, calcium. magnesium, sodium, hardness, conductivity. sodiumabsorptron tab,totaldissolved solids. and turn. - Series 4. Water Characterization 500ml sample minimum pH. calcium. magnesium, sodium. hardness, sodium absorp- I tion m k , andconductivity. Study Directoh Management 'I I SMpEinTmHaOntDIOF &SIHCI\PMENT: FedExpress 0 I I * &$/ohter / instructions: COPY OF ORIGINAL BACK TO MAIN 7 iver Sediment USE LOG Gross wt/vol after Purpose (enter standard number) Balance I D Initials Date i 3M Environmental Laboratory Page 640 of 703 BACK TO MAIN ' bCR-00065-070 I withdrawal 11 131.39 Gross wt/vol I (mass or vol) I after withdrawal 160.0 g 11071.3 g Purpose (enter standard number) IIE00-1311Sorption Balance I D I1904 Initials IILCG Date I~11/13/2000 II 3M Environmental Laboratory Page 641 of 703 BACK TO MAIN Before 1592.99 withdrawn after 1256.169 1336.749 Purpose (enter standard number) IE00-1311Sorption Studies Balance ID Initials Date I , I I 1904 ILCG ~11/28/2000 3M Environmental Laboratory Page 642 of 703 BACK TO MAIN '' I--River Sediment (TCR-00065-070 USE LOG Gross wtjvol Purpose (enter standard number) Balance I D Initials Date after 3M Environmenlal Laboratory Page 643 of 703 BACK TO MAIN I iver Sediment USE LOG Before 263.23 g withdrawn after (75.54 g 187.69 g Purpose (enter standard number) Balance ID Initials Date E00-1311 PFOS AdsorblDesorb 904191 4 CMC 0112412001 3M Environmental Laboratory Page 644 of 703 BACK TO MAIN Test Control and Reference Substance Log < ISubstance trade name /DomesticSludge ITCR Substance # ITCR-00065-025 Domestic Sludge name: ILoVbatch #: 2781 Received from: NlST )3M # IExDiration date: INA 110/31/2005 I I I IAmount received (wt. or 140 g (per vendor) (Inihals: LCG Iof 15 7 containers freeze- dried /Retain Date: Shipper: MSDS ( Y h ) Date of Retain 1010312000 UPS - 9Y-N Ipurity: r- \Recordsrecenred: Locabon of synthesis, fabncation, or derivabon records: Std Location/Storage: Molecular Formulii: Comments NA certificateof analysis SRM 2781 NA Container stored ambient (IO-30C)in TCR-CO2. LCG 12/26/00 3M Environmental Laboratory Page 645 of 703 BACK TO MAIN ' eomestic Sludge! ,: omestic Sludge! CR-00065425 Before withdrawn after 423.66 g USE LOG Purpose (enter standard number) Balance ID Initials Date E00-1311 Suitable Analytical 904 LCG 10/25/2000 3M Environmental Laboratory Page 646 of 703 BACK TO MAIN TCR Substance # TCR-00065-026 15ubstance/chemlcal name: ILoVbatch #: Expirabon date: Domestic Sludge 2781 NA 10/31/2005 IInihals: LCG 2 Of 35 7freeze-dried IRetain Received from: NET Amount received (wt. or 40 g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (vln) - SYWN Date of Retain \Punty: IRecords received: fabncation, or deirlvabon records: SM Locabon/Storage: Molecular Formula: Comments NA Certificate of Analysis SRM 2781 NA Container stored ambient (IO-30C) in TCRG02. LCG 12/26/00 domestic sludge.pdf 3M Environmental Laboratory Page 647 of 703 BACK TO MAIN USE LOG Gross wt/vol Purpose (enter standard number) Balance I D Initials Date I I I I I after withdrawal (massorvol) withdrawal 1164.61 g 119.12 g 1145.49 g IE00-1311 gSuitable Analytical 1904 IILCG I110/25/2000 II 3M Environmental Laborafory Page 648 of 703 BACK TO MAIN Test Control and ReferenceSubstance Log Domestic Sludge 15ubstance/chemil:al Domestic sludge name: ILotjbatch #: 2781 NA 1013112005 `p IcConotainnedrs:ition: LCG 30f15 freeze-dried IRetain TCR Substance # TCR-00065-027 Received from: NlST Amount received(wt. or 40 g (per vendor) vol): Date: I010312000 Shipper: UPS MSDS (Vn) - L)YmN Date of Retain [Records received fabrication, or deiwation records: Std Locabon/Storage: Molecular Formula: Comments certificateof analysis SRM 2781 NA containerwas stored ambient. LCG 12/26/00 domestlc sludge.pdf 3M Environmental Laboratory Page 649 of 703 BACK TO MAIN USE LOG omestic sludge Before 125.389 withdrawn after 3.509 121.88g Purpose (enter standard number) Balance ID Initials Date Sorption E00-1311 904 LCG 11/13/2000 3M Environmental Laboratory Page 650 of 703 BACK TO MAIN -"or reference# Substance/chemical ILot/batch #: Initials: -NI - 1containers: [Retain Test Control and Reference Substance Log Domestic Sludge Domestic Sludge 2781 NA 10/31/2005 LCG 4 Of 15 freezedried TCR Substance # TCR-00065-028 Received from: NlST Amount received (wt. or 40 g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS Wn) Date of Retain 2YmN Ipurity: riecords received fabrication, or derivation records: IMolecular Formu1,s: NA Certificateof analysis SRM 2781 NA Container was stored ambient. LCG 12/26/00 I domestic sludge.pdf 1 3M Environmental Laboratory Page 651 of 703 BACK TO MAIN I omestic Sludge I withdrawal 1164.749 I (massor vol) 141.569 Gross wt/vol I atler withdrawal 1123.189 Purpose (enter standard number) I IE00-1311 Sorption Study Balance I D Initials Date I1904 IILCG I~11/13/2000 1I 3M Environmental Laboratory Page 652 of 703 BACK TO MAIN Domestic Sludge 1n5aumbset: ance/chemsal lLot/batch #: Domestic Sludge 2781 NA 1013112005 IInittals: 7 containers: 7 IRetain LCG 50f15 freeze-dried TCR Substance # TCR-00065-029 Received from: NlST Amount received (wt. or 40 g(per vendor) vol): Date: Shipper: MSDS (Y/n) 10/03/2000 UPS -dYmN Date of Retain IPunty: IRecords received: fabricahon, or derivahon records: Std Locahon/Storage: Molecular Formula: Comments NA Certificateof analysisSRM 2781 NA Container stored ambient (10-3OC) in TCR-C02. LCG 12/26/00 domestic sludge.pdf 3M Environmental Laboratory Page 653 of 703 BACK TO MAIN omestic Sludge! I withdrawal 1162.699 Gross wt/vol I after 1~:rnassorvol) withdrawal 115.389 1147.319 Purpose (enter standard number) I IE00-1311Sorption Study Balance ID I1904 Initials IILCG Date I~11/13/2000 II 3M Environmental Laboratory Page 654 of 703 BACK TO MAIN USE LOG I Before 147.06 g withdrawn afier 125.06 g 122.00 g Purpose (enter standard number) Balance ID Initials Date E001311 Sorption Study 904 CMC 01/24/2001 3M Environmental Laboratory Page 655 of 703 BACK TO MAIN or reference # name: ILoVbatch #: 1 3 #~ IInitials: INumber/sizeof Test Control and Reference Substance Log Domestic Sludge TCR Substance # TCR-00065-030 2781 NA LCG 6 of 15 Received from: vol): Date: