Document JNoZZme5Jwm7BaMz3qyER7J0a

BACK TO MAIN AR226-1030A030 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: E00-1311 Total Number ofPages 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 Adsorption/Desorption Study of Potassium Perfluorooctanesulfonate (PFOS) Study Identification Number: E00-1311 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 Adsorption/Desorption of Potassium Perfluorooctanesulfonate (PFOS) Study Identification Number: E00-1311 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 9/19/00 11/07/00 4/18/01 5/11/01 5/14/01 5/17/01 5/22/01 5/25/01 Phase Protocol In-phase Data (Tier I) Data (Tier II&III) Data (Tier II&IH) Data (Tier II&III) Data (Tier II&III) Final Report Date Reported to Management Study Director 9/20/00 9/20/00 11/07/00 11/07/00 4/18/01 4/18/01 5/11/01 5/11/01 5/14/01 5/14/01 5/17/01 5/17/01 5/22/01 5/22/01 5/25/01 5/25/01 QA U Represemative 1 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............................................................................................................................10 Chemical Characterization.............................................................................................................. 10 Method Summaries.........................................................................................................................11 Specimen Collection and Analysis................................................................................................... 14 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 E00-1311- ................................................................................................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 o f Soil Samples for Screening (Tier II) and Advanced (Tier III) 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-Electrospray/Mass Spectrometry" .......................................... 133 ETS-8-110 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Water Extracts Using HPLC-Electrospray/Mass Spectrometry/Mass Spectrometry" ...................................... 142 Appendix C: Sample Preparation Sheets.............................................................................................. 27 Appendix D: Individual 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 II Studies....................................................8 Table 3. Summary Table of PFOS Adsorb/Desorb Tier III 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-E00-1311........................................... 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, 1:5SoihSolution Ratio,48 hour Time Point...........20 Table 13. Desorption Kinetics of PFOS, 1:5SoihSolution Ratio,48 hour Time Point.......... 21 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 adsorption/desorption 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 Laboratory 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 II) and Advanced (Tier III) 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 Adsorb/Desorb Tier I Studies Q uestion Is th e a n a ly tic a l m e th o d a p p ro p ria te /a d e q u a te fo r th e stu d y ? W h a t is th e b e st te st v essel to u se? W h a t is th e e q u ilib riu m tim e an d am o u n t ad so rb ed at eq u ilib riu m ? W h a t is a s u ita b le d e so rp tio n so lv en t? W h a t is th e o p tim a l so ih so lu tio n ratio ? C onclusion T h e m ethods E T S -8 -1 5 9 and E T S -8 -1 6 0 p ro v id e su fficien t reco v ery o f th e test su b stan ce. P o ly p ro p y len e tubes w ill b e used th ro u g h o u t th is study. T h e 1:5 so ih s o lu tio n ra tio sh o w s a > 5 0 % a d so rp tio n fo r b o th so ils tested . T h e eq u ilib riu m tim e is 4 8 hou rs. M eth a n o l is a su ita b le d e so rp tio n so lv e n t. T h e o p tim a l s o ih s o lu tio n ra tio n is 1:5 Is th e te st s u b s ta n c e s u ffic ie n tly s ta b le d u rin g th e s tu d y p e rio d ? T h e test su b sta n c e is sta b le d u rin g th e co u rse o f th e stu d y . 3M Environmental Laboratory Page 7 of 703 BACK TO MAIN Table 2. Summary Table of PFOS Adsorb/Desorb Tier II Studies Soil Type Average Distribution C oefficien t, K{|, L /g Percentage of O rganic C arbon in Soil, % oc C lay (S T -l) C lay L o am (ST-2) S an d y L o am (ST-3) R iver S edim ent (ST-Sed) D om estic Sludge (ST-SIg) 0.0183 0.00972 0.0353 0.00742 < 0 .1 2 0 2.6 2.6 2.8 1.3 NA A v e r a g e O r g a n ic C a r b o n N o r m a l iz e d A d s o r p t io n C o e f f ic ie n t , K o C, L /g 70.4 37.4 126 57.1 NA Table 3. Summary Table of PFOS Adsorb/Desorb Tier HI Studies Soil Type Sandy Loam Desorption Coefficient, Kdes> ml/g 0.0349 K adSp. 0.0919 C lay L oam 0.0158 0.0421 C lay 0.0471 0.0560 R iv er S edim ent 0.0100 0.0094 D om estic Sludge < 0.237 0.0568 Introduction R desp 0.104 0.082 0.222 0.039 29.5 P o t a s s iu m P e r f l u o r o o c t a n e s u l f o n a t e (PFOS) CAS Number: 2795-39-3 Chemical Formula: C8F17SO3K 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 infonnation on the environmental relevance of the adsorption of a chemical.! OECD guideline 106 is aimed at estimating the adsorption/desorption 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 soihaqueous 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 II: 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 K j and Koc 1.2.2 The preparatory methodology for Tier II is described in the 3M Environmental Laboratory Method ETS-8-160: Preparation of Soil Samples for Screening (Tier II) and Advanced (Tier III) Sorption Studies for Fluorochemicals as the Test Substance (based on OECD Guideline 106). 1.3 Tier III: 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 1 According to OECD Guideline 106 3M Environmental Laboratory Page 9 of 703 BACK TO MAIN and sludge. b) study desorption by means of determining desorption kinetics/Freundlich desorption isotherms 1.3.2 The preparatory methodology for Tier III is described in the 3M Environmental Laboratory Method ETS-8-160: Preparation of Soil Samples for Screening (Tier II) and Advanced (Tier III) 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 Source Expiration Date Storage Conditions TCR Identification Number Physical Description Purity PFOS 3M Specialty Chemicals, Bldg. 2361B-10 8/31/2001 Frozen TCR-00017-046 White Powder 97.9% THPFOS SynQuest Labs none Frozen TCR-00017-047 White Powder TBD Solvent PFO S Solubility ASTM Type I W ater N atural Seaw ater A queous Solution o f 3.5 % Sodium C hloride (Corrected for Purity) 680 ug/mL * 12.7 ug/mL ** 20.2 ug/mL ** n-O ctanol 56.0 ug/mL *** * As reported by 3MEnvironmental Laboratory Report UE00-1716 Phase: Solubility o f PFOS in Water, ** Phase: Solubility o f PFOS in Natural Seawater and an Aqueous Solution o f 3.5% Sodium Chloride, and * * * Phase: Solubility o f PFOS in n-Octanol. All solubility determinations ofPFOS TCR-00017-046 were conducted at 22-25C. For PFOS stability information refer to 3M Environmental Laboratory report W-1878 (PFOS hydrolysis study). 3M Environmental Laboratory Page 10 of 703 BACK TO MAIN Soil T ype C lay Source Expiration Date Storage Conditions Chemical Lot Number Physical Description % Organic Carbon % Sand % Silt % Clay Agvise 12/31/2015 Room Temperature 00-2407 Dried and sieved 2.6% 16% 22% 62% Barnes Loam Agvise 12/31/2015 Room Temperature 00-2404 Dried and sieved 4.9% 39% 50% 11% C lay L oam Agvise 12/31/2015 Room Temperature 00-2405 Dried and sieved 2.6% 21% 46% 33% Sandy Loam Agvise 8/1/2015 Room Temperature 99-2564 Dried and sieved 2.8% 58% 22% 20% R iver Sedim ent Agvise 12/31/2015 Room Temperature 00-2046 Dried and sieved 1.3% 39% 42% 19% D om estic S lu d g e NIST 10/31/2005 Room Temperature 2781 Dried and sieved N/A N/A N/A N/A Method Summaries ETS-8-159 "Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicals as the Test Substance" Suitable Analytical Method: A soil of high adsorbability (high organic carbon and clay content) is agitated with an appropriate volume of 0.01 M CaCl2 solution at a 1:5 (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 500mg/L PFOS in a 10ml 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 HPLC/MS. 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. Suitable (Minimally Adsorbing) Container Up to five containers comprising a variety of materials are exposed to a 0.01 M CaCl2 aqueous solution dosed with the test substance at a concentration of O.lOmg/L and l.Omg/L for a minimum of 24 hours. The resulting solution is analyzed for the test substance using HPLC/MS. 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. 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 500mg/L PFOS to a concentration of 5.0mg/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 soilsolution ratio 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 II) and Advanced (Tier III) Sorption Studies for Fluorochemicals as the Test Substance" Tier II: 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 CaCl2- 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 III: 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 CaCl2 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. Tier III: 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 CaCl2 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. Tier III: 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 CaCl2 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 III: 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 Population 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 II "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 Total 45 Selected for LRN-E00-1311 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 spikes 144 + 48 Matrix Spikes 36 + 12 matrix spikes 15 18 + 6 Matrix Spikes 9 + 3 matrix spikes 60 + 16 Matrix Spikes 29 + 8 matrix spikes 171 + 57 Matrix Spikes 63 + 21 matrix spikes 139 + 48 Matrix Spikes 36+12 matrix spikes 3M Environmental Laboratory Page 13 of 703 BACK TO MAIN Tier III "Desorption Kinetics" Tier III "Adsorption Isotherms" Tier III "Desorption Isotherms" Tier III "Mass Balance" Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks Test Substance Solutions Control Blanks 126 + 42 Matrix Spikes 126 + 42 Matrix Spikes 180 + 60 Matrix Spikes 36+ 12 matrix spikes 90 + 30 Matrix Spikes 18 + 6 matrix spikes 90 + 30 Matrix Spikes 18 + 6 matrix spikes 115 + 42 Matrix Spikes 126 + 42 Matrix 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 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 Step Tier I "Suitable Analytical Work" Tier I "Suitable Container" Tier I "Suitable Desorption Solvent" Procedure Each of tire three soils, the sediment, and the sludge are equilibrated with 0.01M CaCl2in 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. R ep lica tes Each "matrix 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. Date(s) Performed Samples aliquotted 11/02/00 Aqueous samples aliquotted 11/14/00 Methanol extractions aliquotted 11/15/00 Methanol extractions aliquotted 1/22/01 3M Environmental Laboratory Page 14 of 703 BACK TO MAIN Tier I "Selection of Optimal Soil: Solution Ratios and Mass Balance" Tier II "Adsorption Kinetics" Tier III "Desorption Kinetics" Tier III "Adsorption Isotherms" Tier III "Desorption Isotherms" Tier III "Mass Balance Determination Two types of soil are prepared in three soil:solution ratios to determine the optimal ratio to use in the remainder of the study. Samples are 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 soiksolution ratio 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 CaCh 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 soiksolution ratio indicated in the Tier I study. The samples are dosed with 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 CaCl2solution 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 portions of methanol, each time the solution is decanted into the same vessel. Each soil/ratio/time combination is prepared in triplicate, one matrix spike is performed, and one control is prepared. Each soil/time 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 spikes). Each soil/concentration/time 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 matrix spike. Aqueous samples aliquotted 11/29/00- 12/4/00 Methanol extractions aliquotted 12/7/00 Aqueous samples aliquotted 2/1/01- 2/7/01 Aqueous samples aliquotted 2/13/01- 2/15/01 Aqueous samples aliquotted 2/14/01- 2/15/01 Aqueous samples aliquotted 2/21/01 Methanol extractions aliquotted 2/22/01- 2/26/01 Diluted samples (i.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 (r^). The coefficients of determination (r^) 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 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 1000 ng 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 Soil Type lia rn e s L oam (ST-1) C lay L oam (ST-2) C lay (ST-3) Soil/O.OIM C aC i.2 Solution ID E 00-1311-0001, -0002, -0003 E 00-1311-0004, -0005, -0006 E 00-1311 -0007, -0008, -0009 Average Recovery of PFO S from m atrix solution, % 115% 115% 99.8% R iver S edim ent (ST-Sed) D om estic S lu d g e (ST-SIg) E 00-1311-0010, -0011,-0012 E 00-1311-0013, -0014, -0015 116% 88.3% % RSD 7.51 4.92 21.81 8.88 15.97 Table 8. Suitable Test Vessel Determination Centrifuge Tube Type P olypropylene P o ly sty re n e G lass A verage Recovery o f 1.0mg/L PFO S After Adsorb Step, % 96.19% 94.51% 96.74% Average Concentration o f PFO S Extracted From Test Vessels D u rin g D e so rb S tep , PPB 244.36ppb 172.43ppb 397.75ppb A v e r a g e M a t r ix S pik e R ecovery for A dsorb and D esorb Steps, % 116.18% 203.04% 206.69% T eflo n 89.49% 94.37ppb 176.45% 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 ofPFOS Soil Type Soil:Solution Ratio Tim e Point, Hours C lay S edim ent l:l 1:5 1:25 1:1 1:5 1:25 24 36 48 24 36 48 24 36 48 24 36 48 24 36 48 24 36 48 A verage Recovery of PFOS (in so l u t io n )% 17.64% 20.98% 12.74% 21.58% 23.51% 19.71% 57.42% 60.15% 66.80% 11.04% 14.32% 10.63% 45.85% 45.01% 42.19% 65.34% 67.31% 68.00% Adsorption Equilibrium Plot ---- 1:1 Ratio (clay) --* -- 1:5 R atio (clay) - A - - 1:25 Ratio (clay)j 3M Environmental Laboratory Page 18 of 703 BACK TO MAIN Adsorption Equilibrium Plot 1:1 Ratio (Sediment) 1:5 Ratio (sediment) 1:25 Ratio (sediment) |! The test substance appeared to reach equilibrium after 24 hours in all of the soilsolution 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 Soil Type C lay S edim ent Theoretical Test Substance Concentration In Extract, ug/L 0.0 100 1000 0.0 100 1000 Average Recovery, ug/L A verage R ecovery o f PFOS% < 25.0 71.2 591 < 2 5 .0 96.0 601 N/A 71.2% 59.1% N /A 96.0% 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 soiksolution 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 Environmental Laboratory Page 19 of 703 BACK TO MAIN Table 11. Stability of PFOS during the Study Period Soil Type C lay Sedim ent SoihSolution Ratio, Tim e P o in t 1:1 1:5 1:25 1:1 1:5 1:25 T im e Point, hours 48 48 48 48 48 48 48 48 48 48 48 48 48 48 48 48 48 48 Total Recovery of PFOS% 4 6 .1 6 53.15 7 1 .3 3 3 4 .2 8 3 5 .6 2 T ube B roke 83.21 9 1 .2 4 9 6 .2 7 4 3 .6 8 4 8 .1 2 2 4 .6 6 5 7 .6 3 7 8 .6 7 5 9 .5 2 7 3 .6 4 87.35 8 3 .0 5 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 II study are presented in Table 12: Table 12. Adsorption Kinetics o f PFOS, 1:5 SoihSolution Ratio, 48 H our Tim e Point Soil Type C lay (ST-1) C lay L oam (ST-2) S an d y L oam (ST-3) A verage Distribution Coefficient, Kq, L/g 0.0183 0.00972 0.0353 Percentage of O rganic C arbon in Soil, % oc 2.6 2.6 2.8 A v e r a g e O r g a n ic C a r b o n N o r m a l iz e d A d s o r p t io n C o e f f i c i e n t , Kq , L /g 70.4 37.4 126 R iv er S ed im en t (ST-Sed) 0.00742 1.3 57.1 D om estic S lu d g e (ST-SIg) < 0.120 NA NA 3M Environmental Laboratory Page 20 of 703 BACK TO MAIN 100 90 80 S? 70 60 1 50 S 40 < 30 20 10 0 0 Adsorption Percentage as a Function of Time 10 20 30 40 Time, hours ---- Clay -- --Clay Laom A -Sandy Loam X River Sediment 50 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 III study are presented in Tables 13 through 15: Table 13. Desorption Kinetics of PFOS, 1:5 Soil:Solution Ratio, 48 hour Time Point Soil Type B arnes L oam (ST-1) C lay L oam (ST-2) C lay (ST-3) Desorption Coefficient, K des' m l/g 0.0471 0.0158 0.0349 R iver S edim ent (ST-Sed) D om estic Sludge (ST-SIg) 0.0100 < 0.237 3M Environmental Laboratory Page 21 of 703 BACK TO MAIN Desorption Percentage as a Function of Time Clay -- -- Clay Loam --A-- Sandy Loam --- X -- River Sediment 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 Soil Type L o g K a(fSp C lay C lay L oam Sandy Loam ! R iver Sedim ent D om estic Sludge -1.2515 -1.3762 -1.0369 -2.0261 -1.246 KadsF 0.0560 0.0421 0.0919 0.0094 0.0568 Regression Constant, 1/n 0.884 0.841 0.829 0.989 1.2581 R egression C onstant, n 1.13 1.19 1.21 1.01 0.795 3M Environmental Laboratory Page 22 of 703 BACK TO MAIN Table 15. Desorption Isotherms Soil Type Log Kdesp C lay C lay L oam Sandy Loam -0.653 -1.084 -0.981 K desp 0.222 0.082 0.104 Regression Constant, 1/n 0.935 0.954 1.01 Regression C onstant, n 1.07 1.05 0.988 R iver Sedim ent D om estic Sludge -1.41 1.47 0.039 29.5 1.02 0.327 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 non linear. 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 Signatures The final draft of this report is a true representation of the data developed in this study. It has been issued by: 3M Environmental Laboratory Page 24 of 703 Appendix A: Study Protocol E00-1311- Soil Adsorption/Desorption Study of Potassium Perfluorooctanesulfonate BACK TO MAIN 3M Environmental Laboratory Page 25 of 703 BACK TO Laboratory Request Number (LRN)--E00-1311 3M STUDY PROTOCOL STUDY TITLE Soil Adsorption/Desorption Study 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 R equest N um ber (L R N )-- E 0 0 -1 3 1 1 3M Environmental Laboratory 3M Environmental Laboratory Page 1 of 19 Page 26 of 703 BACK TO MAIN Laboratory Request Number (LRN)--E00-1311 Protocol Signatures Study Director: Mark E. Ellefson 3M Environmental Laboratory Protocol Approval Sponsor: William K. Reagen, Ph.D. 3M Environmental Laboratory ____________So//?ypo Date: 3M Environmental Laboratory ^^^nvirnmnfT^^mlry Page 2 of 19 Page 27 of 703 BACK TO MAIN Laboratory Request Number (LRN)--E00-1311 STUDY IDENTIFICATION Soil Adsorption/Desorption Study of Perfluorooctanesulfonate (PFOS) Te s t S u b sta n c e Sponsor S p o n s o r R e p r e s e n t a t iv e S t u d y D ir e c t o r Te s t F a c il it y P r o p o s e d S t u d y Tim e t a b l e 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 55106 (651)778-6565 Mark E. Ellefson 3M Environmental Laboratory 935 Bush Avenue, Building 2-3E-09 St. Paul, MN 55106 (651)778-5405 3MEnvironmental Laboratory 935 Bush Avenue, Building 2-3E-09 St. Paul, MN 55106 Experimental Start Date Experimental Termination Date 18 October 2000 15 December 2000 3M Environmental Laboratory 7$!TinvronmemT^ Page 3 of 19 Page 28 of 703 BACK TO MAIN Laboratory Request Number (LRN)--E00-1311 1.0 Introduction and Purpose/Objective 1.1 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; leaching through the soil profile; volatility from soil; and run-off from land surfaces into natural waters. Adsorption data can also be used for comparative and modeling purposes.1 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 1.2 The target substance for this study is presented in Table 1.1 Table 1.1 Target Substance Target Substance Perfluorooctanesulfonate Acronym and Structure PFOS C8 F17SO3 3M Environmental Laboratory Identification Number TCR-00017-46 2.0 Regulatory Compliance_______________________ 2.1 By complying with the requirements of OECD/OCDE 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 40 CFR Part 792. According to OECD Guideline 106 3M Environmental Laboratory 3M Environmental Laboratory Page 4 of 19 Page 29 of 703 BACK TO MAIN Laboratory Request Number (LRN)--E00-13111 3.0 Test Substance 3.1 Iden tification : Perfluorooctanesulfonate, C8F17SO3' (PFOS) 3.2 Source: 3M Specialty Materials Division 3.3 D escrip tio n : white powder 3.4 3 M E n viro n m en ta l L a b o ra to ry ID # : TCR-00017-46 3.5 Storage C onditions: PFOS should be stored at ambient temperature or lower. 3.6 P u rity: 97.3% 3.7 E xpira tio n D a te : 2010 3.8 R etention Sam ple: A retention sample of the test substance (0.34 g) has been taken and stored frozen at -20C 5C. The sample will be archived for at least the period as required by the EPA GLPs, Section 792.195. 3.9 S a fety P re c a u tio n s: 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 Identification: 1H, 1H, 2H, 2H-Perfluorooctane Sulphonic Acid, CgHsFnOsS (THPFOS) 5.1.2 Source: SynQuest Labs 5.1.3 D escription : Fluffy, white crystals 5.1.4 3 M E n viro n m en ta l L abora to ry ID # : TCR-00017-047 5.1.5 Storage C onditions: THPFOS should be stored at ambient temperature or lower 5.1.6 5.1.7 E xp ira tio n D a te : 2010 R etention S am ple: A retention sample of 0.27 g of THPFOS has been taken and stored frozen at -20C5C. The compound will be archived for at least the period as required by the EPA GLPs, Section 792.195. 5.1.8 S a fety P re c a u tio n s'. 3M Environmental Laboratory Page 5 of 19 3M Environmental Laboratory Page 30 of 703 BACK TO MAIN 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 using the 3M Environmental Lotus Notes TCR database. 5.2 PFOS 5.2.1 Id en tifica tio n : Perfluorooctanesulfonate, Q F 17S O 3 "(P F O S ) 5.2.2 Source: 3M Specialty Materials Division 5.2.3 D escrip tio n : White powder 5.2.4 3 M E n viro n m en ta l L abora to ry ID # : TCR-00017-46 5.2.5 Storage C onditions: PFOS should be stored at ambient temperature or lower 5.2.6 P urity: 97.3% 5.2.7 E xp ira tio n D a te : 2010 5.2.8 R etention S am ple: A retention sample of 0.34 g PFOS has been taken and stored frozen at -20C 5C. The compound will be archived for at least the period as required by the EPA GLPs, Section 792.195. 5.2.9 S afety P re c a u tio n s: 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 CaCl2 aqueous solution. 6.2 TGhueidcerliitneersia1f0o6r.selection of the soils are based on Table 1 of the OECD 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 adsorption/desorption 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 3M Environmental Laboratory Page 6 of 19 3M Environmental Laboratory Page 31 of 703 BACK TO MAIN Laboratory Request Number (LRN)--E00-1311 in order to cover as widely as possible 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, 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 vessels c) the equilibration time for adsorption and the amount of test substance adsorbed at equilibrium d) a suitable desorption solvent e) the soihaqueous 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: P reparation o f Soil Sam ples fo r Prelim inary (Tier I) Sorption Studies fo r F luorochem icals as the T est Substance (based on OECD Guideline 106). 7.1.2 Tier II 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 sin gle concentration b) determination of distribution coefficients Kj and KoC 7.1.2.2 The preparatory methodology for Tier II is described in the 3M Environmental Laboratory Method ETS-8-160: P reparation o f Soil Sam ples fo r Screening (Tier II) and A dvanced (Tier III) Sorption S tu dies f o r F luorochem icals a s the T est Substance (based on OECD Guideline 106). 7.1.3 Tier III: 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 EnvironrnenfeTLaboratory Page 32 of 703 BACK TO MAIN Laboratory Request Number (LRN)--E00-1311 adsorption onto the soils, sediment and sludge. b) study desorption by means of determining desorption kinetics/Freundlich desorption isotherms 7.1.3.2 The preparatory methodology for Tier HI is described in the 3M Environmental Laboratory Method ETS-8-160: P reparation o f Soil Sam ples fo r Screening (Tier II) and A dvanced (Tier III) Sorption Studies f o r F luorochem icals a s the T est Substance (based on OECD Guideline 106). 7.2 The adsorption/desorption studies will be conducted according to a modified version of the OECD Guideline for the Testing of Chemicals 106 "Adsorption Desorption 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 II and III. The study plan outlined for Tier I is an attempt to meet these criteria. The procedures used in the 3M Environmental Laboratory for Tier n and Tier IE will 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 E more than one aliquot is taken from a study sample during the course of a section, a designator of SI, S2, S3, etc. will be included to uniquely identify that aliquot. 3M Environmental Laboratory . Page 8 of 19 3M Environmental Laboratory Page 33 of 703 BACK TO MAIN Laboratory Request Num ber (LR N)-- 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 of the SI, 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 l, Prelim inary Study This section details the general methodology used to determine the 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 1:1 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-8-110 for the analytical methodology. 8.2.3 Acceptable analytical method performance criteria is identified in 3M Environmental Laboratory 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 Environmental Laboratory Method ETS-8-154. 8.3 Suitable Container: 8.3.1 A minimally adsorbing container for the test substance is desirable for Tiers II and III of 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 II and III is the most suitable container of those tested. 3M Environmental Laboratory 3M Environmental Laboratory Page 9 of 19 Page 34 of 703 BACK TO MAIN Laboratory Request Num ber (LR N)-- E00-1311 8.3.2 Test a reasonable variety of materials/containers. They may include, but are not limited to, the following: Teflon centrifuge tubes, Pyrex glass 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 mg/L). 8.3.4 Equilibrate 12.5 mL of a 0.01 M CaCl2aqueous solution containing the test substance (at concentrations of 0.1 mg/L and 1 mg/L) for approximately 24 hours with the container. After that time, dilute a portion of the aqueous solution with methanol and analyze using HPLC/MS/MS 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 II and HI. 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 Soil: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 soiksolution 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 Page 10 of 19 ^J^FnvImnmenfa Page 35 of 703 BACK TO MAIN Laboratory Request Num ber (LR N)-- O-1311 1 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 containing test substance 8.5.2 Dose the test substance such that the final concentration of test substance in solution is approximately 1 mg/L. 8.5.3 Prepare control samples containing only the test substance in 0.01 M CaCl2solution (no soil) in order to check the stability of the test substance in the 0.01M CaCl2solution. 8.5.4 Prepare background control samples containing soil and aqueous 0.01M CaCl2(no test substance) using the same soiksolution 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 additional test substance in 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 K<j value at equilibrium. Based on this Kdvalue, select appropriate soiksolution 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 II 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 CaCl2solution (no soil) in order to check the stability of the test substance in 0.01M CaCl2solution. 8.6.2 Include background control samples containing soil and aqueous 0.01M CaCl2(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. 3M Environmental Laboratory P a g e 11 of 19 Page 36 of 703 BACK TO MAIN Laboratory Request Num ber (LRN)-- E00-1311 | 8.6.4 Select three soil types using the guidance given in Table I of OECD method 106, one sediment and one dried sludge. 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. S ectio n C : T ie r 111 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 CaCb 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 CaCl2(no test substance) in the same soil-.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 mg/L for each of the selected three soil types, sediment and sludge. Use the 3M Environmental Laboratory Page 12 of 19 3M Environmental Laboratory Page 37 of 703 BACK TO MAIN Laboratory Request Num ber (LRN)-- E00-1311 same soiksolution ratio as that used in the Tier n study. (If the amount o f adsorption o f the test substance onto the soils w ill produce concentrations in the adsorption solvent which w ould b o rd er on, o r be below, the quantification limits o f the test substance, the concentration levels m ay need to be increased. The criteria that should be m et are that the concentration range should span two orders o f 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 CaCb 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 Perfluorooctanesulfonate or Other Fluorochemicals in Water Extracts Using HPLC-Electrospray/Mass Spectrometry/Mass Spectrometry 9.2 Additional methods may be developed at a later time and will be listed as protocol amendments. 3M Environmental Laboratory ^^^nvm nrnem aT^Erlfy Page 13 of 19 Page 38 of 703 BACK TO MAIN Laboratory Request Num ber (LR N)-- E00-1311 10.0 Data Quality Objectives___________________ 10.1 T ier l on ly--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 soil:solution ratio. Tier I is also for range-finding in order to successfully proceed to Tiers II and III of the adsorption/desorption study. 10.2 L in earity--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 L im its o f D etection /Q u an titation --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 M a trix S pike F req u en cy--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 A ccep ta b le R ecoveries--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 U se o f R e fe re n c e M a teria ls-- 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 50% deviation in standards and calibration checks. THPFOS is not used for quantitative purposes because the magnitude of rt heesproens pseo nms eaya mnootnbgeacos innsgisletegnrtobueptwi seeenx psetcatneddartodsbaencdo nsas mis tpelnets., TaHlthPoFuOgSh 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 o f C on firm atory M eth ods--No confirmatory methods will be used. The analytical method uses a very selective detector (mass spectrometer) with a chromatographic separation method. 3M Environmental Laboratory Page 14 of 19 3M Environmental Laboratory Page 39 of 703 BACK TO MAIN Laboratory Request Num ber (LRN)-- E 00-1311 10.8 D em o n stra tio n o f S p ecificity-- 10.8.1 HPLC/MS/MS--Unique and characteristic product ions are monitored for each analyte. In addition, a chromatographic separation method is employed. 10.9 P recisio n -- 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 Q uality C on trol B lan ks--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. 10.11 L aboratory C ontrols--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. 11.0 Subcontracted Analysis 11.1 Not Applicable. 12.0 Statistical Methods and Calculations 12.1 mSteaatinsst,icsatlanmdeatrhdoddesvfioartitohnesa, nreallayttiivcealsrtaesnudlatsrdwdiellvbiaetiloimnsi,teadndtoptehrececnatlcruelcaotvioenriseos f (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 Laboratory Request Num ber (LR N)-- E0 0 -1 3 1 1 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 performing the 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. 12.4.10A 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. 12.4.11 Statistical methods used to evaluate the data, if applicable. 12.4.12The 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 Environmental Laboratory Quality Assurance Unit will audit this protocol, the study conduct, and the final report in accordance with GLP regulations and 3M Environmental Laboratory standard operating procedures. 3M Environmental Laboratory Page 16 of 19 3M Environmental Laboratory Page 41 of 703 BACK TO MAIN Laboratory Request Num ber (LR N)-- E 00 -1 3 1 11 14.0 Location of Raw Data, Records, and Final Report_____________ _ 14.1 Original data or copies thereof, will be available at 3M Environmental Laboratory. When the final report is completed (Tiers II and III), all original paper data, including those items listed below, will be retained in the archives of 3M Environmental Laboratory 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 LC/MS 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 II and Tier III study 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 II and Tier HI 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 Page 17 of 19 ^M Tinvironm er^ Page 42 of 703 BACK TO MAIN Laboratory Request Num ber (LRN)-- E00-1311 16.0 Protocol Amendments and Deviations__________ 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-Desorption Using a Batch Equilibrium Method," OECD Guideline 106 Adopted 21 January 2000 17.2 United States Environmental Protection Agency. OPPTS 835.1220 Sediment and Soil Adsorption/Desorption 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 835.1110 Activated Sludge Sorption Isotherm. Prevention, Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-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 II and Tier III) Sorption Studies for Fluorochemicals as the Test Substance 17.6 3M Environmental Laboratory Method ETS-8-110: Analysis of Perfluorooctanesulfonate or Other Fluorochemicals in Water Extracts Using HPLC-Electrospray/Mass Spectrometry/Mass 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 High Performance Liquid Chromatography/Tandem Mass Spectrometry (HPLC/MS/MS) 18.0 Attachments 18.1 A tta ch m en t A : Eample Numbering Scheme 3M Environmental Laboratory Page 18 of 19 3M Environmental Laboratory Page 43 of 703 BACK TO MAIN - + ,, , *' __________________ ____________ ______________ __________________________ _ _ _ ___________________________________________ Laboratory R eq u est N u m b e r (L R N )-- E O O -1311 Attachment A: E xam ple N um bering S chem e Matrix Solutions E00-1311-0001 EOO-1311-0002 EOO-1311-0003 Analytical Samples made from Matrix Solutions E00-1311-0004 E00-1311-0005 E00-1311-0006 Suitable Container E00-1311-1016 -- E00-1311-1017 -- E00-1311-1018 -- E00-1311-1018 MS SI SI SI SI S2 S2 S2 S2 Suitable Desorption Solvent EOO-1311-201O -- SI E00-1311-2011 -- SI E00-1311-2012 -- SI E00-1311-2012 MS SI Optimal Ratio EOO-1311-3094 -- SI EOO-1311-3095 -- SI E00-1311-3096 -- SI EOO-1311-3096 MS SI Optimal Ratio-Mass Balance E00-1311-3094 -- S2 E00-1311-3095 -- S2 E00-1311-3096 -- S2 E00-1311-3096 MS S2 Adsorption Kinetics-One Concentration E00-1311-4031 -- SI E00-1311-4032 -- SI EOO-1311-4033 -- SI EOO-1311-4033 MS SI Desorption Kinetics-One Concentration EOO-1311-4031 -- S2 S3 S4 S5 S6 S7 S8 E00-1311-4032 -- S2 S3 S4 S5 S6 S7 S8 E00-1311-4033 -- S2 S3 S4 S5 S6 S7 S8 E00-1311-4033 MS S2 S3 S4 S5 S6 S7 S8 Adsorption Isotherms-Multiple concentrations EOO-1311-5058 -- SI EOO-1311-5059 -- SI EOO-1311-5060 -- SI E00-1311-5060 MS SI Desorption Isotherms-Multiple concentrations E00-1311-5058 -- S2 S3 EOO-1311-5059 -- S2 S3 E00-1311-5060 -- S2 S3 E00-1311-5060 MS S2 S3 3M Environmental Laboratory Page 19 of 19 Attachment A: Example Numbering Scheme___________________________________________ 3M Environmental Laboratory Page 44 of 703 BACK TO MAIN Study Title Soil Adsorption/Desorption Study of Perfluorooctanesulfonate (PFOS) - Test Control Reference #TCR-00017-46 PROTOCOL AMENDMENT NO. 1 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 Environmental Laboratory Study LIMS #E00-1311 3M Environmental Laboratory 3M Environmental Laboratory Page 45 of 703 BACK TO MAIN Protocol #E00-1311 Amendment 1 This amendment modifies the following portion(s) of the protocol: 1. Protocol reads: Section 8.2.1: Previous work with the test substance in a variety of matrices have strongly 1 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. Amend to 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 1:1 ratio. Reason: Some of the samples in this study were diluted at a level other than 1:1. 2. P rotocol reads: Section 8.2.1: The resulting aliquot can then be analyzed using HPLC/MS/MS. Amend to read: The resulting aliquot can then be analyzed using HPLC/MS. R e a s o n : 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 R eads: Section 8.4.2: Dose the test substance (at 2ug and 20ug) onto 2.5 grams of a strongly adsorbing (high clay content) soil. Amend to Read: Dose the test substance (at 0.75ug and 7.5ug) onto 2.5 grams of a strongly adsorbing (high clay content) soil. Reason: The test substance concentrations were modified to more closely resemble the concentrations used in the rest of the study. 4. PROTOCOL Reads: Section 8.4.5 If this process cannot recover 80% or more of the test substance, investigate a m in im u m o f th re e o th er solvents. Amend to 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 Soil: 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 #E00-1311 Amendment 1 5. Protocol Reads: Section 8.5.2 Dose the test substance such that the final concentration o f test substance is approximately Img/L. Amend to Read: Dose the test substance such that the final concentration of test substance is approximately { 5mg/L. Reason: The test substance showed strong adsorption in earlier portions of the study, and it was necessary to increase the concentration. 6. Protocol Reads: Section 9.2 Additional methods may be developed at a later time and will be listed as protocol amendments. Amend TO Read: ETS-8-155. Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Wastestream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry. Reason: This method was also used in the analysis of the study samples. 7. Protocol Reads: Section 10.5 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 30% of the theoretical value. Reason: Acceptable criteria were decided upon after the signing of the protocol. 8. Protocol Reads: Section 10.8.1 HPLC/MS/MS Amend to read: 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. 9. P rotocol Reads: Section 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 standards. Amend TO 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 Reason: Acceptable criteria were decided upon after the signing of the protocol. Protocol #E00-1311 Amendment 1 1 10. Protocol Reads: Section 12.2 Percent recoveries will be calculated using the following equation: [(AB)/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 Amend to 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. Reason: Clarification 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 R eads: Section 15.4 HPLC/MS/MS Amend to read: 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. 12. P rotocol Reads: Section 17,8 N/A (there was no previous section 17.8) Amend to Read: 3M Environmental Laboratory Method ETS-8-155: Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Wastestream or Water Extracts Using HPLCElectrospray/Mass Spectrometry. Reason: This method was not referenced in the protocol, but was used in the analysis of the study samples. 3M Environmental Laboratory 3M Environmental Laboratory Page 48 of 703 BACK TO MAIN Protocol #E00-1311 Amendment 1 Amendment Approval t 3M Environmental Laboratory 3M Environmental Laboratory Page 49 of 703 BACK TO MAIN Appendix B: Analytical Methods This appendix presents the analytical methods used in the present study: ETS-8-159 "Preparation o f Soil Samples for Preliminary (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 o f Water Extracts Using HPLC-Electrospray/Mass Spectrometry" ETS-8-110 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Water Extracts Using HPLC-Electrospray/Mass Spectrometry/Mass Spectrometry" 3M Environmental Laboratory Page 50 of 703 BACK TO MAIN 3M Environmental Laboratory M ethod Pr e p a r a t io n o f So il Sa m p l e s f o r Pr e l im in a r y (T ie r I ) So r p t io n St u d ie s f o r F l u o r o c h e m ic a l s a s t h e T e s t Su b s t a n c e (B ased o n OECD G u id e l in e 106) M eth o d N u m b er: ETS-8-159.0 Author: Linda Goodspeed, Cindy Carlson, MarkEllefson Adoption Date: R evision Date: Date 3M Environmental Laboratory ETS-8-159.0 Tier I Sorption Studies Page 1 of 13 Page 51 of 703 BACK TO MAIN 1.0 TH t 1.2 1.3 1.4 1.5 1.6 1.7 1.8 Sc o pe an d A pplicatio n By complying with the requirements of the OECD Guideline 106, "Adsorption Desorption Using A Batch EquilibriumMethod", the data will meet the testing requirements of the European Community and Canada. This method complies with OPPTS 835.1220 "Sediment and Soil Adsorb/Desorb 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. 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 III) portions of the Sorption Studies. This method is based on the "Preliminary" subsection of OECD Guideline 106: "Adsorption - Desorption Using A Batch EquilibriumMethod". 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 soihaqueous ratio 1.5.6 the stability of the test substance during the study period In addition, this internal 3M method (ETS-8-159) will address determination of an approximation of the statistical variance of precision and accuracy data that may be expected from the continuation of the procedure to the screening and advanced tiers of OECD Guideline 106. 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. 2.0 S u m m a r y o f M ethod 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 CaCU solution at a 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 HPLC/MS. 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 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 HPLC/MS. 2.2.2 If the extraction results in a total of >80% desorption, no further testing of solvents is necessary. Otherwise, up to three other solvents will be investigated in a similar manner until the criteria (>80% desorption) are met. 2.2.3 If the criteria are not met, the most suitable solvent among those tested will be chosen. 2.3 Suitable (Minimally Adsorbing) Container 2.3.1 Up to five containers comprising a variety of materials are exposed to a 0.01 M CalCh 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 fromthose tested. 2.4 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 optim al 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 soil:solution ratio per soil that gives a depletion of the test chemical above 20% and preferably above 50% at equilibrium. 2.5 In all cases, adequate quality assurance samples are prepared and analyzed. 3.0 D efin itio n s 3.1 Test Substance: Any substance (mixture or controlled compound) added or administered to the test system for the purpose of biological or chemical measurements. 3.2 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 aby-product of that chemical. 3.3 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 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 fromthe 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. 4.0 W a r n in g s a n d C au tio ns 4.1 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. 4.2 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 fluorochemicals from the glassware. Clean all spills immediately to avoid present or future contam ination. 4.2.2 Use disposable glassware whenever possible. 5.0 In ter fer en c es . 5.1 Any compound that co-elutes with the test substance or the reference material during the HPLC/MS analysis can interfere with quantification. 6.0 E q u ipm en t 6.1 Balance capable of weighing to 0.1 mg, such as OHAUS Brand Model GA200 6.2 Centrifuge capable of maintaining 4,000 200 rpm, such as Jouan Brand Model C412 6.3 Orbital shaker capable of a gentle rotation and temperature controlled capable of maintaining 23 3 C, such as Lab-Line Model Environ-Shaker 6.4 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 S u ppl ie s a n d M a t er ia ls 7J 15-mL polypropylene centrifuge tubes, such as VWRbrand Centrifuge Tubes, catalog number 21008-089 7.2 15-mL polystyrene centrifuge tubes such as VWRbrand Centrifuge Tubes, catalog number 21008-202 7.3 15-mL styrene butadiene centrifuge tubes such as VWRbrand 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 VWRbrand 20171 7.7 Syringes, 10 uL, 25 uL, 1000 uL 7.8 Volumetric flasks, 10-mL, 100-mL, 1-L, 5-L, Nalgene and/or glass 7.9 Automatic or manual dispenser, capable of dispensing liquid with 0.1 mL accuracy 7 .10 250-1000 uL 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 # 224211-01 7.13 GC/HPLC autovial crimper(s) and decrimper(s) 7 .14 Appropriately sized storage containers with tight-fitting caps for solutions 7 .15 Glassware, miscellaneous 7 .16 150-mL Nalgene bottles or equivalent 7 .17 pH paper capable of distinguishing pH to 0.5 units. 8.0 R e a g e n t s, S o lu t io n s a n d Sta nd ar ds 8.1 Reagents 8.1.1 Methanol, HPLC grade, such as J.T. Baker #9093. 8.1.2 ASTM Type I water, 18.0 MQ or better. 8.1.3 CaCL, Anhydrous, to meet ACS specifications (>96% pure), such as J.T. Baker #1311. 8 .1 .4 Soils: Appropriate soil types selected from Table 1below. (Soils should be airdried at ambient temperature and sieved to a particle size <2 mm.) Table 1 Soil Types 1 pH range (in 0.01 M CaCI2) 4.5-5.5 Organic Carbon content (%) 1.0-2.0 Clay Content (%) 65-80 Soil Texture Clay 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 Loamy sand 6 >7.0 <0.5-1.0 40-65 Clay loam/clay 7 <4.5 >10 <10 Sand/loamy sand NOTE: It may not be possible to obtain soils that match all criteria. Soi s will be used that match as closely as possible the parameters as listed. Exceptions will be noted. ETS-8-159.0 Tier I Sorption Studies Page 5 of 13 3M Environmental Laboratory Page 55 of 703 BACK TO MAIN 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 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 HPLC/MS 8.1.8 Reference Material: THPFOS, 1H, 1H, 2H, 2H- perfluorooctanesulfonic Acid 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 CaC^ Solution 5.550.02 grams of CaCl2dissolved 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 CaCl2Solution Dissolve 0.050 0.005 grams of test substance in 1.0 liter of 0.01 M CaCl2. Use volumetric flask and record weight. Immediately transfer into a Nalgene 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 and/or adsorption to the container. 9.0 S a m p l e H a n d l in g 9.1 All study samples generated andprepared for analysis by HPLC/MS 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 Q u a l i t y C o n t r o l 10.1 Matrix 10.1.1 Blanks 0.01 M cCoanCsiLstiinngc oonfttahcet fwoiltlhoweiancgh toyfptehse ws eillle bc tee dprseopial rteydp efos r the study: 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 CaCl2and 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 CaCl2only 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 C a l ib r a t io n a n d S ta n d a r d iza tio n 11.1 This section is outside the application of this method. " i 12.0 12.1 12.2 Procedures Labeling of Samples (Centrifuge Tubes) and Antovials--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 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 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 fromthe 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." Suitable Analytical Work 12.2.1 Each soil used in this study must be tested for the suitability of the proposed analytical work. Carry 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 CaC^ 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 aPurteopvaiarle. bPyraelpiqarueoottninegM1a.OtrOixmBLloanf kthfeoMr eaatcrhixMSoalturitxioSnodluirtieocntl.y into an 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. 12.2.11 Calculate 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 types/materials of centrifuge tubes to use in the study fromthe Supplies and Materials section of the method (up to 5). 12.3.2 Prepare 100 mL of each of the following solutions: 12.3.2.1 0.0 mg/L of test substance in 0.01 M CaCU (i.e., Solution A). 12.3.2.2 ~0.05 mg/L of test substance in 0.01 M CaCh. (Dilute 100 uL of Solution B to 100 mL with Solution A in a Nalgene volumetric flask.) 12.3.2.3 --0.50 mg/L of test substance in 0.01 M CaC^. (Dilute 1000 uL of Solution B to 100 mL with Solution A in aNalgene volumetric flask.) 12.3.3 Prepare Time "0 hr" samples: 12.3.3.1 Dispense l.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 Cone. Test Substance, mg/L 0.0 -0.05 -0.50 Solution 12.3.2.1 12.3.2.2 12.3.2.3 No. of tubes Cent. Tube, Type 1 3 3 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.OOmLof 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 centrifuge tube. 12.3.4.8 Transfer 1.0 mL 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 12.3.8 Choose the most appropriate container based on minimal adsorption as well as convenience and cost. 12.4 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 pg -10 pg Matrix Soil only Soil only Soil only pL of Stock Test Substance 0.0 20 200 Amount of Soil (grams) 2.50 0.05 2.50 0.05 2.50 0.05 # of Tubes # of Tubes with Soil with No Soil 33 33 33 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 andremove as much of the solvent layer as possible, without 12.4.11dPilsatcuerbthinegsothlveesnotlildasyelaryienrto. 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 l.OOmL of the study sample and dispense into a prelabeled autovial. 12.4.14Spiking: Referto section 12.6 for spiking. 12.4.15Add THPFOS internal standardprior 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. 12.4.18Ifthe total test substance recovery from the soil is >80%, no further testing of solvent is necessary. 12.4.19If the test substance recovery from the soil is <80%, 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 Selection of Optimal Soil: Solution Ratios 12.5.1 Select two soils fromthe 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 Cone. Test Substance, mg/L Soil: Solution Ratio Soil (grams) mL of 0.01 M CaCI2 Solution Number of Time Points No. of Tubes with No Soil (Control Sample) No. of Tubes with Soil Type 1 No. of Tubes with Soil Type 2 pL of 50 mg/L ' , Stock Test Substance* 0.0 NA 0.00 25.0 0.2 2 3x2 =6 NA NA 0.00 -0.5 NA 0.00 24.75 0.2 8 3 x 8 = 24 NA NA : ; r . 250* ( ' 0.0 1:1 5.00 0.05 5.0 0.1 2 NA 3x2=6 3 x2 = 6 0.00 0.0 1:5 2.50 0.05 12.5 0.1 2 NA 3 x2 = 6 3 x2 = 6 0.00 0.0 1:25 1.00 0.05 25.0 0.2 2 NA 3 x2 = 6 3 x2 = 6 0.00 -0.5 1:1 5.00 0.05 5.0 0.1 8 NA 3x8 = 24 3x8 = 24 . 50* -0.5 1:5 2.50 0.05 12.4 0.1 8 NA 3x8 = 3x8 = 24 24 125* -0.5 1:25 1.00 0.05 24.75 0.2 8 NA 3x8 = 24 *To be added in after the study sam ples have equilibrated for 12 hours. 3x8 = 24 250* 12.5.3 Document the pH of the stock test substance solution, using pH paper. Record to 0.5 pH units. 12.5.4 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 3 C using a gentle rotation. Record start and stop times/dates on appropriate data forms. 12.5.5 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). 12.5.6 For Time "0 hr" study samples only, gently mix and proceed directly to 12.5.10. 12.5.7 The rest of the study samples are then placed back on the orbital shaker 23 3 C using a gentle rotation. Record start times/dates 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. 12.5.1 lDocument the pH for one of each sample set per time point. Record to 0.5 pH units. 12.5.12 Withdraw l.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.) 