Shipper: NlST 10103/2000 UPS Iknty: [Records received fabncatron, or deiivabon records: Std Location/Stor,sge: Molecular Formul,i: Comments NA certificateof analysisSRM 2781 NA Container stored ambient (10-3OC) in TCR-COZ. LCG 12/26/00 domestic sludge.pdf 3M Environmental Laboratory Page 656 of 703 BACK TO MAIN USE LOG Before withdrawn aRer 123.400 g Purpose (enter standard number) Balance I D Initials Date 00-1311 AdsrblDesorb 914 CMC 01/24/2001 3M Environmental Laboratory Page 657 of 703 BACK TO MAIN Test Control and Reference Substance Log ;3 ISubstance trade iiame IDomestic Sludge ITCR Substance # ITCR-00065-031 I Lot/batch #: 3M # Expiration date: I IInitials: INumber/size of 2781 NA 10/31/2005 I ILCG 17 of 15 Received from: NET I I Amount received (wt. or 40g (per vendor) Ivol): IDate: 110/03/2000 IShiDDer: IUPS I IPunty: IRecords received fabncation, or denvation records: Std Locabon/Storsge: Molecular Formula: Comments NA Certificateof analysis SRM 2718 NA Container stored ambient (IO-3OC) in TCR-COZ. LCG 12/26/00 I I domestic sludge.pdf 3M Environment(a1Laboratory Page 658 of 703 BACK TO MAIN omestic Sludge USE LOG I I1 Gross Wt./Vol. Amnt. I I Before withdrawal I withdrawn (massorvol) 1163.78 g 17.82 g I Gross wt/vol I I after withdrawal 1155.96 g II Purpose (enter standard number) I - IE00-1311 PFOS AdsorblDisorb II Balance I D I 1914 II~ Initials IICMC II -D-a_te- I101/24/2001 3M Environmental Laboratory Page 659 of 703 BACK TO MAIN ....... Standard Reference Material" 2781 Domestic Sludge This Standard Reference Material (SRM) is intended primarily for use in the evaluation of methods used for the analysis of sludges and other materials Of a S h i h matrix. S R M 2781 is a dried and pulverized domestic sludge. A unit of S R M 2781 consists of 40g of the dried material. Certified V ~ U C ST:he certified values for 10elementsare listed in Table 1 two or more analytical methods. are based on concordant results from Analytical mediods used for the characterizationof this SRM are given in Table 3. All values are reported as mass fractions [I], c o a dry mass basis and are based on measurements using a sample mass of at least 100 mg. Noncertified Values: Noncertified values for eleven additional elements are listed in Table 2 and were derived . from a combmition of results from NIST and collaborating laboratories. These results may have sources of bias yet to be inves1:igated and do not meet NIST criteria for certification. . Expiration of CertWcation: This certification is valid for five years from &e date of shipment from NIST. However, the certificationwill be nullified if the S R M is contambtedof modifmi. Should any of the values change before the expirationof the certification. putchasers will be notifiedby NET. Return of the attached registration card will facilitate nlotification. . Stability: This material is considered to be stab!e: .however. its stabdity ha9 not been rigorously assessed. NIST will conrinuously monitor this material and rrponbuy substantive changes in certification to the purchaser. - Use: A minimum sample mass of 100 mg (dry mass see Instructions for Drying) should be used and sample preparation procedures should be designed to effect completedissolution for analytical determinationsto be related IO the certified values provided. .. f: Instructionsfor Drying: When nonvolatile elements an to be determined. samplesshould be vacuum dried at r&m temperature for 24 h or oven dried for 2 h at 110 "C. Volatile elements(e.g.. arsenic. mernuy. and selenium) should be determined on samples as received; separate samples should be dried according to these htrUCtiOIE to obtain a .. correction factor for moisture. Moisture corrections;LIC then made to measurement values before comparing them to the certified values. [Note thatthe mass loss ondryingat the time of cenificationwas found to be in the range of 4.7 % to 6.6 46 when using the recommended drying procedures.] Statisticalconsultation was provided by L.M.Gill of the MST Statistical Engineering Division. The overall direction and coordinationof the analyses were under the chairmanship of J.D.Fassett of the NIST Analytical Chemistry Division. The technical and supportaspects involved in the original preparation. certification, and issuance of this SRM were coordinated through the Standard Reference Materials Program by J.S. Kane. Revision of this certificate was coordinated thrixqh the Standard Reference Materials Program by B.S. MacDonald. Gaithersburg. h4D 20899 Certificate Issue Date: October 25, 1996 (Revisionof certificatedated 6-22-95 to include addendum) Thomas E. Gills, Chief Standard Reference Materials Program Page 1 of 4 3M Environmentisl Laboratory Page 660 of 703 BACK TO MAIN Source and Preparation of MatertPI: The U.S.Geological Survey (USGS). under contract to NIST, obtained .C partially dehydrated sewage cake material from the Metropolitan Dmver Sewage Disposal District No. I . The material (approximately 182 kg) was placed inplastic-lincddnrmsud transponcd to the USGS facilitiesin Lakewood. 8 Co for processing. It was dried at ambient tempcraw in a forced air chamber, ground to p w a 74 m. (200 mesh) sieve, blended for 24 h to assun homogeneity of the pulverized material after which test samples were taken from the blmkr for p r c l h h y homogeneity analyses. The matcnal was then radiation sterilired. The sterilized material i W ~ sShipped in bulk 10 NIST,where the material was bottled in40 g units after reblending for 4 h. Analysis: The homogeneity was assessed at USGS on 10 replicate samples of bulk material for over 40 elements using x-ray fluorescence (XRF) andlor inductively coupled plasma atomic emission spectrometry (ICP-AES). -m Homogeneity was funber asusedduring certifmtion analysis; at sample s S S Of 100 mg or greater. No sample-to- sample variations in excess of those expected from the analytical measurements were detected. Certified Values and UanrtnlntK* I.: "he certified values ye the mcivtsof the results from two or more indepmdcnt analytical methods as described by Schiller and Ebcrhardt [21. The unccnainty is based on a 95 X contidence interval for the uue valw, and