12.5.20Centrifiige 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 l.OOmL of the study sample solution into the same 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 soil'.solution 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 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 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 D a t a A n a l y sis a n d C al c u la tio n s 13.1 Data analysis and calculations should be done using the templates provided from OECD Guideline 106. 14.0 M eth o d P er fo rm a n ce 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 cone, analytical - Sample cone, analytical) x 100 (MS Spike cone, 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 P o l l u t io n P r e v e n t io n a n d W aste M a n a g em en t 15.1 Dispose o f 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 R ec o r d s 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 A t t a c h m en ts 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 R e f e r e n c e s ETS-8-159.0 Tier I Sorption Studies page 12 of 13 3M Environmental Laboratory Page 62 of 703 BACK TO MAIN 18.1 I 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 Adsorption/Desorption Isotherm, EPA 712-C-98-048, January 1998. 19.0 A ffe c t ed D o c u m e n ts 19.1 ETS-8-160.0 Preparation of Soil Samples for Screening (Tier II) and Advanced (Tier III) Sorption Studies for Fluorochemicals as the Test Substance (Based on OECD Guideline 106). 20.0 R ev isio n s Revision Number. Reason For Revision Revision ' Date 3M Environmental Laboratory ETS-8-159.0 Tier I Sorption Studies Page 13 of 13 Page 63 of 703 BACK TO MAIN Sample ID Original Matrix Solution ;onc. of Test Substance 100 uL of Stock Test Substance Added I.OOmL of Study Sample Comments Sample ID Soil Type (High Slay/High %CC) Soil weight, jrams (20 g) 100 mL CaCI2 solution Equilibrate 4 lours (Yes/No) Comments Suitable Analytical ETS-8-159 Section 12.2 1 E00-xxxx-0001 E00-xxxx-0002 EOO-xxxx-0003 2 Col. 2 Soil ID #: 34 Col. 3 Col. 4 Col. 5 Col. 6 Balance ID ___________________________ T /D /l___________________ / _ _ _ _ / _____ 0.01 M CaCI2 Soin ID # :_______________ T /D /l___________________ / / ____ Inc. ID _______________________________ Start T /D /l___________________ /______ / Stop T /D /l___________________ / _ _ _ _ / T /D /l___________________ / _ _ _ / ____ Qc>n a 'o Bc ?Oa)i ub 56 1 E00-XXXX-0004 EOO-xxxx-0005 EOO-xxxx-0006 EOO-xxxx-0007 EOO-xxxx-0008 E O O -xxX X -0 009 EOO-xxxx-0010 E00-xxxx-0011 E00-xxxx-0012 E00-xxXX-0013 E00-XXXX-0014 E00-xxxx-0015 2 EOO-xxxx-0001 EOO-xxxx-0002 E 0 0 -x x x x '0 0 0 3 EOO-xxxx-0001 EOO-xxxx-0001 E O O -xxxx-O O 01 EOO-xxxx-0002 EOO-xxxx-0002 EOO-xxxx-0002 EOO-xxxx-0003 EOO-xxxx-0003 EOO-xxxx-0003 Col. 4 Test Substance = T/D/l Col. 5 Matrix Solution ID #: T/D/i Col. 6 T/D/l Internal Standard ID Number T/D/l 3 0.0 0.0 0.0 1 1 t 1 1 1 1 1 1 / / / / c2 .2 -J DE o ~ 'S* Xe TM 5 TtaJt> T<rJ .52C >O 45 M '-- --- / / / / 6 GLP Study Number: 3M Environmental Laboratory Test Substance: 7 7 Page 64 of 703 BACK TO MAIN Suitable Analytical ETS-8-159 Section 12.2 Test Substance: 5ample ID Soil Type Soil weight, jrams (20 g) 100 mL CaCI2 solution Squilibrate 4 lours (Yes/No) Centrifuge [Yes/No) Comments Sample ID Original Matrix Solution cone, of Test Substance 100 uL of Stock Test Substance Added 1.00 mL of Study Sample Comments 1 E00-xxxx-0016 E00-xxxx-0017 E00-xxxx-0018 2 3 456 Col. 2 Soil ID #: Col. 3 Col. 4 Col. 5 Col. 6 Balance ID ,___________________________ T /D /l___________________ / _ _ _ / _____ 0.01 M CaCI2 Soin ID # :___________ ____ T /D /l___________________ / _ _ _ / _____ Inc. ID _______________________________ Start T /D /l___________________/ _ _ _ / Stop T /D /l___________________ / _ _ _ / T /D /l___________________ /_ _ _ _ _ / cS .2 -1 5E o 1 E00-xxxx-0019 EOO-xxxx-0020 E00-xxxx-0021 E00-xxxx-0022 E00-xxxx-0023 EOO -x x x x - 0 0 2 4 EOO-xxxx-0025 EOO-xxxx-0026 E00-xxxx-0027 EOO-xxxx-0028 E00-xxxx-0029 EOO-xxxx-0030 2 EOO-xxxx-0001 EOO-xxxx-0002 EOO-xxxx-0003 EOO-xxxx-0001 EOO-xxxx-0001 E OO-xxxx-OO01 EOO-xxxx-0002 EOO-xxxx-0002 EOO-xxxx-0002 EOO-xxxx-0003 EOO-xxxx-0003 EOO-xxxx-0003 J-S t-Oj ao 2 <> 3 45 0.0 0.0 0.0 si 1 1 1 1 1 1 1 1 1 Col. 4 Test Substance = _________________________ ID #: T /D /l___________________ /______ / ______ Col. 5 Matrix Solution ID #: T/D/l // Col. 6 T/D/l // Internal Standard ID Number T/D/l // 6 GLP Study Number: 3M Environmental Laboratory 7 7 Page 65 of 703 BACK TO MAIN 10.0 m Lo fT estS ub st. Soin. 1.00 mL sample 2.0 mL Methanol Spike Soin Addition Comments Suitable Container ETS-8-159 Section 12.3 Cot 3 C T -1 _________________ C T -4 _______ C T-2_________________ C T -5 _______ C T -3 _________________ pl 7 IIP/]____________ /---- / -- (a) 0.0 mg/L Test Subs. Soin ID ______ t (b) 0.1 mg/L Test Subs. Soin ID ______ (f) 1 mg/L Test Subs. Soki ID ______ Col 8 Inc. ID ________________________ Start T/D /l_________________ /_____ /,, Stop T /D /l_________________ / r Col-9 T /D /l_______________ /___ / _ O 1 1 EOO-wood 001 EOO-wood 002 : EDO-ox-1003 ' E00ooood004 EOO-woodOOS EOO-mom-IOO EOO-woodOQ? E00-wood008 EOO-xxxx-1009 EOG-wcodOlO EOO-ax-1011 EOO-wood 012 E00ooax-1012 EOO-Max-1013 E00-wood014 EOO-woa-1016 EOO-XXMC-101S EOO-wax-1016 EOO-xxw-1017 EOO-caw-101 & EOO-mocx-1019 EOO-woodOl9 EOO-wo-1020 EQO-woa-1021 E00-wood021 EOO-woa-1022 EOO-xxa-1023 EOO-wood 024 EOO-wood 024 EOO-wood 025 EOO-woa-1020 E00-o-1027 EOO-xxxx-1027 E00-ood028 E00-wood 029 E00-xxxx-1030 EOO-wood 030 EOO-wood 031 EOD-wood 032 eoe-a. 1033 eOO-xxxx-1033 EOO-wood 034 EOQ-woa-1035 EDD-wood033 E00-woodC38 EOO-woa-1037 EOO-woa-1038 EOO-wood 039 E00-eo-1038 EOO-wood 040 EOO-xxwc-1041 EOO-wood 042 E0O-XWO6-1042 EOO-Moa-1043 EOO-wood 044 EOO-wax-1046 EOO-woa 1045 EOO-wax 1046 EOO-wax-1047 EOO-coot-1048 EOO-wood 048 EDO-wood 049 EOO-woa-1050 EQO-xxxx-1051 E00-oa-1051 EOO-woodOK EQO-Woa-1053 EOO-wooc-1054 EOO-wood 054 1 S 1 -fe e. I1 23 4 -- NA 0 hr -- NA 0 hr MA 0 hr NA 0 hr NA : OTw NA Ohr -- NA Ohr _ NA : Ohr -- NA Ohr _ CT-1 24 hr -- CT-1 24 hr -- CT-1 24 hr MS CT-1 24 hr CT-1 24 hr -- CT-1 24 hr -- CT-1 24 hr MS CT-1 24 hr CT-1 24 hr _ CT-1 24 hr _ CT-1 24 hr MS CT-1 24 hr _ CT-2 24 hr _ CT-2 24 hr _ CT-2 24 hr MS CT-2 24 hr -- CT-2 24 hr _ CT-2 24 hr -- CT-2 24 hr MS CT-2 24 hr -- CT-2 24 hr -- CT-2 24 hr -- CT-2 24 hr MS CT-2 24 hr -- CT-3 24 tv _ CT-3 24 hr _ CT-3 24 hr MS CT-3 24 hr _ CT-3 24 hr _ MS _ _ MS -- _ _ MS _ _ _ MS _ _ _ MS _ _ MS _ _ -- MS _ ._ MS CT-3 CT-3 CT-3 CT-3 CT-3 CT-3 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-4 CT-S CT-5 CT-5 CT-5 CT-5 CT-5 CT-5 CT-S CT-6 CT-5 CT-5 CT-S 24 hr 24 tv 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 tv 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 hr 24 tv 24 hr 24 hr 24 tv 24 hr 24 hr I 5 O.G o.o 00 0.05 0.05 0.05 0 .5 05 0.5 00 00 0 .0 0 .0 0.05 005 0.05 0.05 0.5 0.5 0.5 0 .5 0.0 0.0 0.0 0.0 0.05 0.05 0.05 0.05 0.5 0.5 0.5 0.5 0.0 0.0 0.0 0.0 0.05 0.05 0.05 0.05 0 .5 0.5 0 .5 0.5 0.0 0.0 0.0 0.0 0.05 0.05 0.05 0.05 0.5 0.5 0 .5 0.5 0.0 0.0 0.0 0.0 0.05 0.05 0 .0 5 0.05 0.5 0.5 0.5 0.5 6 " St S1 S1 S1 S1 S1 St S1 St SI S1 St si St S1 S1 St St S tf St :: 'S 1;r Jit" :V - S t S1 S1 31 SI St S1 S1 S1 SI S1 S1 S1 : S1 St S1 S1 S1 SI Si S1 S1 S1 S1 S1 SI 1 Ss1t; SI St -S i-! SI S1 S1 = s.1r S t S1 si SI S1 St S1 St S1 SI SI 7 -- -- -- -- -- GLP Study Number: ! <5 s 1 e -- _ -- ~ -- -- -- -- Col 10 Spike Soin ID ____________________ T/D/l_______________ /___ / COM2 ' MeOH Dil Soin ID ________________ T/D /l_______________/___ / Col 13 ' T/DA _______________/ ___ / .9l 14 Spike Soin ID ____________________ Internal Standard ID_______________ _ T/D/l_______________/___ /_ i 1 t f Sl _ ig _ 9 to ____ ti t2 -- ---- -- ---- ~ ~-- -- ---- -- ---- -- ---- ---- _ ---- _ ---- -- S2 -- S2 -- S2 S2 -- S2 _ S2 -- S2 S2 -- S2 -- S2 _ S2 S2 _ S2 _ S2 -- S2 S2 -- S2 S2 -- S2 S2 -- S2 -- S2 -- S2 S2 _ 2 _ S2 -- S2 S2 -- S2 -- S2 -- S2 S2 -- S2 -- S2 -- S2 S2 . : : S2 - . -- , S 2 -IV: -- . S2 : S2 ' -- S2 -- S2 : -- S2 S2 -- S2 -- : S2 -- S2;. S2 -- S2 -- S2 _ : S2 S2 _ . S2 _ S2 -- S2 S2 S2 -- : S2 -- 52 S2 E 8 13 -- -- -- -- -- -- -- -- -- 14 -- __ -- -- -- -- -- -- -- -- -- -- -- ---- -- -- -- -- -- -- -- -- -- -- -- -- --.. _ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- _ -- -- _ _ -- -- 3M Environmental Laboratory Test Substance: 16 Page 66 of 703 BACK TO MAIN Desorption Solvent ETS-8-159 Section 12.4 Test Substance C o l 4 Soil ID 1 Soil ID 2 C o l 6 B a la n ce ID t /d n I C o l 7 T e st S ubsL S oin ID # T /D /l / C o l.8 MeOH ID # TD/I / / / / 0 1 1 EOO-joooc-2001 EOO-xxxx-2002 EOO-xxxx-2003 EOO-xxxx-2003 EOO-xxxx-2004 EOQ-xxxx-2005 EOO-xxxx-2006 E00-)ooa-2006 EOO-xxxx-2007 EQO-xxxx-2008 E00-x>oo<-2009 EOO-xxxx-2009 EOO-xxxx-2010 EOO-xxxx-2011 EOO-xxxx-2012 EOO-xxxx-2012 EOO-xxxx-2013 EOO-xxxx-2014 EOO-xxxx-2015 EOO-xxxx-2015 EOO-xxxx-2016 EOO-xxxx-2017 EOO-xxxx-2018 EOO-xxxx-2018 EOO-xxxx-2019 EOO-xxxx-2020 E00-xxxx-2021 E00-xxxx-2021 E00-xxxx-2022 EDO-xxxx-2023 EO O-xxxx-2024 EQQ-xxxx-2024 E00-xxxx-2025 E00-xxxx-2026 E00-xxxx-2027 E00-xxxx-2027 30 1 23 -- Cntrl _ Cntrt -- Cntrl MS Cntrl -- Cntrl _ Cntri _ Cntrl _MS Cntrl Cntrl _ Cntri C n trl MS Cntrl _ Smpl _ Smpl _ Smpl MS Smpl _ Smpl _ Smpl _ Smpl MS Smpl _ Smpl -- Smpl -- Smpl MS Sm pl _ Smpl _ Smpl _ Smpl MS Smpl Smpl _ Smpl _ Smpl MS Smpl Smpl _ Smpl _ Smpl MS Smpl 4 NA NA NA NA NA NA NA NA NA NA NA NA S1 S1 S1 S1 S1 S1 S1 S1 S1 S1 S1 S1 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 Typ o f So (High Clay Conten or shidge) Test Substance, ug So Weight, grams Vdd methanol, record /ohim added in mLs Centrifuge & Transfer hdd methanol, record /olume added in mLs 1.00 mL o f Study Sample Spike Amount Col 9 T/D/l C o l 10 M eOH ID # T /D /l C o l 11 T /D /l C ol 12 MeOH ID # T /D /l // // // // COM3 ' T/D/I C ol 15 Study Sam ple T /D /l C o l 16 S pike soln ID # Tim e/Date/Initials In te rn a l S ta n d a rd ID # Tim e/Date/Initials / / / / // II l ) e .5 i li . Sj , i jS s s 3 < ( ' ! 5S -- ...0 PPP!...0 M n~ ~0 _0 --1 7 8 9 10 11 12 13 14 15 ' -r-M 1 1 1 10 10 10 10 ... _ _ -- -- _ 0 Q 0 0 _ _ r n is i n ' -j 1 1 1 sw 1 10 10 10 --10 0 0 _0 0 1 mm w^il SIPnw SS 1 1 1 p u10 10 Ktfi 10 m m 10 I 1 GLP Study Number: 3M Environmental Laboratory Page 67 of 703 BACK TO MAIN Optimal Ratio E TS -8-159 Section 12.5 S ol Typ Sol:So*i Ratio 3.01 M CaCI2 Addition EquHbrat 12 hours Remove 1.00 mL Study Sampl J liR iifS lif f 1 34 n j 3 6m ? ,,^ a s 2 XZ i ?, B !" S il I 9 10 1 1 12 10 14 3 fl 15 3 ! 1 a0 18 17 E0-5CK-3001 EGQ-ioc 3C02 EGO-joooc-3003 m H ft " **i , " 1 EGO-xxxx-3004 E0O-XXXX-3OOS HWP ~ -- 0.0 0 0.0 0 f m S & m 0.0 W S 0 i | 0.0 0 f t r f mm0.5 0 i i i ? f l p 0.5 0 t e m p s ip p a s s e s * p g I? # M $l : : r i 4S em BS1 1S E00-uooc<3C0ff i l ~ EOO-xxxx-3006 MS - EOO-JOOoc-3007 t e - E00-mx-3006 f t - E00.mx.3009 SiiSi. EOO-mob 300S - : . :: - EOO-XXXX3Q11 :U5 - H iI K - { mE00W O1K - 0.5 0,5 i W 0 il1 0 te P S 0.0 I f c i 48 t e - f u ffl0.0 I M ' 48 t e m s m m 0.0 48 0.0 1 5 5 48 M i l rrffm 0.5 _48 l l r s s s p s s 0.5 p s 48 i 0.5 S \ H _48 l a .'t M its tS s s 0.5 48 sial S H ! mm ii fLM M J' mm 9 ^ p is s W E fe i:' i B is # . 3W iftlli a* H MH Q m ksM mu ft il HC/LO & hs&i18 s l HC/LO m sstm i i l f tE O tm tii? ftE 0 ; 3 b i^ : HC/LO HC/LO HC/LO teE o o -m x -jb irf teo o -m x.3 0 1 f tE O -m x-M IO ? HC/LO HC/LO HC/LO EO.xxw-3019'- f t HC/LO O & i o S f t HC/LO 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1:1 0 1:1 0 1 1:1 0 1 1:1 0 1:5 0 1:5 0 S I 1:5 0 i t 1:5 0 1 1:25 0 w 1:25 0 s i i g iffiS 0 iU PS1 tP fl mm flH iK w m ;^ r .. B B H 9K sa ! 1 * IM E0-X)of*3O2t fl I f t HC/LO E O O -xm -tol: HC/LO Sisiyii 0 3 0 2 2 * HC/LO OO.oix.3023-5 SI IisIE O O -x m ^ in ? BE O O * a -te 4 r- H C /L O H C /L O H C /L O MSEO-xm-3025 : ME0O-m3O6S HC/LO H C /L O H HC/LO EOO-JOoa-3027 > H C /L O EOO-xxxx-303- HygtEO-a-3029'` SpSE0-X500C-33O" sEO-w-3030 - HC/LO HC/LO H C /L O HC/LO 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 1:25 0 m 1:25 0 i m1:1 48 m 1:1 48 i l1:1 48 a1:1 48 l1:5 48 1m1:5 48 1:5 46 n1:5 48 a1:25 48~ 1:25 48 !1:25 48 1:25 48 g& i M H i IlHigfptif r. Hg ft HK mm zz zz mm M BIKI (tw liril mm w M :itfn rn> 8uHm C IIBMW Soil Tvoe 1 (HC/LOl Soil Tvoe 2 LC/HO) Coi B Balana ID T/D/l Col 9 CaCCSolniD T/D/l // // Col 10 4B hrt Inc. ID Start T/D/I StOD T/D/l // // Col 11 TeslSubst.lD T/D8 Col 12 Inc. ID Slari T/D/l StOD T/D/l // // // Col 13 T/D/l Col 14 T/D/l Col 15 Balance ID T/D/l Col 16 T/D/l Col 17 Spike Soin ID T/D/l Internai Standard ID T/D/l /i // // // /! // Test Substance I! s 18 GLP Study Number: 3M Environmental Laboratory 1of 5 Page 68 of 703 BACK TO MAIN Optimal Ratio E TS -8-159 Section 12.5 Test Substance 101 M C a C C Addition EquMbrate fo r x hours centrifuga (Y/N ) Remove 1.00 m l Study Sample |iO 1KL , ' 1 % O ?1 oe vi- , i .; - { S i 3 e o o * x x ^ Q 3 i: S i HC/LO 4 0.5 S 67 p 11 0 E0O-MW .3032 8 HC/LO 0.5 11 0 S E00-M0C*>3033 f e HC/LO E0-JOXX-3033 S I HC/LO 0.5 0.5 11 0 1 1 0 f EOOooor-3034- K H C /L O E O O - i o o a J O iif e i i HC/LO 0.5 0.5 t 5 0 $jf! 15 0 m B t o t ' P HC/LO 0.5 15 0 E 0 0-lo o 303e - M i H C /LO 0.5 15 0 Et n S O lT ! S H HC/LO 0.5 1 25 0 r i t E0CftKX-303 . S B HC/LO EOO.of-4J039 :i HC/LO 0*tox330 -! HC/LO 0.5 0.5 0.5 1 25 | _ _ 1 25 0 f i l 1 25 0 I E0(Moeo<.304b ' g E O O -W M 1 ! I M HC/LO H C /L O 0.5 0.5 11 2 r i: 11 2 s E00*x-3042 : H HC/LO E 0 frX M *5(2 ! M S HC/LO E0tot4043'- B HC/LO 0.5 L l 1 0.5 1 1 0.5 r 5 2 ri 2 ri 2 fs f t i & e M ' i I M HC/LO (SBE ( * * x - 3 0 4 5 ' H C /L O 0.5 0.5 i 5 2 iS i 15 2 r i E O m a o t-3 0 1 E S # HC/LO EO-xax.SO-: B Q HC/LO 0.5 0.5 15 2 r i 1 25 2 r i ! cMa i 1 HC/LO 0.5 1 25 2 s d ix x - S 0 4 S '` I S j HC/LO 0.5 1 25 2 r i Eoo-xo(-304a-.' m S O to x -a -W S ' . m HC/LO H C /L O 0.5 0.5 1 25 2 r i 11 4 r i EOO-xxxx-3050 ' f e i HC/LO E00*)ocof-305t i f e HC/LO E00-cb(.3C5i K HC/LO *SSfEdo-SeaJOM ' H C /L O E O io a x J O !- m HC/LO 0.5 0.5 0.5 0.5 0.5 11 4 r i 1 4 1 1 4 pu 15 4 r i 1 5 4 E 00-M w i54( y HC/LO 0.5 5 4 ri EOMoea-3094 S i HC/LO 0.5 5 4 ri fffigE 0 x * 3 W S ' H C /LO EOO-XMQhSOS ' S HC/LO O.S J , 25 0.5 25 4 ri 4 il ' SjE O O O & t a f H C /LO 1 0.5 i S iE O -M X W O S r HC/LO 0.5 25 25 4 4 SSi EO MdBoOM 'i HC/LO : HE00-oc*3059 HC/LO tp$lE 0 0 & a x i0 6 0 . HC/LO 10.5 P0,5 11 _10.5 : a ~s| 8 8P S EOO-XXXX-306 HC/LO 0.5 11 8 BXHoooiOM)-: HC/LO eto obobteott'-? S HC/LO \i KEIXVoW 0fl3 HC/LO ' iffiiE00-M M-3033 HC/LO iggEOiMooiJOM-i 8 0 EOOocooc-3065 H C /L O HC/LO 'SEOO*ooc30BS H C /LO ' EHtfE0-X0OW08S H C /LO 0.5 5 0-5 S O.S 5 0.5 S 0.5 25 0.5 _1 25 0.5 _1 25 0.5 _ 1 25 8 ir 8 Sf 8 :jg| 8 8H 8S 8 il 8S ! a T/O/l // Col 10 2 hrl Inc. ID Start T/D/l Stod T/D/l Col 10 (4 hrl Inc. ID Start T/D/l StOD T/D/l Cot 10 (8 tvt Inc. IO Start T/D/l Stop T/D/l i ti TS11 3 X a 10 11 12 13 14 a i 1 M iis 15 IE S m SU m U.;u mm ta I i i J_ 16 1 1 ; i-JS p $$$$ i Ip f #4! r i i w W n m fm iX m S N ftS S iS : # ir :< i B a fc fc S S a || (M 1 P I IS H r a S f^ tfte U W m 8m e s o n i :k M w? i ffl is s * s S O rJi Si iiii s s y -y S ta* PI M m m Wk P P l# tW B im a f K // // IJ // // // . HH H E S iS ; n SlS-S^ ffetlSr w a h u mm s m m s gHSy-S1:. m s IM B W W 1S 411,41 ^ tr H M f& tth M lHi ip m p B g M is g l fe m m Tji- .W imi sp ? w Mw iy m fQ f f iil m S i C d 11 Test Subst. ID T/D/l C d 12 Inc. ID Start T/Dfl StOD T/O/l C d 13 T/D/l c o l 14 Tran Col 15 Balance ID - T/D/l C d 16 T/D/l Col 17 SoikeSdnlD T/D/l // // // /i is // // // GLP Study Number: 7/D/l _/ / \ i si _______ .t................ - , t - - m =' : ' " 2of5 3M Environmental Laboratory Page 69 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 Test Substance SoH:Soln Ratio SoBWeight (grams) D.01 MCaCI2 Addition Test Substance AddKlon Remove 1.00mL Study Sample II HBj u P1m s 13 iF 34 E 0 0o o a *30 67 -' ^ > S HC/LO 0 5 E00-ooc-306? H C /L O E0iitbi368 S f f i HC/LO 05 0.5 Eoo-jooo^aoe-4: s s HC/LO Eo&oboe&ora p i i HC/LO 0.5 0.5 B & io o ft& M | HC/LO E00.WMW3072' ' i t e HC/LO 0.5 0.5 f t HC/LO 0.5 E 0 O -X ttfr3 O W ^ HC/LO 0.5 l i HC/LO 0.5 ESJia.3075^ HC/LO 0.5 EO<^>ooiMKff S i HC/LO 0.5 H C /L O e a f c & i & 3|i; HC/LO 0.5 0.5 S i HC/LO 0.5 S Q flS ab fe HC/LO 0.5 E 0 0 i 3 0 7 S V ; m HC/LO 0.5 EOfrxiotteti* f t HC/LO 0.5 E 0 0 *x w *3 0 6 1 - f t HC/LO 0.5 EO koo^M H Jit 8 1 HC/LO 0.5 E 0 4 ja x .3 0 B 2 H C /L O xftote083> m H C /L O f tEOO^x w W O W t - p i l HC/LO H C /L O 0.5 0.5 0.5 0.5 G OO wM idNS? HC/LO 0.5 E00-c*308^ H HC/LO 0.5 E-V00^3087:- HC/LO 0.5 E ^ - 3 0 8 7 * 8 HC/LO 0.5 E ^X3*30M t f i j HC/LO E 0 fr 0 o t - 3 0 8 9 i* : H C /L O 0.5 0.5 EOotod4MO. HC/LO 0.5 E0-M` 3 0 0` ' HC/LO 0.5 E00*c*3091 $ !ijw ? 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ID // Start T/D/l // Stop T/D/l // Col 13 T/0/1 /i Col 14 T/D/1 / Col 16 MeOH Dim Soh ID / T/D/l Col 15 Balance ID / ... t T/Ort // Col 17 T/D8 // Col 18 Spike Soin ID _________________ T/D /l_______________ / ____ / _____ 3of 5 3M Environmental Laboratory Page 70 of 703 BACK TO MAIN Optimal Ratio E TS -8-159 Section 12.5 Test Subs. cono., mg/L Soi Weight (grams) Equiltorate 12 hours EquWbrate fo r x hours Remove 1.00 mL Study Sample m IS m 1O 3 E 0 0 . 3 - LC/HO o c tiN d a u ti R i l c /h o E00.xx3105 LC/HO . 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LC/HO E00-oc*-3132 m LC/HO E00-*cot'3133-1 E 0 0 - xx-3 i3 4 fi LC/HO LC/HO EOOoooot-313> LC/HO E00xa-3135< f f l LC/HO EOO-xxia-3136 > LC/HO EOOxa-3137- LC/HO ' p j|| E00-iooa313'` LC/HO EOO-mx-3138 ; [ B LC/HO 0.5 0.5 0.5 0.5 0.5 O.S 0.5 0.5 0.5 0.5 0,5 0.5 0.5 O.S 0.5 0.5 0.5 0.5 0.5 ni K o K toU m5 fh 1:1 0 3 M1.1 0 i 1:1 0 S 1:1 0 1:5 0 m 1:5 0 1:5 0 S f 1:5 0 R 1:25 0 1:25 0 S i1 1:25 0 w 1:25 0 4 L 1:1 2 1:1 2 1:1 2 R 1:1 2 1:5 ? 31 1:5 2 i s s 1:5 ? -S1 1:5 2 S I 1:25 2 R 1:25 2 Sii 1:25 ? H 1:25 2 R 1:1 4 n i m1:1 4 1:1 4 1:1 4 i l 1:5 4 R 1:5 4 1:5 4 S 1:5 4 i l 1:25 4 t t 1:25 4 R 1:25 4 * 1:25 4 8 m1:1 6 1:1 81:1 8 a 1:1 K 81:5 "m 81:5 ' i i 1:5 R ' S ! 81:5 1:25 R " 1:25 R ' i l i 81:25 ' a 1:25 __ 8_" R 8 c0 1< O LS U j > ii X j n Zf 1 fl Jsi 9 10 11 12 1 14 15 5 i 1 X 18 17 X r iM (JIfs ms 81 1M mt mm ta p n tS LI is P I ms vm ttHIEIH"" i i tl y t/fr * w bm w B H B in V.AAt r3 jf erriti.'V *iiWMf S e ife * s# rm lE:1m 12:r: L uu I L * i M k l: sse# m ____ $ iiS M $ S S S S fllS S itS t. mtOmTIM1Dttt FtfHyayjrTHfyrt-r' wm g r,,,A . cl, mu ....... rP if LU pSi ~~ W M a ftv .-sy fA iv Mlj ~~ i __ ___ _' h s i f f f ia tM _ Soil T 1 (HCA.O)___________________ Soil Type 2 a c /H O )___________________ Col 8 Balance ID_________________ _ T/D/l____________ /____ f ____ Col 3 C&C12 Soin ID_______________ T/D/l____________ /____ ! ____ Col 1Q (2 hr) Inc. ID _______ Start T/D /l___________ ! __ /_ Stop T/D/l________ -- /- / Col 10 (4 hr) Inc. ID____ ________ Start T/D /l_______ --/ __ J .. Stop T/Df l _________/ Col 10 (8 hr) Inc. ID ___________ Start T/D/l ./ / Stop T/D/l // GLP Study Number: C o l l i Test Subst. IO _____________ T /D /l________________ / ____/ _ _ Col 12 Inc. I D ____________________ Start T /D /l____________ Stop T/D/l / / C o l 13 T /D /l_______________/____/ . Col 14 T /D /l_______________/____/ . C o l1 6 MeOH Difn Soin ID ________ T /D /l__________________/ J Col 15 Balance I D ________________ T /D /l__________________ / J Col 17 T /D /l________________ / I Col 18 Spike Soin I D _____________ T /D /l__________________ /____ / Test Substance i t .Li . - _______ __ ` Y r ' X : i-.;" - 1. 4of 5 3M Environmental Laboratory Page 71 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 Test Substance Sol Typt Sol:Solrt Ratio 9.01 CaC(2 AddKionM EquBbrate 12 hours Equilibrate fo r x hours tem ovel.OO mL Study Sample iu <A Ll .-."` 1 . J V m E00-XXXX-3139: JL t VC -S - l " ' 3-7 ' i i ' . ."5'V: ! > ! M LC/HO 0.5 1:1 16 E00.xm -3140 S B E 0 O * m - 3 l 4 t LC/H O LC /H O 0.5 1:1 0.5 _ 1 1 16 m16 EOO.JOCCt-3141 : LC/HO 0.5 __ 1 16 w E O O *m -31 42 - i s t i LC/HO 0.5 5 16 EOO-joooc-31 43 H LC /H O EOO-joooc- 3 1 4 4 LC/H O EOO-looot-31: f e t e LC/HO EOO-1000C-3145T;: M LC/HO E00.kjoot.3f461.: LC/H O EOO-ioooMU? s s LC/HO EOO-xxxx^HT [ 0 5 LC/HO E00-xm .3t4'r' M LC/H O 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0,5 5 5 5 25 _1_ 2 5 _1_2 5 1 25 11 16 i f 16 a 16 16 m 16 s 16 m 16 | 24 EOO.Jooot.3l49.r- 8 5 LC/HO EOO-Jooot.3150:: 5 K LC/HO E00.jocct.3150 S S LC/HO 0.5 1 1 0.5 _ 1 1 0.5 1 1 24 m 24 24 E 0 0.x -31 51i 5 5 5 J X /H O 0.5 __t S 24 i l e o s -x c u -j i s : i 8 5 LC/HO EO-kcot-3153. S J LC/HO 0.5 0.5 1 5 24 i 1 5 24 m E00-joca-3t53:r f e t e LC/HO E 0 0 .*x -3 1 5 4 v LC /H O 53EQO-JCCa-31551 LC/H O EOO-XMt-3156 LC/HO 0.5 0.5 0.5 0.5 15 1 25 1 25 1 25 24 a 24 3 5 24 m24 EOO.JOOOt-3156 f e t e LC/HO EOO.joooc.3157 fatte- LC/HO EOO.JOo-3156- 5 5 LC/HO EOOoCOa-3159 S 5 LC/HO E 0 0 .x m .3 1 5 9 '5 S S LC/HO 0,5 0.5 0.5 0.5 0.5 1 25 11 11 11 11 24 i l 36 36 P i 36 l i t 36 l EOO-Jocct-3160 * f f i LC/H O 0.5 1 5 36 f S E00.jooa.3161 i ; fe tte LC/HO EOO-Jooa-3162 p f f LC/HO E00.xm .3162. w LC /H O 0.5 __L S 0.5 S 0.5 5 36 w 36 36 a EOO-woot-3163 l EOO-XJOa-3164 - B EOO.XXK-3185 LC/H O LC/H O L C /H O EOO-XJoa-3165 l LC/HO 0.5 0.5 0.5 0.5 1 25_ 36 1 25_ 36 a 1 25_ 36 1 25_ 36 i l EOO-oax-3186 I j j LC/HO EO O-m x-3167 - 3 S [ LC/HO E00-oa-0i60 mfeteEOO-XJoa-3168 LC /H O LC/HO EOO.Jtm.369 I S LC/HO EOG-xm-3170 E O O -x m .3 1 7 1 B w LC/H O LC/H O 0.5 1_ 48 i l 0.5 1 1 48 a _0.5 _ 1_ 48 a 0.5 1 46 s i m0.5 _ 5_ 48 _0.5 5_ 46 a m.0.5 5__ 48 E0O.J0txx.3171'' EOO.iooa-3172 M LC/H O L C /H O 0.5 0.5 5 _ 48 5 m.1 25_ 48 E 0 0-m x -3 17 3 : S LC/HO EOO.Joaa-3174 E00-xm -3174 H I LC/HO M LC/HO 0.5 0.5 0.5 1 25_ 48 1 25_ 46 1 25_ 46 B I' s i % 3| 5 8 9 10 11 ____ ____ .... Soil Tvoe 1 (HC/LOJ Soil Type 2 (LC/HO) Col 8 Balance ID T /D /l Col 9 CaCt2 Soin ID T /D A // // Col 10 (16 hr) Inc. ID Start T/D/l Stop T/D/l Col 10 (24 hr) Inc. ID Start T/D/l Stop T/D/l Col 10 (36 hr) Inc. ID Start T/D/l Stop T/D /l Col 10 (48 hr) Inc. ID Start T/D/l Stop T/D/l // // // // // // // // GLP Study Number: z ? S 12 13 14 i O S il? 15 3 % V) S w JL 16 17 B bal i s m ad a tti lie s i mm ftO S tillia m m f raBBWBtfterfii oe soe & m m m iK i M K M W SW i5 18 am n S U K th te o a fs is iit: 8^2 Sea. ft U IP tm H i iM iE a llll m m 4i||i]fi'(irrr*rr; H a iiH M S A i- ati . 354 BsiiS m m m slOt-oa* ____ VW UuSUtSii ir a ffi . * |-- -- ------------------------------------------------------------- S SwWawBpPf 5WW j% ili S PS & 1 Col 12 Inc. ID Col 16 MeOH DlTn Soin ID T /D /l / / T /D /l Col 17 T/D/l Col 18 Spike Soin ID // // 3M Environmental Laboratory Page 72 of 703 BACK TO MAIN Optim al R atio/M ass Balana ETS-8-159 Section 12.5 (co n t) a ! ' EOO.xxxx.3D07 EOO-aoa-3008 EOO-xxxx-3009 EOO-xxxx-3009 EO-xxxx-3010 EOO-xxxx-3011 EOO-xwx-3012 EOO-xxxx-3012 EOO-xxxx-3022 EOO-xxxx-3023 EOO-xxxx-3024 E00-X30O-3024 EO-xxxx-3025 E0O-XXXX.302 EOO-ioooi-3027 EDO.wxx-3027 E00-xxxx-3028 EOO-xxxx-3029 EO-)ooa-3030 E00-oa-303 EO-xxxx-3004 EOOooooc-3095 E00-co<-30S u! 1 _2 _3 __ _,, MS _ _ __ -- _ t 3 n 4 0.0 0.0 0.0 0.0 0.5 0.5 0.5 MS 0.5 - HC/IO 0.0 _ HC/LO 0.0 ,, HC/LO 0.0 MS HC/LO _ HC/LO _ HC/LO _ HC/LO 0.0 0.0 0.0 0.0 MS HC/LO 0.0 HC/LO 0.0 _ HC/LO 0.0 _ HC/LO 0 0 MS HC/LO 0.0 HC/LO 0.5 _ HC/LO HC/LO 0.5 0.5 e1c ImoA * I ! 5 ?. NA 46 S2 UA 48 S2 NA 48 S2 NA 46 S2 NA 46 S2 NA 48 S2 NA 48 S2 NA 48 S2 48 S2 48 S2 48 S2 48 S2 48 52 48 S2 48 S2 48 S2 1 5 48 S3 1 5 48 S2 1 5 48 S2 1 5 48 S2 48 S2 48 :S2. 48 S2 3 % = li I li 8 E00-KOO-30M EOO-xxxx-3097 EOO-xxxx-3098 E0-w-30M ECO-mx-3099 EOooocx-3100 EOO.xxxx.3lOt EOO-aooi-3102 E0-wxx-302 E00.xxxx.3160 EOO-xxxx-3187 _MS HC/LO HC/LO H C /I O __ HC/LO MS HC/LO HC/LO _ HC/LO HC/LO _MS HC/LO LC/HO _ IC/HO 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 40 $2 5 48 S2 5 48 S2 5 48 S2 5 40 S2 1 5 48 S2 1 25 48 s i 1 5 48 S2 1 5 4B S2 1 48 S2 48 S2 E 0.xm -3t 8 LC/HO 0.5 E00.xxxx-31e: MS LC/HO LC/HO EOO-xxxx-3170 ; W LC/HO 0.5 0.5 0.5 EOO-woo-3171 LC/HO 0.5 EOO-noot-3171 MS LC/HO EOO.wxx-3172: - L i LC/HO 0.5 0.5 EOO-xxxtf-3173 LC/HO 0.5 EOO-xxxx-3174: L L LC/HO 0.5 EOO-xxxx-3174 MS LC/HO 0.5 1 48 S2 4B S2 5 48 S2 5 48 S2 5 48 S2 5 48 S2 25 48 S2 25 48 S2 25 48 S2 25 48 $2 C o l l Baiane* ID _____________________________ Col 13 MeOHID, S i= f i_ S ii hz 9 * 5 u 9 si i -s a 9 ts fl fls x ? - ! 1 lL iO ?3 iS IF S 5 10 11 12 13 14 15 1 1) o 1# (2) (2) * i r (2) f (2) . (2) (2) (2) # (2) .. (2) l p | 0 - m(2) (2) (?) (2) (2) (2) . 8 B (2) . . (2) (2). . S S S (2) n (2) 0(2) . m _____ f t $ 0 - (3) .... (3) (3) SS m I* ft dpi S (3) . (3) . (3) (2) (2)__ . (2>_......... 0 ______ (2) L 0 _____ (3) . 0 ______ (2) 0 ______ (2) 0 ______ (2) (?) [ 0 _____ (?) 0 ______ 0__. (2) (2) (2) (2) (2) (2) 0 _____ (2) (2). (2) (2)' (3) (3) ^ (3) (3) 0 (3) (3) (3) (2) _ (3) 0 _ ... _ (2) 0 ______ (3) (2) (2) (2) (2) (2) _ (2) . (2) ... (2) (2) (2) (2) . . (2) (2) _ .. (2) (2) (2) (2) (2) (2) 0 ______ (2) (3) (3) (3) ( 3 ) ....... (3) (3) (3) (3) (3) <21_______ <21______ (2) 0 _______ (2) (3) 21______ 0 _ . ..... (2) (2) 0 _____ (2) (2) 0 ______ (2) 'i (2) 0 _ ... (2) (2) (2) (2) (2 ). (2) (2) 0 ______ 0 _____ (2) ( WM ns ^ 3IS w flfc li s p Si & . WM isS* C o l l M*OH ID T/Dfl Col 11 MbOHID von Col 12 TrtM // // // // Col 14 T/D/l CollST/D A Col 16 Spike Sold IO T/D/l Internal S tan d a rd ID T/D/l // // // // Test Substance: i I n GLP Study Number: 3M Environmental Laboratory Page 73 of 703 BACK TO MAIN 3M Environmental Laboratory M ethod Pr e p a r a t io n o f So il Sa m p l e s f o r Sc r e e n in g (T ie r II) a n d A d v a n c e d (T ie r III) So r p t io n St u d ie s f o r F l u o r o c h e m ic a l s a s t h e T e s t Su b s t a n c e (B a sed o n OECD G u id e l in e 106) Method Number: ETS-8-160.1 Author: Cindy Carlson, Mark Ellefson foAdoption Date: / /3/ Revision Date: ETS-8-160.1 Tiers II and III Sorption Studies 3M Environmental Laboratory Page 1 of 15 Page 74 of 703 BACK TO MAIN 1.0 1.1 ; 1 1.2 1.3 1.4 1.5 Sc o pe and A pplica tio n 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 Adsorb/Desorb 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. 2.0 S u m m a r y o f M eth o d 2.1 Tier II: Adsorption Kinetics (One concentration): 2.1.1 Appropriate soils and/or sediments and/or 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 CaCU- 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. 2.2 Tier III: 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 CaCh 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. 2.3 Tier III: Adsorption Isotherms (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 CaCl2 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 fromthe 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. ETS-8-160.1 Tiers II and III Sorption Studies Page 2 of 15 3M Environmental Laboratory Page 75 of 703 BACK TO MAIN 2.4 Tier III: Desorption Isotherms: 2.4.1 The study samples fromthe 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 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. 2.5 Tier III: Mass Balance: 2.5.1 The study samples fromthe 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. 2.6 In all cases, adequate quality assurance samples are prepared and analyzed. 3.0 D e f in it io n s 3.1 Test Substance: Any substance (mixture or controlled compound) added or administered to the test system for the purpose of biological or chemical measurements. 3.2 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. 3.3 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. 3.4 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 3.5 administered or added for study. Study sample: A sample containing the test substance in contact w ith t h e tes t s y ste m , o r any of the subsequent samples generated fromthe initial set up. 3.6 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. 3.7 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 fromthe initial matrix blank set up. In most, but not all cases, matrix blanks go through all of the same processes as the study samples. 3.8 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 II and III Sorption Studies 3M Environmental Laboratory Page 3 of 15 Page 76 of 703 BACK TO MAIN 4.0 W a r n in g s a n d C au tio ns 41 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. 4.2 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 fromthe glassware. Clean all spills immediately to avoid present or future contamination. 4.2.2 Use disposable glassware whenever possible. 5.0 I n t er fer en c es 5H Any compound that co-elutes with the target analyte(s) or the reference material during the HPLC/MS analysis can interfere with quantification. 6.0 E q u ipm en t 6.1 Balance capable of weighing to 0.1 mg, such as OHAUS Brand Model GA200 6 .2 Centrifuge capable of maintaining 4,000 200 rpm, such as Jouan Brand Model C412 6.3 Orbital shaker capable of a gentle rotation and temperature controlled capable of maintaining 23 3C, such as Lab-Line Model Environ-Shaker 6.4 Vacuum Pump, such as Gast #DOA-P104-AA (Optional) 7.0 S u pplies a n d M a ter ia ls ^L1 15-mL polypropylene centrifuge tubes, such as VWRbrand Centrifuge Tubes, catalog 7.2 n1u5m-mbLerp2o1ly0s0t8y-r0e8n9e centrifuge tubes, such as V W Rbrand Centrifuge Tubes, catalog number 21008-202 7.3 15-mL styrene butadiene centrifuge tubes, such as VWRbrand 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 VWRbrand 20171 7.7 Syringes, 10-pL, 25-p.L, 1000-pL . 7.8 Volumetric flasks, 10-mL, 100-mL, 1-L, 5-L, Nalgene and/or glass 7.9 Automatic or manual dispenser, capable of dispensing liquid with 0.1 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 # 224211-01 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 II and III Sorption Studies Page 4 of 15 3M Environmental Laboratory Page 77 of 703 BACK TO MAIN 7.15 Glassware, miscellaneous 7.16 150-mL Nalgene bottles or equivalent 7.17 pH paper capable of distinguishing pH to 0.5 units 1 8.0 8H R ea g e n t s, Solutions and Standards Reagents '" 8.1.1 Methanol, HPLC grade, such as J.T. Baker #9093. 8.1.2 ASTM Type I water, 18.0 MQ or greater. 8.1.3 CaCb, Anhydrous, to meet ACS specifications (>96% pure), such as J.T. Baker #1311. 8.1.4 Soils: Appropriate soil types selected fromTable 1 below. (Soils should be air- dried at ambient temperature and sieved to a particle size <2 mm.) Table 1 pH range (in 0.01 Soil Types M CaCI2) Organic Carbon content (%) Clay Content (%) Soil Texture 1 4.5-5.5 1.0-2.0 65-80 Clay 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 Loamy sand 6 >7.0 <0.5-10 40-65 Clay loam/clay 7 <4.5 >10 <10 Sand/loamy sand NOTE: It may not be possible to obtain soils that match all criteria. Soi s will be used that match as closely as possible the parameters as listed. Exceptions will 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, 1H, 1H, 2H, 2H-perfluorooctanesulfonic Acid, and/or PFBS, Potassium Perfluorobutanesulfonate. 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 CaCh Solution: 5.550.02 grams of CaCl2 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 CaCl2 Solution: Prepare an appropriate concentration of test substance in 0.01 M CaCE in sufficient quantity to be used through out the study. Use volumetric flask and ETS-8-160.1 Tiers II and III Sorption Studies Page 5 of 15 3M Environmental Laboratory Page 78 of 703 BACK TO MAIN record weight. Immediately transfer into a Nalgene container(s). This solution may be stored for up to 6 months at roomtemperature. 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 S am ple H andling 9.1 All study samples generated and prepared for analysis by HPLC/MS (in tightly capped vials) may be left at roomtemperature 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 Q u a l it y C o n t r o l 10.1 Matrix Blanks consisting of the following types will be prepared for the study: 10.1.1 0.01 M CaCl2 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 CaCb 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 CaCL 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 C a l ib r a t io n a n d St a n d a r d iz a t io n 11.1 This section is outside the application of this method. 12.0 P r o c e d u r e s 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 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 II and III Sorption Studies Page 6 of 15 3M Environmental 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." 1 12.2 Adsorption 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 material/type 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: If the soiksolution 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 No. of Tubes with Cone., mq/L Soil:Solution Ratio Soil, qrams mL of 0.01 M CaCI2 Solution Number of Time Points No Soil (Control Sample) 0.0 NA 0.00 12.5 0.1 2 3x2 = 6 Only need ilone from this set. -0.5 0.0 0.0 NA 0.00 12.5 0.1 1:1 5.00 0.05 5.0 0.1 1:5 2.50 0.05 12.0 0.1 8 3 X 8 = 24 2 NA 2 NA 0.0 1:25 1.00 0.05 25.0 0.2 2 NA Only need one from this set. - 0 5 1:1 5.00 0.05 4.95 0.1 8 NA -0 .5 1:5 2.50 0.05 12.4 + 0.1 8 NA -0.5 1:25 1.00 0.05 24.75 0.2 8 NA. *7o b e a d d e d in a f t e r th e s tu d y s a m p le s h a v e e q u ilib ra te d fo r 12 hours. No. of Tubes with Soil/Sediment/ Sludge NA NA 3 x 2 = 6 (x 5) 3 x 2 = 6 (x 5) 3 x 2 = 6 (x 5) 3 x 8 = 24 (x 5) 3 x 8 = 24 (x 5) 3 x 8 = 24 (x 5) pL of 50 mg/L Stock Test Substance* ; 0.00 200* 0 00 0.00 0.00 50- I 125* ;V : 250* 12.2.4 Weigh the soil and record on the appropriate data form. 12.2.5 Add the appropriate volume of 0.01 M CaCl2 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 0.5 pH 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 times/dates 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 II and III 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 3 C using a gentle rotation. The "0 hr" study sam ples p ro ceed directly to 12.2.12. 12.2.9.1 NOTE: If using the serial method centrifuge the tubes after the addition of 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 date/time. 2 hr 16 hr 48 hr 4 hr 24 hr 8 hr 36 hr 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 CaCl2 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 0.5 pH units. 12.2.12.Centrifuge until the aqueous layer appears clear 12.2.13 Withdraw 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 D12e.s3o.1rptDioensoKrpintieotnicKs--ineSteicrsiaSl tMudeythSoadmples will be generated according to the follow ing grid (Table 3). Table 3 Hour 48 Study Samples* - Cone., mg/L Number of Time Points No. of Tubes with No Soil (Control Sample) No. of Tubes with Each Soil/Sludge/ Sediment 0.0 -0.5 1 3x1=3 3 x 1 = 3 (x 5) 7 3 x 7 = 21 3 x 7 = 21 (x 5) *A c tu a l S tu d y S a m p le S e t m a y d iffe r fro m th is b a s e d o n re s u lts fro m s e c tio n 12.2. 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 II and III 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 CaCh solution containing no test substance. This is done by refilling with fresh Solution A until the weight of the container + contents is equal to the weight (0.1 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 removal constraints. See section 12.7 for spiking. 12.3.7 Replacement of 0.01 M CaCl2solution to study samples: Add an equal amount of fresh 0.01 M CaCl2solution (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. 12.3.11Make the appropriate calculations as defined in the calculations section. 12.3.12Determine the Desorption Kinetics. 12.4 Determination of Freundlich 12.4.1 Select appropriate soils Aandds/oorrpsteidoinmIesnottshaenrdm/osr sludges using the soils/sediments/sludges listed in section 8.1. Use the centrifuge tube material/type and soil:solution ratio determined for use from Method ETS-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/concentration combination 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 Cone., mg/L 1 o.o Soil:Solution Ratio Soil, grams mL of 0.01 M CaCU Solution (Solution A) Number of Time Points No. of Tubes No Soil (Control Sample) NA 0.00 12.5 0.1 2 3 No. of Tubes Each soil (or sediment or sludge) NA (JL O f 50 mg/L Stock Test Substance 0.00* ETS-8-160.1 Tiers II and III Sorption Studies Page 9 of 15 3M Environmental Laboratory Page 82 of 703 BACK TO MAIN -0.05 -0.2 -0.5 -1 -5 NA NA NA NA NA 0.00 0.00 0.00 0.00 0.00 12.5 + 0.1 12.5 + 0.1 12.4 + 0.1 12.25 + 0.1 11.25 + 0.1 2 2 2 2 2 3 3 3 3 3 NA 12.5* NA 50* NA 125* NA 250* NA 1250* 0.0 1:1 5.00 0.05 5.0 0.1 2 NA 3 (x5) 0.00* 0.0 1:5 2.50 0.05 12.5 + 0.1 2 NA 3 (x 5) 0.00* 0.0 1:25 1.00 0.05 25.0 + 0.2 2 NA 3 (x 5) 0.00* -0.05 1:1 5.00 0.05 5.0 0.1 2 NA 3 (x 5) 5.0* -0.05 1:5 2.50 0.05 12.5 + 0.1 2 NA 3 (x 5) 12.5* -0.05 1:25 1.00 0.05 25.0 0.2 2 NA 3 (x 5) ; 25* n o fo J r CM 1:1 5.00 0 .05 5.0 0.1 2 NA 3 (x 5) 20* 1:5 2.50 + 0.05 12.5 + 0.1 2 NA 3 (x 5) ; : 50* : -0.2 1:25 1.00 0 .05 24.9 0.2 2 NA 3 (x 5) 100* -0.5 1:1 5.00 0.05 5.0 0.1 2 NA 3 (x 5) 50* : -0.5 1:5 2.50 0.05 12.4 + 0.1 2 NA 3 (x 5) 125* -0.5 1:25 1.00 + 0.05 24.8 0.2 2 NA 3 (x 5) : : 250* : Only need one from -1 1:1 5.00 0.05 4.9 0.1 2 NA 3 (X 5) 100* this set. -1 1:5 2.50 0.05 12.25 + 0.1 2 NA 3 (x 5) 250*- -1 1:25 1.00 + 0.05 24.5 + 0.2 2 NA 3 (x 5) 500* Only need lione from this set. -5 1:1 5.00 0.05 4.5 0.1 2 -5 1:5 2.50 0.05 11.25 + 0.1 2 -5 1:25 1.00 + 0.05 22.5 + 0.2 2 NA NA NA To be adde d in a fte r the stud y sam ples have equilibrated fo r 12 hours. 3 (x 5) 3 (x 5) 3 (x 5) 500* : : 1250* : 2500* 12.4.4 Weigh the soil and record on the appropriate data form. 12.4.5 Add the appropriate volume of 0.01 M CaCk 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 +0.5 pH units. 12.4.7 The study samples are equilibrated with 0.01 M CaCh 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 times/dates 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 II and III Sorption Studies Page 10 of 15 3M Environmental Laboratory Page 83 of 703 BACK TO MAIN 12.4.9.4 Withdraw an aliquot fromthe test vessel and dispense into a prelabeled autovial. Replace the amount aliquotted with fresh 0.01M CaCh 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 times/dates on appropriate data forms. 12.4.10.2 Remove sample sets after 48 hours and record the date/time. 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 Cone., mg/L 0.0 -0.05 -0 .2 ~0.5 -1 -5 Number of Time Points 1 1 1 1 1 1 # of Tubes w/ No Soil (Control Samples) 3x1=3 3x1=3 3x1=3 3x1=3 3x1=3 3x1=3 # of Tubes w/ Each Soil (or sediment or sludge) 3 x 1 = 3 (x 5) 3 x 1 = 3 ( x 5) 3 x 1 = 3 (x 5) 3 x 1 = 3 (x 5) 3 x 1 = 3 (x 5) 3 x 1 = 3 (x 5) 12.5.2 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. 12.5.3 Replace the volume of solution removed with an equal volume of fresh 0.01 M CaCh solution containing no test substance. This is done by refilling with the aqueous solution until the weight of the container + contents is equal to (0.1 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. 12.5.4 Place the tubes back in the orbital shaker and gently rotate at 23 3 C for 48 hours. Record date/time on the appropriate data form. 12.5.5 Remove the tubes fromthe shaker after 48 hours and record date/time. ETS-8-160.1 Tiers II and III 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. 12.5.8 Spiking: Refer to Section 12.7 for spiking. 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 and/or PFBS internal standardprior 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 0 1 Weight of Soil, grams ~1.0 ~2.5 ~5.0 mL of MeOH to use 2.0 2.0 4.0 5.0 No. of Extractions 3 3 3 4 Total mL of Methanol 6.0 6.0 12. 20. 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. Centrifuge 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 of the study sample from step 12.6.10 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 II and III Sorption Studies Page 12 of 15 3M Environmental Laboratory Page 85 of 703 BACK TO MAIN 12.7 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 D a t a A n a l y s is a n d C a l c u l a t io n s 13.1 Data analysis and calculations should be done using the templates provided from OECD Guideline 106. 14.0 M e t h o d P e r f o r m a n c e 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 cone, analytical - Sample cone, analytical) x 100 (MS Spike cone, 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 Po l l u t io n P r e v e n t io n a n d W a s te M a n a g e m e n t ______________________ ________ 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 R ec o r d s 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 A t t a c h m e n t s 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 SoihAqueous Optimal Ratio Data Form . ETS-8-160.1 Tiers II and III Sorption Studies Page 13 of 15 3M Environmental Laboratory Page 86 of 703 BACK TO MAIN 18.0 18.1 { 18.2 R eferences 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 Adsorption/Desorption Isotherm, EPA 712-C-98-048, January 1998. 19.0 A f fe c t e d D o c u m e n ts 19.1 ETS-8-159 Preparation of Soil Samples for Preliminary (Tier I) Sorption Studies for Fluorochemicals as the Test Substance (Based on OECD Guideline 106) ETS-8-160.1 Tiers II and III Sorption Studies 3M Environmental Laboratory Page 14 of 15 Page 87 of 703 BACK TO MAIN 20.0 R e v is io n s Revision t Number. Reason For Revision 160.1 R equirem ents for specific test substance concentrations were taken out to accom m odate less soluble species and m atrix effects. The 1.00 m L sam ple size was elim inated to accom m odate dilutions o f the original sam ple. The 1:5 ratio sam ple size was adjusted to be consistent w ith the ETS-8-19.0 sam ple size. The adsorption kinetics section was revised to accommodate a serial sam ple preparation rather than ju st the parallel method. Revision Date ETS-8-160.1 Tiers II and III Sorption Studies 3M Environmental Laboratory Page 15 of 15 Page 88 of 703 BACK TO MAIN OECD/OCDE 106 Adopted : 21" January 2000 OECD GUIDELINE FOR THE TESTING OF CHEMICALS A dsorption - D esorption U sing a Batch Equilibrium M ethod 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 Umweltbundesamt (UBA), the University of Kiel, 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 States participated (3). An OECD Workshop on Soil Selection was held at Belgirate, Italy, in 1995 (4). The Workshop agreed on the main elements of the updated Test Guideline 106 for an adsorption/desorption test and, in particular, on the characterisation and selection ofthe soil types for use in the test. 2. Other guidelines concerning adsorption/desorption exist only at national level and are mainly focused on pesticides testing (5)(6)(7)(8)(9)(10)(11). These documents as well as an extensive relevant literature were considered when developing this Guideline. SIGNIFICANCE AND USE 3. 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 (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 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 (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 adsorption of a chemical. SCOPE 5. This Guideline is aimed at estimating the adsorption/desorption 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 function 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 substance with naturally occurring soils. 6. In this Guideline, adsorption represents the process of the binding of a chemical to surfaces of soils; 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 pm) generated by the soils is not fully"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 die adsorption/desorption 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 content and soil texture, and pH. It comprises three tiers: Tierl: Preliminary study in order to determine: - the soil/solution 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. Tier 2: Screening 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 Kre. Tier 3: Determination of Freundlich adsorption isotherms to determine the influence of concentration on the extent of adsorption on soils. Study of desorption by means of desorption kinetics/Freundlich desorption 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. PRINCIPLE OF THE METHOD - 10. Known volumes of solutions of the test substance, non-labelled or radiolabelled, at known concentrations in 0.01 M CaCl2 are added to soil samples of known dry weight which have been pre equilibrated in 0.01 M CaCl2. The mixture is agitated for an appropriate time. The soil suspensions are then separated by centrifugation 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 scintillation counting. However, liquid scintillation counting is an unspecific technique which cannot differentiate between the test chemical and its transformation products; therefore it should be used only.ifthe test chemical is stable for the duration ofthe study. INFORMATION ON 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 composition and radio-purity, is recommended. In the case of short half-life tracers, decay corrections should be applied. _ 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 105]; (b) vapour pressure [OECD Guideline 104] or/and Henry's law constant; (c) abiotic hydrolysis as a function ofpH [OECD Guideline 111]; (d) n-octanol/water partition coefficient [OECD Guidelines 107 and 117]; (e) ready biodegradability [OECD Guideline 301] or aerobic and anaerobic transformation in soil; (f) pKa of ionisable substances; (g) direct photolysis in water (i.e. UV-Vis absorption spectrumin water, quantum yield) and photodegradation on soil. APPLICABILITY 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 10), 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 preliminary study; if a transformation in the time scale of the test is observed, it is recommended that the main study be performed by analysing both soil and aqueous phases. 15. Difficulties may arise in conducting this test for test substances with low water solubility (Sw<10"`g 1"'), 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 reagents 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 OECD/OCDE - 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 pm from aqueous solution. The containers should be capped during agitation and centrifugation to avoid volatility and water losses. To minimise adsorption on them, deactivated caps such as PTFE (Teflon) lined screw caps should be used. (d) Optional: filtration device; filters of 0.2 |im 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. (f) Laboratory oven, capable of maintaining a temperature of 103 to 110 C. Characterisation and selection o f soils 18. The soils should be characterised by three parameters 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 adsoiption/desorption 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 CaCl2 (that is the solution used in adsorption/desorption testing) according to the corresponding ISO method (ISO 10390-1). It is also recommended that the other relevant soil properties be determined according to standard methods (for example ISO "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 adsorption/desorption 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 "Performance of the 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 characterised by 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. 3M Environmental Laboratory 4/45 Page 92 of 703 BACK TO MAIN OECD/OCDE 106 Table 1: Guidance for selection of soil samples for adsorption-desorption Soil type 1 2 3 4 5 6 7 pH range (in 0.01 M CaCl,) 4.5-5.5' >7.5 5.5-7.0 4.0-5.5 < 4.0-6.0* >7.0 <4.5 Organic carbon content (%) 1.0-2.0 3.5-5.0 1.5-3.0 3.0-4.0 <0.5-1.5s* <0.5-1.0s* > 10 Clay content (%) 65-8020-40 15-25 15-30 < 10-158 40-65 <10 Soil texture* clay clay loam silt loam loam loamy sand clay loam/clay sand/loamy sand * According to FAO and the US system (85). The respective variables should preferably show values within the range given. If, how ever, difficulties in finding appropriate soil material occur, values below the indicated minimum are accepted, f Soils w ith less than 0.3% organic carbon may disturb correlation between organic content and adsorption Thus, it is recom m ended the use o f soils with a minimum organic carbon content o f 0.3%. Collection and storage of soil samples 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 ISO standard on soil sampling (ISO 10381-6) should be followed with respect to the description of the sampling site; (b) the sampling site has to be exactly defined by UTM (Universal Transversal Mercator- Projection/European Horizontal Datum) or geographical co-ordinates; this could allow re collection of 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 b e co llected . E sp ecially fo r the soil no. 7 , i f a O h h o riz o n is p re sen t as p a rt o f th e soil, it sh o u ld be included in the sampling. - 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 preparation of soil samples for the test 5/45 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 possible. The soils are sieved to a particle size <2 mm; recommendations of the ISO standard on soil sampling (ISO 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 moisture content of each soil is determined on three aliquots with heating at 105C until there is no significant change in weight (approx. 12h). For all calculations the mass of soil refers to oven diy mass, i.e. the weight of soil corrected for moisture content. Preparation of the test substance for application to soil .28. The test substance is dissolved in a 0.01 M solution of calcium chloride (CaCl2) in distilled or de ionised water; the CaCl2 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 preparedjust before application to soil samples and should 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 (Sw< 10"*g l'1), 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 0.1%); 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 CaCl2 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 the test substance and co-solvent concentration would not be exactly the same in all tests. PREREQUISITES FOR PERFORMING THE ADSORPTION/DESORPTION 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 ofboth 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 appropriate volume of 0.01 M CaCl2, e.g. 100 cm!, is agitate_d 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 soil/solution ratio of 1:5 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 ofthe pre-equilibration solution. The solution is analysed. 35. One blank ran consisting of the system soil + CaCl2 solution (without test substance) must be included, in order to check for artifacts in the analytical 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 carrying 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 soil/solution ratios 38. Selection of appropriate soil to solution ratios for sorption studies depends on the distribution coefficient K4and the relative degree of adsorption-desired. The change of the substance concentration in the solution determines the statistical accuracy ofthe 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 Ka 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 Kd 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 Kdin the form of equation (1): " C f ( e q ) Kd'CjVeq) 7/45 3M Environmental Laboratory Page 95 of 703 BACK TO MAIN 106 OECD/OCDE Vq = ( m -l)Kd m soil ms(eq) m f(eq) or in its logarithmic form assuming that R = rno/V0and A %/100 = (A e q % /100) log R = - log K d + log (1 -A e q % /1 00) (1) (2) 0,1 1 10 100 1000 Distribution coefficient K (cm3 g-1) d Fig. 1 Relationship between soil to solution ratios and Kdat various percentages of adsorbed test substance 40. Fig. 1 shows soil/solution ratios required as a function of Kufor different levels of adsorption. For example, with a soil/solution ratio of 1:5 and a Kd of 20, approximately 80% adsorption would occur. To obtain 50% adsorption for the same Kd, a 1:25 ratio must be used. This approach to selecting the appropriate soil/solution ratios gives the investigator the flexibility to meet experimental needs. 