includes an allowance for differraces bet~mthe merhodo wed [3]. Table 1. Certifd Mass Frac.tions Element Mass Fraction (in mgflrg) Element Mass Fraction (in %) Arsenic Cadmium Copper Lead Mercury Molybdenum Nickel Selenium Zinc 7.82 12.78 627.4 202.1 3.64 46.7 80.2 16.0 1273 f 0.28 f 0.72 f 13.5 f 6.5 f 0.25 f 3.2 f 2.3 f 1.6 f 53 Nitrogen 4.78 f 0.11 Noncertifled Values and Uncertainties: The noncertified values are the means of the results frcm two or more independent analytical methods as described by Schiller and Eberhardt [2]. The uncenainty is based on a 95 % confidence interval for the mean, and includes an allowarre for differences between the analytical methods used [3]. As the accuracy of the measurements could not be asscssed from the data, the uncenainty associated with a nonccnified value may fail to include all sources of uncertainties and may represent only a measure of the precision of the mcasunment methods. Element Chromium Silver Table 2. Noncertified Mass Fractions Mast Fraction (in m d k g ) Element 202 f 9 98 f 8 Aluminum Calcium Iron Magnesium Phosphorus Potassium Silicon Sodium Titanium Mass Fraction (in R) 1.6 f 0.1 3.9 f 0.1 2.8 f 0.1 0.59 f 0.04 2.42 f 0.09 0.49 f 0.03 5.1 0.2 0.21 f 0.02 0.32 f 0.03 Page 2 of 4 3M EnvironmentcaLl aboratory Page 661 of 703 BACK TO MAIN Table 3. Methods wd for the Analysis of SRM 2781. Aluminum Arsenic Cadmium Calcium Chromium Copper Iron Lead Magnesium Mercury Molybdenum Nick1 Nitrogen Phosphorus Potassium Selenium Silicon Silver sodium Titanium Zinc INAA. ICP-AES, XRF RNAA, Hyd. AAS,INAA ID-ICPMS, YGAA,RNM. INAA. TXRF INAA, TXRF, ICP-AES. XRF INAA, TXRF, ICP-AES IPICPMS, RNAA. MAA, TXRF INAA. TXRF. ICP-AES, XRF ICP-AES, ID-ICPMS, TXRF INAA, ICP-AES. XRF m-cv-Ms,RNAA, WAA [PICPMS, ICP-AES. TXRF. INAA ICP-AES, IDICPMS, INAA. TXRF KJeldaM, PGAA Color. ICP-AES. XRF INAA, TXRF.ICP-AES Hyd. AAS,RNAA, INAA, TXRF XRF RNAA. I N M ,TXRF INAA. ICP-AES, XRF INAA. TXRF, XRF ICP-AES, ID-ICPMS, INAA, TXRF Methods FIA-CV-AAS Hyd. AAS ICP-AES ID-ICPMS INAA PGAA RNAA TXRF XRF NIST AIUIYS~S M.H. &an E.S. Beary C.M.Beck I1 D.A. Becker M.S. Epsrein K. Garrity R.R. Gremberg R.M.Lmdstrom E.A. Mackey Flow injection analysis cold vapor atomic absorption spectrometry Hydrih generation atomic absorptionspcctromeuy Inductively coupled plasma atomic emission spectrometry Isotope diiution inductively coupled plasma mass spectrometry Instrumenral neutron activation analysis Prompt gamma activation analysis Radiochemical neutron activation analysis Total reflecrance x-ray fluorescence Wavelength dispersive x-ray fluorescence J.R. Moody B.R. Nonnan P.J. Paulscn M.S. Rearick T.A. Rush R. Saraswati J.M. Smeller R.L. Waners. Jr. L.J. Woad Page 3 of 4 3M Environmental Laboratory Page 662 of703 BACK TO MAIN Cooperating Annlys~sand Laboratories: F, S. Landsherger and D. Wu; Universiry of Illinois. Nuclear Engwcring Department, Champaign, IL S.A. Wilson. D. Siems, and P. Briggs; USGS. Lakewood. CO l i I A. Prange, U. Reus. and R. Neidergesiss;GKSS Research Center. Institute of Physical and C h e w m y r i c s , Geesthacht. Germany REFERENCES [ I ] Taylor, B.N.,'Guide for the Use of the International System of Units (SI)." NIST Special Publication -L 811., 1995 Ed., (April 1995). [2] Schiller, S.B. and Ekrhardt. K.R., Combining Data from Independent Chemical Analysis Methods. Spcfitmhlmid Actn, 468(12), p~ 1607-1613, (1991). [31 Guide IO the Expressh of Uncertainty in M e a w e m n r . ISBN 92-67-10188-9. 1st Ed. ISO. Geneva. Swiizerland. (1993): see also Taylor, B.N. and Kuyao. C.E.. 'Guidelines for Evaluating a d Expressing the Uncertainty of MST Measurement Results,' NIST Tcchical Note, 1297. U.S. Government hinting Office, Washington D.C..(1994). . Page 4 of 4 3M Environmental Laboratory Page 663 of 703 BACK TO MAIN Addendum to Standard Reference Material@2781 i t Domestic Sludge Leachable Mass Fractions Using U.S.EPA and NJDEP Methods for Flame Atomic Absorption Spectrometry and Inductively Coupled Plasma Atomic Emission Spectrometry -L The certi.ficd concentrationvalues of constiruent elemern in certificate are given as totd ma~sfractions. TO obtain total mass fractions, either subsamples of the SRM must k complercly decomposed. or the sample must be analyzed directly in its solid form. For mixed acid dissohnion. hydrofluoric acid must be included in the acid mixrurr to torally dissolve siliceous material present in sludge. For a nurnber of environmental monitoring purposes. acid exmaable mass fractions of elemenu an o k n uud rather than total mass fractions. Acid extractable methods do not necessarily result in total decomposition of the sludge. It should be noted that results obtained using acid leach conditions are often depicted in reporu as total resutu. However, reponed acid labk or extractablemass fractionsof elements M generally lower than total masf fractious. Results are often presented as measured mass fractions in the leachate in comparison to the total or cenified mass fractions. The recovery of an element as a pcrcent of total is a function of several factors such as tbe mode of occurrence in the sample, leach medium. leach time. temperature conditions, and pH of the sample-leach medium mixture [I]. In its monitoring programs. h e U.S..Epvironmental RotecdonAgency (US.EPA) has established a numkr of leach methods. such as Methods 3015. 