41. Areas which are more difficult to deal with are those where the chemical is veiy slightly or highly adsorbed. Where low adsorption occurs, a 1:1 soil/solution ratio is recommended, although for some very organic soil types smaller ratios may be necessary to obtain a slurry. 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 Kd, one can go up to a 1:100 soil/solution ratio 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 Powvalues (Annex 4). This could be useful especially for low adsorbed/polar chemicals with Poi> < 20 and for lipophilic/highly sorptive chemicals with Pd>> 104. 8/45 3M Environmental Laboratory Page 96 of 703 BACK TO MAIN OECD/OCDE 106 PERFORMANCE OF THE TEST Test conditions 42. All experiments are done at laboratory ambient temperature and, if possible, at a constant temperature between.20 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 centrifugation conditions is given in Annex 5. . 44. If the centrifugation facilities cannot guarantee the removal of particles larger than 0.2 pm, a combination of centrifiigation and filtration with 0.2 pm 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 soil/solution 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 corresponding to theseratios can be different with respect to laboratory facilities: - 50 g soil and 50 cm' aqueous solution of the test substance (ratio 1/1); - 10 g soil and 50cm' aqueous solution of the test substance (ratio 1/5); - 2 g soil and 50cm' aqueous solution of the test substance (ratio 1/25). 47. The minimum amount of soil on which the 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 CaCl2solution (no soil) is subjected to precisely the same steps as the test systems, in order to check the stability of the test substance in CaCl2 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 50 cm' 0.01 M CaCl2solution (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. 9/45 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 cm3of 0.01 M CaClj overnight (12 h) before the day of the experiment. Afterwards, a certain volume of the stock solution of the test substance is added in order to adjust the final volume to 50 cm3. This volume of the stock solution added: (a) should not exceed 10% of the final 50 cm3volume of the aqueous phase in order to change as little as possible the nature of the pre-equilibration solution; and (b) should preferably result in an initial concentration of the test substance being in contact with the soil (C0) at least two orders of magnitude higher than the detection limit of the analytical method; this threshold safeguards 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 (C,,) 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 p.g cm'3and 90% adsorption are assumed; thus, the initial concentration of the test substance in contact with the soil should preferably be 1 |ig cm'3 (two orders of magnitude higher than the detection limit). Supposing that the maximum recommended volume of the stock solution is added, i.e. 5 to 45 cm30.01 M CaCl2equilibration solution (= 10% of the stock solution to 50 cm3total volume of aqueous phase), the concentration of the stock solution should be 10 fig cm'3; 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, 48 h). However, times of analysis should be considered with flexibility with 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. (af Parallel method: Samples with the same soil/solution 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 completely as 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. fbl 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(t,), 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 Kdvalue at equilibrium is also calculated. Based on this Kdvalue, appropriate ^ soil/solution ratios are selected from Fig.l, so that the percentage adsorption reaches above 20% and 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 A t or C^! 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. 61. 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. If no 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 and/or 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 soil/solution 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 of the 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 ofthe 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 extractions are 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 o f the concentration o f the test substance in the aqueous phase ( C ^ s ) versus time could also be used to estimate the achievem ent o f the equilibrium plateau (see Fig. 2 in A nnex 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, talcing into account the unstability of the test substance; in this case it is recommended to 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 Table 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 soil/solution 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 10) and 24 h contact time; the agitation time may be extended to a maximum of48 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 CaCl2 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 CaCl2solution (without soil) is subjected to the same test procedure, serving to safeguard against the unexpected. The test runs as described in paragraphs 52-59. 68. The percentage adsorption is calculated at each time point A, 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 adsorption kinetics test 69. The linear Kd 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 Kd < 1 cm5g'1are considered to be qualitatively mobile. Similarly, a mobility classification scheme based on values has been developed by McCall et al. (16). Additionally, leaching classification schemes exist based on a relationship between Kk and DT-503(32)(79). 70. Also, according to error analysis studies (61), Kd values below 0.3 cm3g'' cannot be estimated accurately from a decrease in concentration in the aqueous phase, even when the mosrfavourable (from point of view of accurancy) soil/solution ratio is applied, i.e. 1:1. 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 Kdis possible with the experimental protocol followed in this Guideline. Accurate determination is possible if the value which results by multiplying the Kdwith the soil/solution 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 kinetics/desorption isotherms 3 DT-50: degradation tim e for 50% o f the test substance. 12/45 3M Environmental Laboratory Page 100 of 703 BACK TO MAIN OECD/OCDE 106 Adsorption isotherms 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 into, 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 ofthe equilibrium concentration ofthe 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 Kp(Freundlich adsorption coefficient) values for different substances is only possible if these Kpvalues 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 desorption process also plays an important role in the behaviour of a chemical in field soil. Moreover, desorption data are useful 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 din 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 soil/solution 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 system to reach desorption equilibrium. In every experiment (one soil, one solution) one blank is run. It consists of the soil and 0.01 M CaCl2 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 CaCl2without 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 equilibriumis reached. 77. fbl 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 CaCl2without 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 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. The volume of each individual aliquot should be less than 1%of the total volume. The same quantity of fresh 0.01 M CaCl2solution is added to the mixture to maintain the soil to solution ratio, and the agitation continues until the next time interval. 78. The percentage desorption is calculated at each time point' Dt and/or time interval DAt (according to the needs of the study) and is plotted versus time. The desorption coefficient of at equilibrium is also calculated. All applicable equations are given in Data and Reporting Section and Annex 6. Results from desomtion kinetics experiment 79. Common plqts of the percentage desorption Dt and 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 cm1of aqueous solution is lg. The soil/solution ratio may be expressed in units of w/w or w/vol with the same figure. Adsorption - 83. The adsorption Ati 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, A,, is calculated at each time point t, according to the equation: A, = O . ) 100 (%) mo where: A t = adsorption percentage at the time point tj (%); (3) mads(t ) = mass ftest substance adsorbed on the soil at the time t (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 106 Detailed information how to calculate the percentage of adsorption A, for the parallel and serial methods is given in Annex 6. 84. The distribution coefficient Kdis 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. 7 Kj Cf(eq) _mf(eq) C (e q ) m(eq) (cm> g') (4) where: Cf(eq) C ( eq) msad!(eq) ma,> q ) content of the substance adsorbed on the soil at adsorption equilibrium (pg g 1); mass concentration of the substance in the aqueous phase at adsorption equilibrium (jig cm'); this concentration is analytically determined taking into account the values given by the blanks. mass of the test substance adsorbed on the soil at adsorption equilibrium (pg); mass of the test substance in the solution at adsorption equilibrium (pg); quantity ofthe soil phase, expressed in dry mass ofsoil (g); initial volume of the aqueous phase in contact with the soil (cm5). 85. The relation between Aiqand Kdis given by: Kd = 100 - A. where: A... Vo (cm'g1) m mil percentage of adsorption at adsorption equilibrium, %. (5) 86. The organic carbon normalized adsorption coefficient relates the distribution coefficient Kdto the content of organic carbon ofthe soil sample: Ko, Kd 100 %oc (cm'g 1) (6) where: %oc = percentage oforganic carbon in the soil sample (g g 1). Kk 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, Kwvalues 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 adsorption isotherms equation relates the amount of the test substance adsorbed to the concentration ofthe test substance in solution at 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 (Cad!(eq), elsewhere denoted as x/m) is calculated. It is assumed that equilibrium has been attained and that Cads(eq) represents the equilibrium value: 15/45 3M Environmental Laboratory Page 103 of 703 BACK TO MAIN 106 OECD/OCDE C -. t o - 21253) rH-enil [C ,, --C?(eq)]-Vo (E gg') The Freundlich adsorption equation is shown in (8): C f (eq) = K f E^ds(eq)l/" (pgg") or in the linear form: lo g C f (eq) = lo g K f + 1/n -IogC ^eq) (7) (8) (9) where: jr* n = Freudlich adsorption coefficient; its dimension is cm' g'1only if 1/n = 1; in all other cases, the slope 1/n is introduced in the dimension of KpJs (|lg (cm1)1* g"'); = regression constant; 1/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 Kpdsand 1/n are calculated by regression analysis using the equation 9. The correlation coefficient r of 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 ofthe 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 "Desorption" 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 (m^ corresponds to the sum of the test chemical masses extracted from the soil and surface ofthe test vessel with an organic solvent: ( 10) (Vrec Q e q ) + ntE) -100 MB (%) Vo Co where: MB mass balance (%); total mass of test substance extracted from the soil and walls of the test vessel in two steps (pg); C0 initial mass concentration of the test solution in contact with the soil (pg cm'1); 16/45 3M Environmental Laboratory Page 104 of 703 BACK TO MAIN OECD/OCDE 106 v ra = volume of the supernatant recovered after the adsorption equilibrium (cm3). Desorption 91. The desorption is defined as the percentage of the test substance which is desorbed, related to the quantity of substance previously adsorbed, under the test conditions: D, n Q t,) 100 (%) m fieq) (ii) where: D t = desorption percentage at a time point t. (%); m dcs(t ) = mass the test substance desorbed from soil at a time point t (pg); m a<l!(eq) =- mass f thetest substance adsorbed on soil at adsorption equilibrium (pg). Detailed information on how to calculate the percentage of desorption Dt. for the parallel and serial methods is given in Annex 6. 92. The apparent desorption coefficient (Kda) 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: ,, . m f ( e q ) - m - ( e q ) VT / , ,u 2) K d c s = ----------------- -------------------------------------------( c m & ) m aq (eq) rnsoil where: Kda = desorption coefficient (cm3g'1); m dos(eq ) = totalmass f thetest substance desorbed from soil at desorption equilibrium (pg); VT = total volume of the aqueous phase in contact with the soil during the desorption kinetics test (cm3). Guidance for calculating the m das(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 VT in the equation (12) is considered to be equal to V,,. Desorption isotherms " 93. The Freundlich desorption isotherms equation relates the content of the test substance remaining adsorbed on the soil to the concentration of 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 equilibrium is calculated as follows: , m"ds(eq) --mf" (eq) C s (eq) = -------------------------- ( p g g ) m .,, . (13) " mf" (eq) is defined as: 17/45 3M Environmental Laboratory Page 105 of 703 BACK TO MAIN 106 OECD/OCDE n C (e q ) = m ? (eq) 0 V.F TMA m aq (Mg) (14) where: C f(eq) -- content of the test substance remaining adsorbed on the soil at desorption equilibrium (Mg g '); < S(eq) mass of substance determined analytically in the aqueous phase at desorption equilibrium (jig); A m q mass of the test substance left over from the adsorption equilibrium due to incomplete volume replacement (|ig); < (eq ) mass of the substance in the solution at adsorption equilibrium (|ig); ' maAq=nC(eq) f vv 0 - VV R ^ (15) v rF volume of the solution taken from the tube for the measurement of the test substance, at desorption equilibrium (cm'); v R = 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 CaCl2solution (cm1); The Freundlich desorption equation is shown in (16): C fs(eq)= K f . C(eq)'/n (qgg') ^ or in the linear form: IogCfs(eq) = lo g K f + 1/n logC^(eq) (17) where: C (eq) Freundlich desorption coefficient; regression constant; mass concentration of the substance in the aqueous phase at desorption equilibrium (Mg cm'). The equations (16) and (17) can be plotted and the value of Kj" and 1/n are calculated by regression analysis using the equation 17. Remark: If the Freundlich adsorption or desorption exponent 1/n is equal to 1, the Freundlich adsorption or desorption binding constant (Kpds and K dcs) will be equal to the adsorption or-desorption equilibrium constants (Kdand KdJ respectively, and plots of C, vs C>qwill be linear. If the exponents are not equal to 1, plots of C, vs C 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 CaCl2); - organic carbon content; . - organic matter content; - nitrogen content; - C/Nratio; - Cation Exchange Capacity (mmol/kg); - all information relating to the collection and storage of soil samples; - where appropriate, all relevant information for the interpretation of the adsorption - desorption of the test substance; - reference ofthe methods used for the determination of each parameter. - information on the test substance as appropriate; - temperature of the experiments; - centrifugation conditions; - analytical procedure used to analyse the test substance; - justification for any use of solubilizing agent for the preparation of the stock solution ofthe test substance; - explanations of corrections made in the calculations, ifrelevant; - data according to the form sheet (Annex 7) and graphical presentations; - all information and observations helpful for the interpretation ofthe test results. 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Chu-Huang Wu, N.Buehring, Davinson J.M., and Santelmann, (1975), "Napropamide Adsorption, desorption and Movement in soils". Weed Science, 23, 454-457. 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.Br, 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, Run off and Erosion from Agricultural Management Systems, Chapter 19, Vol. Ill: Supporting Documentantion, USDA Conservation Research report. 50. ISO Standard Compendium Environment: Soil Quality - General aspects; chemical and physical methods of analysis; biological methods of analysis. First Edition (1994). 51. Scheffer F., and Schachtschabel P., Lehrbuch der Bodenkunde, F. Enke Verlag, Stuttgart (1982), 11th edition. - 52. 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Mller, (1995), "HPLC - screening method for the determination of the adsorption coefficient on soil - results of a ring test". Chemosphere 30(71.1373-1384. 76. W. Kordel, J. Stutte, G. Kotthoff, (1993), "HPLC - screening method for the determination of the adsorption coefficient on soil - comparison of different stationary phases. Chemosphere, 27(121. 2341-2352. 77. Hance, R.J., (1967), "The speed of Attainment of Sorption Equilibria in Some Systems Involving Herbicides". Weed Research, 2, PP- 29-36. 78. Koskinen W.C., and Harper S.S., (1990), "The retention processes: mechanisms" in Pesticides in the Soil Environment: Processes, Impacts and Modelling (ed. H.H. Cheng). Soil Sei. Soc. Am. Book Series, No. 2, Madison, Wisconsin. 79. 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 ofpesticides surface areas of soils". J. Chem. Soc., 3973-93. 82. Calvet R., Terc M., and Arvien J.C., (1980), "Adsorption des pesticides par les sols et leurs constituants: 3. Caractristiques gnrales de 1'adsorption". Ann. Agron., 31,239-251. 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., (1985), "Adsorption/desorption", in Joint International Symposium, Physicochemical Properties and their Role in Environmental Hazard Assessment, July 1-3, Canterbury, UK. 85. Soil Texture Classification (US and FAO systems): Weed Science, 33, Suppl. 1 (1985) and Soil Sei. Soc. Amer. Proc., 26, 305 (1962). 23/45 3M Environmental Laboratory Page 111 of 703 106 OECD/OCDE ANNEX 1 TESTING SCHEME BACK TO MAIN prerequisite ______ Tier 1 Tier 2 Tier 3 3M Environmental Laboratory 24/45 Page 112 of 703 BACK TO MAIN OECD/OCDE 106 Sym bol \ A. m r-fti) m f(eq ) ' m m'S( t .i ) < S( e q ) c,, c,, O ,) C :d!(e q ) c ; ds(e q ) v,, A va K, K,,, KKf 1/n D,, V ANNEX 2 DEFINITIONS AND UNITS D efinition a d so rp tio n p e rc e n ta g e a t th e tim e p o in t t. U nits % adsorption percentage at adsorption equilibrium m a s s o f th e te s t s u b sta n c e a d s o r b e d o n th e s o il a t th e tim e t. % M-g m ass o f the test substance adsorbed on the soil during the tim e in te rv a l At, -m ass o f the substance adsorbed on the soil at adsorption equilibrium m ass o f the test substance in the test tube, at the beginning o f the adsorption test Hg Hg ng m ass o f the substance m easured in "an aliquot ( v ^ ) at the tim e p o in t t. m ass o f the substance in the solution at adsorption e q u ilib riu m quantity o f the soil phase, expressed in dry m ass o f soil m ass concentration o f the stock solution o f the substance initial m ass concentration o f the test solution in contact w ith the soil m ass concentration o f the substance in the aqueous phase at the tim e t| th a t th e a n a ly sis is p e rfo rm e d content o f the test substance adsorbed on soil at adsorption equilibrium an equilibrium m ass concentration o f the substance in the aqueous phase at adsorption equilibrium initial volum e o f the aqueous phase in contact w ith the soil during the adsorption test v o lu m e o f the aliq u o t in w h ich th e te st su bstance is m easu red Hg M-g g Hg cm '1 d g cm '1 p g cm '1 gg g ' p g cm '1 cm 3 cm 3 ' distribution coefficient for adsorption organic carbon norm alized adsorption coefficient organic m atter norm alized distribution coefficient Freundlich adsorption coefficient Freundlich exponent d e s o rp tio n p e rc e n ta g e a t a p o in t tim e t, d e s o rp tio n p e rc e n ta g e c o rre s p o n d in g to a tim e in te rv a l At, cm 1 g'1 cm 1 g'1 1 -1 cm g pg (cm ) g %, % apparent desorption coefficient cm 1g'1 25/45 3M Environmental Laboratory Page 113 of 703 BACK TO MAIN 106 OECD/OCDE Sym bol K d=s m at ( A t i ) < s(eq) ma"(eq mf(A t.) m ,Aq C fs(eq) C(eq) vT V D va v; vrF MB mE VTM p~ pKa Sw D efinition Freundlich desorption coefficient m a s s o f th e te s t su b sta n c e d e s o r b e d fro m so il a t th e tim e t. U nits .. ^ M/il / lxIfti "I M-g (c m ) g tig m ass o f the test substance desorbed from soil during the tim e At, m ass o f substance determ ined analytically in the aqueous phase at desorption equilibrium total m ass o f test substance desorbed at desorption equilibrium tig tig tig m ass o f the substance rem aining adsorbed on the soil after the tim e in te rv a l At, m ass o f the test substance left over from the adsorption equilibrium due to incom plete volum e replacem ent tig tig content o f the test substance rem aining adsorbed on the soil at desorption equilibrium ' m ass concentration o f the substance in the aqueous phase at desorption equilibrium total volum e o f the aqueous phase in contact w ith the soil during the desorption kinetics experim ent perform ed w ith the serial m ethod volum e o f the supernatant rem oved from the tube after the attainem ent o f adsorption equilibrium and replaced by the sam e volum e o f a 0.01 M C aC lj solution volum e o f the aliquot sam pled for analytical purpose from the tum e (i), during the desorption kinetics experim ent perform ed w ith the serial m ethod volum e o f the solution tak en from the tube (i) for the m easurem ent o f the test substance, in desorption kinetics experim ent (parallel m ethod) tig g ' tig cm '1 cm 3 cm 3 cm 3 cm 3 volum e o f the solution taken from the tube for the m easurem ent o f the test substance, at desorption equilibrium m ass balance total m ass o f test substance extracted from the soil and w alls o f the test vessel in tw o steps * volum e o f the supernatant recovered after the adsorption e q u ilib riu m octanol/w ater partition coefficient cm 3 % tig" cm 3 dissociation constant w ater solubility g i'1 3M Environmental Laboratory 26/45 Page 114 of 703 BACK TO MAIN OECD/OCDE 106 ANNEX 3 Influence of Accuracy of Analytical Method and Concentration Change on Accuracy of Adsorption Results From the follow ing table (part o f ref. 84) it becom es obvious that w hen the difference betw een the initial m a s s (m ,, = 110 p g ) a n d e q u ilib riu m c o n c e n tr a tio n ( m `* (e q )= 100 p g ) o f th e te s t s u b s ta n c e in th e s o lu tio n is v e r y sm all, an error o f 5% in the m easurem ent o f equilibrium concentration results in an erro r o f 50% in the calculation o f th e m a s s o f th e s u b s ta n c e a d s o r b e d in s o il ( m "dl(e q ) ) a n d o f 5 2 .4 % in th e c a lc u la tio n o f th e K d. A m ount o f soil V olum e o f solution m ^, = 10 g V,, = 1 0 0 cm 1 < ( e q ) "C"ds(eq) (pg) (pg cm3) For A = 9% R mf(eq)* (Fg) Cf(eq) R' *(gg g'1) K * R' 100 1.000 101 1.010 B o 105 1.050 109 1.090 o For A =55% o Z; 5 0 .0 ii 50.5 o U 52.5 0.500 0.505 0.525 o bi) 5 5 .0 0.550 For A =99% true value 1% 5% 9% 10 1.00 9 . " : ; : 0 .9 0 ;5; : ' 0.50 : l,V : : 0.10 true value 1% 5% 10% 60.0 59.5 57.5 55.0 6.00 5.95 5.75 5.50 true value 10% 50% 90% 1 0.891 0 .4 7 6 0.092 true value 0.8% 4.0% 8.3% 12.00 11.78 10.95 10.00 10.9% 5 2 .4 % 90.8% 1.8% 8.8% 16.7% ii 1 .1 0 0 o B 1.111 1.155 1.21 0.011 0.01111 0.01155 0.0121 true value 1% 5% 10% 108.9 108.889 108.845 108.790 10.89 true value 990 10.88 0.01% 980 1.0% 10.8845 10.8790 0.05% 0.10% 942 899 4 .8 % 9.2% 1 * m f(eq) m f(eq) < (eq ) C fS(eq) O eq) R R* [C,, - CgS(eq)] V0 _ m,,- mfVeq), Cf(eq) = Kd m,, m:ds(eq) V0 mads(eq) msou = m ass o f the test substance in the soil phase at equilibrium , pg; = m ass o f the test substance in the aqueous phase at equilibrium , pg; = c o n te n t o f th e te s t su b sta n c e in th e s o il p h a se at e q u ilib riu m , p g g '1; - = m a s s c o n c e n tra tio n o f th e te st s u b sta n c e in th e a q u e o u s p h a se a t e q u ilib riu m , p g c m '3. = a n a ly tic a l e rro r in th e d e te rm in a tio n o f th e m "ds ( e q ) ; = calculated error due to the analytical error R. 27/45 3M Environmental Laboratory Page 115 of 703 BACK TO MAIN 106 OECD/OCDE ANNEX4 Estimation techniques for Kd 1. Estimation techniques permit prediction of Kdbased 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 erfHPLC on reversed phase* (74-76). As shown in Tables 1 and 2, is the K. oriC^ that are calculated from these equations and then, indirectly, the Kdfrom the equations: Ko, 100 K d %oc (cm3g 1) K. Kd 100 (em'g 1) 1.724 %oc 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 applicable in cases where the organic matter content of the soil is very small (12). In addition, although satisfactory correlations have 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 solubility are given in Tables 1and 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. Compounds Vl7 ;: Correlations :T Substituted ureas K,,m= 0.69+ 0.52 log Aromatic chlorinated Kk= -0,779+0.904 log Various pesticides log Km= 4.4+ 0.72 log PTO Aromatic hydrocarbons K^ = -2.53 + 1.15 log Pw Authors Briggs (1981) (Ref. 39) Chioueia/. (1983) (Ref. 65) Gerstl and Mingelgrin (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. Compounds ; l :Correlations:: . . ; : " Various pesticides log Kum= 3.8 - 0.561 log S,, Aliphatic, aromatic K = (4.040 +/- 0.038) chlorinated substances (0.557 +/- 0.012) log Sw a-naphtol logK. = 4.273 - 0.686 log S,, Cyclic, aliphatic logK = - 1.405 - 0.921 log S aromatic substances - 0.00953 (mp-25) Various compounds Km= 2.75-0.45 logS. Authors. Gerstl and Mingelgrin (1984) (Ref. 66) Chiou et ol. (1979) (Ref. 70) Hasset et al. (1981) (Ref. 71) Karickhoff(1981) (Ref. 72) Moreale van Blade (1982) (Ref. 73) D raft O EC D T est G uideline "Estim ation o f A dsorption C oefficient (Koc) on Soil and on Sew age Sludge using H igh P erfo rm a n ce L iq u id C hrom atography (H PLC ) " , 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 I. The centrifugation time is given by the following formula* assuming spherical particles: t = 7 1----- r ]ln ( % ) dr rP (i) For simplification purposes, all parameters are described in non-SI units (g, cm), where: Co = rpm = p= rp = p, = = R, = R^ = R^-R, = ^rotational speed (=2 rcrpm/60), rad s'1; revolutions per minute; viscosity of solution, g s'1cm'1; particle radius, cm; soil density, g cm1; solution density, g cm'3; ' 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 soil/solution 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 (p) and the density (p^) of the solution as equal to the viscosity and density of water at 25 C; thus, p = 8.95 x 10'3g s 'cm'1and P,,=l-0gcm '3. Then, the centrifugation time is given by the equation (2): /=____ ^ --------In* (rpm) -rp1 ( p , - \ ) Rt . (2) 3. From the equation (2) it becomes apparent that two parameters are important in defining the centrifugation condition, i.e. time (t) and speed (rpm), in order to achieve separation of particles with a specific size (in our case 0.1 pm radius): (1) the density of the soil and (2) the length of the mixture in the centrifuge tube (R^-R,), i.e. the distance which a soil particle covers from the tojr 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. la 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 cm3soil density, while it is only 50 min for 2.0 g cm3. Similarly, from Fig lb, for a classical centrifugation of 3000 rpm the centrifugation time is approx. 50 min 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 soil/solution phases, it is important to consider the possible existence of a third "pseudo-phase", the colloids. These particles, with a size less than 0.2 pm, can have an important impact on the whole adsorption mechanism of a substance in a soil suspension. When centrifugation is performed 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 adsorption/desorption 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. c uOJ Fig. la Variations of centrifugation time (t) versus centrifugation speed (rpm) for different soil densities (p,). R, = 10 cm, -R, = 10 cm, T| = 8.95 x 10'3g s'crn' and p>q= 1.0 g cm'3at 25C. 3M Environmental Laboratory 30/45 Page 118 of 703 OECD/OCDE BACK TO MAIN 106 Centrifugation speed (rpm) Fig. lb Variations of centrifugation time (t) versus centrifugation speed (rpm) for different lengths of the mixture in the centrifuge tube (Rb -Rt) = L; R, = 10 cm, T] = 8.95 x 10'3g s'cm'1, p = 1.0 g cm'1 at 25C and p_= 2.0 g cm'3. " 3M Environmental Laboratory 31/45 Page 119 of 703 BACK TO MAIN 106 OECD/OCDE ANNEX 6 CALCULATION OF ADSORPTION A (%) and DESORPTION D(%) 1. The time scheme ofthe procedure is: At} At2 At,,_-i At r-- i-- r. . . . . . . . . . i-- i t() tj ti t n-2 hi-1 Time t 2. For all the calculations it is assumed that the test substance is stable and does not adsorb significantly to the container walls. ADSORPTION A(%) a) Parallel method 3. The percentage adsorption is calculated for each test tube (i) at each time point (t), according to the equation: A,, = 100 (%) mo X ( 1) The terms of this equation may be calculated as follows: mo = Co V0 (jig) m f ( t i) = mo - O , ) Vo (//g) where: Ah = adsorption percentage (%) at the time point t; = mass of test substance on soil at the time ( that the analysis is performed (pg); C,, C(t,) V. = mass of test substance in the test tube, at the beginning of the test (pig); = initial mass concentration of the test solution in contact with the soil (pg cm3); = mass concentration of the substance in the aqueous phase at the time t that the analysis is performed (pg cm'3); 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 (cm3). - The values of the adsorption percentage At or C^s(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 applicable to both direct and indirect m ethods. All the other equations are applicable only to indirect method. 32/45 3M Environmental Laboratory Page 120 of 703 OECD/OCDE BACK TO MAIN 106 Fig. 2 Mass concentration of the test substance in the aqueous phase (CJ 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 the soil is calculated as follows: - for the first time interval At, = t, - 10 33/45 3M Environmental Laboratory Page 121 of 703 BACK TO MAIN 106 OECD/OCDE m s (At,) = mo --m^s(t,)- ( vvo vA V Va y - for the second time interval At^= q - 1, m ^ A t^ m (V K..A J i v 0- v M l Va ) for the third time interval At3= t3- 12 m .- ( A t,) = m i ( t 2). 'V0- v * ' -m,,rcad. tj)s- | V 0 - 2 ' V a V for the n* time interval At rt = t n - 1, n-l m r(A t,, ) = m" s (t11_l) ^V0--(n--2)-v* (Vq~(n~ l)'vA) (4) (5) (6) (7) The percentage of adsorption at each time interval, AAt. , is calculated using the following equation: m ;J,(At,) A*, = m,, 100 t ( 8) while the percentage of adsorption (A, ) at a time point t, is given by the equation: _ j*Aq 100 (% (9) The values of the adsorption A t. or AAti (with respect to the needs of the study) are plotted versus time and the time after which the sorption equilibrium is attained is determined. At the equilibration time teo: - the mass of the test substance adsorbed on the soil is: m f(e q )= X m l* (At,) Atj=l - the mass of the test substance in the solution is: ( 10) t m aq'(eq) = m 0 -- m "ds(At,) ( 11) and the percentage of adsorption at equilibrium is: 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 A= -too (%) t m. t ( 12) The parameters used above are defined as : m "d!(At,), mass of the substance adsorbed on the soil during the time intervals At,, At2,..., Atnrespectively (pg); m *(t,), m i ( t 2) ...... m * (t.) ,, a*JS m (eq) ,,n^aaqds (=q) A. A,,,, mass of the substance measured in an aliquot ( VA) at the time points t,, t2....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 (cm1); percentage of adsorption- corresponding at a time interval At (%); percentage of adsorption at adsorption equilibrium (%). DESORPTION D (% ) 5. The time t0that 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 of0.01 M CaCl2solution. a) Parallel m ethod 6. At a time point ti, the mass of the test substance is measured in the aqueous phase taken from the tube i (Vr`), and the mass desorbed is calculated according to the equation: ^aq (tj) -- m m (V } y j J m aq (13) At desorption equilibrium ts-- and therefore m|Jqs(ts) = m ^ s(eq) . T h e m a s s o f th e te s t s u b s ta n c e d e so rb e d d u rin g a tim e in te rv a l (Atj) is g iv e n b y th e e q u a tio n : < ( A t i ) = m ad" (ti) - m ^ a ) j=i 7. The percentage of desorption is calculated: at a time point t, from the equation: D < ( t,) 100 (%) m ds(eq) and during a time interval (At) from the equation: (14) (15) 35/45 3M Environmental Laboratory Page 123 of 703 BACK TO MAIN 106 OECD/OCDE t 100 (%) m fs(eq) where: (16) = desorption percentage at a time point t (%); D*. < (h ) = desorption percentage corresponding to a time interval At,(%); = mass of the test substance desorbed at a time point t, (pg); nC(At{) mass of the test substance desorbed during a time intervals At. (jig); ^0^ mass of the test substance analytically measured at a time t, in a solution volume V `, which is taken for the analysis (|lg); mass of the test substance left over from the adsorption equilibrium due to incomplete volume replacement (fig); < = < !(eq). v ,, - v R (17) < (eq ) mass of the test substance in the solution at adsorption equilibrium (jig); V = 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 CaCl2solution (cm'); v ; = volume of the solution taken from the tube (i) for the measurement of the test substance, in desorption kinetics experiment (cm5). The values of the desorption Dt| or D4t (according to the needs of the study) are plotted versus time and the time after which the desorption equilibrium is attained is determined. b) Serial m ethod: 8. The following equations take into account that the adsorption procedure, which was preceded, was carried out by measurements of the test substance in small aliquots ( vA) of the aqueous phase (serial method, paragraph 58). It is assumed that: a) the volume of the supernatant removed from the tube after the adsorption kinetics experiment was replaced by the same volume of 0.01 M CaCl2solution (VR) and b) the total volume of the aqueous phase in contact with the soil (VT) during the desorption kinetics experiment remains constant and is given by the equation: VT = V o -X (i) i=I 9. At a time point t. : (18) the mass of the test substance is measured in a small aliquot (v ) and the mass desorbed is calculated, according to the equation: < (ti) = (v0 i(VT-(i-l). ,)j _A l V." J ^ a q l VT J (19) At desorption equilibrium t, = t and therefore m^s(t ) = m^s(eq). The percentage of desorption D, is calculated, from the following equation: 36/45 3M Environmental Laboratory Page 124 of 703 BACK TO MAIN OECD/OCDE 106 D, = < ( , t , _)n 100 (%) m f(eq) 10. At a time interval CAtl: During each time interval the amount of the substance desorbed is calculated as follows: for the first time interval At, = t, - 10 maqS(At i) = (t,) and m f ( t ,) = (e q )-m ^ (A t | ) (20) ( 2 1 ). for the second time interval At, = t, - 1, VT ) = < '( t 2) |- (Vt- , D \ \ (A t,) -m,, (Vt- v.DP VT VT < '(t2) = m f (eq) - [m (At, ) + (At, )] (22) and - for the n"1time interval At = t - 1 , des... . maq (A t,,) -- des ^ I -IX mm On ) '| d (vT- ( n - l ) v aP)A - n-i x i=l,n*l f (vT - (n- Q- vf ) VT des 1maq (Atj) V and m i-(tB) = m f ( e q ) - m ^ A t , ) (23) Finally, the percentage of desorption at each time interval, D At , is calculated using the following equation: mijVAt.) D.ti= - ^ 7 - ^ - i 00 (%) 1 m s (eq) (24) while the percentage of desorption D t| at a time point t. is given by the equation: Z < (J) D- m t,,eqj S 100 = ^ tH'100(%) nC (eq) (25) where the above used parameters are defined as : mJ" (At,), m ^ iA tj).... ,m sd"(Atn) = mass of the substance remaining adsorbed on the soil after the time intervals At,, At,,..., Atnrespectively (jJ-g); md" (At,), md" (At2) ,... ,md" (AtJ < cs(t,), m d" (t2),... ,m d" (t,,) = mass of the test substance desorbed during the time intervals At,, At,,..., Atnrespectively (|lg); = mass of the substance measured in an aliquot ( v p ) at time points t,, t,,..., tn, respectively (pg); 37/45 3M Environmental Laboratory Page 125 of 703 106 vT V, 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 (p.g); V o - v ,A(i) - V R (26) ^ A_ V ,,-X vaA(i) < s(eq) V = 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 CaCl2solution (cm3); = volume of the aliquot sampled for analytical purpose from the tube (i), during the desorption kinetics experiment performed with the serial method (cm3); vf < 0.02-VT (27) 3M Environmental Laboratory 38/45 Page 126 of 703 BACK TO MAIN OECD/OCDE 106 ANNEX7 A D SO R PT IO N -D E SO R PT IO N IN SO ILS: D A T A R E PO R T IN G SH EETS Substance tested: * - Soil tested: D ry m a s s c o n te n t o f th e s o il (105C , 12 h ) : ......................................................................................................................................................... % T e m p e ra tu re : ................................................................................................................................................................................................................. " C Suitability ofthe analytical method W eighed soil Soil: dry m ass V olum e o f C aC l2sol. N om inal cone, final sol. A nalytical cone, final sol. g g cm ' pg cm ' M-g c m ' Principle o f the analytical m ethod used: C alibration o f the analytical m ethod: 3M Environmental Laboratory 39/45 Page 127 of 703 BACK TO MAIN 106 OECD/OCDE Substance tested: Soil tested: D ry m a s s c o n te n t o f th e s o il (105C , 12 h ) : ..........................................................................................................................................................% T e m p e r a tu r e :....................................................................................................................................................................................................................."C A nalytical m ethodology followed: Adsorption test: test samples Indirect D irect I I Parallel s" ` Symbol Units Tube No. Weighed soil Soil: dry mass Water vol. in weighed soil (calculated) Vol. 0.01 M CaCl to equilibrate soil Vol. stock solution -- v ws g g cm1 cm1 cm' Equilibration Equilibration Equilibration Equilibration Time Time Time Time Total volume of aq. v. phase in contact with cm' soil Initial concentration C0 Test solution P-gcm' Mass test subst. at m, beginning o f test Pg After agitation and centrifugation Indirect Method Parallel method Cone, test subst. aq. phase Blank correction included Serial method Measured mass test subst. in aliquot v * O tJ mJfCt.) - M-gcm'1 pg I Directmethod ` M ass test su b stan ce adsorbed on soil '**' * ` * -*> > , -* ..... ` .. . Calculation of adsorption Adsorption A >, % % Means Adsorption coefficient K., cm' g'1 11 Means Adsorption coefficient K_ cm' g 1 1 1 r1 Means 40/45 3M Environmental Laboratory Page 128 of 703 BACK TO MAIN OECD/OCDE 106 Substance tested: Soil tested: D r y m a s s c o n te n t o f th e s o il (1 05C , 12 h ) : ......................................................................................................................................................... % T e m p e r a t u r e : ...................................................................................................................................................................................................................."C A d so rp tio n test: blanks an d control Sym bol U nits T ubeN " - W eighed soil W ater am ount in w eighed soil (calculated) V olum e o f 0.01 M C aC l solution added V olum e o f the stock solution o f the test substance added T otal volum e o f aq. phase (calculated) Initial concentration o f the test substance in aqueous phase ,V. .V-*:- V^ - :o'rV." ' A fter agitation a n d cen trifugation , / C oncentration in aqueous phase g cm 1 cm 1 cm 1 cm 1 p.g cm '' H-g c m '1 4 B lank 00 R em ark: A dd colum ns if necessary .1 . ' !I B lank S tij C ontrol 00 -- -- 3M Environmental Laboratory 41/45 Page 129 of 703 BACK TO MAIN 106 OECD/OCDE Substance tested: , Soil tested: t D r y m a s s c o n te n t o f th e so il (1 05"C , 12 h ) : ......................................................................................................................................................... % T em perature: ........................................................................................................................................................................................................." c M ass balance * Symbol U nits - Tube No. W eighed soil Soil: d ry m ass - ms* W a te r v o lu m e in w e ig h e d soil Vws (calculated) g g ml V ol. 0.01 M C aC l2 sol. to equilibrate soil ml V olum e o f stock solution T o tal vol. o f aq. phase in contact w ith soil Initial concentration T est solution v0 c,, cm 3 cm 1 pg cm 1 E quilibration tim e A fte ra g ita tio n 'a n d c e n trifu g a tio n t h '1 C one, test subst. aq. phase at adsorption equilibrium blank correction included C (eq ) P g cm '1 E quilibration tim e v"*' Sv R em oved volum e aq. phase A dded volum e o f solvent 1st e x tractio n w ith solvent ? ;.v > u ,, .* * V. AV , '>: l" h -~v a cm 3 cm 3 ' 'C Signal analyzer in solvent var. C one, test substance in solvent M ass subst. extracted from soil & vessel walls .................................................. R em oved volum e o f solvent CF, AV, P g cm '5 Pg cm 3 A dded volum e o f solvent '2 n d e x t r a c t i o n w i t h s o l v e n t ' Signal analyzer solvent phase C one, test subst. in solvent &M ass subst. extracted from soil vessel walls AV' ` s* cE! \ mH T otal m ass test subst. extracted in tw o m E steps cm 3 ` var. p g cm '5 Pg Pg M ass balance MB % " 42/45 3M Environmental Laboratory Page 130 of 703 BACK TO MAIN OECD/OCDE 106 Substance tested: Soil tested: D r y m a s s c o n te n t o f th e s o il (1 05C, 12 h ) : ......................................................................................................................................................... % T e m p e r a tu r e :...................................................................................................................................................................................................................."C A dsorption isotherm s Sym bo 1 U nits Tube No. W eig h ed soil Soil: d ry m ass W ater volum e I n w eighed soil (calculated) m s d. VwS g g cm 3 V olum e 0.01 M C aC l sol. to equilibrate the soil V olum e o f stock solution added Total volum e o f aq. phase in contact w ith soil (calculated) V, cm 3 cm 3 3 cm C oncentration solution C. p g cm '1 E quilibration tim e -h A fter agitation and centrifugation < C one, test substance in aqueous phase, blank correction included T em perature C ^(eq) Pg cm ' *C A dsorbed m ass per unit soil C fieq ) Pgg' ' '* 1 ' ' v > '. - V " Regression analysis: value of Kpds: v a lu e o f 1/n: re g re s s io n c o e ffic ie n t r1: 3M Environmental Laboratory 43/45 Page 131 of 703 BACK TO MAIN 106 OECD/OCDE Substance tested: Soil tested: D r y m a s s c o n te n t o f th e so il (105C , 12 h ) : ......................................................................................................................................................% T e m p e r a t u r e : ......................................................................................................................................................................................................................"C A nalytical m ethodology followed: D eso rp tio n test Indirect Parallel EHseriai Sym bol U nits T ube N o. com ing from adsorption step Tim e in te rv a l Tim e in te rv a l T im e in te rv a l T im e in te rv a l M ass o f substance adsorbed on soil at adsorption equilibrium m ffeq ) Rg R em oved volum e aq. phase, V replaced b y 0.01 M C aC l2 cm 3 Total volum e o f aq. PM phase in co n tact w ith soil SM M ass test subst. left over the ad sorption equilibrium due to incom plete volum e replacem ent v0 V, m . D esorption kinetics ' : isj j cm 3 cm 3 M-g ' y - - 'y - M easured m ass o f substance d e s o r b e d fr o m s o il a t tim e t. V olum e o f solution taken from the tube (i) for the m easurem ent o f the test substance PM SM -reo v; V? M-g cm J cm 3 M ass o f substance desorbed fro m s o il a t tim e t, (c a lc u la te d ) M ass o f substance desorbed fro m s o il d u rin g tim e in te rv a l At, (calculated) D esorption percentage > y ! ; y itg [K- y y 'v: 'Ci' .Al- D esorption at tim e t % D , D e s o rp tio n a t tim e in te rv a l At, D a>, % A pparent desorption coefficient PM : Parallel m ethod SM : Serial m ethod ' r y yyy E-: - :vt --i -, ! "( 44/45 3M Environmental Laboratory Page 132 of 703 BACK TO MAIN 3M Environmental Laboratory M ethod A nalysis of Potassium Perfluorooctanesulfonate or Other Fluorochem icals in W aste Stream or W ater Extracts U sing H PLC -Electrospray/M ass Spectrometry Method Number: ETS-8-155.0 Author: Mark L. Anderson, Mark E. Ellefson Approved By: Adoption Date: ltj(o(co Revision Date: Laboratory Manager 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-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 133 of 703 BACK TO MAIN 1.0 Sc o p e a n d Ap p l ic a t io n _________________________________________ ____________ 1.1 Scope: This method describes the analysis ofwaste stream of water extracts using HPLCelectrospray/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 Su m m a r y o f M e t h o d ______________________________________________________ _ 2.1 This method describes the analysis offluorochemicals or other electrosprayionizable compounds extracted fromwater, using HPLC-electrospraymass spectrometry (HPLCES/MS). The analysis is performedbythe mass selection ofa single ion characteristic ofa particular compound, such as the perfluorooctanesulfonate (PFOS) anion, m/z = 499 or perfluorooctanoate (PFOA), m/z = 413. 3.0 D e f in it io n s _____________________________________________________________ _ 3.1 Atmospheric Pressure Ionization (API): The Micromass PlatformLCZ single quadrupole system and other commerciallyavailable LC/MS systems allow for various methods of ionization byutilizing a varietyof sources, probes, and interfaces. These include but are not limited to: ElectrosprayIonization (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 ofionization performed at atmospheric pressure, wherebyions in solution aretransferredto the gas phase via tiny charged droplets. These droplets are produced bythe application ofa strong electrical field. 3.3 Mass Spectrometer (MS): The PlatformLCZand other commerciallymanufactured ES/MS systems are equipped with a single quadrupole mass selective detector. Ions are selectively discriminated bymass to charge ratio (m/z) and subsequently detected. 3.4 Conventional vs. Z-spray probe interface: The Micromass Platform LCZ system utilizes a "Z -spray" conform ation. T he spray em itted from th e 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 ofoperation, cleaning, and maintenance are the same. However, Zspraycomponents 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 commerciallymanufactured ES/MS systems mayhave similar features. 3.5 Mass Lynx Software: Systemsoftware designed for the specific operation ofMicromass LCZMass spectrometer. CurrentlyMassLynx 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 PlatformLCZUser's Guide). ETS-8-155.0 Page 2 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 134 of 703 BACK TO MAIN 4.0 W a r n in g s and C a u tio n s_____________________________________________________ 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 ofapproximately 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 abackpressure of400 bar (5800 psi). Ifthe backpressure exceeds 400 bar, the HP1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences______________________ ;____________________________ 5.1 To minimize interferences when analyzing samples, Teflon shouldnot be used for sample storage or anypart of instrumentation that comes in contact with the sample or extract. 6.0 E q u ipm e n t _________________________________________________ 6.1 Equipment listed belowmaybe modified in order to optimize the system. Document any modifications in the rawdata as methoddeviations. 6.1.1 Micromass PlatformLCZMass Spectrometer equipped with an electrospray ionization source. 6.1.2 HP1100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler. 7.0 Su p p l ie s a n d M a t e r ia l s_____________________________________________________ 7.1 Supplies 7.1.1 High purity grade nitrogen gas regulated to approximately 100 psi (or house air system.). 7.1.2 HPLCanalytical column, such as a Betasil C18 column (50x2mm, 5 pmparticle size) or equivalent. 7.1.3 Capped autovials or capped 15 mLcentrifuge tubes. ETS-8-155.0 Page 3 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 135 of 703 BACK TO MAIN 8.0 R e a g e n t s and Stan dards____________ ;______________________________________ _ 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent. 8.1.2 Milli-QTMwater (ASTMtype I), all water used in this method should be Milli-QTM water or equivalent, andmaybe provided bya Milli-Q TOC Plus systemor other vendor. 8.1.3 Ammonium acetate, reagent grade or equivalent. 8.1.3.1 When preparing different amounts thanthose listed, adjust accordingly. 8.1.3.2 2.0 mMammonium acetate solution: Weigh approximately 0.300 g ammoniumacetate. Pour into a 2000 Lvolumetric flask, add the appropriate volume ofMilli-Q water, mix until all solids are dissolved. Store at roomtemperature. 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 Sa m pl e H an d lin g ___________________________________________________ 9.1 Standards and sample extracts are stored in capped autovials or capped 15 mL centrifuge tubes until analysis. 9.2 If analysis will be delayed, standards and sample extracts maybe refrigeratedat approximately4 Cuntil analyses can be performed. 10.0 Q u a l it y C o n t r o l _________________________________________________________ _ 10.1 Solvent Blanks, Method Blanks and Matrix Blanks 10.1.1 Solvent blanks, methodblanks, andmatrix blanks areprepared and analyzed with each sample set to determine contamination or carryover. 