3050. and 3051 12.31 for thc determination of acid labile or extractable mass fractionsof elements. The New Jersey Depamnenf of the En- (NJDEP) has developed its own leach method. NJDEP 100 for state use [4]. The NIDEP and the U.S. EPA preparedsamples of SRM 2781 using the NJDEP 100 method and EPA Methods 3050 and 3051 and analyzed the resulting leachates by flame atomic absorption spectrornc:try (FAAS) and inductively coupled plasma a@micemission spectrometry (ICP-AES). Reference values have been establishedfor the acid-leachable mats fractionsof several elements in SRM 2781. These vaiues an: thc means of all results from Ihc di&ran kactl mcasmenn~mrhaQ andcombinatioasused. ?berefvalm are listedinTable 1, almgwithtkrmCataintieSwtrirb an bavd ~a 95 % confidarcinavalsof thc maus of d t s . For some of the elements(copper. iron, silver, vanadium). no statisticallysignificant differences were found among - - - - results from the two laboratoriesusing lhreeor four combinationsof sample preparation and insvumental measuremenf ttchniques (NJDEP 100 FAAS;NJDEP 1M) ICP-AES: EPA 3050 ICP-AES; EPA 3051 ICP-AES). For all other elements. statistically significant between-laboratory differences were identified and are included in b e stated uncertainlies. These differences are small in comparison to control limits for many environmental monitoring programs. Therefore, the reference values are meaningful. despite the between-laboratory differences found. Reference Values- and UnccrtPintier: The reference values given in Table 1 are MV NIST cenified but are provided as a reference for U.S. EPA 3050 and 3051, and NJDEP 100 methods. The uncertainties are based on a 95 Z confidence interval for the mean and include an allowance for differences berween the analytical methods used. Gaithenburg. MD 20899 Addendum Issue Date: October 25, 1996 Thomas E. Gills, Chief Standard Refereme Material Program Page I of 2 3M EnvironmentlslLaboratory Page 664 of 703 BACK TO MAIN 1 1 -9 .. Element Al~inum Barium Cadmium Calcium Chromium Copper Iron Lead Magnesium Manganese Nickel Silver Vanadium Zinc Table 1. Reference Leach Values for SRM 278I Leachable rnass fraction (in mglkg) 8040, f 980 570 f 65 11 f 2 36440 f 1830 143 f 14 601 f 16 24300 f 2100 183 f 15 4850 f 290 745 f 33 12.3 f 6.3 86.3 f I .7 81.9 f 3.8 1 120 f 34 96 Leach Recovery* 5-0- 86 93 71 96 87 91 8--2- 90 8--8- 88 K Leach Recovery = 100 L Leach Value Certified or Noncertified Value Cooperating Analysts and Labomtories: S.J. Nagoumey; New Jeney Department of the Environmeot, Trenton. NJ. J. Birri, K. Pcist; U.S. Environmental Protection Agency, Edison, NJ. REFE~ENCES 111 Kam.J.S.. Leach Data vs Total: Which & b m t for SRMs, FreseniusJ. Anal. Chcm. 352: pp 209-213. (IWS). [2] U.S. EPA 1991 Code of Federal Regulations. Title 40,Pan 136. Paragraph 33. [3] Federal Register 1-13-95 SW-846 update#2. Final. [4] New Jersey AdministrativeCode, 1994. N.J.A.C. 7:14-4. Page 2 of 2 3M Environmental Laboratory Page 665 of 703 BACK TO MAIN Test Control and Reference Substance Log Soil: Sandy Loam 13-1 name: Soil: Sandy Loam 7 ILoVbatch #: ,<.. .. [Initials: 99-2564 TNA-4621 0810112015 LCG 1-500ml(2 of 3) 7- containen: [Retain Dried and sieved TCR Substance # TCR-00065-009 Received from: Anvise Amount received (wt. or 448 g net weight vol): Date: 09/14/2000 Shipper: MSDS (Vn) Date of Retain SY-N [purity: IRecords received: fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA NA container stored ambient in cabinet TCR-CO2. LCG 12/26/00 weight of container wlcap 66.49 LCG 9/14/00 3M Environmenta/ Laboratory Page 666 of 703 BACK TO MAIN USE LOG Before withdrawn Purpose (enter standard number) Balance ID Initials Date after E00-1311 PFOS adsldes 904 CMC 01/31/2001 3M Environmental Laboratory Page 667 of 703 BACK TO MAIN - 05/23/01 WED 153113 FAX 1 701 587 6013 AGVISE LABORATORIES LA 8 0 R4T 0 RIE9 t May 23,2001 @I002 Highway 15 P.0. BOX 510 Northwood, ND 58267 oou 587-6010 FAX (700 587-6OU emall: agvise@polarcornin.com nomepage agviselabrcom Mr. Mark Ellefson 3M Corporation Re Soil Characterizationfor Agvise South Soil collectedfrom the site Agvise South has tested as follows~ Percent Sand Percent Silt Percent Clay USDA Textural Class (Hydrometer method) 58 22 20 Sandy Loam Bulk Density(disturbed) g d c c 1.05 Cation Exchange Capacity (mew100 g) 23.3 % Moisture at 113 Bar 27.9 Percent Organic Matter 4.8 p~ in 1:I soilwater ratio 7.8 Extractable Iron (ppm) 10.3 Extractable Zinc (ppm) 1.59 ExtlactableManganese (ppm) 11.9 Extractable Copper (ppm) 0.24 Base Saturation Data Cation Percent PPm Calcium Magnesium Sodium Potassium Hydrogen a& Robert Deutsch c Soil Scientist 79.5 10.0 0.8 2.5 7.2 3700 280 41 231 17 3M EnvironmentasL/ aboratory Agriculturul Testing Page 668 of 703 BACK TO MAIN 12/11/00 MON 15:17 FAX 1 701 587 6013 AGVISE LABORATORIES ~001 * u t L A e o II A T o R I K S AGVISE S o i l Characterization Report Highway 15 P.0. Box 510 Northwood, ND 58267 1701) 587-6010 F A X (7011587-6013 I emall: agvis&poiarcornm.com Homepage: agviselabs.com Submitted By: BOB DEUTSCH P.O. BOX 316 111 1ST AVENUIS NORTHWOOD ND 58267 Results Reported To: BOB DEUTSCH P.O. BOX 316 111 1ST AVENUE NORTHWOOD ND 58267 - PrOtOcOl/StUdy NO = Specimen ID = Purchase Order Trial or Test NO = AGVISE SOUTH Depth = Date Received = 9/20/00 Date Reported = 9/22/00 AGVISE Lab NO = AGVISE Ref NO = 27,767 6,633,357 Percent Sand Percent Silt Percent Clay w USDA Textural Class (hydrometer method) % Organic Matter (Walkley-Black) 58 22 20 SANDY LOAM 4.9 p H (Water) 7.8 W , .. .. . . 3M Environmental Laboratory Agricultural Testing Page 669 of 703 - iz/ii/oo MON i5:ia .FAX 1 701 587 6013 AGVISE LABORATORIES BACK TO MAIN Bo02 c 3M Environmental Laboratory Page 670 of 703 BACK TO MAIN ISubstance/chemcal or reference# name: IH, IH, 2H, 2Hperfluorooctanesulfonic Acid TCR Substance # TCR-00017-047 ILot/batch #: 9-75-30 Received from: SynQuest Labs NIA Amount received (wt. or 80 g, 428.04 g gross wt. vol): [Initials: PMR Date: 0511 512000 7 INumber/sizeof 1/ 250 mL jar Shipper: UPS Jcontainers: I I I_ I lgoodl white powder ~ S D (Sv/n) PYUN \Retain 10.2762 g IDate of Retain l05/17/2000 [Purity: TBD IRecords received: MSDS SynQuest Labs fabrication, or derivation records: ! Std Lmtion/Storage: F19, Frozen IMolecular Formula: C8H5Fl303S 3M Environment,alLaboratory Page 671 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log IStandard ID# 101001-03-07 IDescription 1500 mglL BookNo. 001 PageNo. 