10.1.2 Analyze a method blankanda matrix blankprior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Matrix spikes are preparedfor each sample set and analyzed to determine the matrix effect on the recovery efficiency. 10.2.2 Matrix spike duplicates are preparedperiodicallyto measure the precision associated with the analysis. 10.2.3 Analyze the matrix spike andmatrix spike duplicate (ifprepared) in the same run as the original sample. 10.2.4 Matrix spike andmatrix spike duplicate concentrations should fall in the mid-range ofthe initial calibration curve or should be prepared at 1.5-5 times the endogenous ETS-8-155.0 Page 4 of 9 Analysis ofPotassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 136 of 703 BACK TO MAIN concentration ofthe 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 (CCV) are analyzed to verify the continued accuracy ofthe calibration curve. 10.3.2 Analyze a mid-range calibration standard after everytenth sample, with a minimum ofone per sample set. 10.4 Internal Standard/Surrogate Standard 10.4.1 An internal standard (IS) maybeused to quantify the target analytes by establishing a relationship between the ratio ofanalyte response to IS response and a known concentration ofthe analyte of interest. The IS shouldbe spiked at an amount that will fall within the mid-range ofthe calibration curve. The IS should be added after the extraction process and before analysis. 10.4.2 A surrogate standard may be used for qualitycontrol. The surrogate is used to quantitativelyevaluate the entire analytical procedure including sample preparation and analysis. The surrogate shouldbe spikedto fall within the low to mid-range of the calibration curve. 1 1 .0 C a l ib r a t io n a n d S t a n d a r d iz a t io n ___________________________________________ 11.1 Analyze the standard curves prior to and following each set ofextracts. The average oftwo standard curves maybe plotted by linear regression (y = mx + b) weighted 1/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 Ifthe calibration curve does not meet acceptance criteria performroutine maintenance or prepare a new standard curve (ifnecessary) andreanalyze. 11.3 For purposes ofaccuracywhen quantitating low levels ofanalyte, it maybe necessary to use the low end ofthe calibration curve rather than the full range. Example: when attempting to quantitate approximately 10 ppb ofanalyte, generate a calibration curve consisting ofthe standards from 5 ppbto 100 ppbrather than the fiill range ofthe curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression w eighting o f high concentration standards. 12.0 P r o c e d u r e s____________________________________________ .________________________ _ 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 ofthe name ofthe instrument (T for Tucker), the year (00 for 2000), the month (04 for April), and the day (T001012 for October 12, 2000). Ifmore than one list is made on the same day, use increasing letters ofthe alphabet starting with A at the end ofthe list. ETS-8-155.0 Page 5 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 137 of 703 BACK TO MAIN 12.1.1.2 Assign a method (MS) file. 12.1.1.3 Assign an HPLCprogram(Inlet file). 12.1.1.4 Type in sample descriptions andvial 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 Typicallythe analytical batch run sequence begins and ends with a set of solvent standards. 12.1.4 Samples are analyzedwith a continuing calibration verification (CCV) injected after everytenth 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 trayaccording to the sample list prepared in Section 12.1.1. 12.2.2 Attach the proper analytical column in the column heater compartment. Ifusing 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 HP1100 using the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.1.1.1 Sample size = 10 |iL injection 12.1.1.2 Flowrate = 300 pL/min. 12.1.1.3 Cycle time = 10.0 minutes 12.1.1.4 Mobile phase components: Solvent A: 2.0 m M A m m onium Acetate Solvent B: Methanol (MeOH) Solvent Gradient: Time (min.l 0.00 1.00 4.50 8.00 8.50 10.0 %B 5.00 % 5.00% 95.0 % 95.0% 5.00 % Stop ETS-8-155.0 Page 6 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass 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 ETS9-36, "Operation andMaintenance ofthe Micromass PlatformLCZ Electrospray/Mass Spectrometer". 12.4.2 Check the solvent level in reservoirs and refill if necessary. 12.4.3 Check the tip ofthe stainless steel capillary at the end ofthe probe with an eyepiece. . The tip should be flat with nojagged edges. Ifthe tip is found to be unsatisfactory, disassemble the probe andreplace the stainless steel capillary. 12.4.4 Turn on the nebulizing gas. 12.4.5 Open the tune page. Click on `Operate' to initiate the desolvation heaters. 12.4.6 Open the Inlet Editor. 12.4.5.1 Set HPLC pump to "On". 12.4.5.2 Set the solvent flowto the desired flow rate. 12.4.5.3 Observe droplets coming out ofthe tip ofthe probe. A fine mist should be expelled with no nebulizing gas leaking aroundthe tip ofthe probe. Readjust the tip ofthe 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 liters/hour 12.4.6.2 ESI nebulizing gas 10-15 liters/hour 12.4.6.3 HPLC constant flowmode, flow rate 10 - 500 |iL/min 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 studybinder with copies taped into the instrument run logbook. 12.4.7.1 All copies must be initialed and dated. 12.4.8 Click on startbutton on the MassLynx toolbar. Ensure start and end sample numbers include all samples to be analyzed. 13.0 D a ta A n a l y sis and C a lc u la tio n s__________________________________________ 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 Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 139 of 703 BACK TO MAIN %Recovery = Observed Result - Background Result x 100 Expected Result < 13.1.2 Calculate percent difference using the following equation: %Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 13.1.3 Calculate actual concentration ofanalyte in matrix (|J.g/mL): On-Column Concentration (|xg/mL) x Dilution Factors = Calculated Concentration 14.0 M e t h o d P e r f o r m a n c e ___________________________________________ _ 14.1 The Limit ofQuantitation (LOQ) is method, analyte, andmatrix 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 blankvalues must be < Vi that ofthe lowest standardused in the calibration curve. 14.3 The coefficient ofdetermination (r2) value for the calibration curve must be greater than or equal to 0.980. 14.4 Continuing Calibration Verification (CCV) percent recoveries must be 30% ofthe standard concentration. 14.5 Internal Standard recoveries should be within 50% ofthe spiked concentration. 14.6 Ifcriteria listed in this methodperformance section are not met, maintenance maybe performed on the system and samples reanalyzed or other actions as determined bythe analyst. Document all actions in die rawdata. 14.7 If data is to be reportedwhen performance criteria have not been met, the data must be footnoted on tables and discussed in the text ofthe report. 15.0 P o l l u t io n P r e v e n t io n an d W a st e M a n a g e m e n t __________________________ 15.1 Sample extract waste and flammable solvent is disposed in high BTUcontainers, and glass pipette w aste is disposed in broken glass containers located in the laboratory. 16.0 R ecords _______________ ;___________________________________________ 16.1 Each page generated for a studymust have the following information included either in the header or hand written on the page: studyor 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 fromMassLynx and other applicable information to include in the appropriate study folder. Copythese 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 of9 Analysis ofPotassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry 3M Environmental Laboratory Page 140 of 703 BACK TO MAIN 16.4 Print data integration summary, integration method, and chromatograms, fromMassLynx, and store in the study folder. t 16.5 Summarize datausing suitable software and store in the study folder. 16.6 Back up electronic data to appropriate medium. Record in study notebook the file name and location ofbackup electronic data. 17.0 At t a c h m e n t s _____________________________________________________ _ 17.1 None 18.0 R e f e r e n c e s _________________________________________________ __ 18.1 Platform LCZ User's Guide, Micromass UKLimited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.2 MassLynx NT User's Guide, Micromass UKLimited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.3 MassLynx NT Guide To Data Acquisition, Micromass UKLimited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.4 ETS-9-36.0, "Operation and Maintenance ofthe Micromass PlatformLCZ Electrospray/Mass Sprectrometer". 19.0 Af f e c t e d D o c u m e n t s_____________________________________________________ 19.1 None 2 0 .0 R e v is io n s ______________________________________________________________________ Revision Number. Reason For Revision Revision Date ETS-8-155.0 Page 9 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-EIectrospray/Mass Spectrometry 3M Environmental Laboratory Page 141 of 703 BACK TO MAIN 3M Environmental Laboratory M ethod Analysis of Potassium Perfluorooctanesulfonate or Other F luorochem icals in W ater E xtracts Using H P L C -E lectrospray/M ass Spectrometry/M ass Spectrometry Method Number: ETS-8-110.0 Author: Kris Hansen, Lisa Clemen Approved By: Adoption Date Revision Date: (LU H Group Leader Date ^ ( Date 1.0 S c o p e a n d A p p l ic a t io n __________________________________________________________ 1.1 Scope: This method describes the analysis ofwater 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 of 9 3M Environmental Laboratory Page 142 of 703 BACK TO MAIN 2.0 S um m a r y o f M e t h o d ________________________________________________ ___________________ 2.1 This method describes the analysis of fluorochemicals extracted from water, using HPLCt electrospray 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/z= 499 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 S03-) 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 D e f in it io n s _____________________________________________________________ ________________ 3.1 Atmospheric Pressure Ionization (API): The Micromass Quattro II triple quadrupole systems and other commercially available LC/MS 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 (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-charged droplets are produced-by-the-applicatien-ofa strong electrical field; --- ----- 3.3 Mass Spectrometry, Mass Spectrometer (MS), Tandem Mass Spectrometer (MS/MS): The API Quattro II triple quadrupole systems and other commercially manufactured ES/MS/MS systems that are equipped with quadrupole mass selective detectors. Ions are selectively discriminated by mass to charge ratio (m/z) and subsequently detected. A single MS may be employed for ion detection or a series (MS/MS) for more specific fragmentation information. 3.4 Conventional vs. Z-spray probe interface: The latest models of Micromass Quattro II 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 (i.e., 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 software designed for the specific operation of the Quattro II 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 II triple quadrupole MassLynx or MassLynx NT User's Guide). ETS-8-110.0 Analysis of Water Extract Using HPLC-ES/MS/MS 3M Environmental Laboratory Page 2 of 9 Page 143 of 703 BACK TO MAIN 4.0 W a r n in g s a n d C a u t io n s ______________________________________________ ___________ _ 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 gloves, eyewear, and clothing. 4.2 Cautions: 4.2.1 Operate solvent pumps below aback 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. 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 Quattro II triple quadrupole Mass Spectrometer equipped with an electrospray ionization source 6.1.2 HP1100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler 7.0 Supplies and Materials_____________________________________________________ 7.1 Supplies 7.1.1 Hsyisgthempu) rity grade nitrogen gas regulated to approximately 100 psi (House air 7.1.2 High purity grade argon regulated to approximately 6 psi. 7.1.3 HPLC analytical column, such as a Betasil C18 column (50x2mm, 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-QTM water (ASTM type I), all water used in this method should be Milli-QTM water or equivalent, and may be provided by a Milli-Q TOC Plus system or other vendor ETS-8-110.0 Analysis of Water Extract Using ES/MS/MS 3M Environmental Laboratory 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 Sample Handling________________________________________________ ____________ 9.1 Standards and sample extracts are stored in capped autovials or capped 15 mL centrifuge 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. 10.0 Quality Control_______________________________________________ __ 10.1 Solvent Blanks, Method Blanks and Matrix Blanks I0.T.T- Solventblanks, method blanks and mtrix blanks are prepared and analyzed with 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 Massaotrciixatsepdikweidthupthliecaatneaslyasries.preparedperiodically to measure the precision 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 C a l ib r a t io n a n d St a n d a r d iz a t io n 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 1/x, not forced t through zero, using MassLynx or other suitable software. 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 (MS) file _____________ ___________ _____ 12.1.1.3 Assign an HPLC program (Inlet file) 12.1.1.4 Type in sample descriptions and vial position numbers 12.1.2 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 MS/MS 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 o f 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 HP1100/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 ES/MS/MS Page5of9 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 = Time 0.00 min. 1.00 min. 4.50 min. 6.50 min. 7.00 min. 9.00 min. MeOH 40% 40% 95% 95% 40% 40% 2.0 mM Ammonium acetate 60% 60% 5% 5% 60% 60% 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 II Triple Quadrupole Mass Spectrometer Fitted with an Atmospheric Pressure 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 the tip. The tip should be flat with nojagged edges. If the tip is found to be ^siclbiy7<lisassem5Il&e probe and replace the stainless steel capillary. 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". 1122..33..66..32 OSebtstehrevefldorwoptolet1s0c-om50i0nguLou/mt oinf tohreatsipapopfrtohperpiartoeb. e. A fine mist 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 liters/hour 12.3.7.2 ESI nebulizing gas 10-15 liters/hour 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/MS/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 ES/MS source is recommended for 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 D a t a A n a l y s is a n d C a l c u l a t io n s _____________________________________ __________________ 13.1 Calculations: 13.1.4 Calculate matrix spike percent recoveries using the following equation: %Recovery = Observed Result - Background Result x 100 Expected Result 13.1.5 Calculate percent difference using the following equation: %Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 13.1.6 Calculate actual concentration of PFOS, or other fluorochemical, in matrix __________ (pg/mL):_______ ___ _____ _______________ ______ fne of PFOS calc, from std. Curve x 0.8 Dilution Factor! x 1 ug (Initial Volume of matrix (mL) + mL of Surrogate Standard! 1000 ng Final Volume (mL) 14.0 Method Performance______________________________________________________ 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, Method 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 r2value for the calibration curve must be 0.980 or better. 14.4 Matrix Spikes 14.4.1 Matrix spike percent recoveries must be within 30% of the spiked concentration. 14.5 Continuing Calibration Verifications 14.5.1 Continuing calibration verification percent recoveries must be 30% of the spiked concentration. ETS-8-110.0 Analysis of Water Extract Using ES/MS/MS 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 R e c o r d s ______________________________________________________________________ ___________ _ 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 fromMassLynx 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 1/x, then print these graphs and store in the study folder. -----16:4--Printdataintegration summary, integrationmethodrand chromatograms, fromMassLyny, 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 Tables. Diagrams. Flowcharts, and Validation Data______________________ 17.1 None 18.0 R e f e r e n c e s _____________________________________________________________________________ 18.1 ETS-9-24.0, "Operation and Maintenance of the Micromass Atmospheric Pressure Ionization/Mass Spectrometer Quattro II Triple Quadrupole Systems" 19.0 Affected Documents________________________________ _______________________ None ETS-8-110.0 ' Analysis of Water Extract Using ES/MS/MS 3M Environmental Laboratory Page 8 of 9 Page 149 of 703 BACK TO MAIN 20.0 R ev isio n s Revision Number. Reason For Revision Revision Date ETS-8-110.0 Analysis of Water Extract Using ES/MS/MS 3M Environmental Laboratory 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 Ratio/Mass 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 SampleID SoilType Soilweight, grams (20g) 100mLCaCI2 solution Equilibrate4 hours (Yes/No) Centrifuge (Yes/No) Comments 1 2 34 E00-1311-0001 E00-1311-0002 ST--1 ST=1 r-CfoOsrv-y MO, 030e]a _/%<?#$$-3- cm c E00-1311-0003 ST=1 EOO-1311-0004 ST--2 jitx, 0,W0MO33-Y E00-1311-0005 ST=2 ' tf. 3TO-7- EOO-1311-0006 EOO-1311-0007 EOO-1311-0008 ST=2 ST=3 Uts>^ ST=3 I .Z.-nCt SC fi. mosytity EOO-1311-0009 ST=3 * EOO-1311-0010 ST=Sed 720>..D0Z3l0<7SV* EOO-1311-0011 ST=Sed 2.0 oDZCjS "g EOO-1311-0012 ST=Sed EOO-1311-0013 EOO-1311-0014 ST=Slg ST=Slg DAS' t)JS 0. M. 0136?^ 9233V EOO-1311-0015 ST=Slgi>5^)^^ Ie!^72- *> 4/ 56 MC'S) u j 'CJyi- "Z \i\) . \ '; <jIU' 1 VAy A i --* 7 Col. 2 ST-1 7 ' C D 0 & r - S ~ 3 ST-2 TLR OP OfeS-fcM ST-3 ~TC fc~0Q 0kt?-7)> Col. 3 Col. 4 Col. 5 Col. 6 ST-SedftOn OltfS - I Q ST-SIg T Z l ? - D O < c ~ - Q ' t $ V- TZ.t2-'OO>$~--o z. U 91(4-Balance I D _____________________________________ <J:3o ,^ T/D/l - ? : 3r/A / J o / a s f -D / - 3 - </?_y 0.01 M CaCI2 Soin ID #: T t t ) \ ' 3 i ' ! T/D/i i'.3>f>/r\ Il 1 I 1 m ) C h i ( L Inc. ID X - I 5>__________________ Start T/D/l U / ni /ht) cm C_ Stop T/D/l/ / 5 D f l ^ O /D.-X (Y ) f i r \ C T/D/l 5?; 0 A tn H /OcX 103 CfO C iC-l-Cci 'O* (-1 iie o)4 rMft - MT<C . ' / i S 'joi OrvC AsUUcJL 13 . 5 ^ 1 - ^ r / s '/ nr/ c*1o* 0 ) iC e io /C So S+eri ocv^ /-1 Im I I ( 3 j ^ C / t < ? 5 SV c.-tr' LviAcUir r^Vric^'ri-''--V\c*-v .V\ GLP Study Number: E^O-1311 *4 / t c\ / o t c i ' ^ c a Vepie. ..r \ h C 0 (ix- A l l e i s i u^-K \ ri. d-ic<y Page__ _ of ' 3 3M Environmental Laboratory Page 152 of 703 Suitable Analytical ETS-8-159 Section 12.2 BACK TO MAIN Test Substance: PFOS SI sojd-H-i* 3M Environmental Laboratory Page 153 of 703 $ ?P c_ P F r> 2 e (QTQ)l <D en - fc . owv) I ( V AddUciL IS. ^..L THPPO) E s O C O O f - 0 9 - o , , / / r / l ( Test Substance: PFOS ETS-8-159 Section 12.2 Suitable Analytical Vi 7s H O s > BACK TO MAIN Suitable Container ETS-8-159 Section 12.3 CT-1 lO ' -fjlY {'u jjP t . C T -4 .j > J 2 _ CT-2,U ; L i C T -5_________________ CT^_HoS--I 0 5 C o ir r i d i '1- "Q a n Z i a J f. (a) 0.0 mg/L Test Subs. Soin ID C u x - o t - ? > - IQ t (b) 0.1 mg/L Test Subs. Soin ID c r. i - 3 -oT (f) 1 mg/L Test Subs. Soin ID-i t - x i w .- ? i - l u 1 -- ( ? ) C o la Inc. ID X - 1 3 _________________ /?7yx, StartT/D/l ________i t / IS /C O r_ r y \ c J Stop T/D/l / J 3 n / H /O O f Col 9 C2> T/O/lJ : o o it / l Li m l C.m C spike Soin id PH5S (5 0 0 0 i * Cam x( 3 ~> T/D/l / 7 / ; ( i/iv /fti f t - MeOH IP T l u f t - * 4 7 / > C J/ T/D/l i '. Tt> M /|S~ / op r e K ' Col 13 ( 2 ; T/D/l 11 3c? Il I I S - ! a ) - C ol14 ,,, Spike Soin I D Q C C O * ~ 3 3 - l t > ______ InternalStandardID C fc t-O t ^ ^ Lf>C 3 ) T/D/l r j O It / IfT / a i 'Z Test Substance: S /^ 3 / o | CS':@ C oen t- 3 3 --o i? 3M Environmental Laboratory Page 155 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 TCOS> T est S u b stan ce SampleID SoilType SoilrSolnRatio , Sampimu g SoilWeight(grams) 0.01MCaCI2Addition Equilibrate12hours Equilibrateforxhours AddSpikeSoin(uL) Comments iE, i co aa oIc K 3z s q ai1an-oao e03 Xa fS !oi I I i 3 Cu ia OE?OCV5) '1 :2.. 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 EOO-1311-3001 krr-l ,, 0 0 NA 0 SI \ u I t I I H w M . CUv ;,w: Oil u l - i l O C* E00-1311-3002 -- 0 0 v.NAi 0 S1 00-1311-3003 -- 0 0 :Ina^ 0 SI I EOO-1311-3003 -- 0 0 :NA' 0 $1 : v>:':y:va ! "l. EOO-1311-3004 y4^- ^Ortr 5 t : 0 St - -'jrr. 600-1311-3005: N r -- s&sr r-xa 0 si EOO-1.311-3006 14<1 -- rimi St EOO-1311-3006 : _ -05 3 i# i 0 St EO-1311-3007 (lM:\ _ 0 0 3 nA:.^ 48 $1 if- --- > ij ;uv Y 5 S :.{} H@Sf - 4 Lus: s | i '4 S I- - "-k te-fj'.r'tf: IS i n i lpi ii * *-' ''i V M 7- M fn ii TIM/t-/1I7> CP\CSy C/VVNC O p. H-'M OmC QOJ - EOO-131.1-3008 i' EOO-1311-3009 -- E00-1311-3009 life. _ E00-1311-3010 - 0 0 W;;: 48 si: : 0.0 fife/: 48 SI 0 0 48 si i s m 3na3; 48 ir S i r ^ m f ' ft K ill rule i l S fl-iiric! II n. SH lSf i ll^ l p i W .S M S i vfiiSip. ST.;.-.` ~T plfmm 600-1311.3011. -- ^rr & im 48 ifi :E00-1311-3012: i;*te - /-OS ?*W 48 ai i'M 00-1311-3Q12 -- *$% INa> 48 SI I f f iP W ft t u lliip n '5 i i % t e s i L 7 pip; c 1M 1 H & ? s H il ;& __ - / "yPJ.~ EOO-1311-3013 Clay 0.0 1:1 0 SI I W i H I . -7 L' E00-1311-3014 i:^\ Clay E00-1311-315: Clay . E00-1311-3015 t Clay E00-.1311-3016' Clay 0.0 00 0.0 0.0 1:1 0 sii:3 7 S ? 11 0 iSt 0 0 5 2 1:1 0 M- -------- 1:5 0 Sf 'J .S 2 1 - - im .., 1 - * - . M i ` " t"Jirm . ` - ' 4 i $K~S'' <"r - ' /--i U ZE E00-131-3017 |U|? Clay 0.0 1:5 0 -St Q .V S ? EOO-1311-3018: 4lr: Clay 0.0 1:5 0 Mi if ! fefr B l f m J' E00-1311-3018 ?MS^ Clay 0.0 1:5 0 a -- P Ip E0-1311-3019 Clay 0.0 1:25 0 Sf / 2 6 V lip t ST _ * ^ ;( o ) .E00-311-3020 Clay 0.0 1:25 0 St A o u > ivM/l ' l# E0-1311-3021 :Li' Clay 0.0 1:25 0 SI D. H <7 0 E0-1311-3021 MS: Clay 0.0 1:25 0 M -- ;.EOO-13.11-3022 Clay 0.0 1:1 48 feti s r o / o l EOO-1311-3023. Clay 0.0 1:1 48 tes 5 7 CoO'i 'E00-1311-3024 lilit-: Clay 0.0 1:1 48 st W i l l EOO-1311-3024 | s : Clay 0.0 1:1 : 48 g E0-1311-3025' .00^1311-3026 EOO-1.311-3027': u Clay 0.0 H U 48 . l i `I a l i t i Clay 0.0 1:5 48 te .S - D 3 Clay 0.0 1:5 ! 48 si 2 . S 2 00-1311-3027 M$ Clay 0.0 --5 I 48 tei E0-1311-3028 '''4ir' Clay 1 o.o : 1:25 I48 Mil) / d o 7 O .EOO-1311-3029 Clay 0.0 1:25 ; 48 J S A O / S i p E00-1311-3030 Ci| Clay 0.0 1:25 I 48 I51 0 . 9 4 $ * -0M311-3030 MS Clay 0.0 1:25 48 i T pfw Cji t r M g ij B r TiSS : U KM Mg Q S 3 _L B l5 g - TS r U m ilila i &*W' f l p lu>.1554 O.b if H e l L l o ) 1 S : SI.l i l l a .iter Jl.lL.l3t, 0*7 ki a i ^.lO,icJ Ir rm io ' 3M vii M u.iu 1 .1 1 j / .... Ir i % -.i- 1 V lU ri^. ----- *^*- H L 2 _ S ^ j ;u\!Z ___________________ -TT36 trf-W (4 8 h r)ln c.lD _ coi 13T/D/i u til / a: r m c >70 Start T/D /I U f f l / C> f W C o n 4 T/D/l /a ? /C o k ) / V Q Q S d P * t ' lcL kC i C ol 8 Baallaannccee iIDd / / ________ T/D/l S . ' l ^ V f n f Y a h y T t L o , ^ Stop T/D/l t&'.CO i < ^ i ( / C C ~>K Co) 11 Test Subst IDtX_V_.-_0^_**'3 - ( f Col 9 CiaCI2 Soin ID T/D/l $' ^ Ji -C7 _jJUC oO T/P/l/_t_f _'J__. _Q____ i ii f / %fj%) / jO C > ^ c 'f iW T Inc. ID 3 " - / 3 Start T/D/l > ' " / * / / v<* C Col 15 Balance ID T/p/i^.'yS ________________ " /QLLCt^ C Col 16 T/D/l J / 6 Q / Col 17 Spike Soin ID T/D/l yP-QO / q2- Internal Standard ID< DO lOffr* PF5 OOo-c - I`i Loppi* T tj-pp-JS Stop T/d V T Z Q U Q \ tCQ Cj# * T/D/l j / IS ' . ! <3- n p Q C-w-i C LrvV-TV TV-' iti - / u ^ k li Sh-sd u,uk , r/./ub'd;, ^ , . 1 ^ ,5 eRo-i ;a fra <) c c H/,<,/ o , (I)AU rPfo,,^ | /,,v,^ beW o <p* kW Cmc M /'ii/fli <aT) f (3>(te) Wep i.ACu-rvcl-^ v' ujwW ir te CW , i 111 O O l s<L ' 6<: S -o g /L Pp3 5p/k>ci. t e r t 4. Due g)(fg)COr\C = 5-O^j//- >iVof O Sm^lu c t- n / n l " I GLP Study Number: T/7Z> - /J / / 3/W Environmental Laboratory >($0) r.l I c b i - S0/,U a fOj S^Ojt//t --- 12$^^ " I!5* d " / ^ C f J s (-c*. / t lot p-S \ it Page 156 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 Test Substance Sample ID Soil Type SoihSoIn Ratio Soil Weight (grams) 0.01 M CaCI2 Addition Equilibrate 12 hours " ^ v je s t Substance Equilibrate for x hours centrifuge (Y/N) Add Spike Soin (uL) Comments U v50j r?x. CN S *0 g AHO* 'i-, to O4L- s 40 JI, J1 N4 -J -x _ 5 > a-2cir3 In t j < t#> - O E .o in3 c. 5 KI a - Is 1 ' t o ' 3 4 5 8 M 8 . E00-1311-3031 0Clay r-O-5 1:1 0 'M : W 5 T E00-1311-3032 Clay 1:1 0 'M . M i t n EOO-1311-3033 i p Clay 1:1 0 S i , O / J EOO-1311-3033 fe l Clay E00-1311-3034 Clay jr 1:1 0 * i i 1:5 0 O S o /4 EOO-1311-3035 I J 4 ' Clay -tfto 1:5 0 W : EOO-1311-3036 g b Ctay E00-1311-3036 Clay s t 1:5 0 l l A . S V 7 & 1:5 0 f ---- ; E00-1311-3037 b i| Clay Q5' 1:25 0 S1 L o / D E EOO-1311-3038 p i ' Clay E00-1311-3039 IUi'1 Clay 1:25 0 f / o o o t 1:25 0 i f e l A / 0 2 . T V E0-1311-3039 f i l s Clay X 1:25 0 - s i EOO-1311-3040 E00-1311-3041 EOO-1311-3042 I# 1 g ii* Clay Clay Ctay EOO-131.1-3042 l i f e 1 Clay 4 5 S.S M X5 1:1 2 l i 4 M t n o 1:1 2 w 4 V h ! 1:1 2 v 4 M X 5 5 1:1 2 si l -- -- E00-1311-3043 JS -: Clay fr5 EOO-131 T-3044 Clay sQ'5 1:5 2 m 1:5 2 f i t Wk EOO-1311-3045 Clay /1 5 1:5 2 Isti Z S 3 1 EOO-1311-3045 life : Clay 1:5 2 3 EOO-1311-3046- 111': Clay EOO-1311-3047 IM .- Clay s s 1:25 2 w /* D h U O 1:25 2 M h o n . EOO-1311-3048 1. E0-1311-3048 ; EOO-1311-3049 il*** EOO-1311-3050 : p : E00-1311-351 - I S EOO-1311-3051 - f e i Clay Clay s t i i Clay .-erb Clay Clay frS' Clay frf? r 1:25 2 1 h 0 2 $ 7- 1:25 2 __ ___ 00331:1 4 ' i t i 5- " 1:1 J J S L a S S " " 1:1 * . t e i r o / m 1:1 4 EOO-1311-3052 Clay 1:5 4 S Z S 0 J EOO-1311-3053 :M lr E00-1311-3054 - i n Clay Clay 0.5 0.5 1:5 4 # z s / oe r 1:5 4 Mi Z c t c o E00-1311-3054 : Clay 1:5 4 t o . : EOO-1311-3055 w Clay ^ 5 ^ 1:25 4 to EOO-1311-3058 PP- Clay 1:25 _ l j S ' / . c h / / E00-1311-3057 Clay 1:25 4 i # L B m z ; EOO-1311*3057 I I E0O-1311-3058 Clay ~ 1 :2 5 Clay n s 1:1 4 ---------- - 8 jj W EOO-1311-3059 ; 4 Clay 1:1 8 si n m s v E00-131-3060 i | l Clay ME00-1311-3060 Clay EO-1311-3061 - Clay EOO-1311-3062 'EOO-1311-3063 ' Clay Clay EOO-1311-3063 | i Clay 4T5 ^3- 1:1 8 I I L h K z 1:1 8 ; -- 1:5 8 "Sil: '.-043 1:5 8 s Z . 5 U Z 1:5 8 to '7 3 W 1:5 8 tofj -- -- EOO-1311-3064 .An Clay ;4- EOO-1311-3065 Clay 1:25 8 I f /. U M 1:25 8 :sf L O O S 4 2*EOO-1311-3066 |ij Clay 1:25 8 /S 205 ~ rr ts 5. X a " c l E 1 1! i3 03 n i a! 10 1 12 13 14 C M - '- T 15 J U J 17 / 18 l ~ < i \ l - u - f H i 11 fS ! ' - , V . l& X 'W 'k - \ " T S ift - M r m V .! 11r ^ y i C i1 3 fo o l -- . : .. * 1 - -O VC.VW C :7^~ wSm if? - j WMk 73 - 3 CQ s j^ i .jfe O - Si \h^ 4i fils ' ili -S - mm ij/ 1L . a -- IS M oPhL -4M-tr; 0 1 r~ ~r -, g l i S - _C _- x !--- 1 g _$ - S fte j L ~ r IJ _ . M fc u L -~ _ 4- m .. i i - r L r >! L l - n __ | i L"_ Z - iS i 75^1 kd i S S iii 2m -a T S i t - 4 s iS a is 3 IpO/g - ';U ': 3PS :| S 1 fe s i? .s S f B i W / -L w SR | S S i li i? . N ~7 L P , O S u 3 L J _________________ A - -- < -- I l __________ n ____ I : 0 > L _ 1 5 !? Pi I 1 1 J l A 'm r t o fa . _t S 3 ji L T j 'iiiiz c l I y j 2. f 4 't _ ) 1 ____ 1 " S iitPi?! [ (y 4 -fei 11S I isSlSl#: i f S j. V p i y L _ ____________ ^v ______ ' V. ^ 4r* i2 ^L *| S ::# : V1S J j L_____________ _________ .> ^ 1Ifru_N_ S i l i __________________________ Soi! Type 1D-T/LOV- 7 Z fr2 .-o ^ o ic S '~ 7 7 Soit Type 2 (Sed) 7 Z j* ~ o c o L>V - 7 O Col 8 Balance ID T/P/lSTj Start T/D/l ( O M tf *1 I*#*IC CwAl' Stop T /D /l/J l JC i l<X) / & ' tn r& Co110 f4Tr?Inc. I D ^ " 3 stari T/D/l ifrc It t i p /CO t > * C sto^T/D /iJ 0 <7 <2.) C # n (* Col li i s S H Inc. ID T - 1 3 Start T/D/l T 00 i l / f.M l' Slop T/D/l T' C u1 il i3l >IC T/D/l/ tJW ./ / 5 -/ f.M -C ("d \C o i-irin C . ID X - t 2 Start T/D/l t o ' n / J 1 C-Ct - M Stop T/D/l 1'.(-jf) 1 hbllC t CjY\ Coi 13 T/D/l i 1: l.'i i 1 lO L yv- C Col 14T/O/l t n o j j lU lO C^~ L 15Col Ralancoin `/`Z TiDni'. <4$ t y - i i 0 0 C ^ 'io - 3 P H ) l j z / J u * Lc^ -- ' 4 --' Ii/o/ot) C.lvX - S-o \L-- 4/rt/ov cj-c- GLP Study Number: CXgg>COCD1- 3 ^ a l CWVK. M( \<\i O \ Col 17 Spike Soin IDCPOO ''<=' 3 P T m fO'OO ID f 7 IQQ (A c Internal Standard ID Oti o J / ~ ~~I *7 T/D/l I/'/to i X ! 1 ! 0 0 C (2>ltoto ? `V.'i.lfiri &*" cVi/M-f, t w / /c .' flA ltji/S , Sfn^enxh'A t-A d~ J- (c) vue q/|C,/o,- _ ^ <?S S-foi-ed C i-r ^ c ^ r m rICD 2iiO<Vcf -finwS ilre lot/Urti (iAtr\ ti^cl 6p/vi (Seenne 4 /io I ci 2 o f/ ? 3M Environmental Laboratory Page 157 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 Test Substance Sample ID Soil Type Soil Weight (grams) 0.01 M CaCI2 Addition Equilibrate 12 hours Equilibrate for x hours centrifuge (Y/N) A dd Spike Soin (uL) Comments a E0 !1 c0 n 1 Mc0 C r tn3 CO li ) 2? i CD 413 s 3 1 a. 0E x a s ic ||x V M >3O. i3 1W * 0: O jz V 's cn dc 1 s . 3 4 5 6 S - 8 00-1311-3067 fe r- Clay r 1:1 16 i i V . ^ 7 / i 00-1311-3068 i g Clay -O lf 1:1 16 W : S . 0 3 5 00-1311-3069 | g Clay " i 1T~ 1:1 16 p 00:1311-3069 ! m s Clay ^ 0 .5 1:1 16 p 00-1311-3070 I t e Clay "0 .5 1:5 16 t * Z . S 2 4 I 00-1311-3071 i n Clay " 0 'sT 1:5 16 S1 2 . V % 8 ' - 00-1311-3072 f 00-1311-3072 g s Clay Clay "O T" 1:5 1:5 16 i t i 7 . S 0 O O 16 t e - ____ 00-1311-3073 1 Clay - o l T 1:25 16 p i A o i f l 00-1311-3074 E j Clay ^oS' 1:25 16 1 9 10 r-nv: J 11 Vv^C \ 12 13 rx v / CM U 14 _ .-- tc 15 _ - ~1 - l ____ - i_ .. ts , -- -. -. _ - 18 ' '- . I - tv A i / i. / IS T M B -L /-7 /C c / a i~ 7 i rsO ML rn V C S t* \^ A C une ^ " < r tX K \X -v ^ '` -d i vJ 2 u S j X $ S A jr s. z $ -XT V. A 0- 1 cr 3V v*J I N C" \ VJ 5: <3 tv \ 'A C 1 -3 a A tV d V ? 1- I Vu. 5 < wV 4 u `U 0"\ V J & % 7t & V/ 00-1311-3075 V . - Clay 1:25 16 Mt O W N ! 00-1311-3075 MS Clay - 03 " 1:25 16 W . EOO-1311-3076. \ h Clay . 00-1311-3077 W M Clay 1:1 24 * , S 7 Q ) Z V 1:1 24 M i 6s - . -- " ' _ - , _ L- ! V IV - rfe j- m i M EOO-1311-3078 | Clay 1:1 24 W W T 3 S S '` H t-- . i fe E0-1311-3078 `MS Clay SG.5 1:1 24 u. .. 1 . ffa jL -00-1311-3079. Clay .JS6S- 1:5 24 S1 - "1 3 fS ^ EOO-1311-3080 : p i i =EOO-1311-3081 M l Clay Clay ^5 " 1:5 24 I p r 2. S O W 21:5 24 S I . y n s n tir : - Q t f --i t r j J r A: 00^1311-3081 Clay S^ r- 1:5 24 S1 - "- ? j ; 5) : EOO-1311-3082 W i\ Clay t r r 1:25 24 : fc l . c & H 11 S fm 00-1311-3003 Clay EOO-1311-3084 iMp b * * ' Clay & $ r 1:25 24 w / D O W JSS 1:25 J A I B 0 / 8 7 X If / _r LS E0-131-3084 M s Clay &3T 1:25 1 7 38$ " 1l r m J - 1 -- 7 ] ------------------- ; -- 1J 00-1311-3085 F EOO-1311-3086 f i l i ; EOtM 311-3087 00^1311-3087 1 $ : : EOO-1311-3088 g 00-1311-3089 m Clay Clay Clay Clay Clay Clay A5 JM r 0T5 e ^ 1:1 36 M 9 7 & I 1:1 36 M t / 1:1 36 M 6:0091 1:1 36 1:5 36 s i 2 . H O 1:5 36 S 2.S 3 0 8 I I \ \ _. . . - * ~ j l? t n Z J iu / J V ih /I m W o< , i/V v e ' 7 o /> 6 ) / / 3 --/ y fA - _ r 1 _ I - _, t T iS l r . VV A . v ' : 00-1311-3090 Clay 03 1:5 36 " i l 7 . H 1 1 \^ K l 1 :1 1 n i ^ VJ > ; E00-1311-3090 i S Clay EOO-1311-3091 Clay EOO-1311-3092 Clay E00-1311-3093 00-1311-3093 . EOQ-1311-3094 Clay f s Clay p Clay : 00-1311-3095 fe' Clay 00-1311-3096 li Clay 00-1311-3096 Clay E0-1311-3087 i r : Clay *0ET 1:5 s*F5 1:25 &US STS' 1:25 1:25 1:25 1:1 - 1:1 jOrS- 1:1 1:1 *--- 1:5 36 36 s i L O N O 36 j 1 f . m y o 36 w , L D f l Z 36 M 48 Sj S c o l t a 48 H W W T 48 :B! 6 7 0 O 7 > 48 st -- 48 2 . W 7 5 \ t. :1 1 I I j - nr FT _ Si r & J - ] ( 'l l ) . I r . l ,.i e . n 0\ . . nT -- T Y ! / li = X ... i N/ ' - - - b,<- i - i - 1 7.040% 7. rO . !a i L 7 c;i?7c _ ,__ - > -i.1 -- b B r/PS w P -- -- 2 it i V * fi i ' -* . - 1 EOO-1311-3098- te ' Clay E0-1311-3099 - i l Clay *OT5~ 1:5 1:5 48 St Z . S / 7 9 48 te 2 . V S 5 7 j _j A.p 5 . h- S f EOO-1311-3099 00-1311-3100 00-1311-3101 EOO-1311-302 MS- Clay ite Clay i~ Clay Clay MS 1:5 AS-- 1:25 *5-- 1:25 & s- 1:25 48 't e 48 O . W 9 48 - 'I l O 5 `1 48 - L P t i l V r~L- O _____-- .; .. A. J - JKlSO ci r S i 1 - S r i c d l j 1 A.5. t _T 7_ _ IT *""L _ -3 - L . < '&t. L S TA m vI ^ ------------- NT irst ti ~JVP2 ----------------------------------j j r ______________________ i j 52 3 Sol! Tvoe 1 rtICA.Cn 1/Z - OOO j - 7 r Soil Type2fSedl TH - c n h t ' - T o Col M (16Urline. ID X -->^ 1 Start T/D/IX wt*- t / ccur .m [ StoD^ T/D/l .1 /3 c /C C > vC 1 Col 11 Test Subst ID 0 C O I s 1 - u s-_ T/(DO/ ,U ___ tJ. s 3 \ ' 3 o i ex' f / P C o l W ine. ID i ~ - i > Col 8 Balance ID i / p C o lio ( 2 % Inc. ID Start T/D/I ? 3c -i U S 1 lii l-z-rfi L-U. Col 9 CaCI2 Soin ID C ^tX -r - S3 -6 T < r T/D/i 5: io u u s / c*-1 Start T /D /I^'-^ S it Oft / er' ColSTtioZffp('3LT6/7pDir/)i'TInc'.QIDa_-* 5 Start X/p/l (S^iy n_ / /OfJ ( ^ sioD rm r M // /^/ /JC O n<Col 13 T/D/I O../0 >%! 1 / C < Col 14 T/D/I L?K O / 2 / /T ^ Xal40>M eQH Dil'n Soin I D ' T N s f t *" M 7 15 3 ( c .'ULnry-ta, ^ W s / ' tH ( i ^ / a/VD O t Q ' v e* ^ V ^ lV i/v C o r r fc U i V\U>V\13^ i t. f(S-"- \ id h lo o u o ' t StopyO,tCK u~~i t C o l4 0 (4 W r) Inc. ID _ Z Start TIDlttMO JtR jeX O H L Stop VOnJD'L'i . 7 / 1 0 -' T/DIt / 0 ; D W / -7 / m C 4 - M Col 15 Balance ID * 7 ^ T/D/I /QW*> i~t ( / C t e H f W h --------------- - T " -- !-- rf>Col^SDkeSolnlD 000OI - 3 3 ' 0 3 lQff*^ ? i (M -^ ^ X n t o ' r ^ c t - e Cvv\<~ u ( l ~ l x> 0 J ( 3 ^ ) C o-vc x 5 . o ,, J l. H / i * 1^11t K C . GLP Study Number: T/D/I J0 on 19/ 7 / 0 0 ,-jL^jt. ry^a /) : O oe )- 3 D - / y J ( y -- T HP P * i l \ ', t> 3 / 7 / 0 0 1 3of/ 6 3M Environmental Laboratory Page 158 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 Test Substance Sample ID . . Soil Type Soil Weight (grams) 0.01 M CaCI2 Addition Equilibrate 12 hours Equilibrate for x hours centrifuge (Y/N) Study Sample | Comments 2 3. r*jo-;V t Eo eo m K 'c*r- cc I-in3<On 5in I V) . . f .. 3 EOO-131 i-3103 . Sed EQO-1311-3104 Sed E00-1311-3105 | p f f Sed o? EOO-1311-3105 Sed - b EQO-1311-3106 1||: Sed E00-1311-3107: Sed ,'VfCp v E0O1311-3108- ' :* r' EOO-1311-3108 00*1311-3109 'XL Sed Sed Sed 4 P (A > $ jrc c/ V is 5 IV"! o *o u 5 u C (y> A. Q. 3 0 J JS v* a EOO-1311-3110: i l l E00-1311-3111 EOO-1311-3111 EOO-1311-31.12 E00-1311-3113: EOO811414 .j: Cj , "J. EOO-13114114 EOO-1311-3115 ' : E00-1311-31:16 f j | . EOO-1311-3117: EOO-131 -3 1 7 : : EOO-13T1-3H8 - l ' E00-1311-3118 ' t f c i E00-13114120 f i l l ' EOO-1311-3120 ;|iS! . EOO-1311-3121 ; 0O-131 i-3122 H it E00-1311-3123 00131=14123 - w : EOO-13114124 H l : EOO-1311-3123 I I ; ; EOO-13114120 EOO-1311-3128 i t e EOO-1311-327 l Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed Sed EOO-1311-3128 Sed v~ ^ 5- - Pr ^ E004311-3129 EOO-1311-3120 =&l$! E0-1311-3130 Sed Sed Sed ; EOO-1311-3131 Sed "O ,1 h ji EOO-1311-3132 : f- Sed E00-1311-3132 f 01311-3133 : i . EOO-131.14134 'Mi Sed Sed Sed EOO-311-3135 Sed " EOO-13114135 MS Sed 00-1311-3136 : | | i ? Sed EOO-131 i-3137 : EOO-13114138 E00-13114138 'Li MS; Sed Sed Sed & 45 0 5~ 1:1 4 4 - 1:1 A S - 1:1 A S - 1:1 -0 5 ^ 1:5 0 4 1:5 1:5 - o s ' 1:5 0 5 1:25 tf5 1:25 A T 1:25 1:25 e r r 1:1 o .- r 1:1 < r r 1:1 ArS 1:1 P 4 - 1:5 A S " 1:5 <5!T 1:5 rO T 1:5 p.s- 1:25 0 .5 ' 1:25 J L 5 - - 1:25 "S- 1:25 A" 0.5 1:1 1:1 S ' 1:1 1:1 A S - 1:5 A S - 1:5 r05 1:5 A 5 " 1:5 A 5 - 1:25 0 4 ^ 1:25 1:25 A 4 ' 1:25 1:1 A 4 - 1:1 -O S ' 1:1 A S 1:1 1rS 1:5 r**' 1:5 1:5 p.s 1:25 r ' Aa /T - 1:25 1:25 1:25 6 :d i 8 0 0 ;H l ^ 9 7 7 4 0 3 0 0 S1 Z . W 5 0 S Z -H 7 5 S 0 #; 0 ml 0 is i L 00*420 fM L O W 0 SS? / . 0 3 2 < i 0 2 Kw r 2 * lif - 7 9 S 7 /T 5 2 s ;c o y * / 2 S -- 2 fc 2 w . ,5 6 )9 5 2 ?st!: 2 .S 3 Z 2 rii 2 ;s f : T S O 2 M l2 0 /7 0 2 1 .D 3 2 3 2 te -- 4 rife* V / S y j g 4 S1 5 T O O S 4 ; < 00211 4 W- 4 1 Y m m 4 2 .0 0 1 1 - 4 2 .5 3 3 ? - 4 s! -- 4 St O o r t 4 .> *430 4 r' l i 7 .0 2 / 4 4 life 8 y .w s z W8 S i B 8 fa n 8 SI 8 'W 2 . 5 0 9 / 8 S 2 .5 k ? 8 's # 2 , 5 0 0 v 8 S1 -------------- 8 si 0 0 7 / 8 s i .0 3 0 3 8 si .0 2 3 2 8 si -- 9 1c Jt3; 5s ft 3 10 11 :^ C Ia 12 13 14 n ( )C H i l f [ z&i ? S -c C -C ? i a 15 _ '" _ :.-Si 5 . ' E 3, OC iQ iSn 2 ' o m o Eu < 16 17 - 1 t ,v - , io < K t v - lio * l ! M a w T K iA - H m 5 ' o w tc i a / X / c o ` -3 9 ^ 3 ]# V M - - C?t ix 44 tifiJ ' ^ lit -- 1 f N li O? 'A - I s - (< _ \ / ao^ f i - -- - ' -- J i U o> h p 33 J 7 .. ko t _ c~ V ....... .... ' l' f l ) i l- 2 Hi t .. (n*2 it e - .......... - . . ' 1 N -- I ' `H i l l ' 4?,< ' - - - U' r -t p ip ifii SS ` i. 1 *-^ ;S \ n" V L : jis S t \ $ l i- i S #' - '- - d te i f 4 'v St a\ J. J A \ 1/ s -51 - -- no :_ _m s * m N r s- > -< s ** . V -' A J-*, 4 jfjfr? '( 0 --3 i t e 5 r :;4 i'iL 4 L ;n `i l r q / s as/ x in t j3 fisnt A ^,,4<0^3 i 8 1 ,0 > fe iv i X sy- VO i'* 4 o 5 *vV? ^c%, 3 > J J ___________________________________ J z X_________________________________ N >> & Soil Tvoe 1 (HOL0 7Z/Z -P O O L 'S - 7 ? Soil Type 2 (Sed) 'T L t Z r O & S L ~ ? Col 8 Balance ID * ? / > . j,. 1T/D/i g . A > - ? P M 1<f a r f c u Coi 9 CaCI2 Soin ID n p K .lt- i< -t> 7 O T/D/I A ; _______ '' / ^ J - / C_^ ~ r 'fVCp Wcjoi^dcH,^ r\La-rsU^er^/-- o u t io h i '0 0 Col iO 2 hrl Inc. JD X - 13 Start T/D/i IO' J t i( I2 ? if O O C*rvC stojD g / i t e J h l- J L !L ! CC~ LtC Col 10 4 hr) inc. ID 4 ' ( Start T /D /l/ ' Zi il iJ to !(j <irt < S M T/D /C j'. i J - ,1 / 7 - i / Y ) C i * ' Col '(8T?r) Ine. IO X - f 3 Start T/D/I '7! OC-' / 3C / C t Stop T /D /l.^ jiA P i ( it o O C O **- ( ^ ) C a n O '- A j f t Li / t / t ( c . Col 11 Test Subst ID O i t " 3 1 1 G_> Ti/oD / iij; J*i, it / ; / --------- 4 ------- "**" DP C o llin e . ID X - Start T/D/I i t f s o o t /d /i N c) Col 13T/D/I i0. '0 H MS / ' *- (/ tc o r w 1 1I h CO f > " C Col 14T/D/1 /.*? : A C / 2 / C f / (PC -Cel 16 M e O f t O if t r S d n lP * ----------------------- * Q) tcJUly-^ T/D/I t M S T ( X ) e u l 17 T/P7I 3 -! / I ex' C'f* C (O fif w t>FoS> GLP Study Number: i OOC?I' '-IM p f i j OD O- C. TtfPpoJ H v 3/W Environmental Laboratory Page 159 of 703 BACK TO MAIN Optimal Ratio ETS-8-159 Section 12.5 Test Substance Sample ID . Soil Type ^3-----------------------------SoihSoln Ratio Soil Weight (grams) 0.01 M CaCI2 Addition Equilibrate 12 hours Equilibrate fo r x hours centrifuge (Y/N) Remove / . mL Study Sample Add Spike Soin (uL) Comments c J u 5 "sVs 1 Oil kL d U) cA *A jr *d (j -- 0 k* "o a E c o i * M _ Ii 1 3 45 E00-1311-3139 M Sed - * 5 * 1:1 EOO-1311-314 Sed 1:1 E00-1311-3141 ( # 7 Sed - 0 3 " 1:1 EOO-1311-3141 Sed U " 1:1 EOO-1311-3142 ;*- Sed s r 1:5 0 t> v VVJ. 4 /-A J 00-1311-3143. Sed ' 600*1311-3144 Sed E00-1311-3144 H43 0 1E00-311-3145 ! # ; EOO-1311-3146 Sed Sed Sed EOO-1311-3147 Sed EOO-1311-31.47 . *MS; Sed EOO-1311-3148 -k .. Sed E0-1311-3149 . Sed E00-1311-3150 %<% '& Sed -55 1:5 1:5 r J*. 1:5 1:25 -o:5~ 1:25 1:25 0 ^ ` 1:25 jx r ~ 1:1 T - 1:1 A S "" " 1:1 to lM s VJ S lJ EOO-1311-3150 rife ; Sed E00-1311-3151 t M Sed EOO-1311-3152 Sed EOO-1311-3153 to.EOO-1311-3153 0:1EOO-1311-3154- Sed Sed Sed EOO-1311-3155 ' EOO-1311-3156: Sed , Sed EOO-1311-3156 f Sed ^ 6 ir -o lT ^05 -tfT -015^ -A ir' 1:1 1:5 1:5 1:5 1:5 1:25 1:25 1:25 1:25 ^r EOO-1311-3157' m EOO-1311-3158 Sed TT5" Sed 1:1 1:1 E0-1311-3156 Sed ; EOO-1311-31S -'M - Sed -0 5 ^ 1:1 1:1 ! EOO-1311-3160 ' Sed A A " 1:5 EOO-1311-3161: f t e Sed E0-1311-3192 A' Sed -ei f oOrT 1:5 1:5 =' 00*1311-3162 Sed 5 " 1:5 EOO-1311-3103 Sed EOO-1311-3164 iM '. Sed 1:25 A 5 - 1:25 ' E 0ft31-3165 ' %$ Sed p * - 1:25 . EOO-1311-3165 Sed 1:25 EOO-1311-3166: Sed A S - 1:1 00-1311-3167 Sed OS" 1:1 EOO-1311-3168 Sed -<*S 1:1 EOO-1311*3168 : MS EOO-131-3169 "%Si EOO-1311-3170 Sed Sed Sed rP-6AS- 1:1 1:5 1:5 EOO-1311-3171 jL |; Sed A S - 1:5 EOO-1311-3171 MS Sed E0O1311-3172 Ml Sed A3-- 1:5 1:25 : E0-1311-3173 M e E01311-3174 Sed Sed A A 1:25 -O S " 1:25 E0O1311-3174 MS Sed 1:25 Soil Type 1 Soil Type 2 ( T7JI - C O O l.T - 7 7 L'7U __-- k L --Col 8 Balance ID T/D/l Col 9 CaC12 Soin ID oc-- T/D/l l_l7i /0 M y<! 'W OX' ! iS II 6 8 9 10 11 12 16 S i f i j n 16 p i M C O u t 1Jt L i * < - 16 i n m 15 w . is 16 I l l I ' S V D -T - 16 S I 216 tu - . S S~l . 16 M 16 m / . o n 7 16 f i l J . O i b X p16 / D U S ' 16 $1 24 5-. 0 7 3 0 24 's i 24 i l 4 7 7 V . 5 - 24 ------------ 24 m z m e r 24 m z * m ? 24 *i Z S - 0 8 3 24 24 t i 24 i l i D t f G 24 I S b . 9 7 i o 24 P I 36 5: 0 1 1 7 . 36 % r W 36 S t t& g > 36 SI 36 k i 2 , 5 0 3 3 36 " i 2 . V 9 2 2 36 s< 7 . S 3 G 5 36 m *------------ 36 / 0 2 S 4 36 m / 0 3 5 ~ 36 o z n 36 48 4 W T 3 48 s l 1 7 ( 5 > 3 ? 48 248 B 4 3 7 5 7 48 -------------feili . 5 3 9 3 r 48 M 2 . 9 9 5 7 2 248 P I . o 48 S it - 048 `- I f . l9 ( c G 48 / . 0 3 8 Z 48 I I / O C 48 1 1 1 ? Y Col tt r (16 hr) Inc. ID X - " < 3 N! / 4/ Start T/D/l 2 ' CC / / & IQ 0C***U' sum jm (s'. if i2 ti r i > c n*C r - ,iCol M (ZThr) Inc. ID, Start TfO/lT W a . 'f V. Stop VDlf l '.`l5 ' i > l ? I V A <i Col t0(3onr)Inc. ID H --t 3________ 3CB X a 1 -X 11r i3 13 14 15 16 17 18 CM l * -o e\ j i lip ii `M t -T''' --9 - t ili fi- '; } t- s ili to * ft: ( o - W f= n i c T \S fT - U - r / T C. m C / .2 / - ) / > ri < A f)D tlu .C < -ri A ^ C -----------, ----YLU. U C<y\ C 1^ 0[ , f$ - k- v - _--Jt- * k l ~W$%>. -- ^ T ji r a p g s X. h r -------------------------------------------------- 1 V >3 SES - fp il m. - ! - ft 3 - t . o8B "CJ i f '#f l l V- :a o J 3 . jl . fe r" - l - . - i l - _7 < 7 - .. fo - a < i*c ' \ fe -- -- <4 r i l r- - ,, 7 7> T'S i-| _ *P ;' n . c r u . ir . o lm i V ao3t' f ____ 3 js S J 3 . 0 1 ,5 1 , 1 :1 & . o m ? 7 . < * * cf s to j 4 v iJ L 2 J ;,rjjt :W t^ r k w - 'U S M ito . --S / 1' . 1 H M S O tq J I ^ S S i! N W l V 7) Col 11 Test Subst. IDn U r . f - n I ~ I I J/D /l / J i> 11 3 g ICC c.f * L Start T/D/l X ^ / / / ? / / C O O k v Stop T/D/l 1-^ 0 tf lr?t I Oi-` CiVX C Col 13 T/D/l t O i t .2.1 ; I V ( Urt b Col 14 T/D/l iQ O ( J / * - / 3b ^ /V = fc > i. 32:v ir />,t* /*>- / -x V> *>CG4vr*,f rrt> .CDStart T/D/l (r-WST If /?< / CO C C Stop, Col(4hr) Inc. ID X - <^ Start T/0/Ic7 c/ ^ t/ !j x ! Q 0 S **.( Stop T/D/l ft> iX - l I tC Col 15 Balance ID. T/p/i/< 9 - 'v V IJ-I > 'Cii-Vn1 CDs 0Col % ik e S o in ID tP c c o j - / s P - O f S /O ^ >n Y - ^> G & )c>nC ii/ ^ ` oc> (jy(P 'Sw|* t'^C Si-utT to-doottcTI') GLP Study Number: CDiSJ0,,0^ _- ,> , ch*. n/icffo, T/D/l |g ,'Q O / / T / Q O C4*_- oepoj->a~H oftfr>^^ THi^S e- *\. _ oh (ot> tin c_ vo uY 3M Environmental Laboratory Page 160 of 703 BACK TO MAIN Optimal Ratio ETS-8-15S Section 12.5 Test Substance Soil Type Test Subs, cone., mg/L Soil:Soln Ratio Soil Weight (grams) 0.01 M CaCI2 Addition Equilibrate 12 hours Test Substance Addition Equilibrate for x hours centrifuge (Y/N) Weigh tubecontents,g (48 hr) Add Spike Soin (uL) Comments Q Q. e 2 a CO. 5 OcJ K XI s. \4) Q. E Xa b o? o3 n E i 2 3 EOO-1311-3175 Sed E00-1311-3176 Sed EOO-1311-3177 Sed E00-131.1-3177 'm s Sed EOO-1311-3178 Sed E00-1311-3178 Sed EOO-13.11-3180 Sed EOO-1311-3180 life Sed EOO-13111-3181 Sed E0-1311-3182 >,U: Sed EOO-1311-3183 :U .j Sed 00^1311-3183 . MS; Sed 4 5 67 8 9 10 11 12 13 14 15 16 17 0.0 1:1 0 s i 0.0 1:1 0 S i 4 9 t 3 Z 0.0 1:1 0 S i; 1J AYL :-- ; :. -- i. x A 1^' V; 'j - jv itt: : C : L o Afa' P .' i _ :j W ;it . 0.0 1:1 0 :S * 0.0 1:5 0 l'ai! 2 . W d s 0.0 1:5 0 ; s if 2 , s v o c ' 0.0 1:5 0 i-s if 2 , 7 1 5 g 0.0 1:5 0 's ii 0.0 1:25 0 : s i j / D 3 7 i _____ 0.0 1:25 0 S I / . b 2 < iu '5 Trt - v' V -'.A I t if trU ir-i a s i-v .tiT -;: pfar' ~ fa':' tL '.T-i- tv f i t t i; pa/ j. t ji.i:;- P aT lfb is it N /to / r/t- 0.0 1:25 0 'S t; L 0 / 0 '3 0.0 1:25 0 ; s i | i l i 7?:'-' i ' . - i p 4 ^ , / u- n ** 18 a IO V : D i ' ) . u u / M y- B T M rt - U T / T f . t v ? C l o / ? ^ tip ? ,!<) l \ * r\V^4 C V ^ C H - (T-ov (' ^ . -- E00-1311-3184 " Sed 0.0 1:1 48 M 7*) EOO-1311-3185 /ii; Sed 0.0 1:1 48 ;S1 W O * ! E00-1311-3186 |-J2; Sed 0.0 1:1 48 3 M 2 ^. EOO-1311-3186 MS- Sed 0.0 1:1 48 S1 ' EOO-1311-3187 f i t ' . Sed 0.0 1:5 48 S1 Z W i O 00^1311-3188 EOO-1311r3l89 Sed 0.0 1:5 48 's i ; Z W O G Sed 0.0 1:5 48 St' Z 5 I 7 C , . EOO-1311-3188. MS' Sed 0.0 1:5 48 S t EOO-1311-3190 " i t i Sed 0.0 1.25 48 s i ' / . D l f a E-1311-3191 j i t : . Sed EOO-1311-3192 Sed E00-1311-3182 MS Sed 0.0 1:25 48 ' S / D 3 A 0.0 1:25 48 S1 / . r tZ 0.0 1:25 48 S1 ---------d Soil Type 1 (HC/LO)___________________ Soil Type 2 (Sedi 7 Z J I -O O t: , - 7 0 TjrtD " r~ Col 1 *(4 8 h r) Inc. ID J ~ l -S Start T / D / l9 : y O j j nt lj*.V . j^ X i u; j\! I ..I'M i / > / W 7 b ttfd :T7 . <3 iC . n e s l(-i 1 . ` U t y m P O tJL 25-10;:! -i2 ,, io ; ____ J is ti <9 t> J- 3 % V V zt tt; L </1 IP 31mctL y j i )r /\ _______ y _5 L . Col 13 T/D/I 01iO $ -4 ( I C O C- Q n iL coi14T/D/iti ! jj 3 i U -Col 8 Balance ID ____________________ ___ t/d/I S': - 3 p m / it C o l 9 C aC t2 Soin ID OCCCH - ? ~Q 7 T/D/i 3 - 3 ^ / s ' I qc- c k c Stop T/D/\ iO'.CO l> U i //A ,1 c o i n TestSubst ID ( 7 C 6 ^/-(| zi<ya --7 -^ > >07", z C o l te.lO T - I T Start T/D/I 3. " t3-i ( Col 15 Balance ID Q N ____________ T/D/I (Q '.m> lo L I 1 I Q C c w < Col 1 6 T/D/I Q '.P O / c?-/ i Co! 17 Spike Soin tDO P O p I " 3 0 - I p n 'v f* F^= T/D/I l<PCO J 2 u j - J c > O v C_ Internal Standard ID OQO O I -- 3 ~~ I I "t j ? stop T/D/i i . ' v o ; I /fcZ/ Q j pyi c T/D/I IV. I "S ' / T / Q Q /L> y . C . (q(vJT)tVi_ sCtr-+ T O pC t y Wc-orrtcA-U^ @C^t/7 UXT,^ >' <w / ^ a/vJ^ fp /r 1'^ cn ^-~d-4 ( A c ) C tt-c `/ - f i - c i ^ /v i 3 ^ ^ Lt^ ^ (3) ftIt rfcc<-Aj>A bi.wS nrx Lah* e-d fapm (Ac the /q - >/ GLP Study Number: E00-1311 3M Environmental Laboratory 1 / / " ''l V Page 161 of 703 BACK TO MAIN Optima! Ratio/Mass Balance E T S -8 -1 5 9 S e ctio n 12.5 (co n t.) 7X7 S Test Substance: Sample ID Soil Type Test Subs, cone., Tg/L SoihSoln Ratio S a m p lin g Remove aqueous m d weigh ube+contents, g MeOH A d dition, ecord m Ls ( 2.0 or }.0 mL) Centrifuge and ransfer MeOH A dd itio n , ecord m Ls ( 2.0 or 3.0 m L) MeOH A d dition, ecord m Ls ( 2.0 o r 3.0 m L) Centrifuge and ransfer 1.00 m L S tudy Sample <\dd Spike S o in (uL) 01 a 12 E00-1311-3007 Etto-1311-3008 E00-1311-3009 ~ E00-1311-3009 MS 3 - 0 oc z 4 5 67 8 0.0 NA 48 S2 J J . ( - / '3 3 . 0.0 NA 48 S2 ( -n r rt 0.0 NA 48 S2 Q > .c i ( P D 0.0 NA 48 S2 -- --------------" 9 10 11 m' (2) /C" (2) 7 { ` f d : ( (2) (2) ! (2) cno oe0 55 5 u uc nc U 12 13 14 - s; * :/ 15 "1 16 :: (2) " X - ! (2) 1 L '& M (2) : 7 o u . I ; . 18 _ i y , | . ic wl 1i I 3 n T W Il EOO-1311-3010 - ~ 0.5 NA 48 S2 ( L H 2 D ? - (2 )" E00-1311-3011 - - 0.5 NA 48 S2 ( o . c 3 o 5 (2 f \ E00-1311-3012 - - 0.5 NA 48 52 ( ? . 9 I 3 6 (5 ! (2) ' (2) (2) m s j 3) (2) .jn:.-... ; Wi 7. SX "S -jV v irrV! . . 1 -X T EOO-1311-3012 MS E00-1311-3022 - Clay EOO-1311-3023 -- Clay EOO-1311-3024 - Clay EOO-1311-3024 MS Clay EOO-1311-3025 - Clay EOO-1311-3026 - Clay 0.5 0.0 0.0 0.0 0.0 0.0 0.0 NA 48 S2 1:1 48 S2 5 . 7 5 % 7 1:1 48 S2 5 . H \ 1:1 48 S2 5 , 3 5 C > 1:1 48 S2 1:5 48 S2 / . 0 1 7 2 . 1:5 48 S2 J / . O G H Ta(3)^ j XZ)-----------...`"'M 1 ! (S) ra (5) ef (7) ` (5 (3 ^ T3)-------- &: (5) . (3J--- 4 - .... t- ..- (3) - (2)v (2 )' (5 ! (2) 6 ) (2) : T~ 'J n ,x m s a t or,u - t if EOO-1311-3027 - Clay EOO-1311-3027 MS Clay EOO-1311-3028 -- Clay 0.0 0.0 0.0 1:5 48 S2 / / . 0 2 0 3 1:5 48 S2 1:25 48 S2 1 5 . ( C 3 2 (27 (2) (2 f & -- (2) (2) (2) (2) -- (2) ff poX m EOO-1311-3029 - Clay 0.0 1:25 48 S2 J S . 5 5 3 0 < zr (2) (2) m EOO-1311-3030 -- Clay EOO-1311-3030 MS Clay EOO-1311-3094 - Clay EOO-1311-3095 - Clay EOO-1311-3096 - Clay EOO-1311-3096 MS Clay EOO-1311-3097 -- Clay EOO-1311-3098 -- Clay E00-1311-3099 -- Clay EOO-1311-3099 MS Clay EOO-1311-3100 -- Clay 0.0 0.0 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 1:25 48 S2 J S . J j l 1:25 48 S2 J1:1 48 S2 5 . (7, 7 7 1:1 48 S2 / S , 2 ? 5 f Z 1:1 48 52 J 5 . 5 2 5 0 > 1:1 48 S2 1:5 48 S2 / / . 0 2 0 7 1:5 48 S2 U . 0 9 7 4 1:5 48 S2 / / . 3 / 1:5 48 S2 1:25 48 S2 (2 )' (2) " (3 )" (3 )^ / (3) (3) ` s' (2) (2) (2) (2) (2) (5) (2) o(3) (3) (3) (2) !& (2) T2J~ (2) (2) O) (S) (S) 0) (2) (S ( 7 (2) f S^ --------------------------------------------1 :. m im m: /3 ) u V ? b Ju. 77 / t z t W o1 ft. EOO-1311-3101 -- Clay 0.5 1:25 48 S2 / 3 jm EOO-1311-3102 /S.Clay 0.5 1:25 48 S2 * ru o (2) 5 /N EOO-1311-3102 MS Clay 0.5 1:25 48 S2 EOO-1311-3166 EOO-1311-3167 EOO-1311-3168 _ - Sed 0.5 Sed 0.5 Sed 0.5 1:1 48 S2 4 . 1 3 7 3 1:1 48 S2 / y - 5 3 3 1:1 48 S2 / 3 , 0 7 5 5 r (3)' or 1 (2) (7) V (2) (i T (5) 0 0 & (5) /6 T2) <^> _ i l J . / S ! P i% s pi X m EOO-1311-3168 MS Sed 0.5 1:1 48 S2 EOO-1311-3169 - Sed 0.5 1:5 48 S2 J D . 5 7 5 5 (3) , -i (2) S T iT (21 ^ (2T ( \r m - n rv-' ' EOO-1311-3170 7 g 3 7Sed 0.5 1:5 48 S2 J O . / o . * t wEOO-1311-3171 -- Sed 0.5 1:5 48 S2 A(2) yA? iJ (2) r P) , H ^ TU (2) \ -- P (2) ^ (2) x: 0- EOO-1311-3171 MS Sed 0.5 1:5 48 S2 (2) I S r j3 r S it3 myEOO-1311-3172 ~ Sed 0.5 1:25 48 S2 ^ XZ) ri P) 3 ' S . (2T A d nP5i--- l j y. EOO-1311-3173 -- EOO-1311-3174 ~ EOO-1311-3174 MS Sed Sed Sed 0.5 1:25 48 S2 7 ^ 2 0 2 P > *0.5 1:25 48 S2 \ (2) 'S 0.5 1:25 48 S2 T2)------- O'sS --X ----- r o >(t' Or; K'i (i J 'f ' , __ Ni (2y /y -sia r /x s '/ Col 8 Balance ID T/D/l /?: &/j- / y 7/ J7~ Jp Col 9 MeOH ID V a /. /d ~V / Col 13 MeOH ID 7 > ^ ^ V7V^ T/D/l iJ & T i'* , i) ~ 3-)T1 C'X> Col 14 T/D/l > 2 ^ 0 c--b iT L h e . 4 -g />2 y C'T> %.-rk,cvvL*J S o .' T/D/l C lb v 7X5* I / J > jiy C Xj, <A-Ll..CoM 0 T/D/l ^ f < fefi sLJ. /-> /.S '/c T i c o m MeOH ip 7 7 V - / ? - d `i o , Col 15 T/D/l <gic<L 6 V 'Z S J 4 -<j / 0 / "Jt / C'X> .Col 18 Spike Soin ID T Y Y . ) "3 " / ^ 7 _,,<' O \f f * tg f b S ik m S '.o o ________ I / `3 /<? I QlO (L. T/D/l ^ 1 ^ V / i - J x l * l5 l S / ,n\ Internal Standard ID QOOQ/ ' 3 2 ~ / V - I C y / r M n 7 7 / / , / t ' S ! 3 . S " ^ _ > 7 " r / f e y ) ( - y i/ J -/ < 7 j t /D /i " "- y>i^< o 'C cse ( >~*~n? Xe5 s-torflri ,,V 'ircp /alo Rod.., T*y> U.A,'I e x+r schon W , , OE c\ m ->r - ,, < 3 S r t i ^ t / S t e n t / M / v i f / - r e ( r . ^ r ^ k ^ r v M d i l u i i * , t 6W o r - , GLP Study Number: J^TJZj ~ / 3 V / ' / 'J ^ c<C u.red ((_*0 \ e r g ^ 0/ <- w - 1; | 3M Environmental Laboratory Page 162 of 703 Optimal Ratio/Mass Balance ETS-8-159 Section 12.5 (cont.) BACK TO MAIN Test Substance: 5Vo r e c \ A r f (^)onc - t - W --ci s-ts * * * *< a t Ycxxn l m i -W \ < ? r t r e> C K a lo - e e ^ o - * ^ Occ ^ r ? A * 8 a "*d lu h i"' a* t * ~ * J v h GLP Study Number: " ^ 3 // 3/W Environmental Laboratory Page 163 of 703 BACK TO MAIN Desorption Solvent ETS-8-159 Section 12.4 Test Substance Col 4 Soil ID 1 _T f a - o c u o --n Soil ID 2 T C Col 6 Balance ID np/\f '.c o i / 32-1 Cl* C Col 7 Test Subst. Soin ID # 0 0 0 0 1 - 7 ^ 0 ' f Test Substance Concentration: | OO / L. T/D/l O I Sf fS' t ! j j ( B Q CDK . Col 8 MeOHID# r u e - H m S T/D/l 11! OB' I /A J /O i CJM - Col 9 T/D/l l i \ S O / // Q/'CMC Col10 MeOH ID tfT T/D/ifl5to-,. Mt 7 t /-^/2~cUr C o lli % T/D/l / / A / O / Col 12 MeOH ID # TV f t - 4 1 1g ___ T/D/l a / C J i y . c't/d/i t 2 \ o j _ jJ Q o / c. Col 14 Study Sample T/D/l U t e s / n a / O l C-8VTT Col 15 Spike soin ID # r W n A ** J*4 7 Time/Date/lnitiBlsJ t f j f / / J A Q i C Spike Solution Concentration: (3 p / U y^ ^ P O ^ Internal standard ID# f t l o o l - >3 ~ I Internal Standard Concentration: r w c I Tlme/Date/lnitlalW . J g t o l O V \C * -- li 5 i H 1 10 f I ? IS 6 =s * 1 5 3 s1 * 1 2 2 jj I a i I I i1 a % ZA . f t E i \i 1 ii j JL i l 1 la4 E00-1311-2001 _ Cntrl NA s 0 e _ r7 _ a a 'K 10 7r , 3 _ 7 _ . "7 u 1 ! * EOO-1311-2002 EQO-1311-2Q03 EOO-1311-2003 EOO-1311-2004 EOO-1311-2005 _ Cntri _ Cntri MS Cntri _ Cntri -- Cntri NA HA NA NA NA 0 0 0 0.75 0.75 ,, -- -- i . f r . j ZT 1 / T T ' u __________________ EOO-1311-2006 _ Cntri NA 0.75 -- r t ? ss EOO-1311-2006 MS Cntri NA 0.75 _ ----- >, EOO-1311-2007 _ Cntri NA 7.5 EOO-1311-2008 _ Cntri NA 7.5 EOO-1311-2009 _ Cntri NA 1 7.5 _ j4 T , -- IfiSlRI __ r * y p 1 Wfgb J 1 mm EOO-1311-2009 MS Cntri NA 7.5 i -- 1 -- . i z 00*1311-2010 _ Smpl S1 0 -V ___ E00-1311-2011 ' _ ' Smpl S1 01 _ , -- EOO-1311-2012 _ : Smpl S1 0 3 < *4 _i ----------- ;--------j j E00-1311-2012 ! MS EOO-1311-213 _ EOO-1311-2014 _ Smpl i S1 0 Smpl Smpl S1 \o 0,75 ~ 2 i f o h a { S1 , 0.75 52 _a. n; E0O-1311-201S _ Smpl 1S1 0.75 4 C o x i j i H t S j <s Q - _l "-- j ; ___ !__ ___ ; X t '~ l& jt . ^1z" i1 X m m E0O-1311-2015 E0O-1311-2016 E00-1311-2017 E0O-1311-2018 EOO-1311-2018 MS Smpl _ Smpl S1 0.75 , S1 ! 7.5 r - 1 -J s -U _ _ Smpl : S1 ' 7.5 i j . s d s S . i J l X 1 3 ""f _ Smpl MS Smpl S1 S1 7A. j 7.5 1 7 5 ? r1 -- .--. i Vf zi 0 z 2 ____i rr. _ <J ______ L J XT OB 2J EOO-1311-2019 ,, Smpl S2 0, _ P n S pS E0O-1311-2020 Smpl S2 0 _\ Hj 600-1311-2021 EOO-1311-2021 EOO-1311-2022 E05-1311-2023 EOO-1311-2024 EOO-1311-2024 EOO-1311-2025 EOO-1311-2026 E00-1311-2027 E00-1311-2027 _ . Smpl MS Smpl _ Smpl _ Smpl _ Smpl _MS Smpl Smpl _ Smpl - Smpl MS Smpl S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S l - C-O 0 __ 0 0.75 -- 7 _ VJ _ io : j ; 0.75 . l -V *- 0,75 i h . H m i 3 0.75 -- 7 ----- - _ci - 7.5 r d . 5 c 0 & \ J T . 1 7.5 . 5 9 - 1 0 .i l A S 1 ___j 7.5 " ~ r" i 7.5 ' ---------- ' J ------- 3 u E=- l Z nt 3 Z tZ ~ (J) S'Lrtvp^'i Sterfci uv-icLi*- uyv+i'l fVrvrl'^Si'i M/iTi/c, ____ 1 r1------ g L r ~ J D - I* V cw<_ 1 L^v \i~d- c , a SeclZ-rkei^-f uw. GLP Study Number 3M Environmental Laboratory Page 164 of 703 BACK TO MAIN Adsorption Kinetics Soil/Sediment/Sludge Description: Km In itial pH o f S tock S o lutio n (p H Paperi Stock Soh ID O C & O I - 3 - S PH j l S T/D/l M I S ' 9-1 ( ! O I C o i f B a| |p____ cola sonipe ip to o m g M - i a r / D u Q l. ^ O y ^ . < S i O i C - I r r v C Cono Inc. ID E * 1 ^ - ____________ sta rt Time T//\S S p / v > / 3 1 0 * n( L Stop Time T/D/l T W O o ^ . /~3. / i O i C VTf coi 1 1 stock som p i C o l - ? f 8* S o s T/D/i B I & Q p c3 / " 7 Q i r m n C Cot 12 ( } EquiSbrate hi>es/contents for designated hours. 3 3 " i 3 - 0L0 h our Start T/D/l 2 hour Stop T/D/t / 3 ? ^ 5 p n r s l / / / O i V i r _Nl 4 hour 8 hour S to p T/D/l ? ' < 3 0 n w v _ S _ / J ____ /O i C / I T C Stop T / D f t j l V b p a , c? l & i>l C l t \ ( e 1 6 hour Stop T/D/I - '/ h - 'n /< / Q > C ^ T C f 24 hour Stop T/D/l '.t-itn i* * XX. ! D - / J l L -LJY'- <- g Other l\J A 38 hour Stop T/D /l Q . W l a ? / 7 / < 0 / C ^ w C `?f=c>Test Substance: Centrilg tubes after removal. O hr T/D/1 c3 / / /7/ C->*X 2 hr T/D/l 4 hr T/D/l , 8hr T/D/i 1a hr T/D/i to . _ . A / i ___/ o i c m / ; ' t IQI l>V^C >$ /QL Qy^C XL t f i / O n ^ 24 hr T/D/l 1 0 I c3 - / <2 / Q> C t^ l C 36 hr T/D/l cX / X Q < Q rr^C. 48 hr T/D/l 1 - c 2 / " 7 / 0 I ^ T r v C-- Col 14 Balance ID T/D/l `J f i n A i 7 I Oi c /ry.c . i pH one rep lca te o f each set. 0 hr T/D/l 3 Q 2 3 tolOpC T/D/l I * Q fa T/D/t _j ___ 8 hr T/D/i B * Q c y * * x r O / /S ' / O I c m L 1 8 h r T/D/l 1 1 ^ O c y v t_____ S _ / ^ ___ <Q L 0 ^ 24 hr T/D/l H - / 7 7 - / .3 / Q / 36 hr T/D/l 7 - / 5 ~ / ^ n 7 . / ~~1 / o i 48 hr T/D/l B C > P < y \ / / 7 / >_(_ a h C d e f g h Col 16 0 hr 2 hr 4 hr 8 hr to hr 24 hr 36 hr 48 hr T/D/l * 7 ' O j / . f / < H TfOfl < - 6 0 A / ( | d / P 4 ~ V t f~ . T/D/l 2 1 X F > X I l / Q I C / H C T /D /l O Q ^ ^ /0 ) t/d/iT : ^ d 3 / X IQ i CV^C. T/D/l J3 & / a t c^ P T/D/t 7 - a* J 3 J Q L - C J A * C T/D/l S O Q Q j Z U Q . L C m C_ 0 hr 2 hr 4 hr 8 hr 16 hr 24 hr 36 hr 48 hr T/D/l O ' 7/ g / o n . T /D /l___ ---------- / _ T/D/1___ ______ /_ = TT/D/l T /D /l /j ___ / J _T/D/t /. 4/T/D/l _____ A & ____ T /D /l/O - / K )t O <-- In u m ai standard IP; Oi ~O / TTM/D/li l ' . ' A t w kCeolu1a9 a L jfL / Q J -jQ H 'X C X v DHutiort Factor (if R equired!: / O * Methano IP:T M f t ~ Q l 5 S D */- <A >o \; ^3 <L-_ 5C ^t<I j u (7)<@o n e i>/;/ol <2.Ho'-Kr 5,-Vtk-r+; 3 d(W di'/IOf 4 w St-oO: \o : o ^ ill,, 8 hou^- si-a^f.' 600-^ 3-ls'ioiv^C 3M Environmental Laboratory ibikirvi*- 3:00f\ 0/ </ot'(J*iC an(j w 3'0 ^ 3 slD , UYVI. q^K^cH'Sk<^+-., i:jopTMb2/ir/t(^vlc Page 165 of 703 BACK TO MAIN f - Adsorption Kinetics Tesi Substance: P F o 5 Soil/Sedim ent/Sludge D escriptio n: .S t J - i - C |a i- \ n ~ j(^ > g - ~ n -- ------------------------------- -- M fc = -- --- .. - ----------- *------- -- ------ Initiai p H o f S to c k S o lutio n (p H Paper) Slock Soin ID O I O D I - _____ pH5.!>rawU.W?3i) !oi_cm f Colf BaiID <Ai<~( T/P/l II'. 3rt<V, I Ia-T IQ( t-n/l( con soi-niDJoeoi-M-I.TiD/ica-3Qyuv I l i I /Q I CWL Col 10 Inc. ID . I T - t o * Start Time T/D/l A * 5 f r V J I / / P i J r V \ C Stop Time T/D/l * 7 * . / A * V \ t Q / I lC> j T f \ C C o i n Stock S o h ID Q iO Q < ' S pP TiDfl 3 - 0 ^ p r - ^ i ICD 1 C^V'XC P9I12(V) Equiibrate tubes/contents fo r designated h o u r s ^ o h o u r s ta rt T/D /l A 1; / " I X~ 2 hour Stop T/D/l i X / l / Q> C r C \C Kivy 4 hour Stop T/D/l 3 \ 8 hour Stop T/D/l /) O I 1 C <3!S tO!CMO 16 hour S top T/D /l 'J O f a n & ! 3 _ Q i f J * lL 24 hour Stop T/D/l J f l . W g f t H / T ? I . I O i > t t C 30 hour Stop T/D /l S jw s o 3 / * 7 / Q C * V 4 - Other C M F - 48 hour Stop T/D /l & /7 COM3 cw nniuge tuoes anar removal. 0 h f T/D/l ri / j b 2 hr T/o/i !<?* `io p * * d^ e -T<hr T/D/l T/D/l T/Ort o*~ if* , n st o w -r r-2- I f i i C ^ f 24 hr T/D/l /Q *Ji>A-tV\ A / < p - f r i e z e . 0 30 hr TT/D/fDlP /' ^l CO0~*^- oQ* - /I ~1/ / OCLt i o t m C h 4 8 hr T/Ort < - r O ^ f W ^ / f r i ^TVi Col 14 Balance ID. q / V raw./-'YQ^tm. (3 ! ~7i.tPLcm-i<_ pH one replcate o f each set. Ohr T/D/l 2hr T/D/l _ 4 hr T/D/l 2: 8hr T/D/l 18 hr 24 hr 38 hr T /D /l~ 2l * '7 48 hr T/D/l / 1 xm c <3 / 5 /t? f c t?l f 1 <S- / 1 I Q I C iV -( / 0 / C /Vl X . SsUZ ohr 2 hr 4 hr a hr 1 6 hr 24 hr 3 0 hr 4a hr Col 18 Spike Soin ID T/D/i J jU Jj o j_ o ~ C T/D/l i'. Q a . / / / a I ^ T/D/l TU- I / a j_ C V G t/d/i2 ss2_s2 i T / I C fv iC T/D/|7 - P 2 /$ IO I T/D/i y j j i T . a t j & A 1 c m T/D/i~7: i x g i i 7 / >I e m c T/D/l '2 ,'O P l 7 / _ O l C j v ^ ~ T/P/tltX 7 / O f / 1 ^ PFc6 ! t tC ^ V t ^ lnt?rpql9tan<jqr<t)P;o1^0*" T/D/i / / ' d Ctetfr. Q - / * Col 19 D ilu tio n Factor (If Required): ^ Q << ^ 1 f U . 'K c X 'l-- MethanolID; T M f t ~ T/D/i3 lQ^?m - L 1-2. I Q i CJYC- Weight o f Sol, grams Stock Test Subst JS F S S & . centrifuge Weigh tube 4 contents, grams Document pH Spike Amount, uL Dutkm Required? IS 1V) S s H0 5 1-* 1tf i 1a. tic 1 1 l tin su0 I ao 5 -1 f w8 E V i it II I^ i{ . !1 B s O U 1 2 3 4 Vf 6 7 8 EOO-1311-4031 _ Smpl so in 0.0 0 1:5 J . S T 7 . EOO-1311-4032 -- Smpl Soll 1 0.0 EOO-1311-4033 _ Smpl Sotl 1 0 0 E0-1311-4033 MS Smp| Soll 1 0.0 0 1:5 0 15 -- 0 1:5 E00-1311-4034 _ Smpl Soll 1 0 0 48 1.5 J - t e l U T ' l EOO-1311-4035 __ Smpl Soil 1 0.0 48 1:5 EOO-1311-4036 -- Smpl Soll 1 0.0 48 1:5 E00-1311-4036 MS Smpl S o llt 0 0 48 1:5 EOO-1311-4037 E00-1311-4038 _ _ Smpl SolM r ^ t T 0 1:5 M I M * Smpl Soll 1 0 1:5 EOO-1311-4039 _ Smpl Soll 1 - r 0 1:6 J ' S o J j i i E00-1311-4039 MS Smpl SolM - r i 0 1 5 - * EOO-1311-4040 _ Smpl Soil 1 " 5 0 - 2 1:5 EOO-1311-4041 -- Smpl Soil 1 > r 2 1:5 b o x i l i EOO-1311-4042 __ Smpl Soil 1 w r 2 1:5 Q . 5 I " H y E00-1311-4042 MS Smpl Soll 1 2 15 EOO-1311-4043 Smpl Soll 1 U S S _ 4 t:5 EOO-1311-4044 EOO-1311-4045 - Smpl Soil 1 Smpl Soil 1 io 4 1:5 a n m j 4 15 9 10 11 12 13 14 r v. s B i H i si < W m lF W m 15 16 S si S1 17 18 I * a MSI i <r B 19 -- r A. J 3 ./Y 1- a a . ia ja q 'W M r 3 3 .0 5 ' lJ - l. o S1 LS1 * S1 s, ,J k fri- -- )_ S1 O S1 A J l _ ffm -S i-' l r h S1 i - i ~i o S1 f) -- -- S1 sfa & . ln i = C 'i S1 A JS1 ^ S S) M, j ^ (g . *y S1 __ _ S1 * 4 -Jj o TS 0 4 -r r S1 r - SI S1 - T 5 19 '3 . S . . L j EOO-1311-4045 MS Smpl Soll 1 r S . 4 1:5 s EOO-1311-4046 Smpl Soil 1 ^ 5 .0 8 1:5 EOO-1311-4047 EOO-1311-4048 - Smpl Soll 1 8 1:5 Smpl Soil 1 > 8 1 5 a A M i j E00-1311-4048 EOO-1311-4049 EOO-1311-4050 MS ,, - Smpi Smpl Smpl Soll 1 r-frO ` Soil 1 - r SolM <^5Tf 8 16 16 15 1:5 T h h T I 1:5 b M W J EOO-1311-4051 Smpl Soil 1 * * 16 1:5 ^ EOO-1311-4051 MS Smpl SolM 4 .0 16 1:5 ^ EOO-1311-4052 -- Smpl SolM y r 24 15 0 ? M i t i l i Q EOO-1311-4053 _ Smpl SolM 24 1*5 a . e o v n s EOO-1311-4054 _ Smpl Soil 1 r^0 24 1:5 2 . t i 9 < f ^ ' EOO-1311-4054 MS Smpl Soli 1 24 1 5 EOO-1311-4055 -- Smpl SoiM 36 1:5 b . 3 0< n q *EOO-1311-4056 _ Smpl Soll 1 36 1:5 > . * ? O l O EOO-1311-4057 _ Smpl Soil 1 $ 36 1 5 3 . H U M : iEOO-1311-4057 ' v MSr- Smpl S o llt: 36 1 5 k EOO-1311-4058 1 EOO-1311-4059 ~ _ Smpl Soll 1 48 1:5 . `/ , * 5 7 a b.^A'kei&oSmpl SolM 48 Tfi EOO-1311-4060 -- Smpl Soll 1 5fl 48 1:5 E 0 0 -3 1 1-4060 : 'MS.' .Smpl S o ll* Q)Ur\. aicu-f: l> 1:5 GLP Study Number StHSCt--!-.' fO- Jo/l-cal/I!0\ enc-c. too-H it g/x. s/cxr-t' 6 : St'loH**'- %'S 0 i l S 5S - i 1 1 's ! 5* . 4 -- -- -- _ S1 i c S1 ws i ^ s! S1 y -- S1 j - ' r -- v r~ S1 j! A S1 j - 4 m s X S1 m -- Si C*&<- S1 t s W m "P J \l '3 f s> " R s i , s ''Z T St 1 r? B l y * -- -- S1 N / S1 / > / -'s S U| S1 v % 8 * S1 i < ^ i -.::':.;" yxv.'.i:-.- %-.y S1 J* {* 'T ia .i'im S! d > iia .a a w t i S1 J ' '5U H * h a i? , 3 3 / 7 ^ - r . o S1 * * S1 Xl) 5^w jnc. LN, l/-1/ ' I oi^K.. St-'l-rt.' " I Ckvvc. 3Uh. hw-t'-2:oOt>d-flo[ CM.C tig'll. Start.' / 0-Op^ l~jo ! iftic T .' 3 M Environmental Laboratory Page 166 of 703 NS i BACK TO MAIN Adsorption Kinetics Test Substance: O P f c S 'oii/SeiJment/Sludge Description: ,SafJ a Cla.<^ Lon**t _m- Ooofrfi - - 3siock soin id n i o o y p j j t/d /i - j 2 . A j / C o lt Balio ^1Y /T/0/1 IA l t Omm i D & t O l CO kC Col 9 S or tpQOOOi -^H ^T /D /l 3 ^ I / 3 I / H CVV3<- cono Inc. ID _ S tari Time T/D/l 2 ' . 3 p * t / 3 J p i c r v \ ^ - Stop Time T/D /l *7 I O a W & / / / C-fr^ C C oM 1 Stock S d n ID O t O C X - 3 - 5 ? `S ' Q r w j j u ^ ~ -- /o\ rjtwc_ 2LU EquIBbrate tubes/contents for designated h o u rs .'X -- (hour Start T/Dri K j A -------------- *--------- 1-----------* cb 2 hour Stop T/D /l < S . ' P v / / / O I C S * l <-- 4 hour Stop T / D /lr ^ .'r g A r v r A 1 1 10 ( I J V C d 8 hour Stop T/D/l g l '.`j 5 f t * f & 1 i C J Y \ C Other NJFV 1 6 hour Stop T /D /l( o ^ P O l K A / Z / O I f j r i t f 24 hour Stop T/P/l /O ! 2 - ! 3 - /> / />V < g 36 hour S top T /D /lIa J S S j UJU r ) / '7 / 0 / O l C r-TA ------- - ---------- ------ 7h 48 hour S top T/D/t / ' - 3 0 ^ - / / / V >\ < . COM3 Centrifugo tubes alter removal. 0 hr T/D/l 3 l 2 hr T/D/l Q iP ^ 4tv T/D/lSnA o^. a hr T /D /IC *.'^ !? 4 m L I I ___ >>( > H <V oi // / C_ 0-/ /r>j vm(_ o / <5 / & l T/D /l I 3 ( ? p | | ^ H--'OLOlnC COM 4 Balance ID, q W T/P/l l ' V ^ n ____ c 2 ./_ J 2 7 _ O i_ C (V v c Col 15 pH one repcate o f each set. 0a hr T/D/l ^ W C P A f H t/i / n i r> *o f 4^2 / / c* * (L c 4 hr T /D /tS .'W O / W i nt rJV\C /0I cm C e 16 hr T/D/i T . ' . a s) a /a. / O l ceJM 24 hr T/D/l 36 hr T/D/l / 7 /O/ Ch-^ 48 hr T/D/l 3:o<ym <3/7 l icm c C ol 17 Ohr fSU t i o i o * '! C 2 hr T /D /l/ - o p / f t a l c w i 4 hr T/o/igly . c 8 hr T2DflSi5P^/oS/H 16hr t /d / i ~ T J o r 3 . / P - / o > o v K ,, 24 hr T/D/l 1 * 1 ______________________ 36 hr T/D/l X j g _ / J 2 . / Q ] _ M \ . 48 hr T/D/|3'PpoI/JX/Qi_OV\(^ 15 Ve Soin ID Q Q Q O H 7 f(j* n __P_F o S a Ohr 2VO/UO^iwu M { t Ot C M <- 2 hr T/D/l _ f 24 hr g 36 hr ^ ----------- Z2d3jQ L P** c In te rn a l S ta n d a rd ID; O / O O i -- O ^ -- O X - j - ^ . T/D/l t ( O f t a fisi c2 / <? / O j O V >C. Vt D ilution Factor fif Required!; Q 2C D i / 0 T/D/l . 'C t y t ~ >9 / 7 / O I C IV IC mL o f 0.01 M CaCI2 Soin O tce 1 * 0 ioc 0c $ % o &1 1 1 M -4 ? ce 1 234 67 8 EOO-1311-4061 -- Smpl Soil 2 0.0 0 1:5 EOO-1311-4062 -- Smpl So 2 0.0 EOO-1311-4063 -- Smpl Soil 2 0.0 EOO-1311-4063 MS Smpl Soll 2 0 0 0 1:5 J - v V / r , 0 1:5 01 . S J t o V 0 1:5 EOO-1311-4064 -- Smpl Soit 2 0.0 48 1:5 EOO-1311-4065 -- Smpl Soll 2 0.0 48 r - 1 2 . a . s \ % l E00-1311-4066 -- Smpl Soll 2 0 0 48 1:5 / . s n t o j - EOO-1311-4066 MS s w Sol)2 0.0 48 1:5 EOO-1311-4067 -- Smpl Soll 2 -& tr 0 1:5 EOO-1311-4068 -- Smpl Soil 2 0 1:5 to rEOO-1311-4069 -- Smpl Soll 2 - . 0 1:5 J - S 8 U ? EOO-1311-4069 MS Smpl Soli 2 .* < r 0 1:5 'v . EOO-1311-4070 -- Smpl Soil 2 j * . 2 1:5 J . v r i P r EOO-1311-4071 -- Smpl Soll 2 2 1:5, EOO-1311-4072 -- Smpl Soi! 2 S o ' 2 1:5. S / V i p W cI EOO-1311-4072 MS Smp! Soll 2 - < s k 2 1.5 4 EOO-1311-4073 -- smpl Soil 2 4 15 EOO-1311-4074 -- Smpl Soll 2 ^ S 5 = 4 1:5 S . n a t i s i EOO-1311-4075 -- Smpl Soll 2 0 EOO-1311-4075 MS Soll 2 4 1:5 r i 4 1:5 " EOO-1311-4076 -- Smpl So 2 M - 8 1:5 EOO-1311-4077 -- Smpl Soll 2 8 1:5 i ^ - EOO-1311-4078 -- Smpl Soil 2 f i * 8 1:5 - EOO-1311-4078 MS Smpl Soll 2 8 15 EOO-1311-4079 j- i. -- Smpl Soil 2 o ' 16 1:5 J . ' H U EOO-1311-4080 -- Smpl Soll 2 ! * r 16 1:5 a . s o < 5 V * EOO-1311-4081 -- Smpl Soll 2 . W EOO-1311-4081 MS Smpl Soll 2 16 1:5 j . S ' u A 16 1:5 J EOO-1311-4082 EOO-1311-4083 _ -- Smpl So 2 X Smpl Soil 2 24 1.5 3 . * T o r ) i u 24 1:5 it ii EOO-1311-4084 -- Smpl Soil 2 ' \ r 1 : E0ri3t1-4084 VSmpl Soll 2 EOO-1311-4085 _ Smpl Soil 2 V , EOO-1311-4086 Smpl Soil 2 V o j EOO-1311-4087 -- Smpl Soil 2 > :00-1311-4087; i-M Sir '"'S/npf ^ :Sli * ' PAT 24 24 36 36 36 36 1:5 5 s a 5 J 15 J 1:5 J . S l i / A c . 1:5 15 3 v i 8 i l 15 \ EOO-1311-4088 ,, Smpi Soil 2 V 48 1:5 O . X r i f e T h s iJ e EOO-1311-4089 -- Smpl Soil 2 48 1:5 p . - 3 r 0 3 < ? EOO-1311-4090 -- Smpl Soil 2 S o 48 1:5 0 ?K- Start- /J 3/i/t *0 . t E00-t1311-4090 MS -i Smpi! Soil A ' ::':'48:': -iW GLP Study Number Eoo t i l l Hk- Sha^L 10 Xo Of-l 01 CAM- gk- U-ar-t '- (r W . P / ' / d e> 3M Environmental Laboratory i a0 1 i5 u I =0 3 | fil 1 || st ! 1 ^1 1 O* = l 15 s Vt l i il fce . !nVe 1 s I 1 oic i 9 10 11 12 13 J 14 15 16 7 18 ... _1_ S1 c tP I H ' !: s i 0 3 t ' a n i s . i S1 b < B # t r _ --j '-- _ S1 f W j ^ _ ^ r a a . iu i7 a I . a s . /S 5 5 3 R M S1 J , n V - ^ P . Ji e l 5 /q (q ,( ) S1 t . TB l SI \ t TTM S1 S1 T) 0 1 S1 1 .1 -- J f? l .rui-f ' * f S1 N P .C S1 ri 5 F S1 V. ttp a sa i v j s ii"5 P O ^ V^ ~ 7f\ J i-J ? _j 0S 1 S1 -^ 3 1 S1 V__ SI 0 0 "O D T u r > S1 1\ w _` P S1 rv - V j . . " ' l < >ri r J S1 4 a SI 17 O T " TJ -I SI * lo . 5 ^ S1 X T S1 7 \ ' -lN * M /T g , i f A .iO -- i-- i3 M li iM IS ,.0 S1 g < S1 i <\ r S1 J 4 ~ c V T TS1 ^ 0 S1 ;i 5 s i --X S1 S S S l 3S1 w ` a r S V ,j^ 5 .tS S1 f i t r ii r i qU ^ X l,r tf !a !io . > S1 T f b m m S1 i. i ':i:;;.:: V V . V v f v ' | xi: V i : S1 W J* j'- x J ''s r T? ? 5? <35*. a ie to V c T q te is i P ? .3 ? 7 o W | S1 S1 S1 J 4 te s s _ V i J : ;: :V :. r ! :v. 1 :V V , : . . ^ | i. V l ! S1 y * . S W i - .-of ,3 0 W CA~C : lo.lii P/I/U. C^C 3^. &ta.rt-3 oo tP/r/o/ c4/< L f ^9 0f 19 .5.U 5 - . 5 j r i ! j DI 3/ < 4 6 k . S V e ^ t - . ' i o ! o 9 - 1 5 ( 0 ! c j v u :~ Page 167 of 703 BACK TO MAIN Adsorption Kinetics f>PoSTest Substance: "oil/Sediment/Sludge Desccrriipptfiloonn: ) - r`Si<cKirT.\cXZai UL.OqcO ~TC\2-oooU .TJ-Qoq -Mu -KB- In a tti p H o f stP 9K ? o |y tip n ipH Stock Soin IDO l O & t " 5 ^ 0 pHS . & T/D/l 12 -V j^ p . / / / 0 / _ O V 1 C- P ( f Pal |p- T /D /ln '.Q ^ A m I / 3< / Q < C M C Col 9 S o r n lP ^ Q O l- '^ W o ^ T / D / l r 3 * 3 0 f J / B I / O ^ C - < n C _ Col 10 Inc. ID X Start Tima T/D /l < 3 / / B L Q l Q T V \C _ Stop Tima T/D /l T / Q V H 3 - / / / O j Col 11 Stock Soin ID Q l O O I - 3 " & S O l A t j ( * - i* P < 3 > C *-C Other Equilbrate tubas/contents tor designated hours. X * 0 hour Start T/D/1 M A 2 hour Stop T/D/l fir>\ r l / / jO t O f * - C y jT V 4 hour Stop T / D / l - / I O l fJT ^i C_ 8 hour Stop T/D/l JX / f i l C M C 10 hour s to p T /D /lL ' J O A i 3 - fJ l lp ( 24 hour Stop T/D/t / O W S f r l t D - iO \ C fh C 36 hour S to p T/D/l >' D S & * \ / 7 /O lC ^C Al ~IO*CJr*~\Mft. 4 8 hour u n TOT I ' / i D ^ V l C . gal-12 b d e h Centnflige tubes alter removal. Ohr T/D/l 2hr T/D/l / 2 i T/D/t r5 . ^5/v\ 8 hr T/D/l ' S'f>rr% 18 hr n o n io I / O 4 r r \ 36 hr 48 hr T/D/l // c 2 . y. / ,/ - j. S 3 - l ^ ,0 3 j -2 /O / C i^ -c ro i .c ((-> 1 r j w ( _ / I r m c _ /O I c > h r / c? t C *u C lO lC A n t O I i~ m r i aJ 0 ~3 fi 4 1 4Balance iD_ T/D/t / ipju*3> _ . / _ 3-i-Q-L cy*n c_ Col 15 pH one replcate of each set. a Ohr T / D / l f < / /9m T/D/l i o Q p n T/D/l c 3 'M o n i l l _____ / O i C * n < c l l( n ( fP m .C OI ( M T/D/l U L p (X w \ TfD/l7 / 5 > W H 0o t / - 3 / < / o u t at Z? >r>/ o n Col 17 b d 18 hr T/D/ic/ . V f l r l f . l O l CJf*-C T/0/1 l o * t 1 1 o f U v i r 1T/pn '. ^ O 3-1 1 a l C 4 4 - lX r TOT 3 1 0 0 2 - l i f t O l (_ T M 7 .J 0 r? -/3 4 O l C *v r^ 0V n U X _ jJ j L O n e h 48 hr t o t %i o q - 3 ( 7 / a / Col 18 Solke Soin ID C O O P ^ -- / < / "7 p f n ^ a Ohr T /D /l /(^ 7 O l_ *J^- 2 hr T/D/l _ 4 hr 7/Dfl _ 8 hr 16 hr T/D/l _ T/D/l _ 2 4 hr T/D/l _ 36 hr T/D/l _ I48 hr T/D/lt C -fl t IntermlSt.nd.rdIP:aoo >-oJ--OS ThPFsP o p f r r - ' T/D/l i i \ ?> IX I ^ / V q n C-- Col 19 w D ilution Factor (if Required!: j Q K 0 I C t - r < Methanol Itii T f O A * t o t S '. C C j t m , . / ~7 / L y * ' t ' a Q 1 s 1 'S ins 0 1 ' 10. &i 1 J 1 M >4 _____ ( ( t a L vt i f1 1 0U fl 1 ! a0 n i fi s s. I 0 U! l 1 S ; S8 M * si l * Weigh tube A contents, grenu Document pH Spite Amount, uL ? 1 ii 0 5 ! e <^3 9 ! L1 1 23 zr 6 7 8 1 ... 9 EOO-1311-4091 -- Smpl Soil 3 0.0 0 1:5 - O . i k i U k s EOO-1311-4092 _ Smpl Soil 3 0-0 0 1:5 a . w N q 10 11 12 13 14 15 ie . 17 z n t .1 9 j 7 ' j a m a m m l B g i a a i S1 " 7 j i j VId' f i i l i i i B ta r i i i S1 " 0 19 6^ ' V L , * * L - J . j p / i ( Ci EOO-1311-4093 _ Smpl Soli 3 0.0 E00-1311-4093 MS Smpl Soil 3 0.0 0 1:5 3 H M 3 - a 0 4:5 ;-- --j E00-1311-4094 _ Smpl Soil 3 0.0 46 1:5 t - i i l i u E00-1311-4095 __ Smpi Soil 3 0,0 48 1:5 i ' i l H a EOO-1311-4096 _ Smpl 1Soil 3 0.0 48 1:5 J . S I S ? r i EOO-1311-4096 MS Smpl Soli 3 0.0 48 1:5 ----------- 7 EOO-1311-4097 _ Smpl Soil 3 0 1:5 C D ci J* EOO-1311-4098 -- Smpl Soil3 ' S ' 0 1:5 B W SI '-- ,, ^ w&m,Z M rj , | | T fc - ti J3E _ t.m p .. S i a s .i^ fs L m m H O .lS H lT y L S P ^T T ^1 i l 4 1 S1 t ta - f i i s i i S1 __ 2 S1 J ~T S1 nriT-Ttvr; JttWi. fZ S1 t _S5i i i l i l S1 \ M J- 7r S1 S S1 " 3 ' r~ r : E00-1311-4099 -- Smpl Soil 3 f C 0 1:5 J m W T J ] j EOO-1311-4099 MS Smpl Soli 3 "Z}/ f h 0 1:5 1 s i E0O-1311-410O -- Smpi : Soil 3 2 1:5 3 M < = y \ E00-1311-4101 -- Smpi ! Soil 3 2 1:5 0 . 4 8 ^ 3 EOO-1311-4102 _ Smpl Soil 3 2 1:5 h ? . 4 < ? S - 7 sH zn im I__ 3 3 U '3 e 3 3 2 S 3 s i; l - \ S1 1->d : S1 _ z S1 L Z S1 ~Q S1 ~L frJ L r & wm . EOO-1311-4102 MS Smpl Soil 3 - d S C 2 1:5 \ EOO-1311-4103 Smpl 1 Soil 3 s i r 4 1:5 - EOO-1311-4104 Smpl Soil 3 3^ 4 1:5 z t m J EOO-1311-4105 SmplH Soli 3 ^ 0- 4 1:5 3 - S c ) o a 3 5 d1 X Z1 1 ~qy~Ti - S1 ^F T iT F R y rS wB r S1 5 S1 J S1 L -- z _s EOO-1311-4105 MS Smpl Son 3 S fi- i EOO-1311-4106 X . EOO-1311-4107 _ _ Smpl Soli 3 r^ \ Smpl Soil 3 i ? EOO-1311-4108 _ Smpl Soil 3 E t 131 ^ 4 1 0 8 MS Smpl Soil 3 ? 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H X 1 S a 8 ' 1:5 0 . 4 9 ^ " r a 1:5 3 - 4 R o l l i a P 5 sJ _c i "Th PS ; /f. ....^ t M f i S- -- V1 \ i ii y 8 1:5 j 16 1:5 & & ( & ) c. 16 1:5 ' 3 . 5 1 3 " 1 3 16 1:5 a w j Q , ( ^ 16 1:5 S 24 1:5 A 2 W I Q c 24 1:5 r Q74) . 5 V 8 o 2 24 1:5 - 4 l | " l 24 1:5 c z 71 7* 36 1:5 a - 5 o ( i i i 7 36 1:5 > . 5 ( ^ / 4 zz --, qZ O S -m & M s w m x: ta c~G^ -X 1 r zt a y / r0 c \ h 1 X M ^ ___~ . : - >X O s ir q v < << zz \/ ^ fr). \ Z :;S b ;P lZ Z :T s v/v c S P z v' j Z iM 36 1.5 I" S \r .2... q r i x t ' W ^ j R 6 > . 8 36 1:5 48 1:5 I 448 1:5 E 5 3 S X m 1 -- ---48 1:5 33 . M U 5 0 c^c 5 >A & . O W - l a - M zi T3 Q a a s y S rl m m 32b " 2 3 -115 ! j t Z Z taIL EEES48 1:5 \ S1 t a S1 n j a t & | S1 J L __ j S1 2 T j ip V -- S1 z L _ J l. S1 Z 8 S ] S1 j m 13 S1 1 S1 p * & ,, L - i S1 1 5 V S1 i r T _a S1 ~ r j "V ta S1 3 K < j s S1 ' j s S1 S1 __ N 4 S1 s rEgsS 2> J - T S l S1 " J S1 S1 i P 4 4 _> Lta/ EOO-// t^aryGLP Study Number Q X & t J - O O o , CY `O L /O ,3^, C4A.I l / y /01 0 oi^ '' otcm-i - . d ie d ri r o t |p k. o n ta r f * o ' . CJUf " 4 1 $ k . & W + : / ' . 4 S t o / l.i o , , c M t ^ 36<. S+r-t-.'? OOfnts lo t o w e 8k Sfar-f:k ta'ta /"/diouf 4k 5tar/-' l i s c i l i , h i a*-t_ ta 3/W Environmental Laboratory Page 168 of 703 BACK TO MAIN Adsorption Kinetics :e: p F o S S oil/Sedlm ent/Sludge D escriptio n: . Vci 1 SrdCmaA-l (. i`ucr) MA-JLfL-OiOUS'riJ.. K3f\- Initial p H o f S tock S o lu tio n (pH Paper! Stock Solo ID n I G O ! " 10HHS . T/D/I M .V 5 - H i 1 / C. c lj aHP B H - __ tidji <3*. f o a w I i d r t i o l C* u . Cot Som IPPOCOI - 3 t f ~ t 3 r m \ U p * I t ? I___t O l O T w C Col 10 Start Time T/D/I 2 * _ J .___ / 3 / ` C Stop Time T /D /I" 7 / O A f t* o L / f / C_ Col 11 Stock Soln ID Q | O O j T/D/I f t ' > > ^ 1 A t & I O i C i v \ Equilibrate tubes/contents for designated hours. 1 - 0 0 h o u r S tart T/D/I ~ I 7 ~~ b 2 hour Stop T / D / I I 9 l / / & / 6 I V \ C - c 4 hour S lo p T/D/W a L 'o ^ O jC w 9 / 1 / D I C > V l C d 8 hour StooT/D /lP l ^ ^ m / > /6 / C /v t< L O th e r K J A - ------------ --------------------------- - ----- e 13 hour Stop T /D / I Q J X tC f 24 hour Stop T /D /I/>: 7 S ^ V 1 t/5 i . 38 hour S to p T/D/I > Q^> r p / "7 /O ' ) C4V> C Other j j V j B : 48 hour Stop T/D/I ) '. 3 0 ^ * 1 A / 7 / 0 ) L Centrifuge tubes after removal. O hr T/D/i 21 T/M 13.' 4 hr T/D/I I l / J _ jL iY lC ,, 8 h r . T/D/I, 16 hr T/D/I ( z , 24 hr T/D/I 30 hr T/D/I ( p ' 0 > A m 40 hr T/D /i l!< f> tm -c2_/_5_/O l_r> n< - ,2 - / /C?/ iC>l . 9 /J 2 /_Q( M C o? / 7 1 0 I <xmr q / VBalance ID _ T/D/i / / * 1 O f t r y o L / 3 - 1 <p 1 . c * x i-- Col 15 pH one repcate o f each set. Ohr i/l^ . '/ x i T A m A t i / Ci C * Y V C 2hr T/D/I / l ( T p f i \ <9 / / / Q / 4hr 'D/lPmO^^, -- q L /-- L j O L C Jy v C & l g /p8 hr t)/ll o si 9! c- 10 hr f 24 hr T/D/I { L __ 9 I _ / J 2 S * C n l r./H L g 36 hr T/D/I *7 - . h 48 hr T/D/1 Col 17 Ohr T/D/I I s t i .- , 2 h r T/D/I < J. / / / O / fW o C 4 hr T/D/^ lp a /1/o urn, 8 hr 16hr T/D/I 3 T /D /i 9 i S lO i CJ / r ) JskJQ j 24 hr T/D/I J 2 _ /^ ./ / /T'tdi36 hr I5~ < 3 / 7 / o j _ t r v \ ^ 48 hr t/d/i3-'0 J./7 /3/ C4VOQ SeUS Spike Soin ID 0 D Q p 3 W 4 / ~7 ) Q ^ v \. _ P F o > a Ohr T /D /I(OaOO<^2 / Q<LOt^f- b 2 hr T/D/I _ c 4 hr T/0/1 _ d 8 hr T/D/I _ e 16 hr T/D/I __ _______ ,/. f 24 hr T/D/I _ g 30 h r T/D/I * h 48 hr T/D/I f a ' *r 5 Inte rnal y q pf a r t IP; Q ( Pol - o ^ ~ o Kn ^ f p ^ o s T/D/I : 2 0 / f a \ . . 1 ^ j O l c w L < _ 9L19 ^ ,v Dilution f actor (If Reaulredl: ^ Q v D i IU - T I M ethanol IDn ~ ! M f T/D/i ^ c x p p t r N 12 1r ^ / / o i q v -C _ Type o f Smpl Weight of Sod, grams Stock Test Subst. 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Sed 1 Smpl S e d i , * i r - Smpl Sed 1 > e r MS Smpl Sed i 5 ^ -- i Smpl i S e d i !J L -- Smpl Sed 1 S4T- -- Smpl S e d i MS Smpl S e d i . ^ r * -- Smpl Sed 1 ,, Smpl Sed 1 J l -- Smpl Sed 1 MS Smpl Sed 1 in Smpl Sed 1 - Smpl Smpl MS : Smpl Sed 1 Sed 1 _ t L Sedi -- Smpl Sed 1 _ Smpl Sed 1 , * r _ Smpl S e d i ; MS Smpl S e d i 3 ! $ - -- i Smpl Sed 1 -- Smpl S e d i _ Smpl iMS Smpl Sed 1 Sed 1 - M - -- 1 Smpl : Sed 1 i fi* _ Smpt S e d i _ Smpl S e d i 07 8 0 1:5 J . S 'J / <, J 11 12 13 J 14 15 10 17 18 1a i 19 r L S . S u i 1 . 5: . 0 1:5 J . S i S l t 0 1:5 j . i t e n e 0 1:5 > 48 1:5 J . g p g R j r 48 1:5 J . T - i J 48 1:5 < 2.6 l o t , J 48 1:5 ! J 5 ? H p iii y ft1 r * L -|L = J P * . -- -- ULJ*V ? J . O ' f e i f=ESt S r Z I - O S I I H ? M .s s b t 7 ? o l : rn j- si S1 S1 S1 si S1 s, ^7 .^ 4" ' C H-lpSfP li.'iS.v f` '.e/E-t 0 " lili \Q O JL ! r-- _ $ M y j o 0 1:5 -- iiJgSjgrrftjcgK V ^ k w H H M l m Si 0 1:5 t e n 0 1:5 U . S o t t i ---- -- H 8 fp p s i vjT -j -- -- 0 1 5 1 -------- ^ ------ --i 1-- -- S1 > ( 2 o J L 2 1.5 b . s o s t o * . 2 1:5 .3 . 5 ( < M i r ;^ / ^ X 3 [S 4 j iB nR rr ^ o 2 1:5 2 13 r Sj -* 1 3 Kj j3 S W ^ ^ S ^ Z c > s i T a M a t e ... ........ ................. ....i s i i ms 4 1:5 2 . S O & , * _A - 7 j L s i J .\ f ^ r i *s\ l` 4 1:5 4 1:5 , L1 .4 * 1 1 \ b rt - fe ^ tn.~y st ^ >? fsil !;} * ri R t ^ T 4 1:5 --------------------------^ n n FO T i i8 8 1:5 I S c r iii 1:5 S o i o i 1 -- 8 15 1 S W / -- -t 3 lii! 1 i Hi A * f e s m -7 . |c p rr s i 3 ids^ii = 7 si T s S 1 V 8 15 n 1 16 1:5 l o / . S O 3 1 Ot 16 1:5 Q l . o a o w ' 16 1.5 P > s o s t i 16 1 3 ___i Iw nii IAi s C Q KJ df O ----- w - 3- s .-- - si G IS1 b j l l j rr --- o--- -----s--,------- 3 7 T -- S1 \ r O O jtL - p 24 1.5 ir .5 Q H ,$ g ___ 24 i 1:5 3 . S M s . 24 1:5 J . j M ; 3 _yE | _ 3 N J M M M M M M 3 ^ M S i- T 6 si ^ - = . si ^ si < < s S g 24 1 5 I1 ^ _ 7 1 -- -- si u 1 36 1 3 ! 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Uv^<- S/v. 5^^/ j/ 'Iiich'C `JJ'Jv.SW. t/iS"/o/cm-c 3M Environmental Laboratory Page 169 of 703 BACK TO MAIN Adsorption Kinetics .Soil/Sediment/SHjdge Description: _ % l ` D' ome.t'ffc S in d c,*____ * o o c ,fr5 -6 io _______ t- oa iiS - n i f lutti! p H o f S tock S o lutio n (pH Paperi Stock S oh IO <3t P O I " 1 ' ? V * j L T/D/l Z i// !Q U r ^ i (# mH rtff.BflHP - - T/P/l 1 Col 9 S o rn lD i-^O I - ^ V -V -2 x r/D /V < 7 /,J ^ > rt / / V /3 ^ >or lO i Co) 10 Inc. IP J T -- / _________ Start Time T/D/l Q - 3 io > n \ ) i 3 J I O t Q h * -* - Stop Time T/D/l 1 . ) < ^> fo v y <- / / / O l C ^ v * C C d 11 Stock Soin ID C * o O j _ ^ 3 - f f ? f= C tS Saur Q> Equfbm te tubes/contents fo r designated hours. 0 h o u r S tart T/D/I M / V I 2 hour Stop T/D /l >0-7 / / O t 4 hour S to p T/D /l f ) O p * & / / iO ) 8 hour Stop 1/ __ C C O ther K l f t Other, l \ J P r 16 hour s to p T /o V ^A J r l t O f CS*C 24 hour Stop T/D/l f / 3 1 Q , 3 . / 3- / >< ^ 36 hour S to p T/D /l ( b . f l S r W 2- / 7 Q I L ^ C-- 48 hour Stop T/Dfl I 1 oL/ 7 / Q ( P F b 'S Centrifuge tubes after removal. 0 hr T/D/l <? ^ c\ A n ^ / ( / Q / 2 hr T/D/l / ? .* 5~ Of>jl 3 . / / / Q l _ C j n C _ 4 hr &T/D/l 3 . 3 q p r n Il ! Ql (JV 1.C . a hr 10 hr t id /^ W ^ m T/D/l l o 'A & A * ^ rP - / J T A i O L l e L fO ( C.P* i C 24 hr 36 hr T/D/l a- O b r t- u g / J /Q i C J W , 48 hr T /D /lJ * Col 14 Balance ID 5 t L T/D/i K * j Q ^ i n a? t~ l j O I CJV\C. t/d/i ^ /j j e x *-- 2 hr t /d / i / A / / Di CJ^ C 4 tv T/Dtt '. I O O l) I A C M - O 8 hr T/0/l3.'OD ftl OTV 10 hr T/D/lT J / J - t O I 24 hr t/d/ii o < r 3 - / 3 / a i c / v ie . 38 hr nanT . I S n m l O H C 48 hr t/d/i3 'C P / ./.X / C L C J v \C _ C o ll Spili*SohID r v r lP O .? ~ N 7 1 0 ^1 ?P 03 oL Orvt-- pH one replicate o f each set 0 hr T/D/t 2 h r T/D/l / ' / Q~y T/D/lp . ^ Q , T/D/l Q ^ -d _ L_/Ja_'QLan<- 2 - ! 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H 1 S H i W M 'X r ? ? /ig a a iM ! g S M S1 S1 r~ -jwrigk S1 J im _2l _Q I l s l ' 5 N l o ^^ lS S1 3 S1 J S X S1 3 1 S jJ I n r _ Smpl Slg 1 e t 2 1:5 J . 5 I X S1 i s 3 _ rt.s !W _ MS Smpl S ig i * r 2 1 5 invilii : S1 ~ v j _ fiO /Jr- 3 r - Smpl Stg t [ e . 4 1:5 ^ 7 7 4 . -- -- Smpl Sk}1 4 1:5 ?. \ I ~1 T T T ~ S1 -- t iS S1 " w m "s, _ 5?mpl MS : Smpl -- ; Smpl Slg 1 g S igi d 4 1:5 a . M - l 5 r j 4 15 8 1:5 0 . 1 1 3 0 ~ rj 3 C ^ a ;;.;:;:; ^ is iii &&& S1 3-- 'J S1 S1 3Pi r M m L ^ -P -, ?> " ' EOO-1311-4167 ' 1 EOO-1311-4168 ) 00-13114168 EOO-1311-4169 EOO-1311-4170 _ ' Smpl Slg 1 -- Smpl Slg 1 y MS Smpl : 3 3 1 -- _ Smpl Smpl S ig i rs'-s T: s ig i 8 1:5 D - H i s S l t 8 1:5 , 2 . y 7 7 i ,t 8 1:5 16 1:5 O i Z o i t j * 16 | 1:5 J - S / T / V TT i__ 11 rS , S1 v r S - ' & T S1 t f I !:-:ib;w r . -'H1:1: ; - . S S1 S1 Z 7r 5 __ ip i ' - l l 7^ -5_ i 4 t ? 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NA Soli Soli Soli Soli ros jo adAj 3 a|duitsjo adAj <n 1 1 1 1 1 1 i | 11111 Wo i | to I I 3 I ws I s 1 r w 1 a I f tos s i IJ SH M 1 n i l 11 1 1 1;i 1 1 ' 1 1 1 i1 ' 1 l i i =Kri)- -is V-o (Ba|dm5 - f If rit in -l5 i5 l i lo i-T?" oI Iri i l l n 1 i l l I 1 1il 21 1 iIjJ Ui j :lill UiJ :: Ui i .;iiu UiJ liij mi uI5 LiLl 1 1 1 I I l i ^ i i . i 6 3M Environmental Laboratory P age 171 of 703 2 of 2 fp ( ^ ) ( p sluauiuj3 1 c;1 5 1 g ey1 O/ ri 4l5 7 ii cv1 >1 ^ /v Al r A V 1 # 1 o< I* o < uojuppv pJHpUBJS|BUJ3)U 11 in `(sejdiuss 1 i uomppmvo3M))O!dTsPxujjBVZH) S $Z 1 s li sjq8frjejjBuo|)dJOse(] 3 \ U(Hoj)dj(ossa|dQu)iB8Ss a s CCOOCcOo:| I u r bsl|;_c, Aft 7 r /fl Y: 1 A <i l l ?/ f c ^ I i '2 0I f 2 1 1 1 j <2 1 L ? 1 1 |5 <CO0a>:M *oqCCOO"0c0okS3> CtoOs w1 s 8 0(00;m1ffi. CwO<c0o C<O08 *jqZE uo|jdJosea y /i- ii | pr 1 , m (7> (s|duns uoijdjosaa)S sjqfz -I0Uuopdiosac KCOWis is &co|^ coto icso. 0 \ i Us/ d lo ft ICsO. 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Multiple Concentrations ETS-8-160 Test Substance: PFOS Page 173 of 703 3M Environmental Laboratory GLP Study Number EOO-1311 1 of 12 BACK TO MAIN Sample ID Type of Sample Type of Soil Cone., Test Substance, mg/L Time Point SoikSolution Ratio Sample Descriptor Weight of Soil, grams (2.50 +/0.05) Equilibration (at least 12 hours) Test Subst Addition (Record voi) Equilibration (48 hours) Weigh container (Record grams) centrifuge (Y/N) Document pH Spike Amount Page 174 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS -- OT 12 E00-1311-5019 -- EOO-1311-5020 -- EOO-1311-5021 -- EOO-1311-5021 MS EOO-1311-5022 -- EOO-1311-5023 -- E00-1311-5024 -- EOO-1311-5024 EOO-1311-5025 EOO-1311-5026 EOO-1311-5027 MS -- _ -- E00-1311-5027 MS EOO-1311-5028 E00-1311-5029 EOO-1311-5030 -- -- _ EOO-1311-5030: MS EOO-1311-5031 -- EOO-1311-5032 -- EOO-1311-5033 _ EOO-1311-5033 MS EOO-1311-5034 -- EOO-1311-5035 -- EOO-1311-5036 -- EOO-1311-5036 ~MS~ 3 Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control Control ; Oo i\ 4 5 6 78 9 10 7 ^ 1 NA 0 48 NA S1 t o ' W s i f f 2 8 7 S 12 NA 0 48 NA S1 12.5 NA 0 48 NA S1 g|Sl5 12.5 . NA 0 48 NA S1 -- . 12.5 NA 0.5 48 NA S1 12.5 12.5uLT NA NA ; na NA NA NA NA NA 0.5 48 NA S1 I T T 1__ 12.5uL 0.5 48 NA S1 12 5 12.5uL 0.5 : 48: : NA KStif -- 12.5 12.5uL 2.0 48 NA S1 I Z 50uL 2.0 48 2.0 48 2.0 :! :4S NA NA NA S1 S1 SKBWSSS 12.5 12.5 73 --V ___L iy. :STu: -- 12.5 m 50uL 50uL 50uL 73 5.0 48 NA S1 l 12.4 \ 125uL NA 5.0 48 NA S1 NA 5.0 48 NA S1 12.4 12.4 j 3 1 125uL 125uL 1 NA!ii 5.0 K48'i NA NA 10 48 NA NA 10 48 NA NA 10 48 NA NA c 10T^1rx 48 I NA m s i= S1 S1 S1 -- [i24~ ~KJ 125uU B a ie g* 1 250uL - j [12I 5 250uL 12.25 -- FiZ25 250uL 5 250uL NA 50 48 NA S1 [T ils 1.25mL NA 50 48 NA S1 11.25 1.25mL NA 50 48 NA S1 aac 'v&so l [T ils 1.25mL mNA 50 I NA :::;:S1:.|:, -- T T 23 Zj N7 1.25mb z _ r~ 1? 14 15 16 \ t . 5 - f s r <4 I 9 . lc ts > 8 S q asssss& f.-n -- iq.ioi& H s oe m m ifc'^5;* to 3 lie ct. m & M S S * M -SU L3d m sm m T. .-- 4VI Oo T < N /<?.(*/4 16.5717 Q e'.8rKaSi::id -- C v )U iS O i - S I K A .ia n r i____ H 55? 3 9 <4 6 6, 5 P tS S % \P S .s -- JsBWlr- S. B -- 19. S X l S Q ?1 ^ . 7 6 9 ! a jcj.S fcV jc 5. s \ ------ ---------7 ~ 1 -- E a > i Tl a 17 /- 18 1 . j $e0 E E0 1V 8 ^ 3 --1 IXU to u t- a s s fe T X SM g > N -1- 0 ______ ' : ^x . . y d 4Sa;K;`;: i uJ\^ r sm sm "J S " \ *:l:>` j Z * ... i _ .. 0 X T ~ y ----------------- ffi i oe sm m WSBSMSft 'x v;"X'':'' TJ Or- am m m 5 >7 1 L __________ Col 9 Balance ID ~ C o in Inc id .4 - - Time/Date/lnitials isbftr- - t - Equil Start T/D/lp ; r O f n p . I -l O l CJrr\( Col 10 0.01 M CaCI2 soin ID n C O o l J - EquilStop T/D/l l . o o r ^ d - Il^ l o i r j n C Time/Date/lnitialsfl.'r'D r . 3 / 13.1 o t ru n.C_ S.pH of Test Soin. S ' Col 12 Test Subst. ID O l o o l - c g - O T Test Substance cone.: 500ug/ml_________ Time/Date/lnitialso>- f l & t o I c m ( L Time/Date/lnitials^ - ^ ? ^ / i S / o i C JY \C- fa? @wu.in- I:/ a^`rgu_cLuAfa4 " X ttioH - cTM ft-475S) < 2 / / 0 / S CHi C- i.'io on jlttfoU (.TNfl " M7J"5"5 <S/ / U /oI o n c C ol13 Inc ID ________ Equil start T/D/i I f t in r M r EquilStop T/D/l o? 1)5 hi c jM c C o l1 4 Balance ID " 5 T 3 ~ Time/Date/lnitials 3 U S '!Of C M C Col 15 T/D/l - 1 / -------- Col 16 T/D/l IQ './Q rt^ cQ / IS~ /P)l f i n C c o M 7 T/p/noM Q Am A / t s - n i f ^ y y Col 18 Spike soin ID # Hi T est Substance cone.: lOfPiyx Time/Date/lnitials IO'. j a a m J /o ld / Ol c t yq C_ Internal Standard ID # c u v - i i - q j - o i Internal STD cone.: ^ O p o /n Time/Date/lnitials H' M Q iw J < 7 0 /0 I c_iv\ C lol.&ylAC* I -i^i^v-VC-rTVCui 3+ct fXcAiiirf-- j /^ oj oi em-c Q S h r tJ lo lit a rH riotrafit*. in -_ U n fc / W w w o/ (2 ) ic ^ u ^ r rC m O i^eA > > il X f . n (TQibiM col /0 X cuA X " \ ~ l M^o/4 CTNW- 3 /lG /o ! C A C - GLP Study Number: EOO-1311 2 of 12 3/W Environmental Laboratory I Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS Page 175 of 703 3M Environmental Laboratory GLP Study Number: EOO-1311 r.loo on H-iOlf TS" 2//(o/M Of^C Q amples S h re J ujicUj- re ri^ ra ^ o t^ iryiL'i. usih( i l u i f j ai/o^ unaJcjieei () ckc. H'M ' O! 3 of 12 BACK TO MAIN Page 176 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-16Q Test Substance: PFOS Sample ID Type of Sample Type of Soil Cone., Test Substance, mg/L Time Point SolkSolution Ratio Sample Descriptor Weight of Soil, grams (2.50 +/0.05) mL of 0.01 M CaCI2 Soin Equilibration (at least 12 hours) Test Subst Addition (Record voi) Equilibration (48 hours) Weigh container (Record grams) Document pH m Lof Sample Spike Amount 1 EOO-1311-5055 EOO-1311-5056 E00-1311-5057 E00-1311-5057 EOO-1311-5058 EOO-1311-5059 EOO-1311-5060 EOO-1311-5060 EOO-1311-5061 EOO-1311-5062 EOO-1311-5063 EOO-1311-5063 EOO-1311-5064 EOO-1311-5065 EOO-1311-5066 EOO-1311-5066 E00-1311-5067 EOO-1311-5068 E00-1311-5069 EOO-1311-5069 EOO-1311-5070 EOO-1311-5071 EOO-1311-5072 EOO-1311-5072 (fi 2 23 45 _ Sample Soil 1 0 67 48 1:5 ~ Sample s o in 0 48 1:5 -- Sample Soil 1 0 48 1:5 MSI Sarhpl: s o in 0 48 1:5 _ Sample Soil 1 0.5 48 1:5 -- Sample Soil 1 0,5 48 1:5 -- Sample Soi) 1 0.5 48 1:5 MS Sample S o ilt 0.5 48 1:5 -- Sample Soil 1 2.0 48 1:5 _ Sample s o in 2.0 48 1:5 -- Sample s o in 2.0 48 1:5 MS Sample s o in 2.0 48 1:5 -- Sample s o in 5.0 48 1:5 -- Sample Soil 1 5.0 48 1:5 -- Sample Soil 1 5.0 48 1:5 MS Sample s o in 5.0 48 1:5 -- Sample Soil 1 10 48 1:5 -- Sample Soil 1 10 48 1:5 -- Sample Soil 1 10 48 1:5 MS Sample s o in ; n 0 7 : 48 1 ::T:5:i _ Sample Soil 1 50 48 1:5 -- Sample Soil 1 50 48 1:5 -- Sample s o in 50 48 1:5 MS Sample s o in 50 :48;x.:. 1:5 8.9 10 S1 4 M 7 12.5 V S1 3 . H 3 8 < d . 12.5 S1 7 . 4 s m j 12.5 S1 12 5 S1 12.5 S1 S M l r f i X 12.5 S1 9 . S o n v M 12.5 * S1 12.5 S1 c ^ . s n D o 12.5 \ S1 19 . S o n i S1 S1 n S1 12.5 . 12.5 12.5 N* 12.4 S1 12.4 v i S1 3 - S o s *j 12.4 S1 12.4 S1 12.25 s) S1 12.25 S1 5 . 4 q a L 12.25 S S1 12.25 S1 3 m Z t j T 11.25 S1 A .V O U 11.25 S1 S1 w 11.25 Zi 11.2S 11 12 IV. a SCTftW d g )% a3 cai 5 e0u 13 14 5 16 17 2 S . i o o T 5 J ft3 t.ll K - m m m ------ 7 V M a E ---------------- 7 . 0E0 18 ------------ \ Si A / o r s m uT ^-- 2i9lsSi>,Bfe 12.5uC Q j . r & b b `V ftaX; "0-- ------ 12.5uL O - i 3 i - L -- 12.5uL s o . n o s o, b . 12.5uL 50uL N ` 3 3 S t a b 1 <\ m z m ! 1 1 TT~ -- 50uL \ S i .m q -* , < 50uL J) / . o q o \ te 5 \j 50uL 'S "5 125uL N . u T i J . I O M S " C V, T $ 'o 125uL V 125uL Vi SJ.5-1 q i> ^ 't 6 125uL < ? 1 1 K j c* * t-- .Q *ci- ---N----7' :^ w 'li j 0 VJ O{ 250uL S 3 . * 4 S ' 01 %&&&&& 0 250uL S O -l.T t-M 250uL J M o lrD b mi c250uL 1.25mL 1.25mL 9 2 .IIV b q 93 u n m m sim S tJ jiU f *T- -- 1.25mL Li--- 1.25mL. js .a o i (a. & 1 -- ___ : J - c Q * i.k >/ t . m x i s Col 9 Balance ID H I i f ______________ Col 11 Inc ID L ' t3->_____________ Time/Date/lnitials ll/S p n , I ISMI 0 1 (_ Equil Start T/D/l 2 ! fO&m. J3. t A -la / C J^t Col 10 0.01 M CaCI2 soin ID UccnOI - - i<3- Equil Stop T/D/l ~ 7 L G r x * * J - 111 b l CJ* c_ Time/Date/lnitials 2 1 <9- / 3-1 l c m c pH of Test Soin. j 7 o Co112 Test Subst. ID * D IC O '- P S - T Test Substance cone.;__500ug/ml_________ T i m e / D a t e / l n i t i a l s l[ -l Q / Ct v C Time/Date/lnitials^ - L / / ft / n< r > / l C i I 3 e- C I Q> hi oa "i&u&tujheaL" J/lb /o i O Col 13 Inc ID J - 1 3 - _____________ Col 16 T/D/l /0 <30** ^ /l*T /Ol TVsif ^ Equil Start T/D/l cJ //3 tat c m c Col 17 T/D/l 10- n W l /l/s /Al r m C- EquilStop T/D/l //q~lft I rfv' C Col 18 Spike spin ID t cuoo.3- |H T ______ Col 14 Balance ID _________ Test Substance cone.: lOfpwv Time/Date/lnitials *3 './Oar* 3- / /5 T o I CtV\ C Time/Date/lnitials i o'-acu-, ^ 19-01 o l cw <_ (^Internal Standard ID # n n n i - csj-o /_____ Col 15 T/D/l T . fo * * . 3~ IIF T I 6 l es n C_ Internal STD conc.- J o ^ , t j cJ LA - Time/Date/lnitials ir /PO/ Ot c 5a*y>/<s SfonrJ uAit-r nrfr,Q(rajS SitZ'A. Uri i d e l u d i curici f 0r 0-f\a.t^Zed <^CM- V'iW-oI T C -^ - O c X iS ' - 7 7 i / c ^ / a i cj*y<L (DJIur-kX li io m " 6'poonfc^" xw/ Hf/f Tnft ' 9 / i U j o I LS*\<- ftffjx io u i la ^e s - rtm o o e d ounS-h -k e s S+amcC .t * T t ^ p U n ht i-SorU S te p .(0 tm c 4-il</-e>l Q ' A u L k ^ i l u ^ kjcL -f GLP Study Number: EOO-1311 3/lu/ol C hC r 4 of 12 3M Environmental Laboratory BACK TO MAIN Sample ID Type of Sample Type of Soli Conc., Test Substance, mg/L Time Point Soii:Solutlon Ratio Sample ^Descriptor Weight of Soil, grams (2.50 +/0.05) mL of 0.01 M CaCI2 Soin -- Equilibration (at least 12 hours) TestSubst Addition (Record voi) Equilibration (48 hours) Weigh container (Record grams) Document pH mLof Spike Amount Page 177 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-16Q Test Substance: PFOS 1 EOO-1311-5073 EOO-13 1 1 -5 0 7 4 E00-1311-5075 EOO-13 1 1 -5 0 7 5 EOO-13 1 1 -5 0 7 6 EOO-13 1 1 -5 0 7 7 EOO-13 1 1 -5 0 7 8 E00-1311-5078 EOO-13 1 1 -5 0 7 9 EOO-13 1 1 -5 0 8 0 EOO-1311-5081 E00-1311-5081 EOO-1311-5082 EOO-1311-5083 EOO-1311-5084 E00-1311-5084: EOO-13 1 1 -5 0 8 5 E00-1311-5086 E00-1311-5087 EOO-13 1 1 -5 0 8 7 E00-1311-5088 E00-1311-5089 E00-1311-5090 E00-1311-5090 (0 2 __ -- -- MS -- -- -- MS _ -- -- MS ._ -- -- MS -- -- -- MS -- -- -- MS 3 Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample S a m ple Sample Sample Sample S a m ple 4 5 67 Soil 2 0 0 1:5 Soli 2 0 0 1:5 Soil 2 0 0 1:5 Soil 2 0 0 1:5 Soil 2 0.5 0 1:5 Soil 2 0.5 0 1:5 Soil 2 0.5 0 1:5 Soil 2 0.5 ^ Q p n lui-;. Soil 2 2.0 0 1:5 Soil 2 2.0 0 1:5 Soil 2 2.0 0 1:5 0Soil 2 2:0 ;r 1:1 Si 1:5 Soil 2 5.0 0 1:5 Soil 2 5.0 0 1:5 Soil 2 5.0 0 1:5 Soil 2 5.0 0 1:5 Soil 2 10 0 1:5 Soil 2 10 0 1:5 Soil 2 10 0 1:5 rSoil 2 KIO: ;:4 1:5;; Soil 2 50 0 1:5 Soil 2 50 0 1:5 Soil 2 50 0 1:5 Soli 2; 50 0 1:5 89 10 11 12 13 14 S1 3 . s a i o n 1 2 .5 " s S1 o. c ja a s r - 6 12.5 Hit S f i S S S1 ol. S1 12.5 12.5 M T -- S1 . ^ l H c j 12.5 12.5u fc S i ' S ftS s ; S1 a . W S1 S1 3 12.5 12.5 ? 12.5 12.5uL 12.5uL 12.5uL S S S m u m m isisrsiS ilS S w -- S1 a . w i i L 12.5 50uL V M 8 W < 3^S i4d4^iitlss: S1 a l . S I H U a 12.5 \S1 2 4 8 4 1 12.5 50uL 50uL fP S S .; s srn sm S1 S1 S1 a ^ f s i S1 12.5 <n 12 4 \ i 12.4 iS 12.4 v L U S*1 50uL 125uL h v r 125uL v i < 125uL --. W K S f S a e i^ g mmm S1 12.4 125uL pJ S1 a s m a 12.25 nS1 e ? . S G J 3 12.25 'eis.250uL jttrrq rc i 250uL \\ S1 12.25 , i 250uL S iS fe S : fflS ^S S iiS S R S1 12.25 250uL S1 JS cpg a 11.25 2S1 q.SdSio 11.25 S1 ry H&t-u y 11.25 S1 11.2 ____ N -- 1.25mL rumsm 1.25mL w m m 1 ,25m L )1 25 m b -- i j j 1i 15 r r 'C----- 16 U. O a iERn -- rV X-- 18 # iS * c-- ffl aq.n- Q 3 ea E E 0 - fr . >> (o .O U J ^ .. ... .T-! i V; 1::-ri---: tJ------ ------ T 5---------- Oi 4 , > S \ a ___ T S 3 V : , - : .. ffis s ia s i ,s .f3 ) L, o -- ^Str^lU Aq..L <s;' J f \ n : /V (a r.:;; .- S iS K S fe ) u . o% s . * s a hOSfSk/ j ??> _ 90*1-N - ____ :S m. C ol 9 B a lance ID t f H o _________________ C o in Inc ID i - - Y c Z - ___________ Time/Date/lnitials 9 & I O *wi I / Z o lQ t Ltx, <_ Equi! Start T/D/l ,3 / ^ A - h 3 / A I1 Caw r C ol 10 0.01 M CaCI2 soin ID # o Equil Stop T/D/IT.cX3cii.^L / 13/01 r j v t t_ T im e /D a te /ln itia ls ^?. <2 1/2- I O c * * c . pH of Test Soin, g Col 12 Test Subst. ID # q o O I - Q S - 7 Test Substance cone.:__500ug/m l__________ Time/Date/lnitials^ l [ 2 _ l C j CJw i. Time/Date/lnitials <??: cX>pA\Jl_HQ Q / r jv > C- Col 13 Inc ID M A Col 16 VDnS '.o o o ^ A i N /O l Equil Start T/D/l N'A - Col 17 T/D/IA.'OOpM <9- I N AatCTvnC Equil Stop T/D/l M A - Co! 18 Spike spin ID # epao 3 - >M1______ Col14 Balance ID t o f Time/Date/lnitialsi\\A - -f--f- Test Substance cone.: /Oppyrx Time/Date/lnitials &o /o l O we. ^Internal Standard ID #c>v oo | - 0 3 - - a 1 Col 15 T/D/lc O p .v i i / IM /O l c m C- Internal STD conc.:r3Dffim.t - ^oU U .a Time/Date/lnitials H'.g / o l (_ Sb,| L ooo^S iSaloi c / n c u.fe(L I'. I o n " w / M < (4 T U ' ' - H~.5\5 & / L e i O t C J ^ L. f w ir " @bKu.rcl no n"S)3A-n|y V-/ PUC14 TKJf t ' MIS'S" 3/ltsc i o ' - <- (S> V*. 3 orv w/Met4 TVlKV-H^D. "i/4/oi " (jg> l '.roo OolrBacLu>j)c4 " L-l M-f>OH TlOA'MOa-' H/h/ c?! cmC GLP Study Number: EOO-1311 d ) i > lu.4ic- / D 3A " u e l u,MeoH TMfWlS^ 3 / its o e m e . stored ur-.c/ir reCriaeraho* s\ (L '3 j u .n h t c `lu -d r d o*. a^a.yeef (g)cetc. V-2c/_0 , 5 of 12 3 M Environmental Laboratory Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS 3M Environmental Laboratory Page 178 of 703 BACK TO MAIN Sample ID Type of Sample Type of Soil Cone., Test Substance, mg/L Time Point Soli:Solution Ratio Sample Descriptor Weight of Soil, grams (2.50 +/0.05) mL of 0.01 M CaCI2 Soin Equilibration (at least 12 hours) TestSubst Addition (Record voi) Equilibration (48 hours) Weigh container (Record grams) 1 centrifuge Document pH Spike Amount | Page 179 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS 1 EOO-13 1 1 -5 1 0 9 E00-1311-5110 EOO-1311-5111 EOO-1311-5111 E00-1311-5112 EQO-13 1 1 -5 1 1 3 EOO-13 1 1 -5 1 1 4 E00-1311-5114 EOO-13 1 1 -5 1 1 5 EQQ-1311-5116 EOO-13 1 1 -5 1 1 7 E00-1311-5117 EOO-13 1 1 -5 1 1 8 EOO-13 1 1 -5 1 1 9 EOO-13 1 1 -5 1 2 0 E00-1311-5120 EDO-1311-5121 EOO-13 1 1 -5 1 2 2 EOO-13 1 1 -5 1 2 3 E00-1311-5123 EOO-13 1 1 -5 1 2 4 EOO-13 1 1 -5 1 2 5 EOO-13 1 1 -5 1 2 6 EOO-1311-5126 W S? 23 -- Sample -- Sample ~ Sample MS Sample -- Sample -- Sample - - Sample MS Sample -- Sample -- Sample -- Sample MS Sample -- Sample -- Sample -- Sample MS Sample -- Sample _ Sample -- Sample MS Sample -- Sample _ Sample -- Sample :m s iSample 4 Soil 3 Soil 3 Soil 3 S oils Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 S o ils Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 Soil 3 5 67 0 0 1:5 0 0 1:5 0 0 1:5 0 0 1:5 0.5 0 1:5 0.5 0 1:5 0.5 0 1:5 0.5 : m r ; =1:5/: 2.0 0 1:5 2.0 0 1:5 2.0 0 1:5 2.0 0 1:5 5.0 0 1:5 5.0 0 1:5 5.0 0 1:5 5.0 iSrO =1:5:i 10 0 1:5 10 0 1:5 10 0 1:5 10 0 1:5 50 0 1:5 50 0 1:5 50 0 |:':50.;; tHQ- 1:5 1:5 89 10 S1 1 2 .5 / S1 5 . S t o i 4 12.5 S1 e l. S a 3 Q a 12.5 S1 12.5 S1 <3. H H 5 8 q 12.5 S1 3 . 12.5 S1 3 . S 8 M 12.5 S1 12.5 SI r a s " o 125 S1 d Q 12.5 S1 3 . H i s a - 3 12.5 S1 12.5 S1 C 12.4 S1 3 . HH1 l 12.4 X S1 . `H K 3 12.4 S1 12.4 X S1 3. S cflg a 12.25 S1 SOlol g 12.25 S1 i . st ; S 12.25 1 12,25 0 S1 a - w i v g 11.25 S1 S1 3 .5 0 1 0 11.25 11.25 <3 S1 11.2 o(0 E sO. E r <H0 ) C(U E o O h 12 13 1 4 16 16 17 18 7 W R t& S t V S i-- iiiii' N " is W H E S i ffl (o .O ? i is s # s 12.5ut i W shS t 12.5uL 12.5uL 12.5uL ' -- C>.c> -- _Ti o 50uL 50uL 50uL S 50uL Jj X 125uL S3fcBBS S S S 125uL K sj 125uL -- > A \u X 5 -> 0 r\ lo.fasS 125uL 250uL 0 OfitbfiaSiS- ^S=trir*'i 250uL 4 S ^SB M i^^SS IS 250uL 0 250uL -- 1.25m l m m s m wsbs^ O -- 9l 3 O ,l r4 AX, Xxs- i/ A 2.0 .*L / il = xJ O /: ; T nm n 0 2nuE T- KSi =.. 1.25mL 1.25mL 1.25m l. -S-"------- -- (p __ N.> -- T 1 3 sk X=':=/ /='/= = /./=='. Col 9 Balance ID 1M___________________ C o l l i Inc ID T - f o k ___________ Time/Date/lnitials It: to iv * . I l3 t / O l C t w Equil Start T / D 3 I 3 - I O I C w f C ol 10 0.01 M CaCI2 soin ID # 00=01- .ZH -/ 3 - ' Equil Stop T/D/H -CP/V A / / 4 IQt Ur~- c Time/Date/lnitials.? / / O p n A. / / J - /0 / m iC - O. ^pH of Test Soin. jr ' Col12 TestS ubst. I D t n i m i - n g - Q T Test Substance cone.:__ 500ug/m l__________ T im e /D a te /ln itia te P , /fct- l t (U rti. Time/Date/lnitials,4 .oOpn* ! \<4 /O l f j v i ( \ 3~ L-OOc-, TC& -OOOleS " ^ t I 3 l / O t CtvT i-- (^DileV^ecC I'i OA fl^LLckcoh-eaI" i^M(OH TMfl- <-155 3 -/ It* jo I CM C- () b'lulti I-t>an rl w/HfW T N fl- `-/ISS 9 / Up ( o { ) i > , l u k i . l'.m u./Mi 0 TNA- 4 7 5 5 3/lL ilo I m.c_ Cot 13 Inc ID S3fV----- ---- ---------------- - Col 16 T/D/l3 !C O p tn r k l N I l CW i - Equil Start T/D/l nyt 4-- -------- Col 17 VOIlA '. a i f ^ S~ II d IQ l f i m. C_ Equil Stop T/D/l Kift / ------------ - Col 18 Spike soln ID norrt.4 - I<4~7 Col 14 Balance ID IVWA - -- -------- Test Substanceconc.: 1 Time/Date/lnitials M lft ---- 1--~7 Time/Date/lnitialslo tS to t^ S /S o lot Cme_ (Jnternal Standard ID t m o o i - 0 3 --01 Col 15 T/D/l ^ 'O O p / n ^ - /) M / D l C^ V x C Internal STD conc.:/?Opn lo t. S W - P | d u W - Time/Date/lnitials li1 /O l on. r G tP Study Number: E00-1311 %-hred u ^ c U s ^ ^ usi CJ*d f s/-- 7 of 12 3M Environmental Laboratory BACK TO MAIN Sample ID Type o f Sample Type o f Soil Cone., Test Substance, mg/L Time Point S o ll:S o lu tio n Ratio Sample D e s c rip to r W eight o f Soil, gram s (2.50 +/0.05) m L o f 0.01 M CaCI2 Soin Equilibration (at least 12 hours) Test Subst Addition (Record E quilibration (48 hours) Weigh container (Record grams) ! Document pH *" !}? m L o f Spike A m ount Page 180 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS 1 E00-1311-5127 EOO-1311-5128 E00-1311-5129 EOO-1311-5129 EOO-1311-5130 E00-1311-5131 EOO-13 1 1 -5 1 3 2 E00-1311-5132 E00-1311-5133 EQO-1311-5134 E00-1311-5135 EOO-1311-5135 E00-1311-5136 E00-1311-5137 E00-1311-5138 E00-1311-5138 EOO-1311-5139 E00-1311-5140 E00-1311-5141 EOO-1311-5141 E00-1311-5142 E00-1311-5143 E00-1311-5144 EOO-1311-5144 w S 23 4 -- Sample Soil 3 Sample Soil 3 Sample Soil 3 MS Sample; Soil 3 -- Sample Soil 3 -- Sample Soil 3 -- Sample Soil 3 MS Sample S o il3 -- Sample Soil 3 Sample Soil 3 _ Sample Soil 3 MS Sample Soil 3 -- Sample Soil 3 ~ Sample Soil 3 -- Sample Soil 3 MS Sample Soil 3 _ Sample Soil 3 _ Sample Soil 3 -- Sample Soil 3 MS Sample Soil 3 _ Sample Soil 3 -- Sample Soil 3 -- Sample Soil 3 MS Sample: Soil 3 5 67 0 48 1:5 0 48 1:5 0 48 1:5 0 48 1:5 0.5 48 1:5 0.5 48 1:5 0.5 48 1:5 0.5 48 1:5 2.0 48 1:5 2.0 48 1:5 2.0 48 1:5 2.0 1:5 5.0 48 1:5 5.0 48 1:5 5.0 48 1:5 5.0 -4 8 '-;: 10 48 1:5 10 48 1:5 10 48 1:5 10 48 1:5 50 48 1:5 50 48 1:5 50 48 1 5 50 48 1:5 89 10 S1 <3.S D I? 8 , 9 12.5S1 3 . 5 0 S & 4 12.5 S1 12.5 S1 12.5 S1 12.5 S1 - S D i t f l l 12.5 S1 S . ^ u s - i 12.5 S1 12.5 * S1 S T s s ^ T i S1 12.5 q 12.5 0 V S1 S1 .S i'll l 12.5 12.5 li S1 e. 12.4 X S1 3 . 5 1 0 1 r. 1 2 4 S1 3 M W C % 12.4 s S1 12.4 l i S1 a .5 C M t> a 12.25 S1 a . s t z K i 12.25 S1 i/.< 4 q s v 2 12.25 S1 12.25 S1 3 . 4 4 8 3 ^ 11.25 S1 11.25 S1 d?. S o M i j 11.25 S1 11.23 ? // 4 a3 o> 5caut 11 12 13 14 15 16 \ ------ 3 2 . 1 3 5 e1 9 ----- 7 s iB is i a a .o ii4 < z q a a . o m a c <q V-'tf ; 'k U .o -- 12.5u J i. 'K t 1 9 ^ 1 2 . 5 u !h 12.5uL 12.5uL 50uL IT P tr S lS V e a K 31. <44 08 g a a . i a e -1 o 50uL *^v 3 / 4 3 a J 50uL 50uL W .I3 0 I 125uL f ij 125uL 125uL a a .rW o A > ja .o ^ a -a ti J .0 4 0 1 ^ 125uL 6 250uL 250uL J 250uL 250uL 1.25ml u q a a .o iis ' i 3 3 . 0 aloS Le ) a a .n o o q 1.25ml 1.25ml B - L--1.25mt ; i-- la .is b z a 2 . iO M <-l a a ISSSSJftt Ic .O X-- V* N n h^ r L .o > rSCi % (o O -- ie s is a ^, Ic .O L, O 1 M J \ ------ Q iai E E o o 18 V?TM`f><' 7 C-------------- 7x -------------------- r ) O . L - '-s. `* M \* * s m p b *L ^ X ^ ) i 5 K5 I c 3 3 to *0 - \J S t itS S R -------- 7 < ( i) N. O* ... A 'C /;:::'1".;; 10) 4 iS & ^ ^ // / B ;:-S- " N ^ 4 lr iS r 0 N ?f~r^Si? 3? A - z - '/ '"1:. C o l 9 B a lance ID I H _________________ C o l 11 Inc ID T T W < 2 - ________________ Time/Date/lnitials I I 1. 9 W I l i t I D I C r t V L Equil Start T/D/LD.' / Qo*. 2 - l / J - l a l r n * C C o l 10 0 01 M CaCI2 soin ID Ut o o g Q i --.3 4 --/ J -- Equil Stop T/D/IT . o O e ^ A / / o l Time/Date/lnitials-? / D f , J1 Usi- l o i C k n C . pH of Test Soin. C ol 12 TestSubst. I D # o lQ O I - 0 3 - 0 4 Test Substance cone.:__500ug/m l__________ Time/Date/lnitialP - / /P-/ 0 / Cl*C - T im e /D a te /ln it ia ls //< / P l r m c S>od **"<3=Sa.Aci>-^ l~-occt*q ('( on " M c t u A t u i * "TCR.- O O olcS- 00\ l / g l / o t O v \-C / liai Oi (^), lu-hii l:/ <5n"<Sp U.lh t l+ - r m - ^ s s - s / / p / oz OMn <_ b/ Co! 13 Inc I D ________________ Col 16 T/D/l J O '.^S h n A / |5~ / o l f f Equil Start T/D/lS .'<4S a^ q i l i l O t C x rs f Col 17 T/D/l i p '. ^ g U , a / |S~ / P I C m L Equil Stop T /D /l ^ ^ . . 3 //T</)l c l * .C - C o l 16 Spike soln ID # -H? C ol 14 Balance ID j Test Substance cone.: i Dppyvx Time/Date/lnitials^ * 58^v<% U S ih l O M.C. Time/Date/lnitials ( in t e r n a l S tanda rd ID / Cm c, ow C ol 15 T/D/l 3 1 f iQ & S \ A !L S L I 01 c m C Internal STD conc.: 3 0 p p ^ , L ^dJLed Time/Date/lnitials ijx / o ju !o / d O l c r vUL- (t} laijtf- rCm-ou^^- 4%Jae% yr* u u n U i cU$orlc> S4e.f. I c*^c_ (o ^ iy u ^ h i- i'ib 0* " d u ckooktaI 1^/H-ett T M f t ' 1-f7 5 'S ' f i/iu h i U rnL' GLP Study Number. E00-1311 5 rcA- u*ichr Rgfb'cfe.raji'^ L\ /2-oZ- i^ih'I cLtL^kd a ^ J / Sr- 8 of 12 (rjc^ahc 3M Environmental Laboratory 1*1 lG)-"0 Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS coO 3M Environmental Laboratory Page 181 of 703 BACK TO MAIN Sample ID Type of Sample Type of Soil Conc., Test Substance, mg/L Time Point SolhSoIution Ratio Sample Descriptor Weight of Soil, grams (2.50 +/0.05) mL of 0.01 M CaCI2 Soin Equilibration (at least 12 hours) Test Subst Addition (Record voi) Equilibration (48 hours) Weigh container (Record grams) Document pH mL of Sample Spike Amount Page 182 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS OT E 1 23 4 5 6 78 9 10 E00-1311-5163 -- Sample Sed 1 EOO-1311-5164 _ Sample S e d i 0 0 48 1:5 S1 a . H i o s L * 12.5r 48 1:5 S1 12.5 E00-1311-5165 ~ Sample Sed 1 0 48 1:5 S1 12.5 EOO-1311-5165 MS Sample S e d i : ;Q EOO-1311-5166 -- Sample S e d i 0.5 E00-1311-5167 -- Sample Sed 1 0.5 EOO-1311-5168 -- Sample S e d i 0.5 48 N135S S1 J 12.5 a.48 1:5 S1 y p s - c. 12.5 48 1:5 S1 j s n J 12.5 48 1:5 S1 12.5 E00-1311-5168 MS Sample Sed 1 0.5 :H48:i=; 1:5 S1 12.5 EOO-1311-5169 -- Sample Sed 1 2.0 48 1:5 b. S7<K<S 12.5 's E00-1311-5170 EOO-1311-5171 EOO-1311-5171 -- Sample Sed 1 2.0 Sample S e d i 2.0 MS Sample S d i 2.0 7 48 48 48 1:5 S1 3 . 3 1 T r a 1:5 S1 a s M i z i 1:5: S1 j 12.5 12.5 \ 12.5 M EOO-1311-5172 -- Sample S e d i 5.0 EOO-1311-5173 -- Sample Sed 1 5.0 EOO-1311-5174 -- Sample Sed 1 5.0 48 1:5 S1 3 q 12.4 S 48 1:5 _S1_< " . o i i j 12.4 n i 48 1:5 S1 ' m o , J 12.4 EOO-1311-5174 MS Sample S e d i 5.0 EOO-1311-5175 Sample Sed 1 10 EOO-1311-5176 -- Sample S e d i 10 EOO-1311-5177 -- Sample S e d i 10 EOO-1311-5177 MS Sample S e d i 10 48 : 1 : 5 : S I V _______ 3 12.4 48 1:5 S1 O* n n a * 12.25 J 48 1:5 S1 3 7 i ? 3 < 12.25 48 1:5 S1 <3- S o O d 12.25 48 1:5 S1 J 12.25 ay E0-1311-5178 -- Sample Sed 1 50 48 1:5 S1 11.25 EOO-1311-5179 -- Sample Sed 1 50 EOO-1311-5180 -- Sample Sed 1 50 48 1:5 S1 . ' i k o 11.25 48 1:5 S1 11.25 : EOO-1311-5180 MS Sample Sed 1 50 48 1:5 S1 : 11.25 j -- -\ 01 01 2 ' 5caj h . 