03 1 IDate Prepared ~0210112001 IAnalyst JCMC ]Stock ID# kR-00014-046 I I I Conc or Purity lnut I Final Conc 1500 mglL Weight or Volume 0.500 g Balance ID 914 Final Volume 1000 ml I [ Storage Location [ ExpirationDate 13rd Floor ~08/0112001 T N A Solvent 0.01M CaClZ 00001-34-12 I 1 Comments: I I Reviewed Bv: Cindv M. Carlson 02/06/2001 3M Environment,alLaboratory Page 672 of 703 BACK TO MAIN ]Standard ID# [00001-19-01 IDescription ITHPFOS Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 19 IDate Prepared IAnalyst 1 (07/05/2000 (KLT lneat I Conc or Purity I Flnal Conc: 1444 ppm I Weight or Volume 0.0111 g Balance ID 1 FinalVulume i i i a i m a i (914) 25ml I Storage Location (3rd Floor I Expiration Date ~01/31/2001 I I I Comments: 1Added Meoh TN-A per KLT on 1/30/01 OK. Updated Balance ID on 2/16/01 per KLT. OK )-gn]enka Krupljanin 0211612001 I TN-A Solvent TNA-4464 Methanol - 3M Environmental Laboratory Page 673 of 703 BACK TO MAIN Environmental Laboratory IStandard ID# lOOOOl-24-03 IDescription ITHPFOS Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 24 !Date Prepared IAnalyst (09/13/2000 (CMC 1 I Conc or Purity Weight or Volume 0.5 m l Balance ID Final Volume 10 ml I Final Conc: 122.2 u g h 1 - I Storaae Location 13rd Floor I ExDiration Date 103/31/2001 i I I Comments: IReviewed By: Cindy M. Carlson 10/19/2000 TNA Solvent tn-a4639 Methanol I I 3M Environmental Laboratory Page 674 of 703 _ . .- . - BACK TO MAIN SINGLE COMPONENT STANDARD PREPARATION LOG W Reviewed By: ?! h3 BACK TO MAIN IStandard ID# IDescrbtion Standards Database SCSPL Single Component Standard PreparationLog BookNo. 001 PageNo. 31 bate PreDared [Analvst I 6.0L milli-q I Comments: I Reviewed By: OlgnjenkaKrupljanin11/21/2000 3M Environmental Laboratory Page 676 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log (Standard ID# 100001-31-11 (Description l5OOmglL PFOS IStock ID# ITCR-00017-046 I Conc or Purity lneat I Weight or Volume 10.0500g JBalanceID I BookNo. 001 PageNo. 31 !Date Prepared [Analyst I 111/01/2000 ICMC I FinalVolume 1 TN-A Solvent IlOOml IOOOO1-31-10 0.01M I CaC12 I i-gnjenka Krupljanln 05/23/2001 3M EnvironmentalLaboratory Page 677 of 703 BACK TO MAIN . - . I I s--7 Y -- 7- SINGLE COMPONENT STANDARD PREPARATION LOG Book NO. 00 001 Page No. 32 Reviewed By: Date: I BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 32 I Conc or Purity 1 Weight or Volume ]Balance ID 1 Final Volume 1 TNA Solvent (00001-31-10 0.01M Final Conc I'lODDlll 1 Storage Location I Expiration Date 1 13rd Floor 105/31/2001 1 Icomments: I 1 Reviewed By: Cignjenka Krupljanin 11/21/2000 3M Environmentisl Laboratory Page 679 of 703 BACK TO MAIN )Standard ID# 100001-32-07 [Stock ID# ITCR-00017-046 !Description llOOmg/L PFOS I Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 32 lDate Prepared (Analyst 1 ~11/13/2000 ICMC L I Final Coni: [100mg/~ 1 I Storage Location 13rd Floor 1 Expiration Date 105/31/2001 Comments: [V Reviewed By Ognjenka Krupljanin 11/21/2000 CaC12 3M Environmental Laboratory Page 680 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log IStandard ID# 100001-32-09 IDescription 10.10rnglL PFOS [Stock ID# 100001-32-07 I Conc or Purity I Weight or Volume 250uL Balance ID BookNo. 001 PageNo. 32 I IDate Prepared 111/13/2000 (Analyst ICMC I Final Volume 250mL TN-A Solvent 00001-31-10 0.01M CaC12 Final Conc: 10.1Omg/L 1 I Storage Location 1 (3rd Floor I Expiration Date 105/31/2001 i I Comments: 1 LReviewed By: Ognjenka Krupljanin 11/21/2000 3M Environmental Laboratory Page 681 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log [ Conc or Purity llOOOppm 1 Weight or Volume 10.25mL /Balance ID I 1 Finalvolume 1 TN-A Solvent 1 1500mL ITNA-4672 Final Cono 1500ppb 1 Storage Location I Expiration Date I [2nd Floor (03/30/2001 I Comments: I Reviewed By: Olgnjenka Krupljanln 11/21/2000 I ~ 3M Environmental Laboratory Page 682 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log t L I Conc or Purity 588 ppm Final Conc: 120 PPm Weight or Volume 850u' -Balance ID Final Volume 25 ml I Storage Location I Expiration Date 1 13rd Floor 105115/2001 I Comments: I Reviewed By: Clgnjenka Krupljanin 11/27/2000 TN-A Solvent tn-a4604 Methanol I ~ 3M EnvironmentislLaboratory Page 683 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log t 1 Conc or Purity I 100 ppm Weight or Volume 5 ml Balance ID Final Volume I O ml TNA Solvent 00001-31-10 0.0lMCaC12 I ' w g n j e n k a Krupljanin 11/27/2000 3M Environmental Laboratory Page 684 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log IStandard ID# 100001-33-07 IDescription 10.01 M CaCl2 (aq) BookNo. 001 PageNo. 33 IDate Prepared ]Analyst 1 ~11/21/2000 ICMC I I p o c k ID# (tn-a4000 I Concorpuritv I Weight or Volume IEalanceID I I I FinalVolume I TN-A Solvent I I I I I Final Coni: 10.01 M I - Storage Location I Expiration Date I 13rd Floor ~03/01/2001 i I Comments: I I i-lgnjenka Krupljanin 11/27/2000 3M Environmental Laboratory Page 685 of 703 BACK TO MAIN :E nvironmental Laboratory i IStandard ID# bOOO1-34-12 1 Description 10.01 M CaCl2 (aq) Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 34 IDate Prepared 11 2/04/2000 ]Analyst (CMC 1 Conc or Purity lneat I Weight or Volume 16.7142 g IBalance ID I NA 1 FinalVolume 16 Liters Final Cono 10.01 M I Storage Location I Expiration Date I 13rd Floor 103/14/2001 I Comments: IReviewed By: Cindy M. Carlson 12/14/2000 1 TN-A Solvent Imilli-q I J 3M Environmenfal Laboratory Page 686 of 703 BACK TO MAIN SINGLE COMPONENT STANDARD PREPARATION LOG BookNo. +.,. 00001 Page No. 34 BACK TO MAIN ]Standard ID# [Ol 001-02-01 Standards Database SCSPL Single Component Standard Preparation Log I Description I20 mg/L THPFOS IS BookNo. 001 PageNo. 02 IDate Prepared ~01/08/2001 IAnalyst ICMC E I Conc or Purity Weight or Volume 850 ul Balance ID NA Final Volume 25 ml TNA Solvent TNA-4715 Methanol I ' [ R e v l e w e d i n d y M. Carlson 02/06/2001 3M Environmental Laboratoty Page 688 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log IStandard ID# 101001-02-02 1 Description IPFOS Stock BookNo. 001 PageNo. 02 IDate Prepared ~01/09/2001 /Analyst IMLA p o c k ID# I I ITCR-00017-046 ineatconc or Purity Weight or Volume 0.1278 g Balance ID 914 Final Volume 10 ml Final Conc: (12780 uglml I 1 Storage Location I 13rd Floor I Expiration Date 101/09/2002 TN-A Solvent tn-a-4755 Methanol [Comments: I I 1 Reviewed By: Cindy M. Carlson 02/06/2001 3M Environmental Laboratory Page 689 of 703 BACK TO MAIN IStandard ID# 101001-02-03 1Description ITHPFOS Stock Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 02 ]Date Prepared ~01/09/2001 IAnalyst IMLA I Conc or Purity lneat Weight or Volume 0.0053 g Balance ID 914 Final Volume I O ml TNA Solvent TN-A4755 Methanol 1 Comments: I m i n d y M. Carlson 02/06/2001 3M Environmental Laboratory Page 690 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log [Standard ID# 101001-02-04 [Description IPFBS Stock IStock ID# ITCR-99030-023 1 Conc or Purity lneat I Weight or Volume 0.0127 g Balance ID 914 BookNo. 