12 13 14 15 y is a s is 3 l.n S 5 t q -- rsssn a i . s - i i . . a i. `lU ifi \ 12.5ulf y 12.5uL 12.5uL 12.5uL 50uL 50uL 50uL N ? 50uL U 125uL r 125uL S 125uL 00 J 7;-0 125uL s i 250uL ? N C 250uL 250uL r 250uL 1.25mL sS) 1.25mL 1.25mL N M L 1.25mb f ___N a u n u a ^>1.89 5 0 6 a a . c d i e o c, a o .c s q q 's 5a.C cO (c q a s .o a u i a ? .o 5 W T q s <aa. N 3 L d ' a s . o u i S ^ as. en y a S l.R R -lt, d a i. ^ > 7 a a a -a iU iR o f3 3 . OT b.^i A (j ( ' -- 16 17 --/ \ 7 .0 Ic&.ifeii. 18 Oi d fu U .b ft C -S l 2 ^ eOI E E o o J Id 7 .0 iS B fe 1 .0 -- a ttf/ijig a b '" Q O v-L. X) s Sv0--; . _ > ----------------- J ---- --- ---------i 1 -------------- 0 " " .... ^ ------------------ il O uL -------- 7 r - S "TT S QS ',yfa 7. O 3 .s z1 731 ^ ---------- 1 .0 f Col 9 Balance ID i U f i Time/Dateflnitials I1 C o l l i Inc ID 01 r jsv\l. Equil Start T/D/I j3 - /Q & m 112-1 b I C-H rt-C C ol 10 0.01 M CaCI2 soin ID t n o j o i - ? / --/ 3 - Equil Stop T/D/l ~7' OCxu^ 5 H \ l o i r j v i r Time/Date/lnitials J .' ! O hm A - / / 7 / Q j_ C iv r C pH o fT e s tS o ln .^ " 7 " Col 12 Test Subst. ID # O I P I -- p a -- o~7 C o l 13 Inc ID T -- 13 - Equil Start T/D/H c W . W d t - l P l o j O w C Equil Stop TIDnk '.L jC y g ^ J i / 15~H CTY\C-- C ol 14 B a lance ID _ 3 i i l ___________ Time/Date/lnitials A //5 7 n i r C o l 16 T/D/l IT C Q o . A / 15~ l o t C r v v C Col 17 T/D/l I f / I 57 01 C a n f . C o l 18 Spike spin ID # o c o o 3 - | H 7 ______ Test Substance cone.: I u p p rv ^ Tim e/Date/lnilials I Q '. ^ O ^ /b o /o > cuu- c ` Tim e /D a te /ln itia ls < T est Substance cone.:__ 500ug/m l__________ y / / - / 0 1 C. * C Time/Date/lnitialsjA W S a n M P t ! C l r w . t __ (^ In te rn a l S ta n d a rd ID # g o o l - r > 3 - - o i C ol 15 T/D/l 7 H S L . A I I S 7 m o w /vO Internal STD conc.: 3 Q jp \ . i 7 . T .-C /V d e L t o S >f>c^ " 2-ioti^ S>ecL m rt4 T 0 2 - OOdbS - 70 I/c?<r / ?}tu. I'.I On. "S-tcACooAra.'f1 TNI- d 1 5 S 2 /ilW o i C M C L ) i l u f f e ! I 1. I a n " s p < c n . t i j " jK i'^ lSS 3/ia/ai cmc Tim e /D a te /ln itia ls / 3 o /cal LICOH? Ia.ue.1- r *^0ed a.ncL s to r e d . - fUx>~~~Ti /y b U ja f il c / e r o c is &fc/> O tc > 4-3M -ot ^^luk^L l ' W o n " u c fc c J^ c c i " c in to li- TNJft-^S'' GLP Study Number: E00-1311 Ohu[\ em e- (*>) ^ &brrcH (JUXcU-s^c?CnGMrcoji**-, \ - ~rL /C^ t ^ ^ c l n e l / >S ' <x*iayz*JL @ c*,c i/,^ -0 1 10 of 12 3M Environmental Laboratory Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS 3M Environmental Laboratory Page 183 of 703 BACK TO MAIN Sample ID Type of Sample Type of Soi! Conc., Test Substance, mg/L Time Point Soil:Solution Ratio Sample Descriptor Weight of Soil, grams (2.50 +/0.05) mL of 0.01 M Equilibration (at feast 12 hours) Test Subst Addition (Record voi) Equilibration (48 hours) Weigh container (Record grams) Document pH * 7 mL of I Spike Amount Page 184 of 703 Adsorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: PFOS i ^9 > 1 a sa> E 1(fi y 1 E(0 W E o o 1 E0O-13 1 1 -5 1 9 9 23 4 _ Sample S ig i 5 0 6 78 48 1 5 S1 9 10 11 12 1? 14 15 16 17 M S'A s 1085.^?; V a i . 1 1 5 ^ et / s w m m 18 E00-1311-5200 _ Sample S ig i 0 48 1 5 S1 A . * 1 12.5 ia a s s s s au s ila ^ ______ E00-1311-5201 _ Sample S ig i 0 48 1 5 S1 a . 5 s y 12.5 T E00-1311-5201 EOO-1311-5202 E00-1311-5203 MS Sample; S ig i __ Sample S i g i _ Sample S ig i 0 0.5 0.5 48 41 5. 48 1 5 48 1 5 S1 S1 3 . ? r 3 i s ; S1 12.5 12.5 12.5 12.5uC 12.5ul_ a i.itio i * /.6 J a i a J o .1H /rw 'T :::' :^.T.:.' J0 T I ___________ \ EOO-1311-5204 EOO-1311-5204 EOO-1311-5205 EOO-1311 - 5 2 0 6 EOO-1311-5207 EOO-1311 . 5 2 0 7 EOO-1311-5208 EOO-1311-5209 EOO-1311-5210 _ Sample S ig i MS Sample S ig i _ Sample S ig i _ Sample S ig i _ Sample S ig i MS Sample S ig i __ Sample S i g i _ Sample S ig i _ Sample S ig i 0.5 48 1 5 0.5 48 r: T i 5 2.0 48 1 5 2.0 48 1 5 2.0 48 1 5 2.0 : 48 1 5 5.0 48 1 5 5.0 48 1 5 5.0 48 1 5 S1 < = ? s l J S I ---------- Q S1 A . S A I I l S1 a . s / a W S1 3 . f f 'H t lf A S1 St 3 .5 0 7 0 9 S1 a . S H i i k S1 . ^ L l - L 12.5 12.5 12.5 12.5 12.5 12.5 12.4 12.4 12.4 > \ T X 12.5uL 12.5UL 50uL 50uL 50uL \ 50uL ;>s -nSJ 125uL C* 125uL T 125uL 's " j 1 .1 1 0 2 a 1. ^ 1 31 .ftS S W Ci 4 ^ ,, S o J ^ S Q T . -J i 3 0 . 3 , 1 4 5 i. lo o a 4 (j2 .5 " V) *xc\ _Ck I .7 < o .5 a O j frz T -4.. 4 ______ U i___________ fL . Tq-is i _______ 1-------------> IFiJfaTpj.i^MUfe 0 VJ . - 4 - m m tm "x. ___________ , EOO-1311-5210 EOO-1311-5211 EOO-1311 - 5 2 1 2 EOO-1311-5213 MS Sample S ig i _ Sample S ig i _ Sample Slg 1 _ Sample S ig i 5.0 10 10 10 EOO-1311-5213 MS Sample Slg 1 : : io 48 !i1 5 S1 J 12.4 48 1 5 S1 12.25 48 1 5 S1 . M 1 S 12.25 v I 48 1 5 S1 H l . S i n 12.25 r* 48 1 5 s v 12.25 125uL 250uL 250uL I 250uL 250uL $ 'Cs i . W o S 3 0 .5 2 4 < e < 3 0 .3 1 7 0 0 d d to . S ' S3ftS5^ISi rt u -------a - Q * L .' s I.' EOO-1311-5213 _ Sample Slg 1 50 48 1 5 S1 A S 3 7 0 0 11.25 125m l S o -ih ie n ^ ____ EOO-1311-5214 _ Sample S ig i 50 48 1 5 S1 11.25 1 .25mL a i.^ l i -J EOO-1311-5215 -- Sample S i g i 50 48 1 5 S1 0 . 11.25 125m l to -sssyf ^ to S~ 4 EOO-1311-5215 MS Sample s i g i ; !!:50T' m:48/t 1 5 S1 11.2/ -- ^ i -- 1.25mb ___ i / -- b-- >l -- Q *L- Ti Col 9 Balance IP C ol 11 Ine IP Time/Pate/lnitials I 1 5 ' / 13-11O lC tm f C ol 10 0.01 M CaCI2 soin IP c o n o / - 3 4 ~ 1 3 ? //3Equi! Start T/D/fc ___ -J l r Equil Stop T/D/l T 't o O r x J - o cj^Zi C. r Col 13 Inc ID Equil Start T/D/l Equil Stop T/D/l! C o l 16 T/P/l i l ' I S T - T ) / i S / r s f to - iC , _ c coi 17 von h . i^ W MS //7 r j r \ r C o l 18 Spike soin ID # o n n o 3 ^ T _______ Time/Date/lnitialsJ ' 3 ^ - . 3 H3- IO / CJn rC . slAOpH of Test S o ln . ^ r . r ''' Col 12 TestSubst.lD#r> lfc > 0 r6 ^ ~ O 7 Test Substance conc.:__ 5 0 0 u g /m l_________ C ol 14 Balance ID mTime/Date/Initials s l / S ~ l i O n C - Test Substance conc.: Time/Pate/lnitials / i ! LOP I n I c / v i r ( in t e r n a l Standard IP t o u s o i ^ o a - Q i no~n~ Time/Date/lnitiais^ - <?O **3 / / 3 - i 0 / C H C Time/Date/lnitials - <9- lf ? ) I Q C Col 15 T/P/l l ' . 5 S r ~ 3 j iS 'in t CJY l c . Internal ST P conc.:<3G>p^)ro , I 3 . d S l c ^ i - L^o<vi e s h c SIn-i.d c ^ TC-- Oti'S"id- 5 a o c f') Q> Dri^-4-cctL i'i O''"Cuct,uWo-/-'' cj bl-?Oft T N A - H T J - S' p/iu>/o | Time/Pate/lnitials ii'.w r a i-- S? & c l a \ Cj v .c _ (je J /*< je r- re n-v^i i-n e t sforeT ot oovt'te'Wf u/ifcnl deSorft, *?p ()CjviC 4-aK-Ot. OQO ' o o 9 - ^ (, 5 a <o - 5 5 U 5 ) ( O'1"Sp-^ " / ^ / e m e s TH-eflW T Wft-4TS~5" 3ll>ll a n C GLP Study Number: E00-1311 (3) .'M * " u//KeOH TMft - 4 ^ 3 / / o joi cftna -v2- SforrcC c-ruT./ r ( / r i C ,e .r a .i - i o I cLc!u-rjeef CxoJ ( maJc^z^zoL-( ^ ) Y'cW-' 0 1 onC_ 12 of 12 3M Environmental Laboratory BACK TO MAIN nternal standard Addition, uL Page 185 of 703 Desorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: 0 1 m n! 2 c. goa :onc., Test Substance, ng/L s;ez. a. 1 2. * c c 11 J e% 5 " ' s Sg 3 ST* a00 5 *0 Ol m O iy o li 1I ! cSI f II C5 3 <c J . S >a 5 (aiE e E I. *1 5 Dw i O0t 'cf0t 1 c So- TTi53__ c Un 3! ! 1 1 >a8 4 ftftft c ... u Z5 1 z1 E a i0 oE To3f o c ? a ca Ea <'XSaE. M C I Eo 2 12 1 21 221 3 4 5 6 78 9 10 11 13 14 15 16 17 18 19 2D 23 A % - r " TA >1 (Si _E00-1311-5019 7 C o n tro l NA 0 48 NA W . 5 5 3 ct g / S2 A ? a a l S3 A j\ E /X \ J< -- V E00-1311-5020 - C o n tr o l NA 0 48 NA E00-1311-5021 _ C o n tr o l NA 0 48 NA F00-1311-502' MS C o n t r o ! r.'A 0 "1 " 43 NA_ . " ..iO-1311-o2o C o n t r o l MA 0.5 48 MA H .le H -lS .------------- -- S2 S2 S2 -- -- |<?.<. ) 5 7 A 0 S2 ... S3 S3 S3 S3 - --- %mm - - - - - - -- E00-1311-5024 E00-1311-5024 E00-1311-5025 E00-1311-5026 E00-1311-5027 EOO-1311-5027 Lu 0-1311 -f:2o EOO-1311-5029 E00-1311-5030 EPO-1311-5030 E00-1311-5031 C o n tro l MS C o n tr o ! _ C o ntro! _ C ontrol __ C o n t r o l MS C o n t r o l C e n tro ! _ C o n tro l C o n tro ! MS C o n t r o l C o n tro l L'E!i ' E1.1_!l i. ECJ-1311-5033 F.00-1311-5034 EO-1311-5035 MS C o C r o l C o n tro l C o n tro l NA 0 5 NA 0.5 NA 2.0 NA 2.0 NA 2.0 NA 2 0 NA 5 0 NA 5.0 NA 5.0 NA A .O x NA 10 NA _ 10 NA 1Q MA .'1 :: NA 50 NA 50 48 48 48 48 48 48 4o 48 43 48 48 A 48 48 48 NA NA NA NA NA NA NA Ci NA NA < NA NA E NA NA 2 NA 1 ^ .5 3 4 3 i^ .u a c S c r l et . 5 S U & i ___ J s TT c M. 5551 o, X -- ri *3 iis i- li? 1 Aj n s v a ir. RI S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S2 S3 > S3 ; S3 S3 n -- : S3 p O .L S3 - A f) S3 < \ : S3 S3 2 g r S3 j S3 o k S3 S3 U 3 q ^ S3 S3 S3 v r- O _Sv C ^I 45ii nX; A \J 0 SL Cr n rj N x! tl ni A <6 v VJ S s "0; tt X ri X w R > `L \ UJ x! uiX k j t\ iS E si _S1 i rXi i. C -4 1 J" A l T\ O -x n _r i E00-1311-5036 . . . C o n tr o l NA 50 48 NA ( c( . 5 LtS 9 u S2 W\ S3 " ___} E00-1311-5036 MS C o n tro l NA 50 48 NA s r s/ S2 ' A O i! S3 Nf A Col 8 T/D/l N f f i C T O C A j q 0 j Col 14 Internal Standard ID # CUCPI - 0 Q \ Col 19 Centrifuge & Transfer L jJ j - >s j_ \ >7 Col 23 Centrifuge & Transfer T/D/l M i ~T vV Col 9 0.01 M CaCI2 soln ID ttO IO O i Internal Std. Cone. ofc>ppr-> T/D/l Col 24 Aliquot Study Sample Balance ID _____________________ T/D/l t o ' t / &&/mryvsc Col 20 MeOH ID # T N S f t T/D/l t 'M Q A m o l // q I Q ( W \ ( Col 15 Spike soln ID # o o o o ^ T/D/l 1 ^ ', $ - ( 3 ^ Col 10 Incubator ID ___________ Spike Sol. Cone. Ip p p ^ ftp o S . Col 21 Centrifuge & Transfer Equil Start 1 g I o l ChnC T/D/l j T/D/l Nft- -- -- ~7 1T53T^\ c.t\t LJl tV i. c T/D/l I '. p o p 9- i S O / a t c ** - C C o l25 Spike soln ID U n m o 'b Spike Sol. Conc.lO p p e n I X O ^ Tmnofrtn f f i i OI M<-- EquilStop T/D/l It:OQfl^ J / I t o c r v CCol 17 T/D/l 13 oO p n . > l3 S - l to! C w C C o l22 MeOH ID # T N f V ~ H '- J . S I C o l 26 Internai Standard ID #f n o r n -rsO .-- Q 1 C o in Centrifuge T/D/i M/ f ) / / (T)-Lfssej-r-** SSL s t i p i t i -iH io rt r jp /i-U TS's / i C ^ - C GLP Study Number: E c O ^ 3 t I 'O'c a la r lo I C o lia MeOH ID ffT N f t -M M S 1________ -- T/p/n a 'R O p ^ a. /aa-/>i rtv-if VDIU S S O p ^ . | 5 - i 3 - S ~ l a \ l k C Internai Std. Conc c> p p < rr\ TTT-QF-O1^ TlD/u : o o ^ i i n cro<? / P S / n i t- lKI^JL I. ' - SucVa^kriccf ' bii'dti- r.l Heoff W H -^ lS S o n "8uckjJ-e i t ` -j a/ Clnc t*n+,l Jubs 54zirccf e^b-at-Ho*- .p c* rcin frvv.p jCJnc H-H-ol sH>rP<J U-Acbr rPfrcjerti4lO*~- (il tirais u-n ( cJi rjindjr *_s\clLi cc( H) Ont H-dtl-O I 1 of 6 3/W Environmental Laboratory BACK t o m a in k / . n L o Study Page 186 of 703 Desorption Isotherms, Multiple Concentrations ETS-8-160 Test S u b s ta n c e ^ V o ^ -f 3i o1 - I t .t<) UC; 4it d* i ? '* 3 i,,:s- a1 tf u A** s a 1 1 E00-1311-5055 EOO-1311-5056 EOO-1311-5057 En0-1_?11-6057 EOO-1311-5059 E00-1311-5060 E00-1311-5060 E00-1311-5061 E 0 0 -1 3 1 1-5062 E00-1311-5063 FOO-1311-506? U 0-1311-5! 0-4 E00-1311-5065 EOO-1311-5060 FntM 311.5n<5 E00-1311-5067 EOO-1311-5069 EOO-1311-5059 E 0 0 -1 3 1 1-5070 E 0 0 -1 3 1 1-5071 EOO-1311-5072 EOO-1311-5072 I 1 i ? o1 \ i: c1t 1 e r hi 1 I r c i gic 5f ": j e1f rM4- 'tTo fe 1 1 0 7C3 . ? a- 1 3 1 ( f ^ J jL _SVi _"1sOI_ * 3 < ta I 23 4 _ Sample Soil 1 5 0 6 78 9 10 1 12 13 14 15 15 48 1:5 V S i . o U 'i f e / \ Os 4 S2 7. :p S3 __ Sample Soil 1 0 48 1:5 t tlJ - o M - li S2 S3 Samp! Soi! 1 MS c T".nf? ScM 0 48 1:5 0 _ 48 1S " d "` .. s?P- D U 0 .Q ./ ^.o C rS C b , --I S2 S2 -- S3 Sample Soil 1 0 5 48 1:5 p !3 .l l7 S2 S3 ... Sample Seif 1 0 5 48 1:5 S2 S3 MS Sample Soil 1 : o m 48 1:5 __ S2 p o ,, ( S3 ... Sample Soi! 1 2.0 48 1.5 -- Sample Soil 1 2.0 48 1:5 .5 3 /7 q 0 - S2 --- 0 S2 S3 l l S3 ... Sample Soil 1 2.0 MS_ ^am nie Soil 1 d :c T ; bet'^oie Soi! 1 f 0 48 48 43 1:5 1:5 1.5 3 j.o a -m S a z .is > % n S> 's . 7 82 t 2 i S2 s. B% -Q 2 0 S3 S^ S3 Sample Soil 1 5.0 Sn.pie Soil 1 5 0 48 43 1:5 :K Jb b 3 3 . 5 t . . -M i l c;j C S2 J: S2 1VS C-.n-^ tc Soi! 1 5 0 _ 4 8 _ _ V5_ h in : Sample Soil 1 10 48 1 5 .0 7 T fc S2 y:L^: - S3 S3 s r ^ a , t ,, S3 S3 S ,. ..,, s r * Sou 1 MS Sample Sosl 1 ... Ser. Die SojI 1 10 10 50 ?5. /5 & ;< - -- 48 1 5 Q l.o d S -z i 48 1:5 46 1.5 _ y -/ W o , s ; _sr- S2 J S3 S2 i l " 2 i t o j _ ? 3 S2 . 5 S3 Sample Soil 1 50 46 1.5 w -b c n Q S2 S3 Sample Soil 1 50 48 1:5 s s .s m ^ to , S2 -'b.iS' S3 MS Sample Soil 1 48 1:5 J5i f _ s . S2 ' ' j c2 9 i S3 S -1j c r-3oi._ 17 i* S. ~7 v l* 3 2- "2 `Z 5 1S 19 fr e I e er f* l <# I ! e< 1 =. tJD c c i a II 20 21 22 23 "- iMs ;l & (T w . / V K Jr y F _' f po 0 1 - P 7 f3 i -- - - -- ~ , -" 0 _r di .t Ti h Ss T pi d) n> r< : r< ! - " ri o b -4 1 ,j F ~X5 <"-si F 4 r i r .1 - J b. r i ..i. ' . bv Wi-; ' -- 'v> s, s i s> X rvi 4 V0 ,r n JcpL -- i - --- - -- --- V ! -Ai -A 2__ ' 3~-- i - ... ................................... ... - c-- r ' d m Ac s f> 1 - A /J # N' C ol 8 T/D/l * 7 '5 0 f t ir t o l f M / 0 / O T iC Col 14 Internal Standard I0 C ol 9 0.01 M CaCI2 soin lO Xn io o / - q S ^ . Internal Std. C o n c ^ o ypA ^ T T fftF -C S Col 19 Centrifuge & Transfer T/0/ lit / l| &->c- T/D/l i g O f)/ J L j J i c L j O l C k k \ C C ol 24 Aliquot Study Sample Balance I T/D/l li Col 20 M eO H ID t) T i N f t ~ ` - / ^ 5 ' l T/D/l P i d - 9 - i O 1 C-W <-- T/D/l ^ ^ 5 rien A f / 9 O / c ^ C - Col 15 Spike soin IO # o n i c i - JU 7 T/D/l j j o I c y * c C o l 25 Spike soln (D ffccxaft 5 ~ft/~7________ Col 10 I n c u b a t o r ID ^ - O - Spike Sol. C o nc.ttf ft |3m . i ^ trO S . . Col 21 Centrifuge & Transfer Spike So!. Cone. I g ^ g t _________ Eauil Start T/D/l n QQwr. A / / q I Q I r A C T/O/U o ' 1 . 9 / w t Equil Stop T/D/l IT0 0 /1 a / loi a n CCol 17 T/D/l p ' O P I 3 A ) OS C W L T/D/l I ' . T i S p ^ Z - ! & ! OS O ^ C J / S&/ o l TM C Col 22 MeOH ID # FN/q-VH~l T/D/i.9: Q pp/v^ 3 / cv c iv .c C o l 26 Internal Standard ID Mm 0 0 1 - 0 0 - 0 1 Col 11 Centrifuge Col 18 MeOH ID# T t S f t - MM:? I T/D/l i ' - M s ' } . P /SV3- / O r <n/i C Internal Std. Conci? T tfftP o S T/D /ljjlS g A ^ v A O ' / O l r t w t, T/D/l $j)l3 o&Zj p/ii/naovc (3) -S 3 S- / 3 3 / o l C * * <. fes d.i^fadL i: i on ` BlcL oJ vd T/D/l L i fa = . !& .1 / d * ci-tufad t.i an 'frli, cLoduilf ' ' ( S S S ^ U s b r l u k TIOO,XS Aditoci, GLP Study N u m b e r.^ Q Q -- f 3 I I MfOH Yfoft--Mi-Sb p l - l o I O^- r) jlj-ta 1CrrvC- 3/iV ol <>'c (S> S ~ ~ P la s it: 1u .4 * A . !, 0 . ^ M. fidkSuA 3f f o l c i c jr tt. A SVi 3 l 3 b | t U ' V ' C _ 2 of 6 3/W Environmental Laboratory BACK TO MAIN Page 187 of 703 Desorption Isotherms, Multiple Concentrations ETS-8-160 Test Substance: ? F o ^ 5 1o a to o Tt w i 5 c 1 23 4 5S E 00- 1311-5091 _ EOO-1311-5092 ~ E 00- 1311-5093 F T - : 31 1-5093 Sample Soil 2 Sample Soil 2 2S a m p le S o il S a m p le S o il 2 0 0 0 48 48 48 E 00- 1311-5095 2 05 46S a m p le S o il EDO -1311-5096 2 0.5 48S a m p le S o il 001311-5096 2 48E - M S S a m p le S o il 'M i ED O -1311-5097 2 2.0 48S a m p le S o il E 00- 1311-5098 2 2.0 48S a m p le S o il ' E O O -1311- 509 2 2.0S a m p le S o il 1 2 2.0r n n - f fie r i M S S a m e le S o il _ 48 4? ! .0". ) 2 50> ._ ii E 00-1311-5101 2 5.0 48S a m p le S o il EDO-1"115102 2 50 4S a m e ie S o il c- 0-'811 5102 5F M S s - n r l S o il p O' E 00-1311-5103 2 10 48S a m p le S o il 10p r .; S p'? s o i l ? . EO P-13115105 2 10 40S a m p le S o l! E 00-5311-5105 M S 2S a m p 'r- S o il 10' 43 E 00- 1311-5105 2 50S a m p le S o il 48 E O O -1311-5107 2 50S a m p le S o il 48 E O O -1311-5108 2 50 48S a m p le S o il 1311-5108 2EOO- M S S a m p le S o il 48 Equilibrate fo r 48h o u rs S Oi ' c i 5- f u 3( ) w \. 3 c >0 1t1e. <* "5 78 3i = ?^ 9 1 5t V sj 1 t> ! OT 5< . c. =a 17 a <Dr 10 11 12 13 14 15 16 17 18 1:5 0V i a . S R t \ a J s I " S2 'K 1:5 _A . 15 i . o S o ^ a S2 S2 75 'cl. > S3 S3 S3 2 4 3S ?q - S " ." j - - 1.5 53 3 , 0 3 - 1 33. u h a 15 3I . A 384 a S2 S2 S3 S3 1:5 -- ------------- S2 S3 1:5 . o M c H ^ 2S - S3 1:5 3 3 . 3 5 U 1 0 S2 O S3 1:5 4 3 2 . i T c - ^S 15 > - L S3 3. S 0 V js .m s r = 1.5 (V * 3& S s- 2 -A S V s7 3S n ' i 22.354^ j. W S2 3S - 1-5 3 3s S 2 o ,y S 5 31 5 2 3V . a g io ia -^ .O g J d A S 23 8..C H ? 3 2S % S3 1:5 15 - 33 47. Q . S M S S2 2- S S3 3- S - N or > O 5V 32 .S L 5 L O 15 QS. 2<93 to cx 1.5 JA.ith 1:5 - (L_ . ) \i; ' S2 S2 S2 S2 t S3 3 S S3 J-- rSVL S 3 >L fi J11t I 'S I 8 1 X E I iO3T J 23 1 5E T V 3Q < t Ta0 T i 5 c 19 20 ~7 21 --> 22 "723 "J7 s Vc V "7 -- -- ' i ? c0 3 0 ..o 'y . O c N \' t n 1b V . 1- Yl n n , f ; ..-X2 r i s. 1ot , V, \j w i * Se 5 0T -V - u -- - - $ _ _f E > __ < rri - - <5 'J-- >( - >/ - A i - L N,( > 1 _ j 1 Col 23 Centrifuge & Transfer ' ------- Col 8 T/D /l7: 7 / / `f lO ( c u r Col 14 Internal Standard ID #raiO) - o g - o i Col 19 Centrifuge & Transfer Col 9 0.01 M CaCI2 spin IO # ftf6 o /-o S - fjT InternalStd. Conc.^ O p p - T U ^ f O ^ T/D/l 1 1 31 / 3 - 5 / a \ CJ/V\ C T/D/l /! 3 q a -`v i A 0 . 0 m Col 24 Aliquot Study Sample 0 ^4- Balance ID 7 / * / _____________________ T/ D/ l i o A / 033 /Q \ U w C Col 20 MeOH ID # ~TKI f t - MM .s '!_______ T/D/l I I W . tW A / 3 5 /OI Q V y ( w VOtW . f o ^ . J l I ET I O I O iC C ol15 Spike spin ID f o e 0 3 - N ~ l T/D/li i ' O t a ^ 0/ / o t C !r r \ L . C ol 25 Spike soln ID tic o o o S - i *71_________ Col 10 Incubator ID Spike Sol. Cone, t o p p ^ 'f r F o 1^ __ Col 21 Centrifuge & Transfer Spike Sol. Cone 'i> rf)ei __________ Equil Start T/D/l l / . o g ^ A H \ ! U O n C T /D /lt e '. i J T A ^ L J A J iJ n l r ia* c T/D/i n . te r ,- v ^ . .2 / A 5 / & i o - v o T/D/l A O O p ^ A i a 2I / S I CW' c EquilStop T/D /IH n a . ^ ,3 /< /0) 6 w <Col 17 T/D/l i n \ n O ^ 1 / J 3 / Q ' C w t Col 22 MeOH ID # T M f t - M 4 . 7 I C o l26 Internal Standard ID # r u n m ~/VT --01 Col 11 Centrifuge Col 18 MeOH ID # T M f t - `-<4 5 1 _________ T/D/l III >,*- ~3 ! A Z ! C>\ r * n C_ Internal Std. Cone.a O p p l-vm T f f f i I" C S jiD n iv .S o A ^ A - 1 A I / n l r i w r t/d /i in- e r f ) / n * A / S ' b i o l C m C | T/D/l r-ff' cT O__ln_o_____^_____l__2__U________ C 0 . M . 3 3 iio o rS / /GLP Study Number: Q G " (3 ). S 3 s a m p le s n 0 ^ ' 3 r ^ H f a + " (T j) - 5 5 b l u 9 ): I on " B i r C t d ^ o f " IvlM eOtt- TN A ''-0 5 'S ' 2t d / o l cj^e- (D @ e* -c /M 0+T T /V fl- / l 5 ` i 3/7%/o\ Or^L, 3, I S AefcW, -S ^ s a -p le s 1 (g>-S5MtSScAxcrJ w^ plA- ^stW^ieefme > 1 -I S P i i W ,' ( t ) S 3 *<> *<5 HS A<LL2ct u 4C ii . | \ I O O , J S A d c W , 3 0 1 CJry\L 3 of 6 H S Atd d a A 3i%> l 6 \ O v C 3M Environmental Laboratory BACK TO MAIN Page 188 of 703 Desorption Isotherm s, M ultiple C oncentrations E T S -8 -1 6 0 Test S ubstance: i 7 1 4 Qi j _ -t Y 3 i 4 Ir?tT. *A^t iU ^ tL TR ^ ^ 9 r\ ~Q > Sj iA i, o 1 M s 5 S S ti w 0 iw 1 i K S e i $ 5* y so t . 'Sno B --f '7 ,, > i K 1 <* E a -i 5 ct ! tt 3 C < e; I c & u. 1 5= aT ... wa 5. IC 0) fr o o -< 1 EQ O -13 1 1 -5 1 2 7 E O O -1311-5128 23 4 __ S a m p le S o il 3 __ S a m p le S o il 3 5 0 0 s 78 9 10 11 12 13 14 15 16 17 18 48 1:5 \ 2 a .im a A. a a S2 A / l "2 S3 / 48 1:5 a a .c m e c ^ S2 f i- S3 E O O -1311 -5 1 2 9 S a m p le S o il 3 0 48 1 5 a a .o M m p c ; S2 S3 S !. 5 c 19 V < V V-0 20 21 r-- \ Ii I ? ? D 5 "d < At u__ f I s JC E1 Ci "D__ . ._ j ..U - 22 23 ' S ! % ) - i t o VL ------- 7 \ ----------------------------------------------- W M A .. JS .) F '0-1 " 11 5 1 2 5 M S S a - '- . r : - S c .- 3 ' '.o. . ..' 4 8 E O O -1311-5131 FOO 1 3 1 1 -5 1 3 2 E 0 0 -1 3 1 1-5132 E 0 0 -1 3 1 1-51 3 3 E O O -1311 -5 1 3 4 E 0 0 -1 3 1 1-5 1 3 5 E O O -1311 5 1 3 5 EO O -13 1 1 -5 1 3 7 ECO " M l 5 58 EO O -1311 -5 1 3 5 E O O -1311-f 13P :V ^ o - ; 1-1: E O O -1311-5141 EO O -13 1 1 -5 1 d l E O O -1311-5 1 4 2 E O O -1 3 1 1-5 145 S a m p le S o il 3 0 5 S a m p ie S o il 3 0 5 M S S a m p le S o il 3 0 5 S a m p le S o il 3 ... S a m p le S o il 3 2 .0 2 .0 S a m p le S o il 3 2.0 M S C a p - r tp . S o H '3 5_2 O ' So;. 3 S a m p le S o il 3 5.0 Sam i S e ll 3 5 0 M S S a m p le S o il 3 ' 5 0 .- S a m p le S o il 3 C ,r T!..i: S c l 3 __ S a m e ie S o il 3 10 10 10 M S S a m p S o il 3 Ho S a m p le S o il 3 50 S a m p i-' S o il 3 50 48 46 48 48 48 48 48 48 48 48 48 es 48 48 48 48 .A .5 . - 15 S ig n 's ^ < ji p n e * . r . - S2 -- f oo oz 15 tn .a M ' A S2 1 :5 ----------------- - ^ - S2 . a 1 5 . o 0 S2 15 15 15 J i A l i o (V i3 m a ___________ 3 0 S2 $ 5 S2 S3 4 15 ja .o in c , \ S2 J 2 .0 '3 i3 C > ^ V " 0 _______ ^ ~ T 1:5 0 s : . 1 1:5 ^ H S O g S2 1_5_ -- - ^ 3 .q i5 5 ~ 9 4 1 .0 1 ______ 2 7 S2 S2 15 - 1c = 3 .1 1 1 ^1 r. S2 S2 P S S3 - Sc _ : . - S ' S 3 \ S3 TS S3 S3 A r S3 - S3 i- :A S3 J S3 J S3 ti S3 S3 -- S3 r20zO - S3 S3 S3 0 >> hsJ O' VJ N p N 'i 'i if k) M \ ,e i 'A r2 A - 0 V o j NS J =T/ Y A .... - ... ------------ :----------------------- N N 0n 0 V v. s? O , c M N 4 ... a -Y ` d J J A 1 Hi 0A 0 lo J -- t t ...................... i A ( (i 2 i _ " -V E O O -1311-5144 E O O -1311-5 1 4 4 S a m p le S o il 3 50 M S S a m p le S o il 3 ' 5 0 ' 48 48 1.5 1 .5 3 S t.\5 a > 4 i / L. / S2 J S2 '5,, . - S 3 ' / Q mL S 3 ' ( 4 V J /s / N J ' 4 V L $ 0 * 1 . > V/ Col 8T/D/l5s-tv>r^. c o l 13 T /D /i ia t U s A l A I / d L S jr o A . / / ? / f j i Clv-C COM4 Internal Standard ID o i Col 19 Centrifuge & Transfer C o l 23 C e n trifu g e & T ra n sfe r T/D/ifr .3 o * r ~ A i 2 ( o i n i ri* , c Col 9 0.01 M CaCI2 soln ID ItO i m i - r A - l C InternalStd. Conc.^ P p p ^ , T H -3 F o S > T/D/l 7 '- S D ~ ^ A - l3 U > / O I C | v v C _ Balance ID *?<*/_____________________ T/D/l to . <7i a, -UllT3- / J O / rai t - t Col 20 MeOH ID # TVjO- C ol 24 Aliquot Study Sample T/D/l 3- ; O i Cv-C T/D/l 10 - 0 0 Hm J n e / n l O n f C o l 15 Spike soln ID # a o n n 3 - / M 7 T/D/l R '. O O a ^ A - I c L (j >I O l Gf r v i C c o l 25 Spike soln ID # c o p o - M U I Col 10 Incubator ID 3 ^ - 1 A-*__________ Spike Sol. Cone. /O o p rv n f ip r iA _______ Col 21 Centrifuge & Transfer Spike Sol. Cone ^Fp5 Equil Start T/D/l IT O iW , A l f l i n l C S n C T/D/l i Q i / y f t M 2- /T - a - to lt^ T/D/l 8 . 7 /3 'V -n cS Q 6 l a l T/D/l. j'. C f r p n o <3 / A 'a / o l r -j EquilStop T/D/l iT n n a . J M i l a i r r m r c o l 17 T/D/l T.QOrrv. A . I 3 U I O l Col 22 MeOH ID # T N f t - M M S ' I C ol 26 Internal Standard ID n i m i -o.T C ol11 Centrifuge Col 18 MeOH ID # T lM ft >Ap..I__________ T/D/l %' A / A U / OV - Internal Std. Conc.d O p p ^ T H ^ b C S . T/D/l /l.'.3 Q f t w 7 / cO < / Q L C m C . T/D/l 4 '. 3 b s w 2 /3 C o / Q t C - W _ T/D/i t o g a cX I Q 1* ! o ) C Jv1c To.be erncTd cuvei uxn d is c u s o1/d />OY3(_ GLP S tudy N um ber: - ~ ) 0 2 > / f ^ 9l--/o I Cv^-c. q-7r" "ulWvjA^orf" (3>53 Ax*Mpl<?s> i1u-Vfti ) I a'' " 0 ^0 ~ L y b ,-fa ^n Cis-S^ S>nplr5 CiUwWd, I-.1000,35 uj/ H oh r N f l- ^ n o S jj^u jo ) C fic te tre i, H i f i d c M 3 l3 o j O l (U n n C 5 3 Sa^vpi<r5 iilo d r c i l.' lO /X 'S ( ^ A e J . HS AckU<* 3 / 3 / OJ C*C 4 of 6 3M Environmental Laboratory BACK TO MAIN Page 189 of 703 D esorption Isotherm s, M ultiple C oncentrations E T S -8 -1 6 0 Test Substance: P F o 5 <& <L % 3 .0 I c *3 7h 1W wAv3/'l -S r V J * fi fa @ i 0 Xt*I <A 3 1C S 1 E 0 0 -1 3 1 1-5163 E D O -1311-5164 23 4 S a m p le S e d 1 S a m p le S ed 1 5 0 0 % Ia ! 0 i IN O) ii ^ *e : - s*5 ? ?r M 5ff f 0 * I HI 5 . i -n < JC t > I a e E 1 a *T c *D <S 6 78 9 10 11 12 13 14 15 16 7 18 T 48 1:5 7 3 i.a 3 U 3 Q 7 S 2 'V T S3 48 1:5 a i.a is ) ^ S2 S3 9 fe I 1J 1 0c V : 19 \ ----- 7(L 21 x- / ] ` t e T c5 T _r P ^ | 711 5 ut 1 s A4 22 23 / \ -7 Ue>~, & ) _______________ ~ ~ 7 1------ s TS^ __ E 0 0 -1 3 ^ "1 0 5 JE00 r- S a m o le S e d 1 0 WE S a m p ie S e d 1 : 0 : ... . n 8 48 EOO- i '1 1 -5 1 6 / E 0 0 -1 :-1 l-S ^G b E 0 0 -1 M 1 -5 1 8 E 0 0 -1 3 1 1-5 1 6 9 E D O -1511-5 1 7 0 EO O -1 3 '1 -5 1 7 1 E p n .1 3 - '.5 17 1 E 00-1 ? 1 1-5173 c r-i E O O -1 3 1 1-5174 F 0 0 -^ 3 1 1-5175 S a m p le S ed 1 0 5 48 S a m p le S e d 1 0.5 M S S a m p le S e d 1 .0 .5 ; 48 S a m p le S ed 1 S a m p le S e d 1 2.0 48 2.0 48 S a m p le S e d 1 M S S a m p i-a S e d 1 2 .0 20 48 48 ,, 7 S a m p le S e d 1 ' S a m p le Sed i :U 50 50 A- 48 n M S S a m p le S e d 1 5 0 ' 48 S a m p le S e d 1 10 48 F5 a i.a s s io Q 'J 1.5 15 - 1 .5 1-5 15 15 3 . lb 5 i -- ici - A _) a .o m n a M .o H S -l n a- a . o S L x d I \ 15 '5 a 1 .5 a a . o ssi e. 1 3 .2 0 5 ^ 0 a a .o .^ x a ________ ) 1 ;5 a a . o s o t a 0 S2 S2 A S2 S2 S2 C S2 S2 S2 S2 - 52 < S2 S2 S2 _ ri) S2 S3 ... S 3 .-- 'e j; < ty rn 4 81 S3 S3 S3' S3 S3 S3 S3 S3 S3 S3 S3 - -- - 0 \ s ') >3 -* X al a 0 lu * ? <1 0 X 0 S q tA -- A X ns X 4. \ n: t 's 'X " r 'l 3 0 ,.!- --\ n? *3 a, S; JT ( sL. X i s -- ^1_. J r^ r - \ dA / --^ eco -r. : i EO O -1 3 1 1 -5 1 7 7 F r 0 V 5 1 51 "7 E 0 0 -13 11-5175 F l !0 - 13 ' 1 5 ^ - 3 E P 0 -1 3 1 1 -^1 8 0 E O O -1311-5 1 8 0 S a m p lv. S e c 1 S a m p le S e d 1 M S S a m n i- S e d 1 S a m p le S ed 1 S s m p 'e S e d 1 S a m o le S ed 1 M S S a m p le S ed 1 10 4 3 10 48 1 0 .18 50 48 50 ^6 50 48 50 : 48 . 5 a i.is iu ^ o 1:5 a i a i a a q _______ y I5 1 5 a - i6 e H _ a 1 5 a l . t S O c J 1-5 a s . l& . Y T a 1:5 N ------------- ^ > S2 S2 S2 S2 S2 S2 1 S2 i S3 S3 - S3 - X ' S 3 S3 S3 / - S3 \y / N/ < 3 0 a* -. ... ( s> S i- 1 d Jr-A / L . i j . / taa. > / ' N Col 23 Centrifuge & Transfer Ta / Co) 8T/D/l (6 o q a m 1 / )A / O i C M ^ Col 14 Internal Standard ID # QLflai - Q Col 19 Centrifuge & Transfer . T/D/l f O ' - J t W J / D (g / Q \ C t ~ < - Col 9 0.01 M CaCI2 soln ID # O iC D i- C V /iT Internal Std. C o n e T t f f r p o S T /D / l 9- & {*-! Oj Col 24 Aliquot Study Sam pie "Balance ID _ J /M _____________________ T/D/l i r > v T Q ^ ^ / r> l r > w CCol 20 MeOH ID # _________ T/D/l / o . 3 0 ^ r?~ / 7 ( p I 0 1 C tM - ( T/D/l /Q ;3 c 3 A m d? , /J f / O iC m C Col 15 Spike soln ID # OQQg& ~ t A 7 T/D/la -.c O W A 3- / (j> /_ O j_ Q w C Col 25 Spike soln ID # c u C o S3i ^ l ________ Col 10 Incubator ID X - I o1--' _______ Spike Sol. Cone. P P -o > _ Col 21 Centrifuge & Transfer Spike Sol, Cone. ? O ff ^ _________ Equil Start T/D/l II A m i m e t i c T/D/l 10 A . /A 3 - / ^ i r ^ C T/D/ltO '.n ^ A m 0> / I G > / p i Ctvn C T/D/l 0- I d ie I O i (.__ Equil Stop T/D/l ll'ortwo J H I /m w i t . Col 17 T/D/l T e d a . X IS U I m r t v^t Col 22 MeOH ID # T N A - S '1 5 'b ' _______ Col 26 Internal Standard ID # c p ip p i - v & - o j C o i n Centrifuge InCol 18 MeOH ID # 'T N ^ L z _ y T S ^ _________ T/D/l '. Q 5 a m , - 7 / t/d/i i^ .'3 o ^ di / r i i D i r m i G> l : l o '. ~IHe&U T N rt-^ lS T f atzaloi eTU<_ i m f r - S o a m X i ( n i ch cm^r Q)(t^ Im -/ oi CJM.C | ( J > - S 3 S a - p U i > | i * + l T-i S u cfco L .K fo i+ ^HirOH TUft-4lSS #pi>ioioKC- af CTH f internal Std. Cone. c-P O pp^ T~Vv r*r o>S T/D/l S', o o ^ J> ! 3(1 I O I CTtn r -S 3 S o 5 t>Uu_-W ci. 1. IOOC3, 3 ^ 5 ftdcW, H3 M liA Crttc -yapj Ot GLP Study Number: ^ C /Q - - / 3 / I ( 3 ) - 3 > - & - M p ii 5 b U i J e t t r . i d ,. 3 5 5 of 6 H 5 TtelsW ' f j 0 ' -c ,, ,r / 6Urt1_^ U 's b i( U 4 * c * L - ): I o c ) > $ f r jjjQ / HS i i ? l 2 l CI c j w C 1 " 3M Environmental Laboratory BACK TO MAIN Page 190 of 703 D esorption Isotherm s, M ultiple C oncentrations E T S -8 -1 6 0 Test Substance: p f o ^ si + C 3V 2; oJ <? n3sI 4* * il $ M'S- 'S ^ aS^-Yc- 0^>-<3 5^ v ^ n > <3 i 0 ! Mn D i 5 5 ! I 1 E 0 0 -1 3 1 1-5199 23 4 S a m p le S lg 1 5 0 67 48 1:5 E 0 0 -1 3 1 1-5200 S a m p le S lg 1 0 48 1:5 1 ' i a ' 2- ; 7 x5 o 3 5c : 89 5 U 3 4^a o ? l.c ? 3 tO A ; 1 1 nt 5 6 f' 10 11 \ 12 13 N S2 S2 c> I < c. S 14 15 16 A -riL'-'fi S 3 " ' S3 e | 0 ~C vC ~ c 17 E TD3 < 18 & I S C 19 5 -1 _< - 20 21 < r "5 f 0 D D 22 r $ 3 - i 0f-- 4? _ 23 m : < 5 < JC '5. ... 15 c S < 1 F n O -1311-5201 S a m p le s ig 1 1 0 43 1 5 itt . H S 5 ' A `5 S2 S3 F O O -1 3 1 1 -5 2 0 1 M S S a m o ir- S iq 1 -O ': 48 15 S2 S3 0 0 -1 3 1 1 -5 2 0 3 E 0 0 -1 3 1 1-5204 EO O -13 1 1 -5 2 0 4 E O O -1311-5 2 0 5 0 0 -1 3 1 1-5206 E 0 0 -1 3 1 1-5207 F O O -1311-5207 F 0 0 -1 3 1 1-5209 rT 0 1? 1 1 -5 2 10 E O O -1311-5 2 1 0 E O O -1311-5211 E O O -1311-5213 E O O -1311-5213 E C O -1311-5213 E O O -1311-52 ]4 E O O -1311-52 ^ 5 E O O -1311-5215 S a m p le S ia 1 0 5 48 S a m p le S lg 1 0 5 43 M S S a m p le S lg 1 " '0 .5 48 S a m p le S lg 1 2 0 48 S a m p le S lg 1 2 .0 48 S a m p le S lg 1 2 0 43 M S S a m n fe S !g j_ : e o ; . s ig 1 S a m p le s ia 1 S a m p le S 'n 1 50 c3 48 :: M S S a m p le S lg 1 S a m p le S lg 1 5 .0 10 48 48 S a m p l e F l a -I 0 43 S a m p le S ia 1 10 43 10M S S a m p le S lg 1 48 S a m p le S lg 1 5 0 48 1 :5 15 15 1 :5 1 :5 5 15 1 -5 1 1 :5 1.5 . 1 .5 15 1 .5 3 1 .1 .3 a t.a L r iM ^ a a i s s s s -) S J I.g O o T a \.a a a M 9 4 -S2 S2 S2 V -S 2 a S2 i.z s u g 1 3 1 n: ss o -fe ia tS " r. o - 3 - I3 O d 3 ' , H S ' <3 --------------- - V S t\ . a S2 N . 3 S "1 54 S2 J v) S3 T S2 S2 3 0 . 5 A - W r> a o ^ v ti -- -E - j S3 S2 S2 3 o .~ 1 .T 7 k n S2 S3 . E 3 S3 S N- 3 0 ! - S 3 T r S3 n S3 , cn S 3 ... *3 3 & t t _ S 3 S3 S3 -J ..- S3 S A J - S3 S3 ' ... g ":% y S3 .Q q S3 S3 S a m p le 1 50 43 1 5 3 t .3 ( .a g 'r f S2 S a m p le S ig 1 50 M S S a m p le S lg 1 : 5 0 .., 48 48 1 .5 1.5 > " / }/i o . M R a --------------------- \ S2 s L S2 COM3 T/D/l l '.IO p ,, A i a \ I O l C Y S3 S3 S3 - --- --- e vL - -- - J 0 i N. A v \ 0 43 -- V Nw - i ' _?V Y \ VJ 'O i iVJ M s > L J K. Y ,\ VJ y i* i C - F '- - Y .-- Y A S -C) Y ^ --- S3 YA > -1 YY 4 M J~ \ ' - -- 'Y ' - a o *L- ... <S> L\ ( 1 L /S - A - --b, \ 3 0 ,L i - `------- C o l 23 C e n trifu g e & T ransfer \y ^\ > Cnl s J im f i'r y n v n 3 1 1 9 / n l n n f. COM4 Internal Standard ID fco n m - o i> - Q I C o lts Centrifuge & Transfer T/D/l U '. c - I O t ^ J /-2C . / D t ^ -- <-- Col 9 0.01 M CaCI2 soln ID Un m i - m - l < Internal Std. Conc./ f o p p m T U - P P o S T/D/l l l S O * * /< 3k I Q i C t*~ C Balance ID _____________________ T/D/l io . -?r>*w t & / a a . / Q l W C Col 20 MeOH ID # T N f t - M 7 g ~ T/D/l f r r ,*iOftwn X / / q I Q I Qwnf C o l 15 Spike soln ID # c p o o ^ - 1 ^ 1 T/D/l ll'.O Q ftr. -a /aiw q) x c- CoMO Incubator IDJ - f 3--____________ Spike Sol Cone. I Opfnv, i ^ P n S ________Col 21 Centrifuge & Transfer C ol 24 Aliquot Study Sample TJD/H /.'S C W ^ 3- / r 6 / o y ^ < C ol 25 Spike soln ID # O J n o V i H l ______ Spike Sol. Conc./ Q ^ p r ^ 03>_________ Equil Start T/D/l U.O m 3 / N l l C h nC T/D/l / o : i, C e t 3- / ? 3 / u l O A C T/D/l ; Q > y ~ . ____g L / Y / 0> ) o - C- Equll Stop T/D/l ir.OiiA' d / a /o ir m t. C o l1 7 T/O/l 7 ' . ^ a / <?far Q \ r j ^ ( Col 22 MeOH ID * T M rq - M .'T .T g ' C oM 1 Centrifuge Col 18 MeOH ID # T l U f t - H 7 < 7 $ T/D/l ll '. 3 Q F f i~ \ ^ / t F O - / 0 / T/D/l ( F 'P O fW v 3 /4 > l /o I C T K I.T/D/l lO 'V O ^ itlio,lu QxggJj/ow/oi c*v,c_() S2. > / /v "B u ckW u * v' J Q t e /O l C-H- C | ^{KeoH *T (>-S3 S ^ f tfS i:i on 5u.6tJo.oJ-" 2ld-0(o\ C&C t~ I H e a r t T t * h - M I S S ' i l a t* ( C KL T/D/l J f O O p u r3 / `t / O t o ~ -C C ol 26 Internal Standard ID # t o ic o I o - c ? \ Internal Std. Cone, T/D/l D ic o jfl ^ ~TFoS r) /r}6 /oj_Of-v EbcW 3 /G LP S tu d y N u m b e r: \ (35-56 frnp WS t>. t u.VrcL V. lo / iSAdAtcSy f\> Ph>ASI. , 3l3o|t>l - 3M Environmental Laboratory 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 II: "Tier II: "Adsorption Kinetics, One Concentration" Tier III: "Tier III: "Desorption Kinetics, One Concentration" "Tier III: "Adsorption/Desorption Isotherms" "Tier III "Mass Balance Calculations" 3M Environmental Laboratory Page 191 of 703 3M Environmental Laboratory BACK TO MAIN S tudy E00-1311 Suitable Analytical PFO S Adsorb/D esorb Tier I "Suitable Analytical Work" S a m p le F ile N am e S a m p le D e s c rip tio n 1010125 040 t0 10125_041 t010125_Q42 1010125_043 t0 1 0 1 2 5 _ 0 4 4 t010125_048 H)10125_049 I0 10 12 5JK 0 tQ10125_051 t01O125_052 t0 1 0 1 2 5 _ 0 5 6 t0 1 0 1 2 5 _ 0 5 7 1010125_058 t010125_059 t01O125_060 310125 064 t010125_065 1010125 066 1010125 067 I010125_068 101012S_072 1010125_073 1010125_074 1010125_075 1010125^076 1010125 080 1010125_081 1010125 082 1010125_083 1010125_0&4 1010125_088 1010125_089 t010125_090 10* E00-1311-0016 IQ x 00-1311-0017 IO x E O O -1 3 1 1-0 01 8 10x EOO-1311-0O19 1 0 x E O O -1 3 1 1-0 02 0 10x EOO-1311-0021 10x E00-1311 -0022 10x E00-1311-0023 . 10x 00-1311-0024 10x E00-1311-0025 10x E00-1311-0026 10x E00-1311-0027 10x EOO-1311-0028 IO xEOO-1311-0029 10xE0O -1311-0030 10 xE 0 0-13 11-0031 1 0 x E O O -1 3 1 1-0 03 2 10x EOO-1311-0033 tOx E00-1311-0034 IO x E O O -1 3 1 1-0 03 5 10x EOO-1311-0036 1 0 x E O O -1 3 1 1-0 03 7 1 0 x E 0 0-13 11-0038 10x EOO-1311-0039 10x EOO-1311-0040 IO xEOO-1311-0041 10x EOO-1311-0042 10xE0O -1311-0043 IO x E O O -1 3 1 1-0 04 4 1 0 x E 0 0-13 11-0045 10x EOO-1311-0046 tO x EOO-1311-0047 1 0 x E 0 0-13 11-0048 O riginal M a trix S o lu tio n 600-1311-0001 EOO-1311-0002 EOO-1311-0003 EOO-1311-0004 E00-1311-0005 EOO-1311-0006 EOO-1311-0OO7 EOO-1311-0008 EOO-1311-00O9 EOO-1311-0010 E0O-1311-0011 EOO-1311-0012 EOO-1311-0013 EOO-1311-0014 EOO-1311-0015 EOO-1311-0001 EOO-1311-0001 EOO-1311-0001 EOO-1311-0002 EOO-1311-0002 EOO-1311-0002 EOO-1311-0003 EOO-1311-0003 EOO-1311-0003 EOO-1311-0004 EOO-1311-0004 EOO-1311-0004 EOO-1311-0005 EOO-1311-0005 EOO-1311-0005 EOO-1311-0006 EOO-1311-0006 EOO-1311-0006 T h e o re tic a l Test S ubstance C o n c e n tra tio n , u g /L 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 M easured O b served S o lu tio n % R S D o f R eco v e rie s D ilu tio n F a c to r C o n c e n tra tio n , u g /L C o n cen tratio n , u g /L A verage (from In s tru m e n t) (m easu red x d ilu tio n facto r) R eco very, % R e c o very, % (A v e rg e d o v e r en tire so il ty p e ) 10 < 4 0 .0 10 < 4 0 .0 <400 <400 N /A N/A 10 < 4 0 .0 <400 N/A 10 < 4 0 .0 <400 N/A 10 < 4 0 .0 <400 N/A 10 < 4 0 .0 10 < 4 0 .0 10 < 4 0 .0 <400 <400 <400 N/A N/A N/A Control Blanks 10 < 4 0 .0 <400 N/A 10 < 4 0 .0 1Q < 4 0 .0 <400 <400 N/A N/A 10 < 4 0 .0 <400 N/A 10 < 4 0 .0 10 < 4 0 .0 10 < 4 0 .0 <400 <400 <400 N /A N/A N/A 10 6 1 5 . 6 6 10 5 3 4 .1 1 10 6 2 3 .1 5 6156.6 5341.1 6231.5 123.1 106.8 124.6 10 5 1 1 . 0 2 10 5 9 9 .0 6 10 5 3 9 . 3 7 10 6 0 2 .7 10 5 4 3 .2 8 10 6 1 5 .4 6 5110.2 599Q.8 5393.7 6027.0 5432.8 6154.B 102.2 119.8 107.9 120,5 108.7 123.1 115.2 Barnes Loam-Sandy Loam 7.51 10 5 6 6 .9 6 10 5 6 1 .3 10 5 8 2 . 0 6 5669.6 5613.0 5820.6 113.4 112.3 116.4 10 5 6 0 .8 1 10 6 2 9 .9 1 10 5 4 8 .4 7 10 5 7 0 . 8 4 10 6 1 4 . 5 4 10 5 4 9 .9 4 5608.1 6299.1 5484.7 5708.4 6145.4 5499.4 112.2 126.0 109.7 114.2 122.9 110.0 115.2 Clay Loam (Carl Broeren) 4.92 Page 192 of 703 Page 1 of 2 C'm c 5 1 ci Pcj'0()3- 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Suitable Analytical PFO S Adsorb/D esorb S a m p le FHe N am e t0 1 0 1 2 5 _ 0 9 1 1010125 092 1010125 096 1010125,097 (01Q125 098 1010125 099 tO10125 100 1010125 104 (01 01 25 JG 5 t010125_106 K)10125_107 t0 1 0 1 2 5 _ 1 0 8 1010125J12 1 0 1 2 5 .1 1 3 IQ 1 0 1 2 5 _ 1 14 t010125_115 t0 1 0 1 2 5 _ 1 1 8 1010125_120 t0 10 12 5_ 12 1 t0 1 0 1 2 5 _ 1 2 2 1010125.123 1010125.124 1010125.128 1010125.129 1010125.130 10125.131 1010125.132 S a m p le D escrip tio n 10x E 00-1311-0049 10x EOO-1311-0050 10x E00-1311-0051 tO x EOO-1311-0052 10x EOO-1311-0053 10x E00-1311-0054 10x EOO-1311-0055 tO x EOO-1311-0056 10x EOO-1311-0057 10x EOO-1311-0058 10x EOO-1311-0059 10x E00-1311-0060 10x EOO-1311-0061 10x EOO-1311-0062 10x EOO-1311-0063 10x EOO-1311-0064 10x EOO-1311-0065 10x EOO-1311-0066 10x EOO-1311-0067 tOx EOO-1311-0068 10x EOO-1311-0069 10x EOO-1311-0070 10x E0O-1311-0071 10x EOO-1311-0072 10x EOO-1311-0073 10x EOO-1311-0074 10x EOO-1311-0075 Original M a trix S o lu tio n EOO-1311-0007 EOO-1311-0007 EOO-1311-0007 EOO-1311-0008 EOO-1311-0008 EOO-1311-0008 EOO-1311-0009 EOO-1311-0009 EOO-1311-0009 EOO-1311-0010 EOO-1311-0010 EOO-1311-0010 EOO-1311-0011 EOO-1311-0011 EOO-1311-0011 EOO-1311-0012 EOO-1311-0012 EOO-1311-0012 EOO-1311-0013 EOO-1311-0013 E 00-1311-0013 EOO-1311-0014 EOO-1311-0014 EOO-1311-0014 EOO-1311-0015 EOO-1311-0015 EOO-1311-0015 T h eo re tic a l T est S u b stan ce C o n c e n tra tio n , u g /L 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 5000 M easured O b s e rv e d S o lu tio n % R S D o f R eco v e rie s D ilu tio n C o n c e n tra tio n , u g /L C o n c e n tra tio n , u g /L A verage (A verg ed o v e r en tire F actor (from In s tru m e n t) 10 6 3 5 .7 7 10 5 3 9 .8 1 10 4 0 2 .3 5 10 4 1 7 .4 7 10 3 5 9 .3 1 10 3 8 0 .9 7 10 6 0 9 .1 10 6 0 3 .9 10 5 4 0 .3 2 10 6 8 0 .8 8 10 5 4 3 .9 7 10 6 1 7 .2 10 5 4 9 .0 2 10 6 0 5 .0 4 10 5 2 9 .2 9 10 6 1 3 .7 4 10 5 3 5 .2 7 10 5 4 7 .4 3 10 3 2 6 .1 10 4 5 7 .5 2 10 5 8 6 .4 7 10 4 1 2 .3 9 10 4 7 3 .0 7 10 3 9 9 .6 10 4 2 8 .0 8 10 4 7 1 .3 9 10 4 1 8 .7 5 (m e a s u re d x d ilu tio n fac to r) R e co very, % R eco very, % so il ty p e ) 6357.7 5398.1 4023.5 4174.7 3593.1 3809.7 6091.0 6039.0 5403.2 6808.8 5439.7 6172.0 5490.2 6050.4 5292.9 6137.4 5352.7 5474.3 3261.0 4575.2 5364.7 4123.9 4730.7 3996.0 4280.8 4713.9 4187.5 127.2 108.0 80.5 83.5 71.9 76.2 121.8 120.8 108.1 136.2 108.8 123.4 109.8 121.0 105.9 122.7 107.1 109.5 65.2 91.5 117.3 82.5 94.6 79.9 85.6 94.3 83.8 99.8 C lay 116.0 Sediment 88.3 Sludge 21.81 8.88 15 .9 7 Page 193 of 703 Page 2 of 2 Page 194 of 703 BACK TO MAIN Study E00-1311 Suitable Container PFOS Adsorb/Desorb Tier I "Suitable Container" Sample Data File s00120 035 S0120 036 S00120 037 S00120 038 S00120 039 s00120 043 S00120 044 500120 045 s00120_046 sX120_047 SX120J351 SX120J352 s0Q12Q_054 sX120_055 sX120_059 sQ0120_061 S00120J362 S X 120 063 S00120 X 8 sX 1 2 0 069 s X 1 2 0 070 sX 120 075 sX 1 2 0 076 sX 120 077 sX 1 2 0 079 sX 1 2 0 083 s00120 084 S X 1 2 0 103 S X 1 2 0 104 s X 1 2 0 105 S X 1 2 0 110 S X 1 2 0 111 s X 1 2 0 112 s X 1 2 0 114 S00120 118 S0120 119 s X 1 2 2 a 035 s00122a 036 s00122a 037 s X 1 2 2 a 042 s00122a 043 s00122a 044 s00122a 046 s X 1 2 2 a 050 s00122a_051 Sample Description EOO-1311-1001 Ohr E0O-1311-1002 Ohr E 00-1311-1003 Ohr EOO-1311-1004 Ohr E00-1311-1005 Ohr E00-1311-1006 Ohr EOO-1311-1007 Ohr E00-13 1 1 -1 X 8 Ohr E00-13 1 1 -1 X 9 Ohr E X -1 3 1 1-1010 24 hour, Omg/L, S I , C-1 E00-1311-1011 24 hour, Omg/L, S1, C-1 E X -1 3 1 1 -1 0 1 2 24 hour. Omg/L. S1, C-1 E 00-1311-1013 24 hour, 0.1 Omg/L. S I , C-1 EGO-1311-1014 24 hour, 0.10m g/L, S1. C-1 E X -1 3 1 1 -1 0 1 5 24 hour, 0.10m g/L, S1, C-1 E00-1311-1016 24 hour. 1.Omg/L, S t, C-1 EOO-1311-10 17 24 hour, 1.Omg/L, S 1.C -1 E X - 1 311-1018 24 hour. 1.Omg/L, S1, C-1 E X - 1 311-1010 24 hour, Omg/L, S2, C-1 E X - 1 311-1011 24 hour, Omg/L, S2. C-1 E X -1 3 1 1-1012 24 hour, Omg/L, S2, C-1 E X -1 3 1 1 -1 0 1 3 24 hour. 0.10m g/L, S2, C-1 EOO-1311-1014 24 hour, 0.1 Omg/L, S2, C-1 E X -1 3 1 1 -1 0 1 5 2 4 hour, 0.1 Omg/L. S2, C-1 E X -1 3 1 1-1016 24 hour, 1.Omg/L. S2, C-1 EOO-1311-1017 24 hour, 1.Omg/L, S2, C-1 EOO-1311-1018 24 hour, 1.Omg/L, S2. C-1 EOO-1311-1019 24 hour, Omg/L, S I , C-2 EOO-1311-1020 24 hour, Omg/L, S1, C-2 E X -1 3 1 1 -1 0 2 1 24 hour, Omg/L, S t. C-2 EOO-1311-1022 24 hour, 0.1 Omg/L, S1. C-2 EQO-1311-1023 24 hour, 0.10m g/L, S1, C -2 E00-1311-1024 24 hour, 0.1 Omg/L, S1, C-2 EOO-1311-1025 24 hour, 1.Omg/L, S I , C-2 EOO-1311-1026 24 hour, 1.Omg/L, S I, C-2 E X - 1 3 1 1-1027 24 hour, 1.Omg/L, S I, C-2 E X -1 3 1 1 -1 0 1 9 24 hour, Omg/L, S2, C-2 EOO-1311-1020 24 hour, Omg/L. S2, C-2 EOO-1311-1021 24 hour, Gmg/L, S2. C-2 E X - 1 311-1022 2 4 hour, 0.1 Omg/L, S2, C-2 EOO-1311-1023 24 hour, 0.1 Omg/L, S2, C-2 E X - 1 3 1 1-1024 24 hour, 0.1 Omg/L, S2, C-2 E X - 1 3 1 1-1025 24 hour. 1 .Omg/L, S2, C-2 E X - 1 311-1026 24 hour, 1.Omg/L, S2, C-2 E X -1 3 1 1-1027 24 hour, 1.Omg/L, S2, C-2 Centrifute Tube Type none none nona none none none none none none Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polypropylene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Polystyrene Theoretical Test Substance Concentration, ug/L 0 0 0 1X 100 100 10X 10X 10X 0 0 0 100 100 100 10X 10X 10X N/A N/A N/A N/A N/A N/A N/A N/A N/A 0 0 0 1X 1X 1X 10X 1QX 10X N/A N/A N/A N/A N/A N/A N/A N/A N/A D ilu tio n Factor 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 Measured Concentration, ug/L (from Instrument) <24.75 <24.75 <24.75 <24.75 <24.75 <24.75 486.97 523.02 544.09 25.86 <24.75 <24.75 <24.75 <24.75 <24.75 462.08 475.12 505.67 <24.75 <24.75 <24.75 <24.75 <24.75 <24.75 1 1 0 .8 7 118.37 137.3 <24.75 <24.75 <24.75 <24.75 <24.75 <24.75 457.51 475.62 484.59 <24.75 <24.75 <24.75 <24,75 < 2 4 .7 5 <24.75 71.39 99.23 88.02 Observed Solution Concentration, ug/L (measured x dilution factor) <49.5 <49.5 <49.5 <49.5 <49.5 <49.5 973.94 1046.04 1088.18 ** Point thrown out <49.5 <49.5 <49.5 <49.5 <49.5 924.16 950.24 1011,34 <49.5 <49.5 <49.5 <49.5 <49.5 <49.5 221.74 236.74 274.6 <49.5 <49.5 <49.5 <49.5 <49.5 <49.5 915.02 951.24 969.18 <49.5 <49.5 <49.5 <49.5 <49.5 <49.5 142.78 198.46 176.04 Average Recovery, Recovery, % % Average Concentration of extractions, ug/L <49.5% <49.5% <49,5% 9 7 .3 9 4 1 0 4 .6 0 4 108.818 <49.5% < 4 9 .5 % <49.5% 92.416 95.024 1 0 1 .1 3 4 N/A N/A N/A N/A N/A N/A N/A N/A N/A <49.5% <49,5% <49.5% 91.502 95.124 96.918 N/A N/A N/A N/A N/A N/A N/A N/A N/A 96.19 94.51 244.36 1 7 2 .4 3 3M Environmental Laboratory Page 1 of 2 c\C M C " 5 / 3 ^ , / c i p i Page 195 of 703 BACK TO MAIN S tudy EOO-1311 Suitable Container PFOS Adsort/D esort S a m ple Data F ile s00120 121 s00120_122 S00120 126 s00120_128 s00120_129 S0Q12Q 130 s00120 135 S00120 136 S00120 137 s00122a_053 s00122a 054 s00122a 058 s00122a_06Q s00122a 061 sO0122a 062 s00122a__067 s00122a 068 s00122a 069 S00120 142 s00120_143 s00120_144 S00120 146 S00120 150 S00120 151 S00120 153 s0012D_154 S00120 158 s00122a 074 s00122a 075 s00122a 076 s00122a 078 s00122a_082 s00122a 083 s00122a 085 s00122a 086 s00122a_090 Sample D escription EOO-1311-1028 24 hour, Omg/L, S1, C-3 EOO-1311-1029 24 hour, Qmg/L, S I , C -3 E00-1311-1030 24 hour, Omg/L, S1, C-3 EOO-1311-1031 24 hour, 0.1 Omg/L, S I , C-3 EOO-1311-1032 24 hour, 0.10m g/L, S1, C-3 EOO-1311-1033 24 hour, 0.1 Omg/L, S1, C-3 EOO-1311-1034 24 hour, 1.Omg/L, S 1 ,C -3 EOO-1311-1035 24 hour, 1.Omg/L, S1, C-3 EOO-1311-1036 24 hour, 1.Omg/L, S I , C-3 EOO-1311-1028 24 hour, Omg/L. 82 , C -3 EOO-1311-1029 24 hour, Omg/L, S2, C -3 EOO-1311-1030 24 hour, Omg/L, S2, C-3 EOO-1311-1031 24 hour, 0.1 Omg/L, S2, C-3 EOO-1311-1032 24 hour, 0.1 Omg/L, S2, C-3 EOO-1311-1033 24 hour, 0.1 Omg/L, S2, C-3 EOO-1311-1034 24 hour. 1.Omg/L, S2, C-3 EOO-1311-1035 24 hour, 1.Omg/L, S2, C-3 EOO-1311-1036 24 hour, 1.Omg/L, S2, C-3 EOO-1311-1037 24 hour, Omg/L, S I, C-4 EOO-1311-1038 24 hour, Omg/L, S1, C-4 EOO-1311-1039 24 hour, Omg/L, S I , C-4 EOO-1311-1040 24 hour, 0.10m g/L, S1, C-4 EOO-1311-1041 24 hour, 0.1 Omg/L, S I , C-4 EOO-1311-1042 2 4 hour, 0.1 Omg/L, S I, C-4 EOO-1311-1043 24 hour, 1.Omg/L, S I, C-4 EOO-1311-1044 24 hour, 1.Omg/L, S I, C-4 EOO-1311-1045 24 hour, 1.Omg/L, S1, C-4 EOO-1311-1037 24 hour, Omg/L, S2, C-4 EOO-1311-1038 24 hour, Omg/L, S2, C-4 EOO-1311-1039 24 hour, Omg/L, S2, C-4 EOO-1311-1040 24 hour, 0.1 Omg/L. S2, C-4 EOO-1311-1041 24 hour, 0.1 Omg/L, S2, C-4 EOO-1311-1042 24 hour, 0.1 Omg/L, S2, C-4 EOO-1311-1043 24 hour. 1.Omg/L, S2, C-4 EOO-1311-1044 24 hour, 1.Omg/L, $2 , C-4 EOO-1311-1045 24 hour, 1.Omg/L. S2, C-4 C entrifute Tube Type glass glass glass glass glass glass glass glass glass glass glass glass glass glass glass glass glass glass Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Teflon Theoretical Test S u b s ta n c e C o n c e n tra tio n , ug/L 0 0 0 100 100 100 1000 1000 1000 N/A N/A N/A N/A N/A N/A N/A N/A N/A 0 0 0 100 100 100 1000 1000 1000 N/A N/A N/A N/A N/A N/A N/A N/A N/A D ilution Factor 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 M easured C o n c e n tra tio n , ug/L (from Instrum ent) 29.19 <24.75 <24.75 <24.75 <24.75 <24.75 465.89 490.88 434.39 <24.75 <24.75 <24.75 <24.75 <24.75 <24.75 261.99 201.55 133.08 442.75 28.04 < 2 4 .7 5 <24.75 < 2 4 ,7 5 <24.75 4 1 7 .8 7 455.03 469.4 < 2 4 .7 5 < 2 4 .7 5 < 2 4 ,7 5 <24.75 <24.75 < 2 4 .7 5 25.99 84.89 30.68 - Observed Solution Concentration, ug/L (measured x dilution factor) 58.38 <49.5 <49,5 <49.5 <49.5 <49.5 931.78 981.76 988.78 <49.5 <49.5 <49.5 <49,5 <49.5 <49.5 523.98 403.1 266.16 885.5 56.08 <49.5 <49.5 <49,5 <49.5 635.74 910.06 938.8 <49.5 <49.5 <49.5 <49.5 <49.5 <49.5 51.98 169.78 61.36 Average R e covery, Recovery, % % Average C oncentration of extractions, ug/L <49.5% <49.5% < 4 9 .5 % 93.178 98.176 98.878 N/A N/A N/A N/A N/A N/A N/A N/A N/A <49.5% <49.5% <49.5% 83.574 91.006 93 88 N/A N/A N/A N/A N/A N/A N/A N/A N/A 96.74 89.49 397.75 94.37 N ote: in atl of the O.tQmg/L test vessels the test substance w as undetected. T h is is due to the nature o f the relationship o f the test substance to the test vessel, som e amount o f adsorption w as expected. In this particular case the amount o f test substance initially present in the test vessels was relatively small, and the analytical method was unable to detect the te st substance in the samples. F o r the rem ainder of the study the am ount of te st substance adm inistered to the test vessels was at least 5 tim es higher than the undetected G,10mg/L level. 3M Environmental Laboratory Page 2 of 2 Study E00-1311 Tier I "Optimal Soil:Solution Ratios" 3M Environmental Laboratory Sam ple Data File S01207.036 S001207.037 S001207.038 S001207_040 s001207_044 S001207.045 301215.037 t001215 038 1001215.039 W01215 041 301215.045 {001215.046 S001207.047 S01207.048 sOO1207.052 S001207.054 S001207 055 s001207 056 S001207.061 S001207.062 $001207.063 S001211.036 S001211.037 $001211.038 S001211.040 S001211.044 S001211 045 S001211.047 $001211.048 S01211.052 S001207.068 S001207.069 sOO1 2 0 7 .0 7 0 5001207.072 S001207.076 $001207.077 S001207.079 S001207.080 S001207.084 Sam ple Description 10x EOO-1311-3001-S1, O.Omg/L, Ohr, No soil, 12/07/00 10x EOO-1311-3002-S1, 0.0mg/L, Ohr, No soil, 12/07/00 10x E0O-1311-3O03-S1, O.Omg/L Ohr, No soil, 12/07/00 10x E0-1311-3004-S1 5.0mg/L, Ohr, No soil, 12/07/00 10x E0O-1311-3OO5-S1, 5.0mg/L, Ohr, No soil, 12/07/00 10x EOO-1311-3006-S1, 5.0mg/L. Ohr, No soil, 12/07/00 10x EOO-1311-3007-SI. O.Omg/L. 48hr, No Soil, 12/07/00 10x EOO-1311-3008-SI, O.Omg/L, 48hr, No Soil, 12/07/00 10x EOO-1311-30O9-S1, O.Omg/L, 48hr, No Soil. 12/07/00 10x E0O-1311-3010-S1, 5.0mg/L, 48hr. No Soil, 12/07/00 10x E00-1311-3011-S1, 50mg/L. 48hr, No Soil, 12/07/00 10x EOO-1311-3012-S1, 5.0mg/L, 48hr, No Soil, 12/07/00 10x E00-1311-3013-S1, O.Omg/L Ohr, 1:1day, 12/07/00 10x EOO-1311-3014-S1, O.Omg/L, Ohr, 1:1day. 12/07/00 10x EOO-1311-3015-S1, O.Omg/L, Ohr, 1:1day, 12/07/00 10x E00-1311-3O16-S1, O.Omg/L, Ohr. 1:5clay, 12/07/00 10xE00-1311-3017-S1. O.Omg/L Ohr, 1:5day, 12/07/00 10x E00-1311-3018-S1, O.Omg/L Ohr, 1:5day, 12/07/00 10x E0O-1311-3019-S1,O.Omg/L Ohr, 1:25day, 12/07/00 10x EOO-1311-302O-S1.0.Omg/L, Ohr, 1:25day, 12/07/00 10x E00-1311-3021S1,O.Omg/L, Ohr. 1:25clay, 12/07/00 10x EOO-1311-3022-S1, O.Omg/L, 48hr, 1:1Clay. 12/07/00 10x EOO-1311-3023-S1, O.Omg/L 48hr. 1:1Clay, 12/07/00 10x E0O-1311-3024-S1, O.Omg/L. 48hr. 1:1Clay, 12/07/00 10x EOO-1311-3025-S1 O.Omg/L 48hr, 1:5 Clay, 12/07/00 10x E00-1311-3026-S1 O.Omg/L. 48hr, 1:5 Clay, 12/07/00 10x E00-1311-3027-S1 O.Omg/L, 48hr, 1:5 Clay, 12/07/00 10x EOO-1311-3028-S1 O.Omg/L 48hr, 1:25 Clay, 12/07/00 10x EOO-1311-3029-S1 O.Omg/L, 48hr. 1:25 Clay, 12/07/00 iOx E0O-1311-303O-S1 O.Omg/L, 48hr, 1:25 Clay, 12/07/00 10x E0O-1311-3031-S1,5.0mg/L, Ohr, 1:1day, 12/07/00 10x EOO-1311-3032-S1,5.0mg/L, Ohr, 1:1day, 12/07/00 10x EOO-1311-3033-S1,5.Omg/L, Ohr. 1:1day, 12/07/00 10x EOO-1311-3034-S1,5.0mg/L,Ohr, 1:5day, 12/07/00 1OxEOO-1311-3035-S1,5.Omg/L,Ohr, 1:5day, 12/07/00 10x EOO-1311-3036-S1,5.0mg/L.Ohr, 1:5day, 12/07/00 10xE00-l311-3037-S1,5.0mg/L,0hr, 1:25day, 12/07/00 10x E00-1311-3038-S1,5.Omg/L,Ohr, 1:25day, 12/07/00 10x EOO-1311-3039-S1.5.0mg/L.Ohr, 1:25day, 12/07/00 SoilrSoluti Soil Type on Ratio No soil No soil No soil No soil No soil No soil No soil No soil No soil No soil No soil No soil Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay none none none none none none none none none none none none 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 Page 196 of 703 Optimal Ratios BACK TO MAIN PFOS Adsorb/Desorb Theoretical Test Time Substance Point, Concentration, Dilution Hours ug/L Factor 0 0.0 10 0 0.0 10 0 0.0 10 0 5 0 0 0 .0 10 0 5000.0 10 0 5 0 0 0 .0 10 4 8 0.0 10 48 0.0 10 4 8 0.0 10 48 5 0 0 0 .0 10 48 5000.0 10 48 5000.0 10 0 0.0 1 0 0 0.0 10 0 0.0 10 0 0.0 10 0 0.0 10 0 0.0 10 0 0.0 10 0 0.0 10 0 0.0 10 48 0.0 10 4 8 0.0 10 4 8 0.0 10 48 0.0 10 4 8 0.0 10 4 8 0.0 10 48 0.0 10 4 8 0.0 10 48 0.0 10 0 5000.0 10 0 5 0 0 0 .0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5 0 0 0 .0 10 0 5000.0 10 0 5000.0 10 0 5 0 0 0 .0 10 Measured Concentration, ug/L (from Instrument) Observed Solution Concentration, ug/L (measured x dilution factor) Amount of Substance Adsorbed, % 0 0 0 0 0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 398.29 449.17 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 26.41 47.72 74.95 366 389.48 390.3 427.38 401.2 450.84 0.00 0.00 O.QO 0.00 0.00 0.00 <250 <250 <250 <250 <250 <250 <250 <250 <250 <250 <250 <250 3 9 8 2 .9 0 4 4 9 1 .7 0 <250 <250 <250 <250 <250 <250 <250 <250 <250 <250 2 6 4 .1 0 4 7 7 .2 0 7 4 9 .5 0 3 6 6 0 .0 0 3 8 9 4 .8 0 3 9 0 3 .0 0 4 2 7 3 .8 0 4 0 1 2 .0 0 4 5 0 8 .4 0 100.00 100.00 100.00 >95% >95% >95% 94.72 90.46 85.01 26.80 22.10 21.94 14.52 19.76 9.83 Page 1 of 5 t\U 5 l53/C>/ ' 6 ^ Study E00-1311 3M Environmental Laboratory Sam ple Data File Sam ple Description s001207_104 s001207_105 s001207_108 SQ01207J11 s001207_112 s001207_113 s001207_118 S001207J19 s001207_120 S001207_122 S001207J26 s001207_127 S001207_129 S001207J30 s001207_134 s001207_136 s001207_137 s001207_138 S001211JJ54 s001211_055 S001211_056 s001211_061 s001211_062 s001211_063 s001211_068 s001211_069 S001211_070 S001207_143 sC01207_144 s001207_14S S001207_150 s001207_151 S001207 152 S001207 154 S001207_158 s001207_159 HII0037.D Hilt0038.D HII0039.0 HH0041.D HH0045.D Hill0046D HII0048.D HII0049.D HHI0053.D 10xEOO-1311-3040-S1,5.0mg/L.2Jir, 1:1day, 12/07/00 10x EOO-1311-3041-S1,5.0mg/L,2hr, 1:1day, 12/07/00 1OxE0O-1311-3O42-S1,5.Omg/L,2hrl 1:1day, 12/07/00 1OxE0O-1311-3043-S1,5.0mg/L.2hr, 1:5day, 12/07/00 10x EQO-1311-3044-S1,5.0mg/L,2hr. 1:5day. 12/07/00 10x EOO-1311-3045-S1,5.0mB/L,2hr, 1:5day, 12/07/00 10xEOO-1311-3046-S1,5.0mg/L,2hr, 1:25day, 12/07/00 10x E00-1311-3047-S1,5.0mg/L,2hr, 1:25day, 12/07/00 10x E00-1311-3048-S1.5.0mg/L,2hr, 1:25day, 12/07/00 10x EOO-1311-3049-S1,5.0mg/L,4hr, 1:1day, 12/07/00 10x E00-I311-3050-S1,5.0mg/L,4hi\ 1:1day, 12/07/00 10x EOO-1311-3051-S1,5.0mg/L,4hr, 1:1day, 12/07/00 10x E0O-1311-3052-S1,5.0mg/L,4hr, 1:5day, 12/07/00 10x EOO-1311-3053-S1,5.0mg/L,4hr, 1:5day. 12/07/00 10x E00-1311-3054-S1,5.0mg/L,4hr. 1:5day, 12/07/00 10x EOO-1311-3055-S1,5.0mg/L,4hr, 1:25day, 12/07/00 10x EOO-1311-3056-S1,5.0mg/L,4hr, 1.25day, 12/07/00 10x EOO-1311-3057-S1.5.0mg/L,4hr, 1:25day, 12/07/00 10x EOO-1311-305&-S1, S.Omg/L. 8hr. 1.1C1ay, 12/07/1X) 10x EOO-1311-3059-S1, S.Omg/L, 8hr. 1:lClay, 12/07/00 10x EOO-1311-3060-51, 5.0n>9/L, 8hr, V.lClay, 12/07/00 10x EOO-1311-3061-S1, 5,0mg/L, 8hr. 1:5Clay. 12/07/00 10x EOO-1311-3062-S1. 5.0mg/Lt 8hr, 1:5Clay, 12/07/00 10x EOO-1311-3063-S1, 5-Omgfl., 8hr. 1:5Clay, 12/07/00 10x EOO-1311-3064-S1, 5.0mg/L, 8hr. 1:25Clay, 12/07/00 10x EOO-1311-3065-S1, S.Omgfl.. 8hr, 1:25Clay, 12/07/00 10x EOO-1311-3066-S1, 5.0mg/L, 8hr, 1:25Clay, 12A37/00 10x EOO-1311-3067-S1,S.Omg/L, 16hr, 1:1day, 12/07/00 10x EOO-1311-3068-S1.5.0mg/L,16hr, 1:1day, 12/07/00 10x E0O-1311-3069-S1,5.0mg/L,16hr, 1:1day. 12/07/00 10x EOO-1311-3070-S1,5.0mg/L, 16hr, 1:5day, 12/07/00 10x E00-1311-3Q71-S1,S.Omg/L, 16hr, 1:5day. 12/07/00 10s EOO-1311-3072-31,5.0mg/L,16hr, 1:5day, 12/07/00 10x E00-1311-3Q73-S1.5.0mg/L,16hr. 1.25day, 12TO7/00 10xEOO-1311-3074-S1,5.0mg/L,16hrt 1:25day, 12/07/00 10xE0O-1311-3075-S1,5.0mg/L,16hr, 1:25day, 12/07/00 10x EOO-1311-3076-S1,5.0mg/L,24hr, 1:1day, 12AD7/00 10x500-1311-3077-31,5 ^ 9 /1 ,2 4 ^ . 1:1day, 12/07/00 10x EOO-1311-3078-S1.5.0mQ/L,24hr, 1:1day, 12/07/00 10xEOO-1311-3079-S1,5.0mg/L.24hr, 1:5day, 12/07/00 10x EOO-1311-3080-S1,5.0mg/L,24hr, 1:5day, 12/07/00 10x EOO-1311-3081-S1,5.0fng/L,24hr, 1:5day, 12/07/00 10x E0O-1311-3O82-S1.5.Omg/L,24hr. 1:25day, 12/07/00 10x EOO-1311-3083-S1,5.0mg/L,24hr, 1:25day, 12A37/00 10x EOO-1311-3084-S1,5.0mQ/L,24hr, 1.25day, 12/07/00 SoiltSoluti So il Type on Ratio Clay 1:1 Clay 1:1 Clay 1:1 Clay 1:5 Clay 1:5 Clay 1:5 Clay 1:25 Clay 1:25 Clay 1:25 Clay 1:1 Clay 1:1 Clay 1:1 Clay 1:5 Clay 1:5 Clay 1:5 Clay 1:25 Clay 1:25 Clay 1:25 Clay 1:1 Clay 1:1 Clay 1:1 Clay 1:5 Clay 1:5 Clay 1:5 Clay 1:25 Clay 1:25 Clay 1:25 Clay 1:1 Clay 1:1 Clay 1:1 Clay 1:5 Clay 1:5 Clay 1:5 Clay 1:25 Clay 1:25 Clay 1:25 Clay 1:1 Clay 1:1 Clay 1:1 Clay 1:5 Clay 1:5 Clay 1:5 Clay 1:25 Clay 1:25 Clay 1:25 Page 197 of 703 BACK TO MAIN Optimal Ratios PFOS Adsorb/Desorb Theoretical Test Time Substance Point Concentration, Hours ug/L Dilution Factor 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 4 5000.0 10 4 5QQQ.Q 10 4 5000.0 10 4 5000.0 10 4 5000.0 10 4 5000.0 10 4 5000.0 10 4 5000,0 10 4 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 8 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 16 5000.0 10 24 5000.0 1Q 24 5000.0 10 24 5000.0 10 24 5000.0 10 24 5000.0 10 24 5000.0 10 24 5000.0 10 24 5000.0 10 24 5000.0 10 Measured Concentration, ug/L (from Instrument) Observed Solution Concentration, ug/L (measured x dilution factor) Amount of Substance Adsorbed, % 144.29 98.63 68.87 <25.0 155.7 140.92 317.1 310.56 326.3 113.88 88.39 92.13 126.4 113.16 136.92 326.15 326.21 319.46 130.4 114.48 111.17 293.97 314.29 287.97 118.92 305.1 128.68 119.29 99.92 166.04 140.62 136 17 152.02 330.98 321.53 346.78 125.10 105.41 34.09 116.70 110.21 96.72 288.55 284.21 288.46 1442.90 986.30 688.70 <250 1557.00 1409,20 3171.00 3185.60 3263.00 1138.80 883.90 921.30 1264.00 1131.60 1369.20 3261.50 3262.10 3194.60 1304.00 1144.80 1111.70 2939.70 3142.90 2879.70 1189.20 3051.00 1286.80 1192.90 999.20 1660.40 1406.20 1361.70 1520.20 3309.80 3215.30 3467.80 1251.00 1054.08 340.90 1166.96 1102.12 967.23 2885.54 2842.13 2884.61 71.14 80.27 86.23 >95% 68.86 71.82 36.58 36,29 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 72.77 69.60 33.80 35,69 30.64 74.98 78,92 93.18 76.66 77.96 80.66 42.29 43.16 42.31 Page 2 of 5 Study EOO-1311 3M Environmental Laboratory Sample Data File Sample Description S001211_072 s001211_076 s001211_077 s001211_079 s001211_080 s001211_084 s 001211_088 s001211_087 s 001211_ o a 8 s001211_093 s0Q1211_094 s001211_095 s001211_100 s001211_101 s 001211_102 s001211_104 s001211_108 s001211_109 HM0055.D H M 0056.D HI0057.D HH0062.D HI0063.D HI0064.D HI0069.D HI0070.D HI0071.D HI0073.D HII0077.D H0078.D HI0080.D HII0081.D niOIOl.D HH0103.D HI0104.D HII0105.D HI0110.D HII0111.D HH0112.D HI0117.D HII0118.D HI0119.D HI0121.D HH0125.D HI0126.D 10x EOO-1311-3085-S1 5.0mg/L, 36hr, 1:1Clay, 12/07/00 10x EOO-1311-3088-S1, 5.0mg/L, 36hr, 1:1Clay, 12/07/00 10x EOO-1311-3087-S1, 5.0mg/L, 36hr, 1:1Clay, 12/07/00 10x EOO-1311-3088-S1, 5.Om0/L, 36hr, 1:5Clay, 12/07/00 10x E0O-1311-3O89-S1, 5.0mg/Lr 36hr. 1:5Clay, 12/07/00 10x EOO-1311-3090-S1, 5.0mg/l_ 36hr, 1:5Clay, 12/07/00 10x E00-1311-3091-S1, 5.0mg/L. 36hr, 1:25Clay, 12/07/00 10x EOO-1311-3092-S1, 5.0mg/L, 36hr, 1:25Clay, 12/07/00 10x E00-1311-3O93-S1. 5.0mg/L. 36hr, 1:25Clay, 12AJ7/00 10x EOO-1311-3094-S1, 5.0mg/L, 48hr, 1:1C1ay, 12/07/00 10x E00-1311-3095-S1, S.Omg/L, 48hr, 1:1Clay, 12/07/00 10x EOO-1311-3096-S1, S.Omg/L, 48hr, 1:1Clay, 12A37/00 10x EOO-1311-3097-51. 5.0mg/L, 48hr. 1:5Clay, 12/07/00 10x EOO-1311-3098-S1, 5.0mQ/L, 48hr. 1:5C!ay. 12/07/00 10x EOO-1311-3099-S1. 5.0mg/L, 48hr. 1:5Clay, 12/07/00 10x EOO-1311-3100-S1. 5.0mg/L, 48hr, 1:25Ctay, 12/07/00 10x E00-1311-3101-S1. 5-Omg/L, 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3102-S1, 5.0mg/L. 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3103-S1, 5.0mg/L. Ohr. 1:1Sediment, 12/07/00 1 0 x E 0 O -1 3 1 1 -3 1 O 4 S 1 , 5 .0 m g /1 , Ohr. 1:1Sedim ent. 1 2 /0 7 /0 0 10x E00-1311-3105-S1. S.Omg/L. Ohr. 1:1Sediment, 12/07/00 10x E0O-1311-3108-S1. 5-OmL, Ohr. 1:5Sedim ent 12/07/00 10x EOO-1311-3107-S1, 5.0mg/L. Ohr, 1:SSediment. 12/07/00 10x EOO-1311-3108-S1. 5.0mg/L. Ohr, 1:5Sediment, 12/07/00 10x EOO-1311-3109-S1. 5.0m g^, Ohr. 1:25Sediment. 12/07/00 10x E0O-1311-3110-S1. 5.0mg/L, Ohr, 1:25Sediment. 12/07/00 10x E00-1311-3111-S1, 5.0mg/L, Ohr, 1:25Sediment, 12/07/00 10x EOO-1311-3112-S1. 5.0mg/L. 2hr, 1:1Sediment, 12/07/00 10x E00-1311-3113-S1, 5.0mg/L, 2hr, 1:1Sediment, 12/07/00 tOx EOO-1311-314-S1, 5.0mg/L, 2 h r, 1:1S e< tim e nt, 1 2 /0 7 /0 0 10x EOO-1311-3115-S1. S.Omg/L, 2hr. 1:5Sediment. 12/07/00 10x EOO-1311-3116-S1. 5.0mg/L. 2hr, 1:5Sediment 12/07/00 10x EOO-1311-3117-S1, 5.0mg/L, 2hr, 1:5Sediment, 12/07/00 10x EOO-1311-3118-S1.5,0mg/L, 2hr. 1:25 Sediment, 12/07/00 10x EOO-1311-3119-S1, 5.0mg/L, 2hr, 1:25 Sediment, 12/07/00 10x EOO-1311-3120-S1,5.0mg/L, 2hr, 1:25 Sediment, 12/07/00 10x EOO-1311-3121-S1. S.Omg/L, 4hr. 1:1 Sediment, 12/07/00 10x EOO-1311-3122-S1. 5.0mg/L. 4hr, 1:1 Sediment, 12/07/00 1Qx EOO-1311-3123-S1, 5.0mg/L, 4hr, 1:1 Sedimerrt, 12/07/00 10x EOO-1311-3124-S1. 5.0mg/L, 4hr, 1:5 Sedim ent 12/07/00 10x EOO-1311-3125-S1, 5.0m g^, 4hr, 1:5 Sedim ent 12/07/00 10x EOO-1311-3126-S1,5.0mg/L, 4hr, 1:5 Sedim ent 12/07/00 10x E00-1311-3127-S1, 5.0mg/L. 4hr. 1:25 Sediment, 12/07/00 10x E00-1311-3128-S1, 5.0mg^., 4hr, 1:25 Sediment, 12/07/00 10x EOO-1311-3129-S1. 5.Qmg/L, 4hr, 1.25 Sediment, 12/07/00 SoiltSoluti Soil Type on Ratio Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Clay Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1 :1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 Page 198 of 703 BACK TO MAIN Optimal Ratios PFOS Adsorb/Desorb Theoretical Test Time Substance Point, Concentration, Hours ug/L Dilution Factor 36 5000.0 10 36 5000.0 10 36 5000.0 10 36 5000.0 10 36 5000.0 10 36 5000.0 10 36 5000.0 10 36 5000.0 10 36 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 48 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 0 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 2 5000.0 10 4 5000.0 10 4 5000.0 10 4 5000,0 10 4 5000.0 10 4 5000.0 10 4 5000.0 10 4 5QQQ.Q 10 4 5000.0 10 4 5000.0 10 Measured Concentration, ug/L (from Instrument) 131.97 138.13 44.59 103.26 119.9 129.42 299.09 313.39 289.04 59.14 62.46 69.43 92.9 107.09 95.6 301.56 331.37 361.05 118.32 121.89 87,39 451.55 442.99 447.69 402.85 428.58 425.08 78.07 B5.B6 59.32 247.50 268.70 331.41 365.63 <25.0 <25.0 <25.0 80.43 63.71 242.86 246.91 245.14 380.34 374.21 368.76 Observed Solution Concentration, ug/L (measured x dilution factor) Amount of Substance Adsorbed, % 1319.70 1381.30 445.90 1032.60 1199.00 1294.20 2990.90 3133.90 2898.40 591.40 624.60 694.80 929.00 1070.90 956.00 3015.60 3313.70 3610.50 1183.16 1218.86 873.87 4515.51 4429.87 4476.92 4028.50 4285.82 4250.83 780.65 858.62 593.21 2475.02 2687.00 3314.09 3656.30 <250 <250 <250 804.32 637.08 2428.62 2469.09 2451.42 3803.38 3742.10 3687.58 73.61 72.37 91.08 79.35 76.02 74.12 40.18 37.32 42.03 88.17 87.51 86.10 81.42 78.58 80.88 39 69 33.73 27.79 76.34 75.62 82.52 9.69 11.40 10.46 19.43 14.28 14.98 84 39 82 83 88.14 50.50 46.26 33.72 26.87 >95% >95% >95% 63.91 87.26 51.43 50.62 50.97 23.93 25.16 26.25 Page 3 o f 5 BACK TO MAIN 3M Environmental Laboratory Study E00-1311 Optimal Ratios PFOS Adsorb/Desorb Sample Data File Sample Description t001215_048 t0012l5_049 (001215,053 (001215,055 (001215,056 t0012l5_057 1001215,062 (001215,063 tO01215,064 t001215_069 t001215_070 (001215,073 t0 0 1 2 1 5 ,0 7 7 (001215,078 t001215_080 (0 0 1 2 1 5 ,0 8 1 t0 0 1 2 1 5 ,0 8 5 (001215,087 (001215,088 t001215_089 t001215,094 (001215,095 (001215,096 t0 0 1 2 1 5 ,1 1 6 t00121S,117 501215,118 (001215,120 t001215,124 (001215,125 t001215,127 301215,128 t0 0 1 2 l5 ,1 3 2 tC 0 1 2 1 5 ,1 3 4 (001215,135 t0 0 1 2 1 5 ,1 3 6 (001215,141 t0012l5_142 (001215,143 t0 0 1 2 1 5 ,1 4 8 (001215,149 (001215,150 (001215,152 t0012l5,156 1001215,157 10* E00-1311-3130-si. 5.0fng/L. 8hr. 1:1 Sediment, 12/07/00 10*EQ0-1311-3131-S1, 5 0mgrt_, Bhr, 1.1 Sediment, 12/07/00 10* EOO-1311-3132-S1, 5.0mg/L, 8hr, 1:1 Sediment, 12/07/00 10* EOO-1311-3133-S1, 5.0mg/L, 8hr, 1:5 Sediment, 12/07/00 10* E00-1311-3134-S1, 5.0mg/L, 8hr, 1:5 Sediment. 12/07/00 10* EOO-1311-3135-S1, 5.0mg/L. 8hr, 1:5 Sediment, 12/07/00 10* E0O-1311-3136-S1, 5.0mg/L, 8hr, 1:25 Sediment 12/07/00 10x E0O-1311-3137-S1, 5.0mg/L, 8hr, 1:25 Sediment 12/07/00 10* E00-1311-3138-S1, 5.0mg/L. 8hr, 1:25 Sediment 12/07/00 10x E00-1311-3139-S1, 5.0mg/l_ 16hr, 1:1 Sediment 12/07/00 10x E00-1311-3140-S1, 5.0mg/L. 16hr, 1:1 Sediment, 12/07/00 10x E00-1311-3142-S1, 5.0mg/L, 16hr, 1:5 Sediment, 12/07/00 10x E00-1311-3143-S1, 5.0mg/L, 18hr, 1:5 Sediment, 12/07700 10x E00-1311-3144-S1, 5.0mg/L, 16hr, 1:5 Sedim ent 12/07/00 10x EDO-1311-3145-S1. 5.0mg/L, 16hr, 1:25 Sediment, 12/07/00 10x E00-1311-3146-S1, 5.0mg/L, 16 hr, 1:25 Sediment 12/07/00 10x EOO-1311-3147-S1, S.Omg/L, 16hr, 1:25 Sediment, 12/07/00 10x E00-1311-3148-S1, 5,0mg/L, 24hr, 1:1 Sedim ent 12/07/00 10x E00-1311-3149-S1. S.Omg/L, 24hr, 1:1 Sediment. 12/07/00 10x E0O-1311-3150-S1, 5.0mg/L, 24hr, 1:1 Sediment 12/07/00 10x E00-1311-3151-S1, 5.0mg/L, 24hr. 1:5 Sedim ent 12/07/00 10 x E00-1311-3152-S1, 5 0mg/L, 24hr, 1.5 Sediment 12/07/00 10x E00-1311-3153-S1, 5.0mg/L, 24hr, 1.5 Sediment, 12/07/00 10x E00-1311-3154-S1, 5.0mg/L, 24hr, 1:25 Sediment. 12/07/00 10x E00-1311-3155-S1, 5.0mg/L, 24hr, 1:25 Sediment, 12/07/00 10x EOO-1311-3158-S1, 5.0mg/L, 24hr, 1:25 Sedim ent 12/07/00 10 x E00-1311-3157-S1, 5.0mg/L, 36hr, 1:1 Sediment 12/07/00 10x E00-1311-3158-S1, 5.0mg/L. 36hr, 1:1 Sedim ent 12/07/00 10x E00-1311-3159-S1, 5.0mg/L, 36hr, 1:1 Sediment, 12/07/00 10x EOO-1 311-3160-S1, 5.0mg/L, 36hr, 1:5 Sediment 12/07/00 10x E00-1311-3161-S1, 5.0mg/L, 36hr, 1:5 Sediment 12/07/00 10x E00-1311-3162-S1, 5.0mg/t, 36hr, 1:5 Sediment, 12/07/00 10x E0-1311-3163-S1, 5.0mg/L, 36hr, 1:25 Sediment, 12/07/00 10x E00-1311-3164-S1. 5.0mg/L, 36hr, 1:25 Sedim ent 12/07/00 10x E00-1311-3165-S1, 5.0mg/L. 36hr, 1:25 Sediment, 12/07/00 10x E00-1311-3166-S1, 5.0mg/L, 48hr, 1:1 Sediment. 12/07/00 10x E00-1311-3167-S1, 5,0mg/L, 48hr, 1:1 Sediment 12/07/00 10x E00-1311-3168-S1, 5.0mg/L. 48hr, 1:1 Sediment 12/07/00 10x E00-1311-3169-S1, 5.0mg/L, 48hr, 1:5 Sediment, 12/07/00 10x E00-1311-3170-S1, 5.0mg/!_ 48hr. 1:5 Sediment 12/07/00 10x 600-1311-3171-S1, 5.0mg/l, 48hr, 1:5 Sediment, 12/07/00 10x 00-1311-3172-S1, 5.0mg/L, 48hr, 1:25 Sediment 12/07/00 10 x E00-1311-3173-S1, 5.0mg/L, 48hr, 1:25 Sediment 12/07/00 10x 00-1311-3174-S1, 5.0mgA_ 48hr, 1:25 Sediment, 12/07/00 Theoretical Test Time Substance SoilrSoluti Point, Concentration, Soil Type on Ratio Hours ug/L Dilution Factor Sediment Sediment S e dim ent Sediment Sediment S e dim ent Se dim ent Se dim ent Se d im e n t Sediment Se d im e n t Sediment Se dim ent Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment S e dim ent Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 8 8 8 8 8 8 8 8 8 16 16 16 16 16 16 16 16 24 24 24 24 24 24 24 24 24 36 36 36 36 36 36 36 36 36 48 48 48 48 48 48 48 48 48 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 5 0 0 0 .0 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 1Q 10 Measured Concentration, ug/L (from Instrument) Observed Solution Concentration, ug/L (measured x dilution factor) Amount of Substance Adsorbed, % 98.66 92.97 87.04 396.95 233.83 271.08 322.07 341.64 340.94 65.07 80.84 248.78 247.05 268.5 355.44 338.22 355.34 71.71 57.44 36.51 229.84 237.34 220.6 355.21 320.83 304.11 83.87 80.37 50.58 208.79 212.87 253.48 319.84 318.04 371.72 68.64 60.37 30.48 198.79 237.42 196.59 304.44 368.92 346.68 9 8 6 .6 0 9 2 9 .7 0 8 7 0 .4 0 3 9 6 9 .5 0 2 3 3 8 .3 0 2 7 1 0 .8 0 3 2 2 0 .7 0 3 4 1 6 .4 0 3 4 0 9 .4 0 6 5 0 .7 0 8 0 8 .4 0 2 4 8 7 .8 0 2 4 7 0 .5 0 2 6 8 5 .0 0 3 5 5 4 .4 0 3 3 8 2 .2 0 3 5 5 3 .4 0 7 1 7 .1 0 5 7 4 .4 0 3 6 5 .1 0 2 2 9 8 .4 0 2 3 7 3 .4 0 2 2 0 6 .0 0 3 5 5 2 .1 0 3 2 0 8 .3 0 3 0 4 1 .1 0 8 3 8 .7 0 8 0 3 .7 0 5 0 5 .8 0 2 0 8 7 .9 0 2 1 2 8 .7 0 2 5 3 4 .8 0 3 1 9 8 .4 0 3 1 8 0 .4 0 3 7 1 7 .2 0 6 8 6 .4 0 6 0 3 .7 0 3 0 4 .8 0 1 9 8 7 .9 0 2 3 7 4 .2 0 1 9 6 5 .9 0 3 0 4 4 .4 0 3 6 8 9 .2 0 3 4 6 6 .8 0 80.27 81.41 82.59 20.61 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 85.66 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 36.03 36.39 25.66 86.27 87.93 93.90 60.24 52.52 60.68 39.11 26.22 30.66 Page 4 of 5 Page 199 of 703 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Optimal Ratios PFOS Adsorb/Desorb Sample Data File Sample Description HII0128.D HH0129.D HII0133.D HM0135.D HII0136.D HM0137.O HII0142.D HMI0143.D HI0144.D (001215_162 t001215_163 t001215_164 t001215_169 t001215_170 t001215_171 t001215_173 t0 0 1 2 1 5 _ t? 4 t001215_178 10x E00-f311-3175-S1,0.Omg/L, Ohr, 1:1 Sediment, 12/07/00 fOx E00-1311-3176-S1, O.Omg/L, Ohr. 1:1 Sediment, 12/07/00 10x EOO-1311-3177-S1, O.Omg/L. Ohr. 1:1 Sediment, 12/07/00 10x EOO-1311-3178-S1, O.Omg/L, Ohr, 1:5 Sediment, 12/07/00 10x E00-1311-3179-S1, O.Omg/L, Ohr, 1:5 Sediment. 12/07/00 10x E00-1311-3180-S1. O.OmgA., Ohr. 1:5 Sediment, 12/07/00 10x E00-1311-3181-S1, O.Omg/L, Ohr, 1:25 Sediment, 12/07/00 10x EOO-1311-3182-S1, O.Omg/L, Ohr, 1:25 Sediment 12/07/00 1Qx E00-1311-3183-S1, 0.0mg/L. Ohr, 1:25 Sediment, 12/07/00 10x EOO-1311-3184-S1, O.Omg/L. 48hr, 1:1 Sediment, 12/07/00 10x E00-1311-3185-S1. O.Omg/L, 48hr. 1:1 Sediment, 12/07/00 10x EOO-1311-3186-S1, O.Orng/L, 48hr, 1:1 Sediment, 12/07/00 10x E00-1311-3187-S1,O.Omg/L, 48hr, 1:5 Sediment, 12/07/00 10x E00-1311-3188-S1, O.Omg/L, 48hr, 1:5 Sediment 12/07/00 10x EOO-1311-3189-S1, O.Omg/L, 48hr, 1:5 Sediment 12/07/00 10x EO0-1311-319O-S1, O.Omg/L, 48hr, 1:25 Sediment 12/07/00 10x E00-1311-3191-S1, O.Omg/L, 48hr, 1:25 Sediment, 12/07/00 10x EOO-1311-3192-S1, O.Omg/L, 48hr, 1:25 Sediment, 12/07/00 Theoretical Test Time Substance SoihSoluti Point, Concentration, Soil Type on Ratio Hours ug/L Dilution Factor Sediment Sediment Sediment Sediment Se dim ent Sediment Sediment Se dim ent Se dim ent Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 0 0 0 0 0 0 0 0 0 48 48 48 48 48 48 48 48 48 0.0 0.0 Q.O 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 Measured Concentration, ug/L (from Instrument) Observed Solution Concentration, ug/L (measured x dilution factor) Amount of Substance Adsorbed, % <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25.0 <25,0 <25.0 <250 <250 <250 <250 <250 <250 <25Q <250 <250 <250 <250 <250 <250 <250 <250 <250 <250 <250 Note: The control samples that did not contain 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. Page 200 of 703 Page 5 of 5 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Adsorption % Charts PFOS Adsorti/Desorb Sample Data File s001207_069 s 001207^076 s001207_080 S001207JO S * 0 0 1 2 0 7 .1 1 2 *001207.118 * 0 0 1 2 0 7 .1 2 6 * 0 0 1 2 0 7 .1 3 0 * 0 0 1 2 0 7 .1 3 7 * 0 0 1 2 1 1 .0 5 5 sD012 1 1 .0 6 2 * 0 0 1 2 1 1 .0 6 9 * 0 0 1 2 0 7 .1 4 4 *001207.151 * 0 0 1 2 0 7 .1 5 8 HU0038.O HII0045.D HiH0049,D * 0 0 1 2 1 1 .0 7 6 *001211.080 * 0 0 1 2 1 1 .0 8 7 S 0 0 1 2 1 1 .0 9 4 *001211.101 * 0 0 1 2 1 1 .1 0 8 Adsorption Kinetics. One Concentration . Calculation o f A (adsorption % at time t) to be plotted vs time Calculation of distribution Coefficient v, C,, m0 A, AverageAm_ K, Sample D escription 10x E00-1311-3t)32-S1,5.0mg/L, Ohr, 1:1d*y, 12/07/00 10x EOO-131 l-SHS-SI.S.Otng/UOhr, 1:5clay, 12/07/00 10x EOO-1311-3038-S1,5.0mjj/L,0tir, 1:25day, 12/07/00 10x EOO-1311-3041-SI .S.0mg/L.2hr, 1:1 day. 12/07/00 10x EOO-1311-3044-S1,5.0mL,2hr, 1:5dy, 12/07/00 10x EOO-1311-3047-S1,5.0mg/L,2hr, 1:25ct*y. 12/07/00 10x EOO-1311-3050-S1,5.0mg/L,4hr, 1:1cby, 12/07/00 10x E00-1311-3053-S1,5.0mg/L,4hr, 1:5day, 12/07/00 10xE00-13A1-3056-S1,5.0m9n.,4hr, V.25ty, 12/07100 10x E00-1311-3059-S1, 5.0m s/l, 8hr, 1:1Ctoy, 12/07/00 10x EOO-1311-3062-S1, 5.0mg/1_. Bhr, 1:5CIy, 12/07/00 10x EOO-1311-3065-S1, 5-Omg/l, 8hr, 1:25Ct*y, 12/07/00 10x E00-1311-3068-S1,5.0mj)/l.16hr, 1:1ctay, 12/07/00 10x EQ0-1311-3071-S1,5.0mgA^ 16ht, V.5day, 12/07/00 10x EOO-1311-3074-S1.50m 9l.16hf, 1:25clay, 12/07/00 10x EOO-1311-3077-S1.5.0mg/L.24hr, 1:1day, 12/07/00 10x EOO-1311-308O-S1,5.0mg/U.24hf, 1:5dy, 12/07/00 tOx E0O-1311-3083-S1,5.0tng/L,24hr. 1:25cl*y, 12/07/00 10x EOO-1311-3066-S1, S.Omgfl. 38hf, V.ICtoy, 17107/00 10x EOO-1311-3089-S1, 5,0mL, 38hf. 1;5Cl*y, 12/07/00 10x E0O-1311-3092-S1, 5.0tr>g/L, 36hr, 1:25Clay. 12/07/00 10x EOO-1311-3095-S1. S.Omg/L, 48hr. 1;1Clay, 12/07/00 IOxEOO-1311-3098-SI, 5.0mg/l_ 48hr, 1:5CJay, 12/07/00 lOx EOO-1311-3101-S1, 5.0mgfi_, 43hr, r.25Clay, 12/07/00 .5 i i 11 1 S} i -j S i1 1 y fl 1 f c 1 8 % ' 'S ' 8 i I' 5 fI 2s |j\ 8j II\ - 15 l> If * r s o-- s 8 e i t ? !> . % ! 1E 1 8. S 1 1? h " *i li 1 !i * i . 11 J .9 If il 5. !1 II: 11 i f 1TM 3 ,3 h J Ji E I 1& ' ! . &> S ? . 'j I s1 I s 1 f: l !| -; 1 o" 1 & ' ' . ' 'S * S' 1 i 1?. 0 j 1 0 5.0 5 25 0.477 2 2 .6 1 9 0 .46 9 0 .06 4 .9875 9 .502 0 12. 5 5.0 6 2 .5 3 .8 9 5 1 3 .8 2 2 2 .10 2 3 .61 2 .4953 1.421 0 25.0 2 5.0 2 12.5 5.0 12 5 4 .0 1 2 2 4 .7 0 1 9 .7 6 1 4 .71 5.0 2 5 0 .9 8 6 2 0 .0 7 8 0 .27 7 9 .21 5.0 6 2 .5 1 .557 4 3 .0 4 6 8 .86 7 0 .34 1 .0 0 0 8 4 .9841 2 .4988 6 .1 52 4 .082 1 1 .062 2 25.0 5,0 125 3.186 4 5 .3 6 3 6 .2 9 3 5 .87 1 .0 0 1 2 1 4 .2 22 4 5.0 5.0 25 4 12.5 - 5.0 6 2 .5 0 .8 8 4 1 .1 3 2 2 0 .58 4 8 .36 8 2 .32 7 7 ,37 8 0 .37 7 4 .90 5 .0085 2 .5105 4 .649 1 7 .021 4 25.0 5.0 125 3 .2 6 2 4 3 .4 5 3 4 .7 6 35.21 1.0241 1 3 .0 0 5 8 5.0 5.0 25 1.145 1 9 .2 8 7 7 .10 7 6 .2 6 4 .9889 3 .3 75 8 12.5 5.Q 6 2 .5 3 . 1 4 3 2 3 .2 1 3 7 .14 40.2 5 2 .5122 2 .940 8 25.0 5.0 125 3.051 4 8 .73 3 8 .98 6 3 . 15 1.0084 1 5 .8 3 7 16 5.0 18 12.5 5.0 25 0 .999 2 0 .0 0 8 0 .02 7 4 .32 5.0 6 2 .5 1.362 4 5 .4 8 7 2 .77 7 1 .41 5 .0035 2 .4968 4 .001 1 3 .3 7 7 16 25.0 5 .0 1 2 5 3 .2 1 5 4 4 .6 2 3 5 .6 9 3 3 .3 8 0 .9 9 6 4 1 3 .9 2 7 24 5.0 5 .0 2 5 1 .Q 54 1 8 .7 3 7 8 .9 2 8 2 .3 6 4 .9963 3 .746 24 12.5 24 25 .0 5.0 6 2 .5 1 .1 0 2 4 8 .7 2 7 7 .96 7 8 .4 2 5 .0 125 2 .8 4 2 5 3 .9 5 4 3 .16 4 2 .5 8 2 .5080 1 .0 0 9 9 1 7 .6 2 7 1 8 .795 36 5.0 5 .0 25 1.381 1 8 .0 9 7 2 .37 7 9 .02 4 .9910 2 ,625 36 12.5 5.0 6 2 .5 1 .1 9 9 4 7 .5 1 7 6 .02 7 6 .4 9 2 .5308 1 5 .6 5 8 36 25.0 5 .0 1 25 3 .1 3 4 4 6 .6 5 3 7 .32 3 9 .85 0 .9 9 4 0 1 4 .976 48 5.0 5 .0 2 5 0 .6 2 5 2 1 .8 8 8 7 .51 8 7 .2 6 4 .9899 7 .0 1 9 48 12.5 48 25.0 5 .0 6 2 ,5 1.071 4 9 .1 1 7 8 .58 8 0 .2 9 5.0 125 3.314 4 2.16 3 3 .73 3 3 .73 2 .5174 0 .9 8 5 9 1 8 .2 1 8 1 2 .904 Adsorption Equilibrium Plot Equilibrium Time, hours Page 201 of 703 Page 1 of 2 S i c5- 3 / 0 i p ` \ 0"^ BACK TO MAIN Co SS' 3' C=D3 sr r- CD O' o *3 Study EOO-1311 Adsorption % Charts PFOS Adsorb/Desort S a m p le D a ta Fite HU0056.D HII0063.D HH0070.0 HIJ0077.D HI0081 .D HU01M.D HilfOUl.D H iiio iia.o HI0126.D W01215_049 ( 0 0 1 2 1 5 .0 5 6 t001215_063 tOOl21S_070 100121 S_077 tooi2is_oai t001215_OSB t001215_095 t001215_117 t001215_124 t001215_128 (001215_135 t001215_142 t001215_149 1001215.156 S am p le D escrip tio n 10x E0O-1311-3104-S1, S.Omg/l, Ohr. 1:1 Sediment, 12/07/00 10x EOO-1311-3107-S1. 5.0mg/L, Ohr. 1:5Sedimeni, 12/07/00 lO x E00-1311-3110-S1, S.OmgiE, Ohr, 1:25S0diment, 12/07/00 10x EOO-1311-3113-SI, 5.0mgA_ 2hr, l:lSedim ent, 12/07/00 10x E00-1311-3116-SI, S.Omg/L, 2hr, 1:5Sedimertt, 12/07/00 10x EOO-1311-3119-S1, 5 . 0 m ^ 2hf. 1:25 Sedim ent, 12/07/00 10x EOO-1311-3122-SI, 5 Om$/L, 4hr, 1:1 Sediment. 12/07/00 10x EOO-1311-312S-S1, 5. Om/l_ 4hr, 1:5 Sediment, 12/07/00 10x E00-1311-3128-S1, -Om^/l, 4hr, 1:25 Sediment. 12/07/00 10x EOO-1311-3131-SI, 5.0mg/L. 8hr, 1:1 Sediment, 12/07/00 10x EOO-1311-3134-S1, S.Omg/L, 8hr, 1:5 Sediment. 12/07/00 10x E00-1311-3137-S1, S.Omjj/L, 8hr, 1:25 Sediment, 12/07/00 10x EOO-1311-314 0-SI. 5.0mg/L, 18M, 1:1 Sediment. 12/07/00 10x EOO-1311-3143-S1, S.Omfl/L, 16hr, 1:5 Sediment, 12/07/00 10x EOO-1311-3146-S1, 5.0mg/L, 16hr, 1:25 Sediment, 12/07/00 10x EOO-1311-3149-S1. S.Omg/L, 24W. 1:1 Sediment, 12/07/00 10x EOO-1311-3152-SI. 5.0mg/L. 24hr, 1:5 Sediment, 12/07/00 10x EOO-1311-3155-S1, 5 Omg/L. 24hf, 1:25 Sediment, 12/07/00 10x EOO-1311-3158-S1, 5.0mg/l, 36hr, 1:1 Sediment, 12/07/00 IQx EOO-131V3161-S1, 5.0m9rt_, 36hr, 1:5 SBdiment, 12/07/00 10x E00-1311-3164-S1, 5.0mg/l, 36hr. 1:25 Sediment. 12/07/00 10x E00-1311-3167-S1, 5 0mfl/L, 48hr, 1:1 Sediment, 12/07/00 10x EOO-1311-3170-S1, 5 Omg/L, 48hr, 1:5 Sediment, 12/07/00 10x EOO-1311-3173-S1, 5.0mg/l_ 48hr, 1:25 Sediment. 12/07/00 Calculation o f A (adsorption % at time t) to be plotted vs time - Calculation of distribution Coefficient, Kj t, v. c,, m0 An AverageA m ** s 1 * i f8 e tV o I* t | | if i 13 18 1 S 1 f| 1 1* j? fs s> ^ ?1 1 5 ' II t i* St '% 2>- * I 1 - I- o 2 . 5i | 1 .1 1i o .1 .- O- 1 L I 0 i* . 1 u* li * l % 3. ? E ? 1 I | E h | l* i l l i I 1 ii 11! 1 2a f I *1 0 5.0 5 .0 2 5 1 .2 1 9 18.91 7 5 .6 2 7 8 .1 6 0 12.5 5.0 62.5 4 .430 7 .1 3 1 1 .4 0 10.52 0 25.0 5.0 125 4,286 17.85 14.28 16.23 2 5.0 5.0 25 0 .859 20.71 8 2 .83 8 5 .1 2 2 12.5 5.0 6 2 .5 2 .6 8 7 2 8 .9 1 4 6.26 4 3 .49 2 25.Q 5.0 125 <250 > 59.38 >95% 2 6 .87 4 5.0 5.0 2 5 0.804 2 0 .98 83.91 85.59 4 12.5 5.0 6 2 .5 2 .469 31.64 50.62 51.01 4 25.0 5.0 125 3 .7 4 2 3 1 .4 5 2 5 .1 6 2 5 .1 1 8 5.0 5 .0 25 0 .930 20.35 81.41 81.42 8 12.5 5.0 6 2 .5 2 .3 3 8 3 3 .2 7 5 3 .23 3 9 .88 8 25.0 5 .0 125 3 .4 1 6 3 9 .5 9 3 1 .6 7 3 3 .0 2 16 5.0 s.o 2 5 0 .808 20.96 8 3 .83 7 3 .69 16 12.5 5.0 6 2 5 2 .685 2 8.94 4 6 .3 0 4 7.73 16 25.0 5 .0 125 3.382 4 0 .45 3 2 .36 3 0,07 24 5.0 5 .0 25 0.574 2 2 .13 88.51 86.96 24 12.5 6.0 62.5 2.373 32.83 5 2 .53 54.15 24 25.0 5 .0 1 25 3 .2 0 8 4 4 .7 9 3 5 .8 3 3 4 .6 6 36 5.0 5 .0 25 0.004 2 0 .98 8 3 .93 85.68 36 12.5 5.0 62.5 2 .129 35.89 5 7 .43 54.99 36 25.0 5 .0 125 3 .1 8 0 4 5 .4 9 3 6 .3 9 3 2 .6 9 4 8 5.0 5 .0 25 0.604 2 1 .98 8 7.93 89.37 - 48 12.5 5.0 62.5 2.374 32.82 5 2.52 57.81 48 25.0 5 .0 125 3 .6 8 9 3 2 .7 7 2 6 .2 2 3 2 .0 0 I I a 1 ! ! .E ( O 4.9 7 7 3 2.4755 1 .0 1 9 9 4 .9 8 0 5 2 .5 0 9 5 1 .0170 5 .0 0 8 1 2.5012 1 .0 4 3 4 4 .9 9 2 4 2 .5 0 6 7 1 .0 3 0 3 4 .9 9 1 6 2 .5 0 4 8 1.0168 4 .9 8 9 6 2 .4 9 8 7 1 .0196 4 .9 7 6 6 2.4922 1 .0 3 1 5 5 .0 0 3 7 2 .4 9 5 4 1 .0 3 8 2 3.116 0 .650 4 .085 4 .8 4 2 4 .2 8 8 > 0 .2 3 6 5 .2 0 8 5 .1 2 3 8 .0 5 4 4 .3 8 5 5 .6 7 6 1 1 .2 4 7 5 ,1 9 4 4 .3 0 3 11.761 7.721 5 .5 3 6 1 3 .6 9 3 5 .2 4 6 6 .7 6 5 1 3 .8 6 6 7 .2 7 7 5 .5 4 0 8 .5 5 6 5 10.00 S. o.oo - 10.00 Adsorption Equilibrium Plot E quilibrium Time, hours 0T)J CO CD ro oro vi oco Page 2 of 2 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Mass Balance Calculation PFOS Adsorb/Desorb Tier I "Mass Balance Calculations" Sample Data Fi Sample Description S01211_093 S01211_Q94 10x E00-1311-3094-S1. 5.0m g/t, 48hr, 1:1Clay. 12/07/00 10x E00-1311 -3095-S1, 5.0mgfl. 48hr, 1:1C)ay, 12/07/00 s001211_095 10x E00-1311-3096-S1, 5.0mg/L, 48hr. 1:1 Clay, 12/07/00 S001211_100 s001211_101 10x E00-1311-3097-S1, 5.0mg/L. 48hr, 1:5Clay, 12/07/00 10x EO0-1311-3098-S1, 5.0mg/L, 480r, 1:5Clay, 12/07/00 S001211_102 10x E00-1311 -3099-S1, 5.0mg/L, 48hr, 1:5Clay, 12/07/00 s001211_104 10x E00-1311-3100-S1, 5.0mg/L, 48hr, 1:25Cfay, 12/07/00 s001211_108 s 0 0 1 2 f1_109 10x EOO-1311-31Q1-S1, 5.0mg/L, 48hr, 1:2SCIay, 12/07/00 10x EOO-1311-31Q2-S1,5.0mg/L, 48hr, 1:25Clay. 12/07/00 t001215_141 10x EOO-1311-3166-S1, 5.0mg/L, 48hr. 1:1 Sediment, 12/07/00 t001215_142 10x EOO-1311-31B7-S1, 5.0mg/L, 48hr, 1:1 Sediment. 12/07/00 t0Q1215_143 10x EOO-1311-316B-S1, 5.0mg/L, 48hr, 1:1 Sediment, 12/07/00 t001215_148 10x E00-1311-3169-S1, 5.0mg/L, 48hr, 1:5 Sedim ent 12/07/00 tOOl215_149 1001215 _ 1 50 10x EOO-1311-3170-S1, 5.0mg/L, 48hr, 1:5 Sediment, 12/07/00 10x EOO-1311-3171-S1. 5.0mg/L, 48hr, 1:5 S edim ent 12/07/00 t001215_152 10x EOO-1311-317 2 -S I, 5.0mg/L, 48hr, 1:25 Sedim ent 12/07/00 t0 0 1 2 1 5 _ 1 56 t001215_157 10x EOO-1311-3173-S1. 5.0mg/L. 48hr, 1:25 Sediment. 12707/00 10x EOO-1311-3174-S1, 5.0mg/L, 48hr, 1:25 Sediment, 12/07/00 I -l -- Desort>Step Observed Solution SoihSolu Concentration, ug/L tion (measured x dilution Soil Type Ratio factor) Final Volume of Solvent added, Dilution ml Factor Measured Concentration, ug/L (from Instrument) Observed S o lu tio n Concentration, ug/L (measured x dilution factor) Volume of CaCI2 Solution, L Volume o f Methanol Solution, L Total Test Substance Recovery, % Clay Clay Clay Clay Clay Clay Clay Clay Clay Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment Sediment 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1:25 1:25 1:1 1:1 1:1 1:5 1:5 1:5 1:25 1 :2 5 1:25 591.40 624.60 694.80 929.00 1070.90 956.00 3 0 1 5 .6 0 3 3 1 3 .7 0 3610.50 6 8 6 .4 0 603.70 3 0 4 .8 0 1987.90 2374.20 1965.90 3044.40 3 6 8 9 .2 0 3 4 6 6 .8 0 9.0 10 95.36 9.0 10 112.93 9.0 10 159.53 6.0 10 163.56 6.0 10 147.93 6.0 10 **Tube Broke 6.0 10 476.98 6.0 10 6.0 10 520.09 501.18 9.0 10 83.19 9.0 10 100.14 9.0 10 51.56 6.0 10 186.19 6.0 10 324.9 6.0 10 210.45 6.0 10 265.72 6.0 10 6.0 10 . 282.72 285.76 953.6 1129.3 1595.3 1635.6 1479.3 4769.8 5200.9 5011.8 831.9 1001.4 515.6 1861.9 3249 2104.5 2657.2 2827.2 2857.6 0 .0 0 5 0 0.0050 0 .0 0 5 0 0.01250 0 .0 1 2 5 0 0.01250 0.0250 0.0250 0.0250 0.0050 0.0050 0.0050 0.01250 0.01250 0.01250 0.0250 0.0250 0.0250 0.0090 0.0090 0.0090 0.0060 0.0060 0 0060 0.0060 0.0060 0.0060 0.0090 0.0090 0.0090 0.0060 0.0060 0.0060 0.0060 0.0060 0.0060 46.16 53.15 71.33 34.28 35.62 83.21 91.24 96.27 43.68 48.12 24.66 57.63 78.67 59.52 73.64 87.35 83.05 Page 203 of 703 Page 1 oi 1 Ci t i r / J ) ? / 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Desorb Solvent PFOS Adsorb/Desorb Tier I "Suitable Desorb S o lvent" Sample Data File 1010122 040 1 0 1 2 2 041 1 0 1 2 2 042 10122 044 1 0 1 2 2 048 10122 049 10122,051 10122,052 1 0 1 2 2 056 10122,058 1 0 1 2 2 ,0 5 9 10122 060 10122 065 1 0 1 2 2 066 10122 067 10122,072 10122 073 10122 074 1 0 1 2 2 076 10122 080 1 0 1 2 2 081 1 0 1 2 2 083 10122 084 10122 088 1 0 1 2 2 090 1 0 1 2 2 091 10122,092 Sample Description E00-1311-2001,0ufl PFO S, control,1122/01 CMC EOO-1311-2002. Oug PFO S, control, 1/22/01 CMC EOO-1311-2003, Dug PFO S, control,1/22/01 CMC EOO-1311-2004, 0.75UB PFO S, control,1/22/01 CMC EOO-1311-2005, 0.75ug PFOS, control, 1/22/01 CMC EOO-1311-2006, 0.75ug PFO S, control,1/22/01 CMC EOO-1311-2007, 7.5ug PFO S, control,1/22/01 CMC EOO-1311-2008, 7.5ug PFO S, control,t /22/01 CMC EOO-1311-2009, 7.5ug PFO S, eontroi.1/22/01 CMC EOO-1311-2010. Oug PFOS, Clay.1/22/01 CMC EOO-1311-2011, Oug PFO S. Clay,1/22/01 CMC EOO-1311-2012, Oug PFO S, Cl ay, 1/22/01 CMC EOO-1311-2013, 0.75ug PFO S, Clay, 1/22/01 CMC EOO-1311 -2014,0.75ug PFO S, Clay,1/22/01 CMC E00-1311-2015, 0.75ug PFO S, Clay.1/22/01 CMC EOO-1311-2016, 7.5ug PFOS, Clay.1/22/01 CMC E 00-1311-2017, 7.5ug PFOS, Clay.1/22/01 CMC E00-1311-2018, 7.5ug PFO S, Clay.1/22/01 CMC EQ0-1311-Z019, Oug PFO S. Sediment, 1/22/01 CMC EOO-1311-2020, Oug PFOS, Sediment, 1/22/01 CMC EOO-1311-2021, Oug PFOS, Sediment, 1/22/01 CMC EOO-1311-2022, 0.75ug PFO S, Sedim ent,1/22/01 CMC E00-1311-2023,0.75ug PFO S, Sediment.1/22/01 CMC EG 0-13H -2024, 0.75ug PFOS, Sediment. 1/22/01 CMC EOO-1311-2025, 7.5ug PFO S, Sediment, 1/22/01 CMC EOO-1311-2026, 7.5ug PFO S, Sediment, 1 /22 1 CMC EOO-1311-2027, 7.5ug PFOS, Sediment, 1/22/01 CMC Desorb Solvent MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH MeOH T est Substance Added to Soil, ug Final (ug/ml solution Volume, cone. X ml added) ml 0 7.5 0 7.5 0 7.5 0.75 7.5 0.75 7.5 0.75 7.5 7.5 7.5 7.5 7.5 7.5 7.5 0 7.5 0 7.5 0 7.5 0.75 7.5 0.75 7.5 0.75 7.5 7.5 7.5 7 S 7.5 7.5 7.5 0 7.5 0 7.5 0 7.5 0.75 7.5 0.75 7.5 0.75 7.5 7.5 7.5 7.5 7.5 7.5 7.5 Measured Concentration, ug/L {from Instrument) < 2 5 .0 < 2 5 .0 < 2 5 .0 9 5 .9 2 9 6 .8 5 9 5.39 8 0 2 .0 1 5 8 7 .7 1 6 7 1 .3 < 2 5 .0 < 25.0 < 2 5 .0 6 3 .7 1 7 5.13 7 4 .7 4 627.98 6 8 2 .4 3 4 6 1 .5 6 < 2 5 ,0 < 2 5 .0 < 25.0 1 09.78 8 9 .7 2 88.5 4 5 6 8 .2 4 6 0 8 .7 5 625 .2 Theoretical Solution Concentration, ug/L (ug added to soil / final volume in Liters) 0 0 0 100 100 100 1000 1000 1000 0 0 0 100 100 100 1000 1000 1000 0 0 0 100 100 100 1000 1000 1000 Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Observed Solution Concentration, ug/L (measured x dilution factor) < 25.0 < 25.0 < 25.0 95.92 96.85 95.39 802.01 587.71 671.3 < 25.0 < 25.0 < 25.0 63.71 75.13 74.74 627.98 6 8 2 .4 3 4 6 1 .5 6 < 25.0 < 25.0 < 25.0 1 09 .7 8 B9.72 88.54 5 6 8 .2 4 6 0 8 .7 5 625.2 Recovery, % N/A N/A N/A 95,92 96.85 95.30 80.20 58.77 67,13 N/A N/A N/A 63.71 75.13 74.74 62.80 66.24 4 6 .1 6 N/A N/A N/A 1 09 .7 8 89.72 88.54 56.82 60.88 62.52 Average Observed Solution Concentraton, ug/L 96.1 687.0 71.2 590.7 96.0 600.7 Average Recovery .% 96.1 68.7 71.2 59.1 96.0 60.1 Note: Solubility of PFO S in soH-tess matrix (C aC l2 ) le** than the matrix w ith a d The organic molecule* in the aoil (bacteria, lipids, proteins) help to keep the PFO S In solution. This is why the recovery of the highest concentration of the soil-less matrix w as low (<80%) Page 204 of 703 Page 1 of 1 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Adsorption Kinetics PFOS Adsorb/Desorb Average Organic Carbon Adsorption Coefficient (at equilibrium), % Tier II: "Adsorption Kinetics. Ona Concentration" Calculation of Au (adsorption % at time t) to be plotted vs time fn .(ti) Calculation of distribution Coefficient K* AverageA M H010222 HO10222 H010222 HO10222 H010222 H010222 H010222 HO10222 H010222 HO10222 H010222 H010222 HO10222 H010222 H010222 HO10222 H010222 HO10222 H010222 HO10222 H01222 H010222 HO10222 HO10222 HILL0045.D HILL0046.D HILL0051.D HILL0053.D HILL0054.D HILL0055.D HILL0057.D HILL0058.D HILL0059.D HILL0O65.D HILL006.D HILL0067.D HILL0069.D HILL0070.D HILL0071.D HILL0073.D HILL0Q74D HILL0079.D HILL0081.D HILL0082.D HILL0083.D HILL0085.D HLL0086.D HILL0087.D 1311-4007-S1 1311-4008-S1 1311-4009-S1 1311-4010-S1 1311-4011-S1 1311-4012-S1 1311-4013-S1 1311-4014-S1 1311-4015-S1 1311-4016-S1 1311-4017-St 1311-4018-S1 1311-4019-S1 1311-4020-S1 1311-4021-S1 1311-4022-S1 1311-4023-S1 1311-4024-S1 1311-4025-S1 1311-4026-S1 1311-4027-S1 1311-4028-S1 13VM029-S1 1311-4030-S1 11 1 m i8f1 I I i " t_ I II? i i 0 0.0125 500.0 6.25 0 0.0125 500.0 6.25 0 0.0125 500.0 6.25 2 0.0125 500,0 6.25 2 0.0125 5Q0.Q 6 .2 5 2 0.0125 500.0 6.25 4 0.0125 500.0 6.25 4 0.0125 500.0 6.25 A 0.0125 500.0 6.25 8 0.0125 500.0 6.25 8 0.0125 500.0 6.25 8 0.0125 500.0 6.25 16 0.0125 500.0 6.25 16 0.0125 500.0 6.25 16 0.0125 500.0 6.25 24 0.0125 500.0 6.25 24 0.0125 500.0 6.25 24 0.0125 500.0 6.25 36 0.0125 500.0 6.25 36 0.0125 500.0 6.25 36 0.0125 500.0 6.25 48 0.0125 500.0 6.25 48 0.0125 500.0 6.25 48 0.0125 500.0 6.25 SUI li j! T i ll - 51.2 55.2 86.0 52.8 52.4 50.9 51.1 52.4 52.6 51.9 50.2 51,4 49.0 50.7 50.2 55.8 49.3 52.2 52.0 49.7 52.2 50.5 53.4 51.0 i3 ! H I !;s LM 10 512.31671 10 551.79408 10 860.1895 10 527.68576 10 524.20684 10 508.90006 10 511.32918 10 523.53991 10 625.56529 10 518.62455 10 501.60536 10 514.18988 10 490.01757 10 507.11023 10 502.12373 10 557.78725 10 492.73867 10 521.86832 10 519.77988 10 496.81929 10 522.22917 10 505.05482 10 534.39476 10 509.70915 !li ii U SI S I! N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A ! None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A None N/A N/A None N/A None N/A Calculation of %oc N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A Page 205 of 703 Page 1 o f 7 C JT Y \C >e\ i f , 7 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Adsorption Kinetics PFOS Adsorb/Desorb Average Organic Carbon Adsorption Coefficient (at equilibrium). % Calculation of A ,, (adsorption % at time t) to be plotted vs me ti , v .. f ' , - i ~ . .. ? Run \ | | \ \A\ :'i H010222 HO10222 H010222 HO10222 H010222 H010222 HO10222 H010222 H010222 H010222 HO10222 H010222 HO10222 H010222 H010222 R010222 R010222 R 0 10222 R010222 R 0 10222 R 0 10222 RO10222 R 010222 R 0 10222 HILL0101.D HILL0102.D HILL0107.D HILL0109.D HILL0110.D HILL0111.D HILL0113.D HILL0114.D H1U.0115.D HILL0121.D HILL0122.D HILL0123.D HILL0125.D HILL0126.D HILL0127.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0041.D RUSH0042.D RUSH0Q43.D RUSH0045.D RUSH0046.D RUSH0O51.D 1311-4037-S1 1311-4038-S1 1311-4039-S1 1311-4040-S1 1311-4041-S 1 1311-4042-S1 1311-4043-S1 1311-4044-S1 1311-4045-S1 1311-4046-S1 1311-4047-S1 1311-4049-S1 1311-4049-S1 1311-4050-S1 1311-4051-S1 1311-4052-S1 1311-4053-S1 1311-4054-S1 1311-4055-S1 1311-4056-S1 311 -4057-S1 (Point thrown out* 1311-4058-S1 1311-4059-S1 1311-4060-S1 I 0 00 2 2 2 4 4 4 8 86 16 16 16 24 24 24 36 36 36 48 48 48 V0 C0 1 I 1f 1 i f i ? i 1 1>i 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 ! 5 1I 5 1c 8 2 E_ 500.0 500.0 500.0 500,0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 m0 1i I l r iflB B ffiM p p 1i | p | l g s 21 I S S S l 1I i m m 8. W fi H l mE M ... )f 6.25 6.25 6.25 6.25 6.25 6 .2 5 6.25 6.25 6.25 6.25 6 .2 5 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 36.6 33.0 28.9 11.7 10.4 11.3 11.5 9.9 10.2 13.6 11.2 12.9 9.5 8.7 10.4 1101..13 11.3 8.9 88 3M 11.3 10.4 10.5 ! i f 1100 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 40 10 10 10 C" ,, w A# * iI II !! i 11 i! H f i. I2I.2! 365.77631 330.16608 288.72178 117.05089 104.31161 112.87498 114.51078 98.86349 101.64917 135.62296 111.91357 Jf 1 S_ f > rg i 15 B Si i1 i I 1E 31 1! ` tI H f i S s. 1 1.677796125 26.84474 2.122924 33.96678 2.64097775 42.25564 4.786863875 76.58982 4.946104875 79.13768 4.83906275 77.425 4.81861525 77.09784 5.Q142Q6375 80.2273 4.979385375 79.67017 4.554713 72.87541 4.851080375 77.61729 129.49094 4.63136325 74.10181 94.80544 86.89825 103.55901 112.90206 5.064932 5.163771875 4.955512375 4.83872425 81.03891 82.62035 79.2882 77.41959 100.99263 4.987592125 79.80147 113.48309 4.831461375 77.30338 89.29487 5.133814125 82.14103 87.70241 5.153719875 82.45952 3 *1FC19725 55.20796 113.11606 483604925 77.37679 104.46575 4.944178125 79.10685 104.74724 4.9406595 79.05055 AverageAtf Calculation of distribution Coefficient, rritoi 0 J * J 1 E I$ 1I S S a& i l i 5 I fl t f f : <1 f 3 2.4919 34.36 2.4894 2.5035 2.4842 77.72 2.4873 2.5199 2.4914 79.00 2.4945 2.4971 2.4871 74.86 2.4893 2.4899 2.4967 80.98 2.4909 2.4866 2.4936 78.17 2.5087 2.4894 2.5097 82.30 2.5090 3r4B14 2.4857 78.51 2.5228 2.4930 6 > X 1' j i 0.001840742 0.002582898 Q.Q3Q5374 0.016462273 0.019063494 0.017012975 0.016890108 0.020332124 0.019617152 0.013503133 0.017413196 0.014364402 0.02139804 0 023856115 0.019243973 0.017187085 0.019685775 0.017102227 0.022908245 0.023421172 0.00616387 0.017199576 0.018761683 0.018919953 1e *Q-test outlier 0.016293737 Calculation of K %oc Koc > S i 1; -S I .e f 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% 2.60% 3.60% 2.60% 2.60% 2.60% i l r. 7.0797782 9.9342243 14.052845 63.316435 73.321131 65.434519 64.961953 78.200479 75.450586 51.935128 66.97383 55.247701 82.300155 91.75429 74.015282 66.104172 75.71452 65.777797 88.108635 90.08143 o-3 7aAAna 66.152214 72.160319 72.769051 Page 206 of 703 Page 2 o f7 3M Environmental Laboratory BACK TO MAIN Study 00-1511 Adsorption Kinetics PFOS Adsorb/Desorb Average Organic Carbon Adsorption Coefficient (at equilibrium). % Calculation of At (adsorption % at time t) to be plotted vs time m.(W Calculation of distribution Coefficient, K j AverageA# K< W I I H H b;Data;Source prfe Sample R 0 10222 R010222 RQ10222 R010222 R010222 R01Q222 R 010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R010222 R 0 10222 RUSH0O65.D RUSH0066.D RUSH0067.D RUSH0069.D RUSH0070.D RUSH0071.D RUSH0073.D RUSH0074.D RUSH0079.D RUSH0081.D RUSH0082.D RUSH00B3.D RUSH0085.D RUSH0086.D RUSH0087.D RUSH0093.D RUSH0094.D RUSH0095.D RUSH0097.D RUSH0098.D RUSH0099.D RUSH0101.D RUSH0102.D RUSH0107.D 1311-4067-S1 1311-406B-S1 1311-4069-S1 1311-4070-S1 1311-4071-S1 1311-4072-S1 1311-4073-S1 1311-4074-S1 1311-475-S1 1311-4076-S1 1311-4077-S1 1311-4078-S1 1311-4079-S1 1311-4080-S1 11-4081-S1 (Point Thrown out* 1311-4082-S1 1311-4083-S1 1311-4084-S1 1311-4085-S1 1311-4086-S1 11-4087-S1 (Point Thrown out** 1311-4088-S1 1311-4089-S1 1311-4090-S1 000 2 2 2 4 4 4 8 8 8 16 16 10 24 24 24 36 36 36 48 48 48 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0 0125 0.0125 0.0125 0.0125 i 1E*_ 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 2 i I ! If If 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 gm M i 39i3 40.8 26.5 18.3 22.2 21.4 20.1 20.6 19.5 21.9 21.3 21.6 18.1 18-.41 19.9 17.8 17.9 15.5 163 vu. 17.1 17.1 16.8 ;!si 4S I? If H Is i~i K I 1s II 10 393.4128 1.33234 21.31744 10 408.06493 1.149188375 18.38701 10 264.88843 2.938894625 47.02231 10 192.79449 3.840068875 61.4411 10 222.39068 3.4701165 55.52186 10 213.99507 3.575061625 57.20099 10 200.94518 3.73818525 59.81096 10 206.36687 3.670414125 58.72663 10 195.19751 3.810031125 60.9605 10 219.44298 3.50696275 56.1114 10 213.05622 3.58679725 57.38876 10 216.3487 3.54564125 56.73026 10 180.50238 3.99372025 63.89952 10 180.82727 3.989659125 63.83455 g; 1991140 314.0S447 2.32431P13S 10 199.45437 3.756820375 60.10913 10 177.74809 4.028148875 64.45038 10 179.00609 4.012423875 64.19878 10 155.09854 4.31126825 68.98029 10 162.77563 4.215304625 67.44487 T340 7 2,04079835 72.65277 10 171.14436 4.1106955 65.77113 10 170.50029 4.118746375 65.89994 10 168.24527 4.146934125 66.35095 28.91 58.05 59.83 56.74 63.87 62.92 68.21 66.01 2.5058 2.4904 2.5286 2.4966 2.5099 2.5022 2.4999 2.4878 2.5214 2.4999 2.4952 2.4921 2.4932 g2.5087 2.5006 2.5269 2.5061 2.5242 24981 2 2.4987 2.5038 2.4910 0.001351513 0.001130818 0.00438774 0.007978026 0.00621686 0.006676637 0.007441502 0.007149236 0.007741275 0.006392737 0.006746946 0.0065762 0.008874371 0.008794743 0,002844366 0.007532387 0.008968349 0.008944181 0.011012187 0.010366443 0,002426376 0.00961255 0.009648067 0.00989488 **Q-test outlier ***Q-test outlier 0.009718499 Calculation of K, %oc Koc S 3 1 I I .5 1 s3 o o 1I 1 '1 2.60% 260% 2.60% 2.60% 2.60% 2.60% 260% 2.60% 2.60% 2.60% 2.60% 2.60% 2.60% 22.^600%% 260% 2.60% 2 60% 2.60% 2.60% 2.60% 2.60% 2.60% 2.60% 5.1981263 4.3493013 16.875923 30.684714 23.910998 25.679372 28.621161 27.497061 29.774135 24.587449 25.949793 25.293078 34.132197 3131..382245^95363 28.970721 34.493651 34.400698 42.354565 39.870934 B.327W1 36.971345 37.107948 38 057232 Page 207 of 703 Page 3 of 7 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Adsorption Kinetics PFOS Adsorb/Desorb Calculation of A* (adsorption % at time t) to be plotted vs time % v,, C0 m0 i g l i llr f M niks - ........M-M . : gg * %,fm.i -L~ ;,a ^ .; it;' I Run f s S S fP P f e t W s c r t p < ^ r - f 1 1 1 R 0 10222 R01Q222 R010222 R010222 R010222 R010222 H010309 H 0 10309 H010309 H 0 10309 H 0 10309 H 0 10309 H010309 H010309 H010309 H 010309 H010309 H010309 H010309 H010309 H010309 H 010309 H 010309 H010309 RUSH0121.D RUSH0122.D RUSH0123.D RUSH0125.D RUSH0126.D RUSH0127.D H1LLOO30.D HILL0037.D HILL0038.D HILL0040.D HILL0041.D HILL0042.D HILL0044.D HILL0045. D HILL0050.D HILL0052.D H1LL0053.D HILL0054.D HILL0056.D HILL0057.D HILL005B.D HILL0064.D HILL0065.D HILL0066.D 1311-4097-S1 1311-4098-S1 1311-4099-S1 1311-4100-S1 1311-4101-S1 1311-4102-S1 EOO-1311-4103-S1 EOO-1311-4104-S1 EQO-1311-4105-S1 EOO-1311-4106-S1 EOO-1311-4107-S1 EOO-1311-4108-S1 EOO-1311-4109-S1 EOO-1311-4110-S1 EOO-1311-4111-S1 E00-1311-4112-S1 EOO-1311-4113-S1 EOO-1311-4114-S1 EOO-1311-4115-S1 E00-1311-4116-S1 EOO-1311-4117-S1 EOO-1311-4118-S1 E00-1311-4119-S1 EOO-1311-4120-S1 1 I $ 0 0 0 2 2 2 4 4 4 8 8 8 16 16 16 24 24 24 36 36 36 48 48 48 I i I f 1 3 .5 i 1 1 i0 5 >s13 1 00125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0,0125 0.0125 0.0125 f 1 s i5 1 1 c I f 8 ! E_ II 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500,0 500.0 500.0 500.0 500.0 500.0 5GQ.0 500.0 500.0 500.0 500.0 500.0 500 0 1 I !* if 'iv -'i } I % & z 1 1 M 1 li i" H 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6 25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 ill - t ir i- 20.6 21.2 31.3 14.B 15.S 14.0 8.012285 6.1696 8.375534 11.534113 11.512441 10.789985 5.573715 5.956354 5.468121 5.548499 5.788465 7.103971 5 890369 6.081276 5.516164 6.353969 6.139234 6.068331 I s i & 1 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 Ai f r s j s. |i ' r i t { -f i " Ii ? a <T z l t SI I a li S8 i f IIj_ 206.27486 211.88812 313.08584 147.54934 155.3989 14Q.39BS2 80.12285 61.696 83.75534 115.34113 115.12441 107.89985 55.73715 59.56354 54.68121 56.48499 57.88465 71.03971 58.90369 60.81276 55.16164 63.53969 61.39234 60.68331 K 1! 1! 3.67156425 3.6013985 2.336427 4.40563325 4.30751375 4.4950185 5.248464375 5.4788 5.20305825 4 808235875 4.810944875 4.901251875 5.553285625 5.50545575 5.566484875 5.543937625 5.526441875 5.362003625 5.513703875 5.4898405 5.5604795 5.455753875 5.48259575 5.491458625 t i 58.74503 57.62238 37.38283 70.49013 68.92022 71.9203 83.97543 87.6008 83.24893 76.93177 76.97512 78.42003 88.85257 88.08729 89.06376 88.703 88.42307 85.79206 88.21929 87.83745 88.96767 87.29206 87.72153 87.86334 AverageA Calculation of distribution Coefficient, K* m*o K. _ i j. ! ! a: i 1 f It !? 51.25 70.44 84.96 77.44 88.67 87.64 88.34 87.63 i 'S . .l E .t C S i 8 1 Z 2 fs 2.5002 2.4849 2.4887 2.4927 2.4999 2.4857 2.4917 2.4963 2.5065 2.4875 2.4927 2.4906 2.5083 2.5139 2.4926 2.4966 2.5180 2.4911 2.5065 2.5096 2.4936 2.5084 2.5358 2.4820 1 .> 1 * ! i \ I 0.0071191B2 0.006839993 0.002998584 0.011978462 0.011088073 0.0128013 0.026289366 0.035573915 0.024784404 0.016758628 0.01676459 0.018238209 0.039721512 0.036767557 0.040840432 0.039313011 0.037916345 0.030299451 0.037345066 0.035971662 0 040424838 0.034230472 0.03521738 0.036460001 o> S 0.035302618 Average Organic Cartoon Adsorption Coefficient (at equilibrium), % CaJculation of K^_ %oc Koc $ :I `. 1i 'I f ' h 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2 80% 2.80% 2 80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 2.80% 25.425649 24.428546 10.709229 42.780221 39.600262 46.000464 93.890593 127.0497 88.515727 59.852245 59873537 65.136462 141.86254 131 3127 145.85869 140.40361 135.41552 108.21233 133.37523 128.47022 144.37442 122.26169 125.77636 126 0808 130.21429 Page 208 of 703 Page 4 of 7 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Adsorption Kinetics RFOS Adsorb/Desort Average O rganic Carbon Adsorption Coefficient (at equilibrium), % Calculation of At (adsorption % at time t) to be plotted vs time~ mfid Calculation of distribution Coefficient, ffWAverageA* Kd Calculation o f K ff ' it II ?a 11 it ^taSotxceF j_SfiB ^eD M C npgon R010314 R1314 R 0 10314 R010314 R010314 R010314 R010314 R010314 R010314 R010314 R010314 R010314 R010314 R010314 RO10314 R010314 R010314 R 0 10314 R010314 R010314 R010314 R010314 R010314 R010314 RUSH0039.D RUSH0045.D RUSH0047.D RUSH0048.D RUSH0049.D RUSH0051.D RUSH0052D RUSH0053.D BUSHOOSa.D RUSH0060.D RUSH0061.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0067.0 RUSH0068.D RUSH0073.D RUSH0075.D RUSH0076.D RUSH0077.D RUSH0079.D RUSH0080.D RUSH0081.D 1311-4127-S1 311-4128-S1 point thrown out*** 1311-4129-S1 1311-4130-S1 1311-4131-S1 1311-4132-S1 1311-4133-S1 1311-4134-S1 1311-413S-S1 11-4136-S1 Point thrown out*** 1311-4137-S1 1311-4138-S1 1311-4139-S1 1311-4140-S1 1311-4141-S1 1311-4142-S1 1311-4143-SI 1311-4144-S1 1311-4145-S1 1311 -414 6 -S 1 1311-4147-S1 1311-4148-S1 1311-4149-S1 1311-4150-SI 0 o 0 2 2 2 4 4 4 8 8 8 16 16 16 24 24 24 36 36 36 48 46 48 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 1 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 !I Ir 8.25 6 ,2 5 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6 .2 5 6.25 6.25 6 .2 5 6.25 6.25 6.25 6.25 6 .2 5 6.25 6.25 6.25 6.25 6.25 6.25 I I 37.0 I pa g 27.3 24.3 21.9 25.0 22.5 23.3 23.7 22.6 23.2 20.7 20.4 210 20.4 21.3 20.7 19.5 19.2 19.0 20.1 20.0 20.2 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 f1!I 369.86485 273.04294 243.429 219.25888 249.69091 224.8773 233.20361 237.39843 N/A 228.30606 232.11374 206.68992 203.85975 209.76708 204.22624 212.60569 207.00305 194.89952 192.10652 189.95595 201.23399 200.41683 201,72713 1626689375 26.02703 -217 6079 2.83696325 45.39141 3.2071375 51.3142 3.509264 56.14822 3.128863625 50.06182 3.43903375 55.02454 3.334954875 53.35928 3.282519625 52.52031 N/A N/A 3.39617425 54.33879 3.34857825 53.57725 3.666376 58.66202 3.701753125 59.22805 3.6279115 58.04658 3.697172 59.15475 3.592428875 57.47886 3.662461875 58.59939 3.813756 61.0201 3.6486685 61.5787 3.875550625 62.00881 3.734575125 59.7532 3.744789625 59.91663 3.728410875 59.65457 I3 35.71 52.51 53,63 53.96 58.65 58.41 61.54 59.77 2.5039 2.526 2.5013 2.5056 2.5166 2.5005 2.5036 2.5179 2.4991 2.5063 2.503 2.5161 2.5031 2.502 2.5051 2.5093 2.5228 2.4993 2.5021. 2.5007 2.5137 2.5048 2.5018 2.5064 0.001756486 0.004153909 0.005258157 0.006359818 0.005011377 0,006108378 0.00567958 0.005532811 N/A 0.005943081 0.005733657 0.007086626 0.007257527 Q.006903897 0.007214488 0.006697774 0.007079099 0.007820553 0.00801137 0.008116468 0.007409123 0.007468625 0.007374101 ****Q-Test outlier ****No internal standard 0.007417283 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1.30% 1-30% 13.511428 31.953146 40.447359 48.921674 38.549051 46.98752 43.689076 42.560087 N/A 45.71601 44.105053 54.512507 55.827131 5 3 ,1 0 6 8 9 8 55.496063 51.521337 54.454607 60.158101 61.625925 62.434367 56.993254 57.450961 56.723053 Page 209 of 703 Page 5 o f 7 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Adsorption Kinetics PFOS AdsorP/DesorP Average O rganic Carbon Adsorption Coefficient (at equilibrium). % Run Data S o u * Fde H0104046x1 HILL0039.D........ H010404ext H1LL0040.D H010404ext HILL0045.D H010404ext HILL0047.D H010404ext HILL0048.D H010404ext HILL0049.D H010404ext H1LL0051.D H010404ext HILL0052.D H010404ext HSLL0053-0 H010404ext HIU.0059.D H010404exl H1LL0060.D H010404ext HILL0061.D H 0l0404ext HILL0063.D H010404ext HILL0064 D H010404ext HILL0065.D H010404ext HILL0067.D H010404ext HILX0068.D H010404ext HILL0073-0 H010404ext HLL0075.D H010404ext HILL0076.D H010404ext HILL0077.D H010404ext HILL0079.D HQ1Q4Q4ext HILL0080.D H010404ext HILL081.D 1311-4157-S1 1311-4158-S1 1311-4159-S1 1311-4160-S1 1311-4161-S1 1311-4162-S1 1311-4163-S1 1311-4164-S1 1311-4165-S1 1311-4166-S1 1311-4167-S1 1311-4168-S1 1311-4169-S1 1311-4170-S1 1311-4171-S1 1311-4172-S1 1311-4173-S1 1311-4174-S1 1311-4175-S1 1311-4176-S1 1311-4177-S1 1311-4178-S1 1311-4179-S1 1311-4180-S1 Calculation of A* (adsorption % at time t) to be plotted vs time v0 c,, m 0 1 " ;; 1! 1i i8 . _ # %f w i 1 ..'i-V -v ' i fjK P jp i % PM I M w. II S5 1I 1 I0 1 I - r ii! * ;I 1: T -i| r i p 5 L ,', f J com 0 J ! 8 i m Sm li r i H ! I i ? if |H ! >1 ! 1 1* l i iE ' 0 0.0125 500.0 6.25 <10.0 0 0.0125 500.0 6.25 <10.0 0 0.0125 500.0 6.25 <10,0 2 0.0125 500.0 6.25 <10.0 2 0.0125 500.0 6.25 <10.0 2 0.0125 500.0 6.25 <10.0 4 0.0125 500.0 6.25 <10.0 4 0.0125 500.0 6.25 <10.0 2 2 2 2 2 2 2 2 4 0.0125 500.0 6.25 <10.0 a 0.0125 500.0 6.25 <10.0 8 0.0125 500.0 6.25 <10.0 s 0.0125 500.0 6.25 <10.0 16 0.0125 500.0 6 2 5 <10.0 2 2 2 2 2 16 0.0125 500.0 6.25 <10.0 16 0.0125 500.0 6.25 <10.0 2 2 24 0.0125 500.0 6.25 <10.0 2 24 0.0125 500.0 6.25 <10.0 24 0.0125 500.0 6.25 <10.0 2 2 36 0.0125 500.0 6.25 <10.0 2 36 0.0125 500.0 6.25 <10.0 2 36 0.0125 500.0 6.25 <10.0 48 0.0125 500.0 6.25 <10.0 2 2 48 0.0125 500.0 6.25 <10.0 2 48 0.0125 500.0 6.25 <10,0 2 1, ) I il n Sn U fl If P : ;i !3 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 A, / f 8` f E* . 1 5 '_ > V i S i S* i 23 3E. *? 1 ' . 8 . E j I 1 >6.0 >6 0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6 0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6 0 >6.0 >6.0 >96% >96% > 96% >96% > 96% >96% > 96% >96% >96% >96% > 96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% > 96% >96% AverageA, ^ :' Calculation of distribution Coefficient K* Ki { ' J* f I J 1 fs . 1 H i! 13 >96% > 96% >96% > 96% >96% >96% >96% >96% f : 1 E t .S i &5 6i 1 i1 13 2.4857 2.4947 2.4959 2.5021 2.5007 2.5137 2.4773 2.5149 2.4956 2.495 2.4831 2.4775 2.5094 2.5171 2.5166 2.5007 2.502 2.4899 2.4893 2.5139 2.4771 2.5021 2.4837 2.5205 f j, J s f ? i: 1 <0.120 <0.120 <0.12Q <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 <0.120 aSe <0.120 Calculation of K; %oc Kc 1 ' f S. E 3 I G 8 & 18 I s N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A Page 210 of 703 Page 6 of 7 3M Environmental Laboratory Study EOO-1311 Adsorption Kinetics BACK TO MAIN PFOS Adsorb/Desorb A verage O rganic Carbon Adsorption Coefficient (at equilibrium). % A d sorptio n Percentage as a F u n c tio n o f Tima Page 211 of 703 Page 7 o f 7 3M Environmental Laboratory 00-1311 Tier HI: "Desorption Kinetics. One Concentration" Calculation of A* (adsorption % a l tim e t) to fa- cytj m*yij . =; ............' -i. * , * s- ; - 'j, .: ` *- H010309 H010309 H010309 R 0 10309 R 0 10309 RQ10309 H010311 H010309 H010309 H010309 R010309 R010309 R010309 H010311 H010309 H010309 R010309 R010309 R010309 R010309 H010311 H010309 HO10309 R010309 R010309 R010309 H010311 HQ10311 H010309 H010309 R010309 R010309 H010311 H010311 Dala Sour Filo H IU0071.D H IL L 01 06 D HILL0136.D RUSH0057.D R U S H 00 93 .0 R U S H 0 1 3 5 .D HILL0058.D HILL0072.D HILL0107.D H IL L 0 1 3 7 .D R U S H 0 0 5 8 .D R U S H 0 0 9 4 .D R U S H 0 1 3 6 .D H ILL0 0 5 9 ,D HILL0080.O H IL L 0 1 1 0 .D R U S H 0 0 3 6 .D RUSH0066.D R U S H 0 1 0 0 .D RUSH0140.D HILL0069.D H1LL0081.D HILL0111.D RUSH0037.D R U S H 0 0 6 7 .D RUSH0101.D H1LL0036.D H IL L 0 0 7 0 .D HILL0082.D H1LL0112.D tube broke RUSH0068.D R U S H 0 1 0 6 .D HILL0037.D HILL0071.D E00-1311-4028-S2 E0 O -1 3 1 1 -4 0 2 8 -S 3 00-1311-4028-S4 1311-4028-S5 1311-4028-S6 1311-4028-S7 E00-1311-4028-S3 EOO-1311-403Q-S2 E0 O -1 3 1 1 -4 0 3 0 -S 3 E0O-1311-4O30-S4 1311-4030-S5 1311-4030-S6 1311-4030-S7 EOO-1311-403O-S8 00-1311-4058-S2 00-1311-4056-S3 1311-4058-S4 1311-4058-S5 1311-4058-S6 1311-4058-S7 0 0-1 311-4058-S8 E 0 C M 3 1 1 -4 0 5 9 - S 2 E0O-1311-4O59-S3 131M 059-S4 1311-4059-S5 1311-4059-S6 00-1311-4059-S7 0 0 -1 3 1 1-4 05 9-S 8 E0O-1311-4O60-S2 EDD-13 1 1- 4 0 6 0 -S 3 1311-4060-S4 1311-4060-S5 1311-4060-S6 00-131 -4060-S7 EOO-1311-4O60-S8 2 4 6 6 24 32 48 2 4 6 6 24 32 48 2 4 6 8 24 32 48 2 4 6 8 24 32 48 2 4 6 6 24 32 48 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 500.0 500,0 500.0 500.0 500.0 500.0 500,0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 ?I? 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 ' l! ll 5 0 .5 0 5 4 8 2 50 .5 0 5 4 8 2 50.505482 50 .5 0 5 4 8 2 50.505482 5 0 .5 0 5 4 8 2 50.505462 5 0 .9 7 0 9 1 5 5 0 .9 7 0 9 1 5 5 0 .9 7 0 9 1 5 5 0 .9 7 0 9 1 5 5 0 .9 7 0 9 1 5 5Q.97Q915 5 0 .9 7 0 9 1 5 1 1 .3 1 1 6 0 6 1 1 .3 1 1 6 0 6 1 1 .3 1 1 6 0 6 1 1 .3 1 1 6 0 6 1 1 .3 1 1 6 0 6 1 1 .3 1 1 6 0 6 1 1 .3 1 1 6 0 6 1 0 .4 4 6 5 7 5 10 .4 46 57 5 10.446575 10 .4 46 57 5 1 0 .4 4 6 5 7 5 10446575 1 0 .4 4 6 5 7 5 1 0 .4 7 4 7 2 4 10 .4 74 72 4 1 0 .4 7 4 7 2 4 10 .4 74 72 4 1 0 .4 7 4 7 2 4 1 0 .4 7 4 7 2 4 1 0 .4 7 4 7 2 4 ir ivis 1S i . 