001 PageNo. 02 [DatePrepared [Analyst I )01/09/2001 [ MLA Final Volume 10 ml TNA Solvent TNA-4755 Methanol P v G d By: Cindy M.Carkon 02/06/2001 3M Environmental Laboratory Page 691 of 703 BACK TO MAIN i ]Standard ID# [OIOOI-02-05 IStock ID# ~01001-02-02 Standards Database SCSPL Single Component Standard Preparation Log 1IDescription 25 ppm (uglml) PFOS BookNo. 001 PageNo. 02 IDate Prepared IAnalyst 1 ~01/09/2001 (MLA Final Conc: 125.048 ua/ml I Comments: NA 25 ml I 1 Storage Location I Expiration Date 13rd Floor 101/09/2002 I TNA-4755 Methannl I 3M Environmental Laboratoty Page 692 of 703 BACK TO MAIN Standards Database SCSPL Single Component Standard Preparation Log t BookNo. 001 Page No. 03 Weight or Volume Balance ID NA Final Volume I 0 0 ml I Final Conc (50 mg1L I 1 I Storage Location I 13rd Floor Expiration Date ~0810112001 I Comments: 1 Reviewed By: Cindy M. Carlson 02/06/2001 T N A Solvent 0.01 M CaC12 00001-34-12 I 3M EnvironmentalLaboratory Page 693 of 703 BACK TO MAIN Environmental Standards Database ILaboratory SCSPL Single Component Standard Preparation Log i ]Stock ID# I ITN-~-4000 I Final Conc 10.01 M I I 1 Storage Location Expiration Date 13rd Floor 108/12/2001 1 I Comments: I Reviewed By: Cindy M. Carlson 02/28/2001 ~~~~ 1 I 3M Environmental Laboratory Page 694 of 703 BACK TO MAIN IEnvironmental ILaboratory 1 I StandardID# I Description Standards Database SCSPL Single Component Standard Preparation Log BookNo. 001 PageNo. 04 I Date PreDared I Analvst I 3M Environmental Laboratory Page 695 of 703 BACK TO MAIN II MULTI-LEVELSTANDARD PREPARATION LOG Book ,No. 00 002 Gl Pa"aeNo. 104 t Description:&is&/ k - k Date Prepared: la/&.I OD &A--o& Prepared By: L.1fi:- Storage Location: I- ExpirationDate: (a Lot#: .- Description: Date Prepared: Prepared By: Storage Location: Expiration Date: 4 G,A 034Jm&? # bf 33' - 011- ,$?? h BACK TO MAIN MULTI-LEVEL PREPARATION LOG BookNo. 01 003 Page Nc'. 7 BACK TO MAIN Prep date: Analyst: Type of the curve: Target analytes: Exact concentration of I .L0/ /tl& P.FrIS p h J CTy-/&/e 'PFOJ,THPFD>C"ZS) pp?fi~s(zr) Standard mix used for preparing the curve: D l m / -d - 5 every point of every analyte Book No: Page No: 01 003 7 Solvent & TN-A #: flpO//, Final Volume of each point: 7 , ~ - A- Y f55 __"-....-..-...........---.. ..-- ........................... I...............". Internal Standards TH'HP.735 PFDs / standard concentration amount used Same amount of Internal standard used in all points, leading to same concentration in every point. BACK TO MAIN Date Frepared: is/,a/0 o Prepared By: Storage 1-ocation: Expiration Date: cw\( 3 6 /o I MULTICOMPONENT STANDARD PREPARATION LOG Book No. 00 003 PageNo. 147 Solvent: t+ 0 H S o u r c e : w sau Lot #: 3MTrace#: m &-L(lL.Io Expiration Date: m o54 I 3M EnvironmenQslLaboratory Page 699 of 703 a ET&S Chemical inventory System ISize: lQty Recorded: IDate Recorded: b a t e ExDired: 14L 112 I5117/00 12005 BACK TO MAIN I I 1 3M Environmentid Laboratory Page 700 of 703 a ET&S Chemical Inventory System I I I ITrace #: TN-A-07f5 Chemical Sort Prefix: Chemical Namo: Methanol CASllD #: 67-56-1 Manufacturer: EM CATIStudy #: MX0475-1 Lot # 40276 Size: 4L Qty Recorded: 12 Date Recorded: 11110100 Date Expired: 11110/05 Storage Requinnents: Flammable Chemical Hazard Class 3 BACK TO MAIN I 3M Environmental Laboratory Page 701 of 703 ET&S Chemical Inventory System E i I Trace #: ChemicalSort Prefix: Chemical Name: CASllD #: Manufacturer: CATIStudy #: Lot #: Size: Qty Recorded: Date Recorded: Date Expired: Storage Requinments: ChemicalHazard Class I TNA-4740 methanol 67-56-1 EM MX0475-1 40276 4L 12 11/27/00 11/27/05 flammable 3 BACK TO MAIN I 3M Environmental Laboratory Page 702 of 703 a ET&S Chemical inventory System Trace #: Chemical Sort Prefix: Chemical Name CASllD #: Manufacturer: CATIStudy #: Lot #: Size: Qty Recorded: Date Recorded: Date Expired: Storage Requirrnents: Chemical Hazard Class TNA-4755 Methanol 67-56-1 EM MX0475-1 4L 12 12/11/00 12/11105 flammable 3 BACK TO MAIN 3M Environmental Laboratory Page 703 of 703 Collection Information BACK TO MAIN ........................................................ ........................................................ BACK TO MAIN AGVISE Soil Characterization Report submitting firm = 3M Protocol or Study No = NA Sample ID. = KITTSON CO CLAY 0-6 Trial ID. = NA D a t e Received = 10-23-00 D a t e Reported = 11-02-2000 AGVISE Lab NO 00- 2407 Percent Sand 16 Percent Si1t 22 Percent Clay 62 USDA Textural Class (hydrometer method) Clay Cation Exchange Capacity (meq/lOO g) 54.5 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen ( 0 ) 2.6 4.5 7.2 0.223 Base Saturation Data Caticrn Calcium Magnesium Sodium Potassium Hydrogen Percent 54.2 34.6 0.9 3.6 6.8 5900 2260 110 771 37 leted in compliance of 40 CFR Part 160. Date Soil Scientist/Analytical Investigator - au Agricultural Testing BACK TO MAIN L A B 0 R A T0-RI e 8 AGVISE Soil Characterization R@port Submitting firm = 3M Protocol or Study No = NA Sample ID. = DON UGLEM-LOAM 0-6 Trial ID. =NA Date Received = 10-23-00 Date Reported = 10-31-2000 AGVISB Lab No 00- 2404 Percent Sand 39 Percent Silt 50 Percent Clay 11 USDA Textural Class (hydrometer method) Loam Cation Exchange Capacity (meq/lOO g) 23.9 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen (%I 4.9 8.4 7.4 0.358 Base Saturation Data Cation Calcium Magnesium Sodium Potassium HyUrogen Percent 52.2 20.9 0.7 3.5 22.7 oom 2500 600 38 324 54 These t e s t s were completed in compliance of 40 CFR Part 160. Arkytical Investigator 10-31-00 Date Agricultural Testing BACK TO MAIN AGVISE Soil Characterization Report: Submitting firm = 3M Protocol or Study No = NA Sample ID. E K BROKREN-CLAY LOAM 0-6 Trial ID. rNA Date Received E 10-23-00 Date Reported = 10-31-2000 AGVISE Lab NO 00- 2405 Percent Sand 21 Percent Silt 46 Percent Clay 33 USDA Textural Class (hydrometer method) Clay Loam Cation -change Capacity (meq/100 g ) 2 4 . 7 Percent Organic Carbon Percent Organic Matter pH in 0-01 M CaC12 Total Nitrogen (%I 2.6 4.4 6.0 0.216 Base Saturation Data Cation Calcium Magnesium Sodium Potassium Hydrogen Eercent 52.7 24.3 0.7 5.8 16.5 ppm 2600 720 39 557 41 These tests w e r e completed in compliance of 40 CFR Part 160. &a1 ytical Gvestigator /&a- 00 Date Agricultural Testing 05/23/01 WED 15:19 FAX 1 701 587 8013 AGVISE LABORATORIES LABORATORIES May 23,2001 BACK T@ O0IM02AIN Highway 15 P.0. BOX 510 Northwood, ND 58267 (701) 5876010 FAX (701)5876013 emall: agvis&polarcommrom nomepage agviselabscom Mr. Mark Ellefson 3M Corporation Re Soil Characterizationfor Agvise South Soil collected from the site Agvise South has tested as follows; Percent Sand Percent SiIt Percent Clay USDA Textural Class (Hydrometer method) 58 22 20 Sandy Loam Bulk Density (disturbed) gm/cc 1.05 Cation Exchange Capacity (meq/100 g) 23.3 % Moisture at 113 Bar Percent Organic Matter pH in 1:1 soikwater ratio 7.8 Extractable Iron (ppm) Extractable Zinc (pprn) Extractable Manganese (ppm) Extractable Copper (ppm) 10.3 I.59 11.9 0.24 Base Saturation Data Cation Percent Calcium Magnesium Sodium Potassium Hydrogen 79.5 10.0 0.8 2.5 7.2 PPm 3700 280 41 231 17 &D*- Robert Deutsch Soil Scientist Agriciil turd Testing LABORATORIES BACK TO MAIN Highway 15 P.O. Box 510 Northwood ND 58267 (701) 587-6010 FAX (701) 587-6013 email: agvise@polarcommcom Homepage. agviselabs.com AGVISE Soil Characterization Report Submitting finn = 3M Protocol or Study No = NA Sample ID. = GOOSE RIVER-SEDIMENT 0-6 Trial ID. = NA Date Received = 10-23-00 Date Reported = 10-31-2000 AGVISE L a b No 00- 2406 Percent Sand 39 Percent Silt 42 Percent Clay 19 USDA Textural Class (hydrometermethod) Loam Cation Exchange Capacity (meq/100 g) 17.5 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen ( % ) 1.3 2.3 7.7 0.101 Base Saturation Data Cation Percent &an! Calcium Magnesium Sodium Potassium Hydrogen 57.2 28.6 4.8 3.4 6.0 2000 600 193 232 10 These tests were completed in compliance of 4 0 CFR Part 1 6 0 . J@ie M. J o w o n Analytical Investigator 18 -J/-OO Date Agricultural Testing BACK TO MAIN Standard Reference Material" 2781 Domestic Sludge This Standard Reference Material (SRM) is intended pnmuily for use in the evllurtiOn of methods uscd for the analysis of sludgesand &r materials of a similar malrix. SRM 2781 is a dried and pulverized domestic sludge. A unit of SRM 2781 consists of 40g of rhe drkd mrterial. C d i Values: The certified values for 10elemem m listed mTable 1 vdarebascd onfoacoTdant results from two or more analytical methods. Analytical methods used for the characterizationof this SRM are givenm Tabb 3- All values arc reported as mass fractions [I], on a dry mass basis and arc based on m t m m w usinga sample mass of at least 100 mg. Noacuttfied Vdocs: Noncertificd values for eleven additional elsmenu arc listed in Tabk 2 and were derived . from a combiDMion of results from NIST and collabontiag 19boratorier. These results may have sources of bias yet IO be investigatedand do not meet NIST criteria for certification. Expiration of CeMratian: This ctmficath is valid for five years from tbe due of Jhipnen from NIST. However, tht certificationwill be nullifiedif the SRM iscmWmat&orlllamd. shoutdpnyofrhcvai~chaage before dle Upiratimof thecenificarion, plrchasers wiubeooti&edbym1.Reaanof the atuched registration card will facilitate notification. stability: This material is amsidered to be stable;boweva, its StSwityhasnMbea!rigorously assessed. NIST will continuously monitor rhis material and report ahy subeuativc cbangcs in certification to the purchaser. - Use: A mixurnurn sample mass of 100 mg (dry m8.w ree [9stmca* olls forDryiIlg)shouldbeased.ndsample preparation procedures should be designed to effect complete dissolutiiopfor analytical derenninatiwsto k related to the certified values provided. &. - 1 lor Drying: W h m n o n v o l a t i b e l e m e n r s a r e a b e ~sampks should k ~cuumdriedamt om temperame for 24 h or oven dried for 2 h at 110 'C. Volntile elermar (e.g., mercury. and selenium) should be &ermined on samples as received, sepmate sampla should be dried according to meSe imfltcti to obtain a correction factor for moisrurt. Moisture comUm' os arc thm made to mwauememvalues befon amparing them to the certifiedvalues. [Notethatthe mass loss andryingat the timC 0fcertiAcaClonwas found to be in the range of 4.7 7% to 6.6 96 when using the rtcommcodcd drykg procedUrrs.1 Statistical consultationwas provided by L.M.Gill of rbe NIST SaWcal snoia#rinsDivision. The overall direction ivnd cOOrdiOatioD of tbe analyses were rmQ tk chahmdu'p of J.D. Fas~mof the NIST Analytical Chemistry Division. The technical and support aspects involved in r k originalpreparation. certification,and issuance of this SRM were coordinated through the Standard Referare Materials Program by J.S. KaDc. Revision of this certificate was coordinated through the Standard Reference Materials Program by B.S. MacDolllld. Gaithersburg, M D 20899 Certificate Issue Dare: October 25, 1996 (Revisionof certificate dated 6-22-95 to include Eddendum) Thomm E. Gills. Chief Standard Reference Materials Program 1 Of4 BACK TO MAIN . I Sourrc sad Repamtiom d We*. The U.S. Geologicrl Swcy (USGS), under cowact to NIST. obuincd pniplly dehydrated sewage cake material from tk Menopoliua Dmer Sewage Disposal District No, 1. Ibe mated(Ipp0ximUcly 182 I r s ) w r , ~ i n p l a r t k - l i ~ r r d o a r r s p a r t a d Ut SoG~S faciiitier ia L;rlrcwood. b CO for proceuina. hum dried &I ambient tcmpeMurr inr forcsdakchamber, grormd tom8 74 m. (200mesh) sieve. blended for 24 h to wun bomogmeity of the pulverizCa material after which test umples were taken h m tbc blender forplimirnry bmoga&y malyJcs. The mmefialwmtitcnndiationslerilited. 'Ibc rterilized moterial WIU shipped inbulk to NUT, where the material was bottled m a g uniu a&r nblendq for 4 h. - Anolysb: The bornoseniry was asscsxd a! USGS on 10 replicate samples of bulk mterial for over 40elements wing x-ray flwesceacc (XRF) and/or iaductively coupled plasma atomic emission spccttomeuy (ICP-AES). Homogarity wy f\atbrr PKualduringcmicrViOaadysis; Isampk Oizcs of 100 mg or greater. No saxnpk-to- sampk variations in excess of thosc expected from the llarlyticzl mwurcmcnts wen detected. Anmic Cadmium copper Lepd Mercury Molybdearmr Nickel z i SClClliWll 7.82 f 0.28 12.78 f 0.72 627.4 f 13.5 202.1 f 6.5 3.64 f 0.25 46.7 f 3.2 80.2 $ 2.3 16.0 f 1.6 1273 f 53 Nitrogen 4.78 f 0.11 Element chromium Silver Mass Fraction (in m m 202 f 9 98 f 8 Element Page 2 of 4 * 1.6 f 0.1 3.9 0.1 2.8 f 0.1 0.59 0.04 2.42 f 0.09 0.49 f 0.03 5.1 f 0.2 0.21 f 0.02 0.32 f 0.c13 BACK TO MAIN Addendum to Standard Reference Material* 2781 Domestic Sludge Leachable Mass Fractions Using US.EPA and NJDEP Methods for Ramc Atomic Absorption Spectrometry and Inductively Coupled Plasma Atomic Emission Spectromeq IL The CenifKd conctntntida values of constin~~ealemcn~in~ thit certificate are @vmas totalmass Froctioas. To obtain total mass fractions, either subsamples of the SRM must be completely decompored or the sample must k amlyzeddirealyiaiusdidfonn. Formixedaciddissdatiaa,hydroffuon- cacidmwbcirrhdtdinbreacidminat to totally dissolve siliceous material prrsent in sludge. For a number ofcnvimuneaolmaiming purposes, acidexaambk ma55 fractiossofclewnts are o f h used rather th?n total mass h;aEti. Acid emactable metbodsdo aof llCCCSSUlyl result in tarl decomposition of thc sludge. It should be noted tb?t d t s obuined using acid lcacb Maditions arc often depicted in repons as mal result). However.reponcd acid labile or urnactablemass fmioos of elements arc gumally lower than tolll mass fractions. Results are often presmcd as measured mass fractioas in the -hate incomparisaatothetotal or certified mass fractions. The recovery of an ekmmt as a pcrcmt oftaal is a imaionof several factors such at the mode of occurrence in the sample. leach medium. leach the. temperature coixiitkms, and pH of the sampk-leachmedium mixture [11. In its moaiurriag programs. thc u.s,Epviroamenut Rotccm. aAgcrry(U.S.EPA)bascsrabli&edanumk+ofkach methods. such as Methods 3015. 3050,ad 3051 [2,3] far the dcttrmiDMioa of acid labile or exmaable mass lractMN of ekmem. The New Jersey -of the mEP)bardmlop!!diuoWnruchmtbod. NJDEP I00 for state UK [4]. Ihe NJDEP and dr U.S. EPA prepad samples of SRM 2781 uaiag h e NJDEP 100 method and EPA Methods 30% Ud 3OSl a d analyzed tht resulting leachates by flame atomic absorption spectrometry (FAAS) and inductively couplea plasma atomic emissioa specvomeuy (ICP-AH). Rcferrncc values havc kcamabhbcd fortbc acid-kdt&lemass baicms ofsevenl ek3nenrr inSRM2781. Ibcse values arc the meylJofpn Iesulaifiom Itr diffka* k d l mQMco3edmtbods ladcmwmthsItssd 'Ibcnkrrnce v a h r s a n l i r s e d i m T a b k l . ~ W i h r b c i r ~ ~ a c b a r e d a9n6%r r n M a r r ~ o f t h c ~ o f r c o u k t . For some of the ekmmts (copper. inn,silver. vanadium), no StrUinicaUy significant differenceswen found unang - - - - Mulufrom tht two labontw. rusiagthneorfourcombiaatiollsofs;llaplepepvaDionaadiasvumenulfnmmmma tcchqws (NJDEP 100 FAAS;NJDEP 100 ICP-AES; JPA 3050 ICP-AES; EPA 3051 ICP-AES). For dl otbtr elelncnts. statistically sipificam bctw#n-laboratory difference were identified and are included in the stated uncertainties. These differraces are s d m cOmpPriSw to control 1imiB for many cmhmmtd monitoring programs. Therefore. the reference valuer an mcani@d. despite t& krwccn-laboramy differences found. . Reference V.lucs md UncerMiakr The rcfermccvahres given mTrbk 1 arc mt NlSTCmitkd but arc provided as a reference for U.S. EPA Mu)and 3051. and NJDEP 100 melhods. The UnCerUintks are based on a 95 5% confiiacc interval for tbe mean and include an allawlnct for diffnrrrcs ktw+mthe pnolyticd methods wed. Gaithenburg. MD 20899 Addendum Issue Date: October 25,1996 Thomas E. Gills, Chief Standatd Referrnee M a r i a l Program Pagelof2 BACK TO MAIN Element Aluminum Barium Cadmium Calcium chromium Copper IrOn Lead Magntsium Maw== Nickel Silver VaMdium Zinc Table 1. Reference h h Values for SRM 2781 Leachable mass f r a c t i (inmg/kg) 8 04q 570 11 36440 143 601 24 30 183 4 850 745 72.3 86.3 81.9 1 120 fm f 65 f 2 *f 1830 14 f 16 f 2100 f 1s f 290 f 33 f 6.3 f I .7 f 3-8 f34 46 Leach Recovery' s-o 86 93 71 96 87 91 82 I - 90 88 -I 88 * % Leach Recovery = 100 x Leach Value Cerdtkd or Noneenifled Value CoopclPtiaLAnnlysQandLPbaotorlcs: . S.J. Nagwmey; New Jcney Dopanment of the EnvinnrmCat Tnntoa NJ. J. Birri, K.kist;US. Environmental Protection Agency, Edison, NJ. RJmitEWEs (1) Kuw, AS., LuchDafa vs Total: Which u d;kvan for SRMs, Frcsadus J. Anal. cbcm. 3 8 : pp 209-213, (199s). [2] U.S. EPA I991 Cock of Federal Regulations. T i 40,Part 136. pprpgrppb 33. [3] Federal Register 1-19-95 SW-846 update y2. Fizul. [41 New Jcrsey Administrative Code, 1994. N.J.A.C. T14-4. Page20f2 BACK TO MAIN T8ble 3. Methods used far the Analysis of SRM 2781* I N M , ICP-AES, XRF RNM, Hyd. AAS, I N M ID-ICPMS, PCM, RNA& INAA. TXRF I N M . TXRF, ICP-AES, XRF I N M . TXRF. KP-AES ID.IcpMs, RNM, INM,lXRF INM.TXRF. m-AES.XRF ICP-AES,ID.ICPMs.TXRF INAA, ICP-AES. XRF rn-Cv-AAS, RNA& INAA ID=ICPMs,ICP-m, "XRF, INM ICP-AES,IDXPMS, INM.TXRF IQ-9 XAA Cdor. ICP-AES, XRF INAA,TXRF. ICP-AES Hyd. Ms, RNAs IN&, TXRF XRF RNM, INM.lxRF I N M . ICP-AES,XRF INAA. TXRF, XRF ICP-AES, DICPMS, MAA, TXRF FIA-CV-AAS nyd. MS ICP-AES ID-ICPMS INAA PGAA RNAA TXRF XRF M.H. Ahsan E.S. Beary C.M.Beck I1 D.A. Baker M.S. Epstein K. Gamty R.R. Greenberg R.M. tiadsrrom E A .Maclrey J.R. Moody B.R. Nonnan P.J. Paulscn M.S. Rearick T.A. Rwh R. Saraswati J.M. Smeller R.L. Waters, Jr. L.J. Wood Page3of4 BACK TO MAIN - [11 Taylor, B.N., 'Guide for the Use of the Intcmuional System ofUnits (SI)." NIST Special Publication 811, 1995 Ed., (April 1995). [2] Schiller, S.B. and Eberbrdt. K.R.. Combining Data from lndependcru Chemical Analysis Metbob, SpeeaoChtmicrl Aao, 468 (12). p~ 1603-1613. (1991). [3] Guide ro the Expnssion of Uncertainly in Mcanmnunr. ISBN 92-6'7-10188-9, 1st Ed. ISO, Geneva. Switzerland, (1993): w also Taylor, B.N.and Kuym, C.E.. 'Gukklks for Evaluating pad w i n g rht Uncertainry of NfsT Measurement Resulu.' NIST Tcchohl Note, 1297. U.S. Government Riming Office. Washington D.C.. (1994).