10 505.05462 N /A N /A 10 505.05482 N/A N /A 10 505.05482 N /A N /A 10 505.05482 N/A N/A 10 505.05482 N /A N /A 10 505.05482 N/A N/A 10 505.05482 N/A N /A 10 509.70915 N/A N/A 10 509.70915 N/A N/A 10 509.70915 N/A N/A 10 509.70915 N/A N/A 10 509.70915 N/A N/A 10 509.70915 N /A N/A 10 509.70915 N/A N/A 10 113.11606 4.8360493 77.37679 10 113.11606 4.6360493 77.37679 10 113.11606 4.8360493 77.37679 10 113.11606 4.6360493 77.37679 10 113.11606 4.8360493 77.37679 10 113.11606 4.8360493 77.37679 10 113.11606 4.8360493 77.37679 10 104.46575 4.9441781 79.10685 10 104.46575 4.9441781 79.10685 10 104.46575 4-9441781 79.10685 10 104.46575 4.9441781 79.10685 10 104.46575 4.9441781 79.10685 10 104.46575 4.9441781 79.10685 10 104.46575 4.9441781 79.10685 10 104.74724 4.9406595 79,05055 10 104.74724 4.9406595 79.05055 10 104.74724 4.9406595 79,05055 10 104.74724 4.9406595 79.05055 10 104.74724 4.9406595 79.05055 10 104.74724 4.9406595 79.05055 10 104.74724 4.9406595 79.05055 Page 212 of 703 Page 1 of 6 BACK TO MAIN P F O S AdsorWDesofb U r\( S l u l t M c t ) ip 3M Environmental Laboratory E00-1311 Tier 111: "Desorption Kinetics. One C We , (: i 1is bon%attmwU" V0 1, fi I 51 Ji ! l S ljj . .. 1 S 1 Run ,,DataSourceFite HHHRO00011110000333300009999 RHHHUIIULLS.HLLQ000011703051667...DD.0D R010309 RUSH0093.0 R010309 R U S H 0 1 3 5 .D H 0 10311 HILL0058.D H010309 HILL0072.D H010309 HILL0107.D H010309 HILL0137.D R010309 R U S H 00 56 .D R010309 R U S H 0 0 9 4 .D R010309 RU5H0136D H010311 HILL0059.D HO10309 HILL0080.D H010309 HILL011D.D R 010309 R U S H 0 0 3 6 .D R010309 R U S H 0 0 6 6 .D R 010309 R U S H 0 1 0 0 .D R010309 R U S H 0 1 4 0 .D H010311 HILL0069.D H010309 HILL0081.D H010309 HILL0111.D R 0 10309 R U S H 0 0 3 7 .D R010309 RUSH0067D R010309 R U S H 0 1 0 1 .D H010311 HILL0036.D H010311 HJLL0070.D H010309 HILL0082.D HO10309 HILL0112.D tube broke R010309 R U S H 0 0 6 6 .D RO10309 R U S H 01 06 .D H010311 H1LL0037.D H010311 HLL0071.D BBBHW i SampleDeecHpon EEEOQO1OO03--1-11131331-1141M10--442O0Q822-2S8885---SSS243 1311-4Q28-S6 1311-4028-S7 E O 0 -1 3 1 1 -4 0 2 8 -S 8 E00-131-4030-S2 EOO-13 1 1 - 4 0 3 0 - S 3 EOO-1311 -4030-S4 1311-4030.S5 1311-4030-S6 1311-4030-S7 E00-1311-4030-S8 E00-1311-4058-S2 EOO-13 1 1-4058-S3 1311-4058-S4 1311-4058-S5 1311-4058-S6 1311-4Q58-S7 E00-1311-4058-S8 EOO-13 1 1 -4 0 5 9 -S 2 E 0 -1 3 1 1 -4 0 5 9 -S 3 1311-4059-S4 1311-4059-S5 1311-4059-S6 'E 0 0 - 1 3 1 1 - 4 0 5 9 -S 7 -1311-4059- 3EDO S EOO-131 1 -4 0 6 0 -S 2 EOO-1311-4060-S3 1 3 1 1 - 4 0 6 0 - S4 1311-4060-S5 1311-4060-S6 EOO-1311-4060-S7 E00-1311-4060-S8 i 3 st % N/A N/A N/A N/A T111020...3351490i0002.3l648050459 N/A 9.9 N/A 9.9 N/A 12.3 N/A 10.758796 N/A 10.082186 N/A 8.300946 N/A 6.2 N/A 9.4 N/A 10.4 N/A 10.4 2.4857 9.632074 2.4857 3.726289 2.4857 9.6 2.4857 27.1 2.4857 29.6 2.4857 27.7 2.4657 29.8 2.5226 10.882623 2.5226 5.345641 2.5226 9.6 2.5226 27.1 2.5226 28.0 22..55222286 25.2 11.5 2.4930 13.560921 2.4930 11.436618 2 .4 9 3 0 N/A 2.4930 32.9 2 .4 9 3 0 27.2 22..44993300 24.5 25.7 1 1 !2222 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 !. it; ISj 22I221040I....076688I071163 19 .6 1 3 19 .7 7 0 24 .5 6 3 21 .5 1 6 20 .1 6 4 16.602 12.400 18.806 20 .8 2 7 20 .8 6 3 19.264 7.457 19.178 54 .1 9 9 59 .1 7 0 55.331 59.581 21 .7 6 6 10.692 19.297 54 .1 4 5 55 .9 5 3 22.950.481 87 27 .1 6 2 22 .8 7 3 N/A 65 .7 0 7 54.492 48 .9 9 3 51 .4 9 5 12 1 0000....0000i111122225555 0.0125 0.0125 0.0125 0 .0 1 2 5 0 .0 1 2 5 0 .0 1 2 5 0.0125 0.0125 0.0125 0.0125 0 .0 1 2 5 0 .0 1 2 5 0 .0 1 2 5 0 .0 1 2 5 0 .0 1 2 5 0 .0 1 2 5 0.0125 0 .0 1 2 5 0 .0 1 2 5 0 .0 1 2 5 Q.0125 0 .0 1 2 5 0 .0 1 2 5 0.0125 0 .0 1 2 5 0.0125 0 .0 1 2 5 0.0125 0 .0 1 2 5 0.0125 0 .0 1 2 5 ri " 1 ry *.''v Du *** 1 i s 1 I I1s^> 1C 1? 0000....23221666 0.25 0.25 0.31 0.27 0.25 0.21 0.16 0.24 0.26 0.26 0.24 0.09 0.24 0.68 0.74 0.69 0.74 0.27 0.13 0.24 0.66 0.70 0.63 0.29 0.34 0.29 N/A 0.82 0.68 0.61 0.64 P . ?cT i i 8 i [\ I| Ic N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A 4.98 1.93 4.96 14.01 15.29 14.30 15 .4 0 5.50 2.70 4.88 13.69 14.15 12.76 5.81 6.87 5.79 N/A 16.62 13.79 12.40 13.03 'r-"W''~v s ii I? N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A 0.09596445 0.255866272 0.096417966 0.03086746 0.027851852 0.030133047 0.027524799 0.085092813 0.176360505 0.096614882 0.031242717 0.030073337 0.Q33S7Q005 0.080306522 0.067949086 0.081629271 N/A 0.025147447 0.031354673 0.035436552 0.033471788 Page 213 of 703 Page 2 of 6 BACK TO MAIN PFOS Adsorb/Desorb N/A 5.73 347 4.92 14.77 14.41 13 .1 5 11.41 0.047134 3M Environmental Laboratory EOQ-1311 Calculation of A, (adsorcin % at time t) to be p V0 - --'.i.'V i ; SISlIBBilalSlIi HHIHHRHHHI H 0 10309 H010309 R 0 10309 R010309 R 0 10309 H010311 H010311 H010309 H010309 R010309 R010309 R010309 H010311 H010311 H010309 H010309 R010309 R010309 R 0 10309 H010311 H010311 H010309 H010309 R010309 R 0 10309 R010309 H010311 H010311 H010309 H010309 R010309 R010309 R010309 H010311 H010311 H010309 H010309 R010309 R010309 R010309 H010311 H010311 P v a Source File HILL0086D HILL0120.D RUSH0410 R U S H 0 0 7 2 .D R U S H 0 1 1 2 .D HILL0041.D HILL0081.D HILL0087.D H IL L 0 1 2 1 .D BUSHOQ42.D R U S H 0 0 7 3 .D R U S H 0 1 1 3 .D HILL0042.D HILL0082.D H fi .t .0 0 9 2 .0 H IU0122.D R U S H 0 0 4 3 .D R U S H 0 0 7 8 .D R U S H 0 1 1 4 .D HILL0043.D HILL0083.D HILL0096.D HIIL0126.D R U S H 0 0 5 1 .D R U S H 0 0 8 2 .D R U S H 0 1 2 4 .D HIIL0051.D HILL0093.D HILL0097.D HILL0127.D R U S H 0 0 5 2 .D R U S H 0 0 8 3 .D R U S H 0 1 2 5 .D HILL0052.D HILL0094.D HILL0098.D HILL0128.D R U S H 0 0 5 3 .D R U S H 0 0 8 4 .D RUSH0126.D HILL0053.D HILL0095.D E00-1311-4088-S2 EOO-1311-4088-S3 1311-4066-S4 1 3 11 -40 88 -S S 1311-4088-S6 EOO-131 1 -4 0 8 8 -S 7 E00-1311-4088-S8 E00-1311-4089-S2 E 0 -1 31 1-4Q 89 -S 3 3 1 1 14089-S4* peint t h iw n aiU 1311-4089-S5 1311-4089-S6 E00-1311-4089-S7 E0 O -1 3 1 1 -4 0 8 9 -S 8 E0O-1311-409O-S2 E00-1311-4090-S3 1311-4090-S4 1311-4090-S5 1311-4090-SO EOO-13 1 1 - 4 0 9 0 - S 7 E00-1311-4090.se E 00-1311-4118-S2 EOO-1311-4118-S3 1311-4118-S4 13 11 -41 18 -S S 1311-4118-S6 EOO-1311-4118-S7 EOO-1311-4118-S8 E00-1311-4119-S2 E 0 0 - 1 3 1 1 - 4 1 19 -S3 1 3 1 1 -4 1 1 9 -S 4 1311-4119-SS 1 3 1 1 -4 1 1 9 -S 6 EOO-1311 - 4 1 19 -S7 EOO-1311-4119-S6 E00-1311-4120-S2 E00-1311-4120-S3 1 3 1 1 -4 1 2 0 -S 4 1311-4120-S5 1 3 1 1 -4 1 2 0 -S 6 E O O -1 3 1 1 -4 1 2 0 ^ 7 E0O-1311-412O-S8 2 4 6 8 24 32 46 2 4 6 e 24 32 48 2 4 6 8 24 32 48 2 4 6 8 24 32 48 2 4 6 8 24 32 48 2 4 6 6 24 32 48 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 Q.Q125 0.0125 0 .0 1 2 5 0.0125 0 .0 1 2 5 0 .0 1 2 5 0.0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0 .0 1 2 5 0 .0 1 2 5 0.0125 U 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0 500.0500.0 500.0 500.0 500.0 500.0 5000 500.0 5000 500.0 500.0 500.0 5000 500.0 500,0 500.0 500.0 500.0 500.0 500.0 500.0 500,0 500.0 500,0 500J] 500,0 500,0 500.0 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 1 7 .1 1 4 4 3 6 1 7 .1 1 4 4 3 6 1 7 .1 1 4 4 3 6 17 .1 14 43 6 1 7 .1 1 4 4 3 6 17 .1 14 43 6 1 7 .1 1 4 4 3 6 17 .0 50 02 9 17 .0 5 0 0 2 9 17 .0 50 02 9 17 .0 50 02 9 17 .0 50 02 9 17 .0 5 0 0 2 9 17 .0 50 02 9 1 6 .8 2 4 5 2 7 1 6 .8 2 4 5 2 7 1 6 .8 2 4 5 2 7 16 .8 24 52 7 16 .8 24 52 7 16 .8 24 52 7 1 6 .8 2 4 5 2 7 6.353969 6.353969 6.353969 6.353969 6.353969 6.353969 6.353969 6.139234 6.139234 6.139234 6.139234 6.139234 6.139234 6.139234 6.068331 6.068331 6.068331 6.068331 6.068331 6.068331 6.068331 c"V(M I 1 1I l : j I*I- ll ,8\ i * 10 171.14436 4.1106955 65.77113 10 171.14436 4.1106955 65.77113 10 171.14436 4.1106955 65.77113 10 171.14436 4.1106955 65.77113 10 171.14436 4.1106955 65.77113 10 171.14436 4.1106955 65.77113 10 171.14436 4.1106955 65.77113 10 170.50029 4.1187464 65.89994 10 170.50029 4.1187464 65.89994 10 170.50029 4.1187464 65.69994 10 170.50029 4.1187464 65.89994 10 170.50029 4.1187464 65.89994 10 170.50029 4.1187464 65.89994 10 170.50029 4.1187464 65.89994 10 168.24527 4.1459341 66.35095 10 168.24527 4.1469341 66.35095 10 168.24527 4.1469341 66.35095 10 168.24527 4.1469341 66.35095 10 168.24527 4.1469341 66.35095 10 168.24527 4.1469341 66.35095 10 168.24527 4.1469341 66.35095 10 63.53969 5.4557539 67.29206 10 63.53969 5.4557539 87.29206 10 63.53969 5.4557539 87.29206 10 63.53969 5.4557539 87.29208 10 63.53969 5.4557539 67.29206 10 63.5 3969 5.4557539 87.29206 10 63.53969 5.4557539 67.29206 10 61.39234 5.4625958 87.72153 10 61.39234 5.4825958 87.72153 10 61.39234 5.4825958 87.72153 10 61 39234 5.4825958 87.72153 10 61.39234 5.4825958 87.72153 10 61.39234 5.4825953 87.72153 10 61.39234 5.4825958 87.72153 10 60.68331 5.4914586 67.86334 10 60.68331 5.4914586 87.86334 10 60.68331 5.4914586 67.86334 10 60.68331 5.4914588 87.86334 10 60.66331 5.4914566 67.86334 10 60.68331 5.4914586 87.86334 10 60.66331 5.4914566 87.86334 Page 214 of 703 Page 3 of 6 BACK TO MAIN PFOS Adsortu'OosartJ PFOS Adsorb/Desorb Page 4 of6 mm 3 * m im Mmmmmnv $ iH s:!;!fH 3 s::3 s u !ii:i3 ;}S 3 !3 !;;:i !i9iiij3ii!HSii:!ii9i9:sii:fiiss::is!!Si lI!IS !IS ilii!lS S llS S IIIS IllillS S iS IS !l!lil laSSBg||i333=||=SSSsi|=Saas|sasaaR| p gsga EOO-1311 3M Environmental Laboratory !IIISl!I!I!ii!!!!!Ii Page 215 of 703 3M Environmental Laboratory BACK TO MAIN 00-1311 Run S H01Q319a H 010319a H010319a H010319a H010319a H010319a H010319a H010319a H010319a H010319a H010319a HO10319a H010319a H010319a HO10319a H010319a HO10319a H01Q319a HO10319a H010319a H010319a R010404ext RO1O404ext R010404ext R0104Q4ext R010404ext R010404exl RQ10404ext R010404exl R010404exl R0lO404ex R010404ext R010404ext R010404exl R010404ext R010404exl R010404ext R010404ext R01G404ext R010404ext R010404ext A* %C alculation of (adsorption a t tim e t) to b e p lo tt e d v s tim e t. v. c,, m, 51 f MW Sowte'Fi*' HILU0035 H1LL0041 D HILL0050 D H IL L 0 0 6 0 .D H IL L 0 0 6 7 .D HILL0078.D H IL L 0 0 8 9 .D H IL L 0 0 3 6 .D H IU -0046.D H IL L 0 0 5 1 .D H IL L 0 0 6 1 .D H IL L 0 0 6 8 .D H IL L 0 0 7 9 .D H IL L 0 0 9 0 .D H IL L 0 0 3 7 .D HLL0047.D HILLO052.D H ILU 062.0 HILL0 0 7 3 .D H IL L 0 0 8 0 .D HILL0091.D R U S H 0 0 3 5 .D RUSH004VD R U S H 0 0 5 1 .D R U S H 0 0 6 0 .D R U S H 0 0 6 7 .D R U S H 0 0 7 8 .D R U S H 0 0 B 9 .D R U S H 0 0 3 6 .D R U S H 0 0 4 6 .D R U S H 0052.D R U S H 0 0 6 1 .D R U S H 0 0 6 8 .D R U S H 0 0 7 9 .D R U S H 0090.D R U S H 0037.D R U S H 0047.D R U S H 0 0 6 2 .D R U S H 0069.D R U S H 0080.D R U S H 0 0 9 1 .D 1311-4148-S2 1 3 1 1 - 4 1 4 8 -S 3 1 3 1 1 - 4 1 4 8 -S 4 1 3 1 1-4 1 4 8 -S 5 1311-4148-S6 1 3 1 1-4148-S 7 1311-4148-S8 1 3 1 1-4 1 4 9 -S 2 1 3 1 1-4 1 4 9 -S 3 1311-4149-S4 1 3 1 1 - 4 1 4 9 -S 5 1 3 1 1-4 1 4 9 -S 6 1311-4149-S7 1 3 1 1 -4149-S 8 1 3 1 1-4150-S 2 1311-4150-S3 11 - 4 1 5 0 -S 4 p o in t throw n out 1311-4150-S5 1 3 1 1-4 1 5 0 -S 6 1311-4150-S7 1 3 1 1 - 4 1 5 0 -S 8 1 3 1 1-4 1 7 8 -S 2 1 3 1 1-4178-S 3 1311-4178-S4 1311-417S-S5 1311-4178-S6 1 3 1 1-4 1 7 8 -S 7 1311-4178-SB 1311-4179-S2 1311-4179-S3 1311*417934 1311-4179-S5 1 3 1 1-4 1 7 9 -S 6 1311-4179-S7 1311-4179-S8 1311-4180-S2 1311-4180-S3 1311-4180-S4 1311-4180-S5 1311-4180-S6 1 3 1 1-4 1 8 0 -S 7 1311-4180-S8 I I I 2 408 24 32 48 2 4 6 8 24 32 48 2 4 6 8 24 32 40 2 4 6a 24 32 48 2 64 B 24 32 48 2 46 8 24 32 48 I l 15 ! ? 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 O.C125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 . 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I ' r t f "'"'* t J 1 li 625 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6 .2 5 6.25 6.25 6.25 6.25 6.25 6.25 6.25 625 6.25 6.25 6.25 6.25 625 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 6.25 .'.I'/:. - life 20.123399 2 0 .1 2 3 3 9 9 20.123399 20.123399 20.123399 20.123399 20.123399 20.041683 20.041663 2 0 .0 4 1 6 8 3 20.041683 20.041683 20.041683 20.041683 2 0 .1 7 2 7 1 3 20.172713 20.172713 20.172713 20.172713 2 0 .1 7 2 7 1 3 20.172713 <100 <10.0 <10.0 <10.0 <10.0 . <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 <10.0 1 sf I 10 10 1Q 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 c r * ' m"\(W A* ' ' : - :' . ' f 1 i !? l ii f r }. I .; i.j ; ! :1 i f i 201.23399 201.23399 201.23399 201.23399 201.23399 201.23399 201.23399 200.41683 200.41663 200.41683 200.41683 200.41663 200.41683 200.41683 201.72713 201.72713 201.72713 201.72713 201.72713 201.72713 201.72713 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 <20 if 3.7345751 3.7345751 3.7345751 3.7345751 3.7345751 3.7345751 3.7345751 3.7447896 3.7447896 3.7447896 3.7447896 3.7447896 3.7447896 3.7447896 3.7284109 3.7284109 3.7284109 3.7284109 3.7284109 3.7284109 3.7284109 >6.0 >6.0 >6.0 >6 0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 >6.0 59.7532 59.7532 59.7532 59.7532 59.7532 59.7532 59.7532 59.91663 59.91663 59,91663 59.91663 59.91663 59.91663 59.91663 59.65457 59.65457 59.65457 59.65457 59 65457 59.65457 59.65457 >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% >96% PFOS A dsorb/De sorto Page 216 of 703 Page 5 o f 6 EOO-1311 .- jd e s y p tio fl* art t o * t ^ BACK TO MAIN PFOS Adsorti/Desorb 3M Environmental Laboratory ill Run TBS W H010319a HO10319a H010319a H010319a H01Q319a H010319a HO10319a H010319a H010319a HO10319a H010319a H010319a H010319a H010319a HQ1 0 3 19a H010319a H010319a H010319a H010319a H010319a R010404ext RQ1Q404ext R 0 1 0 4 0 4 ext R010404ext R 010404ext R010404ext R010404ext R010404ext R010404ext R010404ext R010404ext R010404exl R010404ext R010404ext R010404ext R010404ext Data S ource Fife H U LK S " HILL0041.D H1LL0050.D H1LL0060.D H IL L 0 0 6 7 .D H ILL 00 76 .0 H IL L 0 0 8 9 .D HILL0036.D H ILL 0O 46 .D HILL0051.D H1LL0061.D H IL L 0 0 6 8 .D HILL0079.D H IL L 0 0 9 0 .D H IL L 0 0 3 7 .D HILL0047.D H IL L 0 0 5 2 .D HILL0062.D HILL0073.D HILL0080.D H1LLO091.D R U S H 0 0 3 5 .D RUSHQ041 D R U S H 0 0 5 1 .D R U S H 0 0 6 0 .D R U S H 0 0 6 7 .D R U S H 0 0 7 8 .D R U S H 0 0 8 9 .D R U S H 0 0 3 6 .D RUSH0046D R U S H 0 0 5 2 .D RUSH0061.D RUSH0068.D R U S H 0 0 7 9 .D RUSHQ090.0 R U S H 0 0 3 7 .D R U S H 0 0 4 7 .D R010404ext R010404ext R010404ext R0!0404ext R U S H 0 0 6 2 .D RUSH0069 O RUSH0080.D R U S H 0 0 9 1 .D 8 iin p lo D a a crip tio if" 1 3 1 1-4 1 4 8 -S 3 1311-414S-S4 1 3 1 1-4 1 4 8 -S 5 1 3 1 1-4 1 4 8 -S 6 1311-4148-S7 1 3 1 1-4 1 4 8 -S 8 1311-4149-S2 1 3 1 1 -4 1 4 9 -S 3 1311-4149-S4 1 3 1 1 -4 1 4 9 -S 5 1 3 1 1-4 1 4 9 -S 6 1311-4149-S7 1 3 1 1 -4 1 4 9 -S 8 1311-4150-S2 1311-4150-S3 11-4150-S4 point thrown out 1311-415Q-S5 1 3 1 1 -4 1 5 0 -S 6 1 3 1 1 -4 1 5 0 -S 7 1311-4150-S8 13 1 1-4178-S2 1 3 1 1 -4 1 7 8 -S 3 1 3 1 1 - 4 1 7 8 - S4 1 3 1 1-4 1 7 8 -S 5 1311-417B-S6 1 3 1 1-4 17 8-S7 1 3 1 1 -4 1 7 8 -S 8 1311-4179-S2 1311-4179-S3 1 3 1 1-4 17 9-S4 1 3 1 1-4 17 9-S5 1311-4179-S6 1 3 1 1-4 1 7 9 -S 7 1 3 11 -41 79 -S B 1 3 11 -41 80 -S 2 1 3 1 1- 4180-S3 1 3 1 1-4 1 8 0 -S 4 1 3 1 1- 4180-S5 1311-4180- S6 1 3 1 1-4 1 8 0 -S 7 1311-4180-S8 2.5046 2.5048 2.5048 2.5048 2.5048 2.5048 2.5048 2.5018 2.501 B 2.5018 2.5018 2.5018 2.5018 2.5018 2.5064 2.5064 2.5064 2.5064 2.5064 2.5064 2.5064 2.5021 2.5021 2.5D21 2.5021 2.5021 2.5021 2.5021 2.4837 2.4837 2 4837 2.4837 2.4837 2.4837 2.4837 2.5205 2 .5 2 0 5 2.5205 2.5205 2.5205 2.5205 2.5205 W 30.5 39.1 131.4 72.9 59.1 60.4 58.6 32.4 38.5 78.0 63.0 64.6 63.2 62.8 30.4 43.7 212.6 79.4 64.2 71.4 36.4 <10.0 < 1 0 .0 <10.0 < 10.0 < 10.0 < 10.0 <10.0 < 10.0 < 10.0 < 10.0 < 10,0 < 10.0 < 1 0 .0 <10.0 < 10.0 <10.0 tube broke <10.0 < 100 < 10.0 < 10.0 Ii 2 61.012 0 .0 1 2 5 2 78.101 0 .0 1 2 5 2 262.770 0.0125 2 145.867 0.0125 2 118.209 0.0125 2 120.703 0.0125 il 0.76 0.98 3.28 1.82 1.48 1.51 2 117.269 0.0125 1.47 2 64 .7 0 6 0.0125 Q.81 2 76.924 0 .0 1 2 5 0.96 2 155.968 0.0125 1.95 2 125.944 0.0125 1.57 2 129.276 0.0125 1.62 2 126.316 0.0125 1.58 2 125.585 0.0125 1.57 2 60 .8 9 6 0 .0 1 2 5 0.76 2 87 .4 2 9 0.0125 1.09 2 425.224 0.0125 5.32 2 158.750 0.0125 1.98 2 128.323 0.0125 1.60 2 142.857 0.0125 1.79 2 72.779 0 .0 1 2 5 0.91 2 <20.0 0.0125 <2.08 2 <20.0 0.0125 < 2 .0 8 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0 .0 1 2 5 < 2 .0 8 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0 .0 1 2 5 < 2 .0 8 2 < 2 0 .0 0 .0 1 2 5 < 2 .0 8 2 < 2 0 .0 0.0125 < 2.08 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0 .0 1 2 5 < 2 .0 8 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0 .0 1 2 5 < 2 .0 8 2 < 2 0 .0 0.0125 < 2 .0 8 2 < 2 0 .0 0 .0 1 2 5 < 2.08 2 N/A 0.0125 N/A 2 < 2 0 .0 0.0125 <2.08 2 < 2 0 .0 0 .0 1 2 5 < 2 .0 8 2 < 2 0 .0 0.0125 < 2.08 2 < 2 0 .0 G.0125 < 2 .0 8 0 li H V 20 .4 2 26 .1 4 87 .9 5 48 .8 2 39 .5 7 40 .4 0 39 .2 5 21.60 25 .6 8 52 .0 6 42 .0 4 43 .1 5 42 .1 6 41 .9 2 20 .4 2 29.31 142.56 53 .2 2 43 .0 2 47 .8 9 24 .4 0 < 0 .2 3 5 < 0.235 < 0.235 < 0 .2 3 5 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 < 0.235 N/A < 0.235 < 0.235 < 0.235 < 0.235 s& m m 0.019447047 i* 2081 0.014099941 27 .0 4 0.000683619 7Q.Q1 0.005231021 48 .0 3 0.007622552 41.91 0.007361997 0.007723675 0.018136497 43 .4 9 35 .1 9 0.014462163 0.004600666 0.006888569 0.00658219 0.00685357 0.006922545 0.019440686 0.012027234 -0.00148895 **bad injectio 0.004383175 refer to QC 0.006605041 0.00542565 0.01545214 <0.237 N/A < 0.237 < 0.237 N/A N/A < 0.237 N/A < 0 .2 3 7 N/A < 0.237 N/A < 0 .2 3 7 N/A < 0.237 < 0.237 < 0.237 < 0.237 < 0.237 < 0.237 < 0 .2 3 7 < 0.237 < 0.237 N/A < 0.237 < 0.237 < 0.237 < 0.237 Page 6 of 6 Desorption Percentage as a Function of Ton Tim e, hours Page 217 of 703 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Tier III: "Adsorption/D esorption Isotherms'* Adsorption Adsorption Isotherms plot to determine K and n PFOS Adosrb/Desorb H010311 H010311 H010311 H010311 H010311 H01Q311 H010311 H010311 H010311 H010311 H010311 H010311 R010402a R010402a R010402a HO10311 H010311 H010311 RO10329a R010329a R010329a R010329a R010329a RO10329a R010329a R010329a R010329a R010329a R010329a R010329a HILL0101.D HILL01O6.D HILL0107.D HILL0109.D HILLO110.D H1LL0111.D H ILL0113.D HILL0114.D HILL0115D H IL L 0 1 2 1 .D HILL0122.D HILL0123.D R U SH 0037. D RUSH0038. D R U S H 00 39 .D HILL0137.D HILL0138.D HILL0139.D R U S H 0 0 3 7 .D R U S H 00 38 .D R U S H 00 39 .D RUSHD041.0 R U S H 0 0 4 2 .D R U S H 00 43 .D R U S H 00 49 .D RUSHO050.D R U S H 0 0 5 1 .D R U S H 00 53 .D R U S H 00 54 .D R U S H 00 55 .D E 0 0 -1311-5004 EOO-1311-5005 E 0 0 - 1 3 1 1-5006 EOO-1311-5007 E00-1311-5008 EO O-1311 -5 0 0 9 EOO-1311-5010 EOD-1311-5011 EOO-1311-5012 EOO-1311-5013 EOO-1311-5014 EOO-1311-5015 1311-5016 1311-5017 1311-5018 EOO-1311-5022 EOO-1311-5023 EOO-1311-5024 1311-5025 1311-5026 1311-5027 1311-5028 1311-5029 1311-5030 1311-5031 1311-5032 1311-5033 1311-5034 1311-5035 1311-5036 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 196.1 197.5 198.5 253.2 183.9 169.5 435.7 403.3 406.6 102.7 110.0 102.9 69.243301 63.879261 64.31529 186.8 193.1 200.3 159.93 152.92 143.26 391.37 230.09 387.34 82.81 85 .1 1 50 .3 3 404.55 414.16 433.98 2 2 2 10 10 10 10 10 10 100 100 100 1000 1000 1000 2 2 2 10 10 10 10 10 10 100 100 100 100 100 100 392.199086 2.59350658 395.05281 2.59665516 396.986296 25 32 .1 7 0 7 2 18 39 .4 4 7 2 5 16 95 .3 3 7 2 9 43 57 .2 8 3 5 6 2.59877552 3.40349298 3.26468734 3.22925611 3.53921582 4033.37088 3.60566816 4065.65759 3.6091308 10270.0043 4.01157063 10996.3071 4.D4124666 10288.8621 4.01236735 69243.301 4.84037776 63879.261 4.80535988 64315.29 4,80831423 373.65555 386.188014 400.617808 1 5 9 9 .3 3 5 3 2.57247144 2.58679879 2.60273025 3.20393952 1529.15715 3.18445212 1432.64531 3.15613868 3913.70145 3.59258769 2300.94744 3.3619067 3873.38636 3.58609082 8281.3209 3.91809961 8510.8829 3.92997359 8037.8359 3.90513914 40454.91 4.60697124 41416.3251 4.61717156 43397.8954 4.63746867 N /A U/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A 0.0125 0.0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0.0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0 0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0.0125 0.0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0 .0 1 2 5 0.0125 0 .0 1 2 5 0.0125 N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N /A N/A N/A N/A N/A N/A N/A N/A N/A ------1____ Page 218 of 703 Page 1 of 16 s '/<3h / ) 3M Environmental Laboratory BACK TO MAIN Study E00-1311 R010329a R010329a R010329a R010329a R010329a RO10329a R010329a R010329a R010329a R010329a RO10329a RO10329a RO10329a R010329a R010329a RO10329a R010329a R010329a R010329b RO10329b R010329b RO10329b R010329b R01Q329b R010329b RO10329b RO10329b RO10329b R010329b R010329b RUSH0065.D RUSH0O66.D RUSH0067.D RUSH0069.D RUSH0Q70.D RUSH0071.D RUSH0077.D RUSH0078.D RUSH0079.D RUSH0081.D RUSH0082.D RUSHQQ83.D RUSH0085.D RUSH0090.D RUSH0091.D RUSH0097.D RUSH0098.D RUSH0099.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 Adsorption Isotherms (")) is' :EI:' plot to determine K and n 1311-5040 1311-5041 1311-5042 1311-5043 1311-5044S1 1311-5045 1311-5046 1311-5047 1311-5048 1311-5049 1311-5050-1S 1311-5051 1311-5052 1311-5053 1311-5054 1311-5058 1311-5059 1311-5060 1311-5061 1311-5062 1311-5063 1311-5064 1311-5065 1311-5066 1311-5067 1311-5068 1311-5069 1311-5070 1311-5071 1311-5072 ii 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 I f! if 99.69 9 6 .20 58.15 460.98 305.78 > 501 183.73 166.25 156.55 359.52 > 501 351.66 211.71 253.43 207.41 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 2 199.378426 2.29967816 2.4853 2 192.408926 2.28422522 2.492 2 116.296416 2.06556633 2.4898 2 921.950724 2.96471148 2.5046 2 611.563282 2.7864414 2.5154 2 N/A N/A 10 1837.31918 3.26418461 2.5162 2.4949 10 1662.52521 3.22076824 10 1565.51161 3.19465629 2.5008 2 .521 10 3595.21967 3.55572543 2.4853 10 N/A N/A 10 3516.5502 3.54611682 2.5132 2.4976 100 21170.5882 4.32573292 100 25342.8747 4.40385588 2.5007 2 .5287 100 20741.2664 4.31683527 2.5065 2 63.66312 1.80388792 2.4936 2 68.302058 1.83443379 1.8183721 2.4697 2 65.5835 1.81673459 2.5098 2 270.25587 2.43177514 2.517 2 282.215634 2.45058107 2.44621055 2.5023 2 285.940358 2.45627546 2.4912 10 831.7832 2.92001014 2.482 10 778.17175 2.89107546 2.90096809 2.5173 10 779.50456 2.89181866 2.5088 10 1795.32634 3.2541434 2.5042 10 1871.04255 3.27208366 3.25364837 2.4816 10 1716.79339 3.23471803 2.4892 100 10122.5113 4.00528827 2 .4872 100 10329.5006 4.01407933 4.01928362 2.5011 100 10926.5554 4.03848327 2.4959 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 1.511998 0.179551 1.542893 0.188336 1.926378 0.284741 5.380307 0.730807 6.899682 0.838829 N/A N/A 15.84573 1.199912 16.68204 1.222249 17.0294 1.231199 32.21332 1.508035 N/A N/A 32.4484 1.511193 144.1067 2.158684 121.8864 2.085955 145.9143 2.164098 2.187284 0.339905 2.184972 0.339446 0.338176 2.163601 0.335177 8.590307 0.934009 8.581027 0.933539 0.934025 8.600572 0.934527 20.99223 1.322059 20.96407 1.321476 1.322114 21.02846 1.322807 40.95456 1.612302 40.94615 1.612213 1.614521 41.59573 1.619049 200.4136 2.301927 198.2653 2.297247 2.296913 195.6882 2.291565 PFOS Adosrto/Desorto Page 219 of 703 Page 2 o f 16 3M Environmental Laboratory BACK TO MAIN Study E00-1311 Adsorption Isotherms RUN R010329b R010329b RO10329b H010405int H010405int H010405int R010329b R010329b R010329b H010405int H010405int H010405int R010312 R010312 R010312 RO10312 R010312 R010312 R010312 RQ10312 R010312 R010312 R010312 R010312 RQ10312 R010312 R010312 R010312 R010312 R010312 Q iib a r a M RUSH0149.D RUSH015O.D RUSH0151.D HILL0039-D HILL0040.D HILL0045.D RUSH0157.D RUSH0162.D RUSH0163.D HLL0047.D HILL004.D HILL0049.D RUSN0030.D RUSH0031.D RUSH0032.D RUSH0038.D RUSH0039.D RUSH0044.D RUSH0046.D RUSHQ047.D RUSH0048.D RUSH0050.D RUSH0051.D RUSH0052.D RUSHQ058.Q RUSH0059.D RUSH0060.D RUSH0062.D RUSH0063.D RUSH0064.D Sam ple D e u rip rio n 1311-5076 1311-5077 1311-5078 1311-5079 1311-5080 1311-5081 1311-5082 1311-5083 1311-5084 1311-5085 1311-5086 1311-5087 1311-5086 1311-5089 1311-5090 1311-5094 1311-5095 1311-5096 1311-5097 1311-5098 1311-5099 1311-5100 1311-5101 1311-5102 1311-5103 1311-5104 1311-5105 1311-5106 1311-5107 1311-5108 A d sorptio n C0 C ^j(eq) plot to determine K and n " W , Vq I C ^ y a q ) 1 1 i \ 1 j! ii 1I ]i l 1! 1 i l | J li 00 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 500 500 500 2000 2000 2000 5QQQ 5000 5000 10000 10000 10000 50000 50000 50000 8 8 1 vV i.t 1i nmF x " 1 r :% -i WMI t s ' 8 lif e 1W i! . iillm w4 If 1 i f c S I 1 2 1 lH '- " l U 75.82 2 75.66 2 95.65 2 96.606457 10 121.213214 91.012507 10 10 238.27 10 236.36 10 226.44 10 52.079333 100 51.355299 100 51.676981 too 289.8 100 268.9 too 269.9 100 49.0 2 54.8 2 46.2 2 191.2 2 249.9 2 239.1 2 153.8 10 140.8 10 138.0 10 321.0 10 306.8 10 305.4 10 180.1 100 176.0 100 170.2 100 J !ii j 1 s ijI j ii j\ i i i II!i f i 1 I f1 ? U jj 1=1 LlL 151.641086 T i o 0 2.18081689 - ae . t ? 151.315862 2.17988446 191.29506 2.28170375 966.06457 2.98500615 1212.13214 3.08354997 910.12507 2.95910108 2382.72209 3.37707339 2363.6275 3.37357903 2264.43015 3.35495893 5207.9333 3.71666541 5135.5299 3.71058526 5167.6981 3.71329713 28984.2339 4.46216183 26891.0326 4.42960748 26991.5171 4.4312273 98.0234 1.99132976 109.688412 2.04016075 1.9989094 92.307648 1.96523769 382.498934 2.58263023 499.850758 2.69884036 2.65371018 478.255482 2.67965996 1537.57668 3.18683735 1408.05483 3.14861957 3.15849757 1380.49807 3.1400358 3209.84698 3.50648433 3067.92472 3.4868447 3.492755 3054.47082 3.48493598 18011.5457 4.25555098 17602.9055 4.24558436 4.24402235 17018.9084 4.2309317 ii !} |[ 1 1i 1\ J i \ \\ 2.5117 2.4893 2.4858 2.4932 2.5126 2.4841 2.497 2.4851 2.4867 2.5197 2.5023 2.5014 2.5000 2.5086 2.4894 2.5032 2.4944 2.4915 2.4779 2.4904 2.5058 2.5149 2.515 2.5018 2.4835 2.4937 2.4917 2.5096 2.4812 2.4857 3 1! j :i li1 I i 4 i 1 i 1! ! 1 - !8 i1 1 : i" ! 1 1 \ I1 l s a! sl 1i 3I t Ji -, ff ' ' ] 1i f f o - - a e i jl _ i_ 0.0125 1.733681 0.238969 - 0.0125 1.750915 0.243265 0.0125 0.0125 0.0125 0.0125 0.0125 1.552342 0.190987 5.18377? 0.714646 3.919585 0.59324 5.484255 0.739118 13.10211 1.117341 0.0125 0.0125 0.0125 0.0125 13.2609 13.751 23.773 24.29999 1.122573 1.138334 1.376084 1.385506 0.0125 24.14799 1.382881 0.0125 0.0125 0.0125 105.0788 2.021515 115.1487 2.061259 115.5323 2.062703 0.0125 0.0125 0.0125 2.007314 0.302615 1.955939 0.291355 0.301584 2 045416 0.310782 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 8.159637 0.911671 7.52966 0.876775 0.869584 7.591111 0.880305 17.20954 1.235769 17.85261 1.251702 1.248259 18.08449 1.257306 0.0125 34.17633 1.533725 0.0125 34.74794 1.540929 1.538925 0.0125 34.84333 1.54212 0.0125 0.0125 0.0125 159.3304 2.202299 163.2128 2.212754 2.211593 165.8541 2.219726 PFOS Adosrh/Desorb Page 220 of 703 Page 3 o f 16 3M Environmental Laboratory BACK TO MAIN Study E00-1311 R010312 R010312 R010312 R010312 R010312 R010312 R010312 R010312 R010312 H010405int HO1O405int H010405int R010412 R010412 R010412 R010412 R010412 R01O412 R010412 R010412 R01O412 R010412 R010412 R010412 R010412 R010412 R010412 R010412 R010412 R010412 RUSH0074.D RUSH0075.D RUSH0076.D RUSH0078.D RUSH0079.D RUSH0080.D RUSH0O86.D RUSHD07. D RUSH0088.D HILL0059.D HILL0060.D HILL0061.D RUSH0032.D RUSH0033.D RUSHQ034.D RUSH0040.D RUSH0041.D RUSH0046.D RUSH0048.D RUSH0049.D RUSH0050.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0060.D RUSH0061.D RUSH0062.D RUSH0064.D RUSH0065.D RUSH0066.D Adsorption Isotherms 1311-5112 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 Adsorption !, I plot to determino K end n v. il 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 500 500 500 22000000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 t 62.4 61.1 66.1 324.3 337.1 303.4 200.5 177.7 204.6 437.953237 503.530246 423.370937 235.149546 235.642534 230.804348 24.842763 18.057138 25.246348 112.234056 133.554484 135.817446 85,185002 76.528101 75.760492 157.041946 155.224502 154.501564 109.207528 99.477125 96.43578 2 124.769652 2.09610896 2.4938 2 122.284226 2.08737045 2.522 2 132.259912 2.12142823 2.5133 22 648.68341 2.81203279 674.288876 2.828846 2 .5Q25 2 .4687 2 606.715152 2.78298484 2.4952 10 2005.16531 3 30215018 2 .4949 10 1777.00509 3.24968867 2.4973 10 2046.33166 3,31097602 2 .4971 10 4379.53237 3.64142774 2 .5098 10 5035.30248 3.70202556 2.5067 10 4233.70937 3.62672104 2 .4949 100 23514.9546 4.37134414 2.4978 100 23564.2534 4.37225368 2.4892 100 23080.4348 4.36324399 2.507 2 49.685526 1.69622989 2.4862 2 36.114276 1.55767891 1.65237912 2.5069 2 50.492696 1.70322856 2.4965 22 224.468112 2.35115465 2 .4891 267.108965 2.42668847 2.40394289 2.4995 2 271.634892 2.43398556 2.5191 10 851.85002 2.93038314 2.4977 10 765.28101 2.88382094 2.89787562 2.5107 10 757.60492 2.87944279 2.4999 10 1570.41946 3,19601567 2.5016 10 1552.24502 3.19096028 3.19196961 2.5128 10 1545.01564 3.18893288 2.4954 100 10920.7528 4.03825258 2.4892 100 9947.7125 3.99772323 4.006738 2.4837 100 9643.578 3.9842382 2.5041 0.0125 0.0125 0.0125 00125 0.0125 0.0125 0.0125 0.0125 0.Q12S 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 1.880816 0.274346 1.872104 0.27233 1.828607 0.26212 6 .749B33 0.829293 6.658653 0.823386 6.979826 0.843845 15.00478 1.17623 16.1324 1.207699 14.76549 1.169836 27.99261 1.447043 24.75714 1.3937 28.89039 1.460753 132.5419 2.122353 132.7522 2.123042 134.222 2.127824 2.26407 0.35489 2.313045 0.364184 0.35713 2.250687 0.352315 8.916536 0.950196 8.666188 0.937828 0.940441 8.576303 0.9333 20.75985 1.317224 21.08336 1.32394 1.322587 21.21282 1.326598 42.12095 1.624498 42.02361 1.623493 1.624958 42.35285 1.628883 196.244 2.292796 201.5757 2.304438 2.300469 201.4517 2 304171 PFOS Adosrb/Desort) Page 221 of 703 Page 4 o f 16 3M Environmental Laboratory Study E00-1311 BACK TO MAIN 5=5T Adsorption Isotherms plot to determine K end n V,, lC " Vaq) PFOS Adosrb/Desorb R010412 R010412 R010412 R010412 RD10412 R010412 R010412 R01Q412 R010412 H010405int H010405int H010405int H010329 H010329 HO10329 HO10329 H010329 H010329 H010329 HO10329 HO10329 H010329 HO10329 H010329 HO10329 HO10329 H010329 H010329 H010329 HO10329 RUSH0Q76.D RUSH0077.D RUSH0078.D RUSH0084.D RJSH0065.D RUSH0066.D RUSH0088.D RUSH0089.D RUSH0090.D HILL0063.D HILL0064.D HILL0065.D HILL0104.D HILL0105.D H1LI0106-D HILL0116.D HILL0117.D HILL0118.D HILL0120.D HH.LQ121.D HILL0122.D HILL0124.D HIU0129.D HILL0130.D HILL0132.D HILL0133.D HILL0134.D H1LL0136.D HILL0141.D HILL0142.D 1311-5148 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 1311-5167 1311-5168 1311-5169 1311-5170 1311-5171 1311-5172 1311-5173 1311-5174 1311-5175 1311-5176 1311-5177 1311-5178 1311-5179 1311-5180 11 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 1QQOQ 50000 50000 50000 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 123.282427 90.083398 152.507888 470.275971 481.768175 461.552835 259.294489 273.244648 260.405148 56.237274 86 08401 87.643563 289.002164 258.39539 266.033394 79.696368 93.228986 94.960207 344.862674 340.759666 365.047259 203.797939 187.700144 194.510276 371.323196 371.174203 389.708739 183.266658 178.291848 179.600507 2 246.564854 2.39193117 2.4887 2 180.166796 2.25567476 2.4762 2 305.015776 2.4843223 2.5142 2 940.551942 2.97338278 2.4733 2 963.53635 2.9838681 2.4881 2 923.10567 2.96525142 2.5389 10 2592.94489 3.41379329 2.4954 10 2732.44648 3.43655166 2.48B 10 2604.05148 3.41564957 2.4932 100 5623.7274 3.75002426 2.4859 100 8608.401 3.93492249 2.4782 100 8784.3563 3.94370994 2.4815 100 28900.2164 4.46090109 2.4861 100 25839.539 4.41228476 2.4832 100 26603.3394 4.42493616 2.5025 2 159.392736 2.20246853 2.4857 2 186.457972 2.27058096 2.25054038 2.4859 2 189.920414 227857165 2.483 2 689.725348 2.83867619 2.5149 2 681.519332 2.83347818 2.84517782 2.5171 2 730.094518 2.86337909 2.5098 10 2037.97939 3.30919979 2.5183 10 1877.00144 327346461 3.29053565 2.5071 10 1945.10276 3.28894255 2.481 10 3713.23196 3.56975208 2.4972 10 3711.74203 3.5695777B 3.57669 2.4823 10 3897.08739 3.59Q74Q14 2.5008 100 18326.6658 426308346 2.479 100 17829.1848 425113149 4.25617417 2.483 100 17960.0507 4.25430756 2.4772 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 1.272929 1.614536 0.208048 0.969415 -0.01349 5.354426 0.728713 5.207104 0.716596 5.301973 0.724438 12.05746 1.081256 11.39245 1.056617 12.01242 1.07963 22.00547 1.342531 7.019202 0.846288 6.123533 0.787002 106.0888 2.025669 121.6196 2.085004 116.8664 2.06769 1.712834 0.233715 1.576602 0.197722 0.208281 1.561013 0.193406 6 512558 0.813752 6.547618 0.816083 0.010292 6.324734 0.801042 14.70248 1.167391 15.57077 1.19231 1.182327 15.39146 1.18728 31.46909 1.497884 31.66548 1.500586 1.494279 30.5048 1.484363 159.7082 2.203327 161.9554 2.209395 2.207121 161.6742 2.208641 p 1 2 Page 222 of 703 Page 5 of 16 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 H010412 H010412 HQ10412 H010412 H010412 HO10412 H010412 H010412 HO10412 HO10329 HO10329 H010329 H010329 H010329 HO10329 H010412 HO10329 H010329 H010329 HILL0031.D HILL0032.D HILL0033.D HILL0035.D HILL0036.D HILL0Q37.D HILL0039.D HILL0040.D HILL0045.D HILL0164.D H1LL0165D HILL0170.D HILL0172.D HILL0173.D HILL0174.D H1LL0047.D HILL0048.D HILL0O49.D HILL0051.D HILL0052.D HILL0053.D HILL0059.D HILL0060.D HILL0061.D HILL0063.D HILL0064.D HILL0065.D HILL0204.D HILL0205.D HLL0206.D C*%(iqTAdsorption f jl fj Adsorption Isotherms ------- v.plot to determine K16an-d;^n ,) 1311-5184 1311-5185 1311-5186 1311-51871311-5188 1311-5189 1311-5190 1311-5191 1311-5192 1311-5193 1311-5194 1311-5195 1311-5196 1311-5197 1311-5198 1311-5202 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 in i 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 500 500 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 5Q00Q 50000 50000 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 11.327739 14.704513 < too 587.353982 375.628336 624.651539 25.400564 16.589279 20.475802 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 <10.0 14.126747 11.420901 < 10.0 14.879531 23.895092 24.461872 8.466139 7.309995 7.707909 2 N/A N/A 2.4775 2 N/A N/A 2.5291 2 N/A N/A 2.4698 2 N/A N/A 2.5167 2 N/A N/A 2.4888 2 N/A N/A 2.5137 10 113.27739 2.05414323 2.4922 10 147.04513 2.16745065 2.4678 10 N/A N/A 2.4517 10 5873.53982 3.76889992 2.5128 10 3756.28336 3.57475835 2.4925 to 6246.51539 3.79563781 2.5286 100 2540.0564 3.40484336 2.5086 100 1658.9279 3.21982751 100 2047.5802 3.31124092 2.5167 2,4766 2 N/A N/A 2.5318 2 N/A N/A N/A 2.4861 2 N/A N/A 2.5256 2 N/A N/A 2.5299 2 N/A N/A N/A 2.5129 2 N/A N/A 2.5416 10 141.26747 2.15004217 2.507 10 114 20901 2.05770037 2.10387127 2.5432 10 N/A N/A 2.5467 10 148.79531 2.17258924 2.5184 10 238.95092 2.37830871 2.31312921 2.4757 10 244.61872 2.38848969 2.5102 100 846.8139 2.92778798 2.537 100 730.9995 2.86391708 2.89288055 24996 100 770.7909 2.88693658 2.5362 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.012S 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A 24.51008 1.389345 24.58138 1.390606 N/A N/A 20.5272 1.31233 31.31252 1.495718 18.55515 1.268465 236.4862 2.373806 240.1015 2.380395 242.0275 2.383865 N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A N/A 24.22583 1.384279 24.01399 1.380464 N/A N/A 48.89615 1.689275 49.28429 1.692708 48.57871 1.686446 242.1816 2.384141 246.3844 2.391613 242.6327 i1 PFOS Adosrto/Desorb Page 223 of 703 P a ge 6 o f 16 Study EOO-1311 Adsorption isotherms BACK TO MAIN PFOS Adosrb/Desort 3M Environmental Laboratory Page 224 of 703 Page 7 of 16 Study EOG-1311 Adsorption Isotherms BACK TO MAIN PFOS Adosrto/Desorto 3M Environmental Laboratory Adsorption Isotherms, Sludge 0 0.5 1 1.5 2 2.5 3 3.5 loflCaq clay day ioam sandy loam sediment sludge Log Kads -1.2515 -1.3762 -1.0369 -2.0261 -1.246 Kads 0.05604024 0.04205329 0.09185441 0.00941673 0.05675446 1/n 0.884 0.8407 0.8288 0.9885 1.2581 n 1.131222 1.189485 1.206564 1.011634 0.794849 Page 8 of 16 Page 225 of 703 3M Environmental Laboratory BACK TO MAIN Study EQO-1311 Adsorption Isotherms sorption/Desorption % i ft EOO-1311-5004 EOO-1311-5005 EOO-1311-5006 EOO-1311-5008 EOO-1311-5009 EOO-1311-5010 EOO-1311-5011 E00-1311-5012 EOO-1311-5013 EOO-1311-5014 EOO-1311-5015 1311-5016 1311-5017 1311-5018 I - f t - ' V ' " M ? W ^ 7 EOO-1311-5022 R010312 RUSH0094.D 11.4 EOO-1311-5023 EOO-1311-5024 R010312 R010312 RUSH0095.D RU5H0100.D 10.7 12,0 1311-5025 R01Q312 RUSH0102.D 27.7 1311-5026 R010312 RUSH0103.D 28.9 1311-5027 R01Q312 RUSH0104.D 23.3 1311-5028 . R010312 RUSH0106.D 56.0 1311-5029 R010312 RUSH0107.D 31.7 1311-5030 R01Q312 RUSH01Q8.D 57.8 1311-5031 1311-5032 I R010312 R010312 RUSH0114.D RUSH011S.D 65.7 66.9 1311-5033 1311-5034 1311-5035 1311-5036 | R010312 R01Q312 R01Q312 R010312 RUSH0116.D RUSH0118.D RUSH0119.D RUSH0120.D 71.2 144.7 235.1 189.2 s i M ft- mms u If ! il- i I I; ! !i j i n n ! mmC??m'Ms i il ! i 2 22.859932 2 21.361226 2 23.972482 2 55.333452 2 57.871888 2 46.678566 2 111.971874 2 63.459182 2 115.682498 2 131.442794 2 133,71768 2 142.403456 2 289.416628 2 470.189976 2 378.410064 PFOS Adosrb/Desorb Page 2 2 6 o f 7 0 3 Page 9 o f 16 Study EOO-1311 Adsorption Isotherm* BACK TO MAIN PFOS AdosrtVDesorb 3M Environmental Laboratory 1311-5041 1311-5042 1311-5043 1311-5D44S1 1311-5045 1311-5046 1311-5047 1311-5048 1311-5049 1311-5050-1S 1311-5051 1311-5052 1311-5053 1311-5054 1311-5058 1311-5059 1311-5060 1311-5061 1311-5062 1311-5063 1311-5064 1311-5065 1311-5066 1311-5067 1311-5068 1311-5069 1311-5070 1311-5071 1311-5072 R010312 R010312 R010312 R010312 H010313 H010313 H010313 H010313 H010313 H010313 H010313 HO10313 R010402a R010402a R010402a RUSH0130.D RUSH0131.0 RUSH0132-D RUSH0134.D HILt.0031 D HILL0032.D HILL0034.D HILL0035.D HILL0036.D HILL0038.D HILL0039.D HILL0040.D RUSH0041.D RUSH0042.D RUSHD043.D 10.9 11.9 29.0 75.7 66.6 53.4 114.7 120.2 188.2 436.9 417.8 333.4 450.789701 305.703229 339.490983 2 21.87378 1.33992384 5.3445614 0.72791207 2 23.09696 1.378379002 1.493715829 5.27526343 0.72224415 0.72042173 2 57.922146 1.762844644 5.14172636 0.71110896 2 151.367756 2.180033373 20.8700746 1.319524 2 133.222922 2.124578955 2.111184944 20.8068022 1.31820534 1.31921844 2 106.891336 2.028942505 20.8894009 1.31992599 2 229.32978 2.360460454 50.9477454 1.70712497 2 240.421642 2.380973559 2.439004249 51.5790063 1.71247297 1.70871815 2 376.338572 2.575578733 50.8811005 1.7065565 2 877.85928 2.943424904 98.176486 1.99200748 2 835.577968 2.92198698 2.896452664 97.403101 1.98857278 1.99380444 2 666.72403 2.823946108 100.191999 2.00083304 10 4507.89701 3.653973985 475.813128 2-67743642 10 3057.03229 3.485300026 3.556700752 480.602804 2.6817863 2.67754223 10 3394.90983 3.530828244 471.415624 2 67340397 Page 10 o f 16 Page 227 of 703 Study EOO-1311 Adsorption Isotherm PFOS Adosrb/Desorb 3M Environmental Laboratory Page 228 of 703 Page 11 of 16 Stuify EOO-1311 Adsorption Isotherms PFOS Adostb/Desotb 3M Environmental Laboratory Page 229 of 703 Page 12 of 16 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Adsorption Isotherms if 1 i ...TOTOffr-Sampfci Description 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 1311-5167 1311-5168 1311-5169 1311-5170 1311-5171 1311-5172 1311-5173 1311-5174 1311-5175 1311-5176 1311-5177 1311-5178 1311-5179 1311-5180 R010402b R010402b R010402b R010402b R010402b RO10402b R010402b R010402b R010402b R010402b R010402b RO10402b RO10402b R010402b RUSH0120D RUSH0121.D RUSH0122.D RUSH0124.D RUSH0125.D RUSH0126.D RUSH0128-O RUSH0129.D RUSH0134D RUSH136.D RU5H0137.D RUSH0138.D RUSH0140.D RUSH0141.D RUSH0142.D 42.932438 43.120798 42.621787 160.750438 149.070084 165.740897 380.66422 374.889478 379.287662 174.993474 163.325091 174.345547 74.086291 79,446466 70.91215 - i l \ Jy H; , !l s a i S V' i i V . .0 > i - :,,0 4 `- | - __ 1__ -- L , 2 85.864876 1.933815547 3.82579656 0.58272187 2 86.241596 1.935716785 1.933397994 3.48562156 0.54228023 0.55414187 2 85.243574 1.93066165 3.44685883 0.5374235 2 321.500876 2.507182161 14.7804527 1.16968774 2 298.140168 2.474420492 2.500687444 15.0004346 1.17610384 1.16625972 2 331.481794 2.520459681 14.2228812 1.15298758 2 761.32644 2.681572053 33.2462776 1.52174303 2 749.778956 2.874933247 2.878834671 35.2992039 1.54776491 1.53520511 2 758.575324 2.879998711 34.3642923 1.5361074 10 1749.93474 3.243021853 69.8251162 1.84401167 10 1633.25091 3.213052909 3.232495207 70.3787407 1.84744149 1.84040647 10 1743.45547 3.241410859 67.5719189 1.82976625 100 7408.6291 3.869737853 358.559734 2.55456152 100 7944.6466 3.900074583 3.87351103 362.13999 2.55887648 2.55846465 100 7091.215 3.850720653 364.716956 2.56195595 PFOS Adosrb/Desorb Page 230 of 703 Page 13 o f 16 < s o o* < C 3M Environmental Laboratory BACK TO MAIN Study EOO-1311 Adsorption Isotherms -------- S S S m s .. -, is s a i 'Y.Y: ' m i11 %.! 1 IS i H i h Mr,: !, 'i.i ! 1.1 j a ^d || ... * ; j 'i" "=*! * ! 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Isotherms -- Least Squares Fit LogCaq day d ay loam sandy loam sediment sludge Log Kdes -0.653 -1.0641 -0.9611 - 1 .4 0 8 6 1 4693 Kdes 0.222330989 0.082394837 0.104447969 0.03901216 29 .4 64 56 27 1 1/n 0.935 0.9544 1.012 1.0164 0.3272 n 1.069516717 1.047778709 0.986142292 0.98386462 3.056234719 P age 16 of 16 Page 233 of 703 BACK TO MAIN PFOS Adosrb/Desorb 3M Environmental Laboratory BACK TO MAIN Study EOO-ASM Desorption isotherms Tier III "Mass Balance Calculations" Run H010316 H010316 H01D316 H010316 H010316 H010316 H010316 H010316 H010316 R010320 RO10320 R010320 R010320 R010320 R010320 H010316 H010316 H010316 H010316 HQ1Q316 H010316 H010316 H010316 RO10320 RO10320 R010320 R010320 R010405 RO1040S R010405 Sanple Dat* Fie H ILL0064.D H LL0065.D H ILL0066.D H ILL095.D H 1L L 0 96.D H ILL0101.D HILL0131.D HILL0132.D HILL0133.D RUSH0055.D RUSH0056.D RUSH0061.D RUSH0083.D RUSH0084.D RUSH0089.D HILL0068.D HILL0073.D HILL0074.D HILL0103.D H IL L 0 1 0 4 .0 HLLD105.D HILL0135.D HILL0136.D RUSH0033.D RUSH063.D RUSH0064.D RUSH0065.D RUSH0032.D RUSH33.D RUSH0034.D Sample Descriptor. -5 0 2 2 -S 3 -5023-S 3 -5 0 2 4 -S 3 -5025-S 3 -5 0 2 6 -S 3 -5 0 2 7 -S 3 -5028-S3 -5029-S3 -5030-S3 1311-5031-S3 1311-5032-S3 1311-5033-S3 1311-5034-S3 1311-5035-S3 1311-5036-S3 -5058-S3 -5059-S3 -5060-S3 -5061-S3 -5062-S3 -5063-S3 -5064-S3 -5065-S3 13113-5066-S3 1311-5067-S3 1311-5068-S3 1311-5069-S3 1311-5070-S3 1311-5071-S3 1311-5072-S3 Adsorb Sta -Llr-;,-', i p r V0 - H ' 'j l .a ; ; S :ir: *1 t ''- . i f : f: 1 ?: : ; i l V' 1L aJ"J - 1 ! J; a. '* v : ' ..r; jj l! i 0 0125 500 CO 373 655S5 0.0125 500.00 386.1880H 0.0125 500.00 400.6 17000 0.0125 2000.00 1509.3353 0.0125 2000.00 1529.15715 0 0125 2000 00 1432.64531 0.0125 5000.00 3913.70145 0.0125 5000.00 2300.94744 0.0125 5000.00 3873.38636 0.0125 10000.00 8281.3209 0.0125 10000.00 8510 8629 0.0125 10000.00 8037.8359 0.0125 50000.00 40454.91 0.0125 50000.00 41416.3251 0.0125 50000.00 43397.8954 0.0125 500 63 66312 0 0125 500 66 302058 0.0125 500 65 5835 0.0125 2000 270.25587 0 0 1 2 5 2000 282.215634 0.0125 2000 285.940358 0.0125 5000 831.7832 0.0125 5000 778.17175 0.0125 5000 770.50456 0.0125 10000 1705.32634 0.0125 10000 1871.04255 0 0125 10000 1718.79339 0.0125 50000 10122.5113 0 0125 50000 10329.5006 0.0125 50000 10928.5554 2l i . I. |I c s If fl 11 ' 3 %I I SfI I ! w 4.670694375 4 .827350175 5 .0077226 19.99169125 19.11446438 17 90806638 48.92126813 2 8 .7 6 1 8 4 3 48.4173295 103.5165113 106.3857863 1 0 0 .47294B 8 505.686375 517 7040638 5 4 2 .4736925 0 .7 9 5 7 8 9 0.853775725 0.81979375 3 .378198375 3.527695425 3.574254475 10.39729 9.727146875 9.743807 22.44157925 23.38803188 2 1 .45991738 126.5313913 129.1187575 136.5819425 E x tr a c ti o n r dii ' M o Balance i. S i i i; H pi : ita 22 859932 2 1 .3 6 1 2 2 6 23.972482 55.333452 57.871888 46.678566 111.971874 63459182 115.682498 131.442794 133 71768 142 403456 2 8 9 416628 470.189976 378.410064 2 1 .8737B 23 69896 57.922146 151.367758 133.222922 106 891336 22 9 32978 240.421642 376.338572 877.85928 835.577968 666 72403 4507.89701 3057.03229 3394.90983 !1 ?1 fi !s '. .. Pl i II 1! s! V ! li 'S JS S 8 #3 J S3 0.28574915 . 0.267015325 0.299656025 069166815 0.7233986 0.583482075 1.399648425 0.79323977S 1.446031225 1 643034925 1.671471 1.7800432 3.61770785 5 .8773747 4 .7301258 0.27342225 0.298737 0.724026825 1 89209695 1.665286525 1.3361417 2 86662225 3.005270525 4.70423215 10.973241 10.4447246 8.334050375 56.34871263 36.21290363 4 2 .4363728 8 ! itS 10 ) II J 1 f2 I s 3 3 5 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 00120 0.0120 0.0120 0.0120 0.0120 0 0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 L iliJ < 5 .0 < 5 .0 < 5 .0 < 5 .0 < 5 .0 < 5 .0 5.6 <5,0 6.0 6.217634 5,939702 7 .8 7 1 9 2 4 22.65781 16.95932 46.22885 42.6 48.9 57.0 159.8 2032 180.8 461.1 285.5 3 4 6 .5 2 6 8 2 9 8 .1 4 4 7 360.5895 3 3 7 .6 6 2 41.69038 35.16084 68.33123 E 200 200 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2 00 2.00 2.00 2.00 2.00 2.00 2 .0 0 2.00 2 .00 2.00 2.00 200 2.00 100.00 100.00 100.00 21 l . II : 8 dt n . I5 :f fi : II !I l i Tf r ii* I H -- 31 li 5 |3 il: < 10 t 58 < 0 12 < 10 < 0 12 < 10 <0.12 <10 <0.12 < 10 < 0.12 < 10 <0.12 11.162706 0.1339525 < 10 <0.12 12051664 0.14461997 12 435268 0.14922322 11 879404 0.14255285 15 743848 0.18892618 45.315612 0 5437B734 33.918642 0.4070237 92.457708 1.1094925 85.102702 1.02123242 97.702736 1.17243283 113.917176 1.36700611 319.525044 3.83430053 406.39942 4 .87679304 361.644534 4.33973441 922.14921 11.0657905 570906 6.850672 693.053616 831664339 596.289326 715547191 721.17904 8 .65414848 675 32394 8 .10388726 4169 0375 50.02845 3518.084 42.193008 6833 1228 81.8974736 * ii 1: 2 1 79.3% 81.5% 8 4 .9% 82.7% 79.4% 74.0% 80.7% 47.3% 80 0% 84.2% 86.6% 82 0% 8 1 .6% 83.8% 87.7% 33.4% 37.2% 46 6% 3 6 .4% 40 .3% 37 .0% 3B.9% 31.3% 36.4% 325% 34.0% 3 0 .3% 37.3% 33.5% 4 1 .8% PFOS Adsorto/Desortj Page 234 of 703 Page 1 of 3 Q j'h C Study E00-1311 Desorption Isotherms BACK TO MAIN PFOS Adsorto/Desorb 3M Environmental Laboratory Run H010316 H010316 M010316 H010316 H010316 H010316 R010320 R010320 R010320 R010405 R010405 R010405 R010405 R010405 R010405 H010316 H010316 H010316 H010316 H010316 H010316 R01O4Q5 R01040S R010405 R01O405 R010405 RO1O405 R010405 R0104 05 R010405 HILL0077.D H IL L U U / .IJ HILL0107.D H IL L O 1O 0.D HILL0109.D RUSH0035.D RUSH0036.D RUSH0037.D RUSH0040.D RUSH0041 D RUSH0046.D RUSH0048.D RUSH0049.D RUSH0050.D HILL0080.D Tube broke HILL0081.D HJLL0115.D HILL0116.D HILL0117.D RUSH0052.D RUSH0053.D RUSH0054 D RUSH0060.D RUSH0061.D RUSH0062.D RUSH0064.D RUSH0065.D RUSH0066.D -5095-S3 -5096-S3 -5097-S3 -5098-S3 -5099-S3 1311-5100-S3 1311-5101-S3 1311-5102-S3 1311-5103-S3 1311-5104-S3 1311-5105-S3 1311-5106-S3 1311-5107-S3 1311-5108-S3 -5130-S3 E00-1311-5131 -5132-S3 -5133-S3 -5134-S3 -5135-S3 1311-5136-S3 1311-5137-S3 1311-5138-S3 1311-5139-S3 1311-5140-S3 1311-5141-53 1311-5142-S3 1311-5143-S3 1311-5144-S3 0.0125 0.0125 0.0125 0.0125 0.0125 0 .012$ 0 0125 0.012$ 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0 0125 0.0125 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 2000 2000 2000 5000 5000 SOCO 10000 10000 10000 50000 50000 50000 109.688412 92.307646 362 498934 499.850750 476.255482 1537.57868 1408.05483 1380.49807 3209.84698 3067.92472 3054.47082 18011.5457 17602.9055 17018.9084 49.665526 36.114276 50.492696 224 468112 267.108968 271.634692 851.85002 765.26101 7S7.6Q432 1570.41 946 1552.24502 1545.Q1564 10920.7528 9947.7125 9643.578 1.37110515 1.1538456 4,781236675 6 .2 48134475 5 .978183525 19.2197335 17.60068538 17 .25622586 40.12308725 3 6 .349 059 38 .18088525 225.1443213 220.0363188 2 1 2 .736355 0.621069075 0 .4 5 1 4 2 8 4 5 0.6311587 2 .8058514 3.3388621 3 .39543615 10.64812525 9.566012625 9.4700615 19.83024325 19 40306275 1 9 .312 6355 136 50941 124.3464063 120.544725 2 5 4 .19996 252.13575 2 7 1 .063 586 669.374834 654.78009 684.0531 1218.44173 1272.33095 1336.30265 6781 1262 8272.7361 8430.3464 53 352096 214.226632 222.57563 212.447768 579.746028 499.345734 552.023624 1053.77362 1141.23143 1032.39784 4919.27102 5090.61312 5130.07645 <1H7Q')<;7,5 0.866075775 3 .1774995 3 .151696875 338823485 8.367185425 8.184751125 8.55073875 15.23052163 15.90413688 16.70378313 84.7640775 78.40920125 105.38683 0.66725075 2.6776329 2.782195375 2.855S971 7.24682535 6 .241821675 8 .9003703 13.17217025 14.26539288 12.904973 6 1 .4908877 5 63 632664 6 4 .1259556 3 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 00120 0.0120 0.0120 0.0120 0.0120 0.0120 57.9 161.9 173.0 194.7 467.7061 3 7 1 .4 1 9 485.0679 < 25 <25 <25 50.04657 61.22001 65.68839 111.6 393.7 375.2 361.3 182.5679 190.9566 242.2879 <25 <25 <25 <25 <25 <25 2.00 2.00 2.00 2.00 2.00 2.00 2.00 100.00 100.00 100.00 100.00 100.00 100.00 2.00 2.00 2.00 2.00 2.00 2.00 10.00 10.00 10.00 1000.00 1000.00 1000.00 1000.00 1000.00 1000.00 115.766982 323.876642 345.931234 389 428652 935 41224 742.836078 970.135824 <2500 <2500 <2500 5004.6567 6122.001 6568.8394 0223.252154 197.580186 787.427278 750.306384 722.513148 1825.67883 1909.56582 2422.87857 <25000 <25000 <25000 <25000 <25000 <25000 I 38920378 3.8865197 4.15117481 4.67314382 11.2249469 891405694 II 6416299 <30 73.464012 78.8260728 02 .67902 58 5 2 .37096 22 3 9 44912734 9 00367661 8.67015778 21.908146 22 9147898 29 0745428 <300 53.6% 54.5% 47.4% 54 2% 56.2% 6 2 ,1% 55.5% 59.9% 4 4 .3% 4 3 .4% 4 3 .9% 5 9 .2% 59.5% 6 3 .5% 6 3 .5% N/A 58.7% 59.7% 60 5% 58.9% 63.7% 6 2 .0% 72.7% 26.2% 26.9% 25.8% 31.7% 30.1% 29.5% Page 2 of 3 Page 235 of 703 Study E00-1311 Desofption Isotherms BACK TO MAIN PFOS Adsorb/Desorb 3M Environmental Laboratory Run H010316 H010316 H010316 H010316 H01D316 R010320 R01D320 R010320 R010405 R010405 R010405 R010405 R010405 R010405 H010316 H010316 H010316 H010316 H010316 H010316 RO10320 R010320 R010320 R010320 R010320 RO10320 R010405 RC10405 R010405 HILL0068.D t iu_u>juaa,u HILL0119.D HILL0120.D H IL L 0 1 2 1 .D RUSH0047.D RUSH0048.D RUSH0049.D RUSH0068.D RUSH0069.D RUSH0074.D RUSH076.D RUSH0077.D RUSH0078.D H IL L 0 0 9 1 .0 HILL0092.D HILL0093.D HILL0123.D HILL0124.D HILL0129.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0080.D RUSH0081.D RUSH0082.D -5167-S3 -5-S3 -5169-S3 -5170-S3 -5171-S3 1311-5172-S3 1311-5173-S3 1311-5174-S3 1311-5175-S3 1311-5176-S3 1311-5177-S3 1311-5178-S3 1311-5179-S3 1311-5180-S3 -5202-S3 -5203-S3 -5204-S3 -5205-S3 -5206-S3 -5207-S3 1311-5208-S3 1311-5209-S3 1311-5210-S3 1311-5211-S3 1311-5212-S3 1311-5213-S3 1311-5214-S3 1311-5215-S3 1311-5216-S3 0.0125 0 .0 1 2 5 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0025 0.0125 0.0125 0.0125 0 0125 00125 0.0125 0.0125 0 0125 0.0125 0.0125 0.0125 0.0125 0.0125 0.0125 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 500 2000 2000 2000 5000 5000 5000 10000 10000 10000 50000 50000 50000 186.457972 189.9204 H 689.725348 681 519332 730.094518 2037.97939 1877.00144 1945.10276 3713.23196 3711.74203 3897.06739 18326.6658 17829.1848 17960.0507 N/A N/A 141.26747 114.20901 WA 148.79531 23695092 244.61872 846.8139 730.9! 2.33072465 2.374005175 8 62156685 8.51899165 9 .126181475 2 5 .47474238 23 462516 24 .3137845 46 4153995 46.39677538 4 8 .71350236 229.0833225 222.86481 2 2 4 .50063 38 N/A 1.765843375 1.427612625 N/A 1.859941375 2.9668865 3.057734 10.58517375 0.13749375 9 63488625 86.241596 85.243574 321.500876 290.140168 331 481794 761.32844 7 4 9 .778956 758.575324 1749.93474 1633.25091 1743.45547 7408.6291 7944 6486 7091.215 N/A 18.140072 18.930076 14.799368 3 2 .934802 4 0 .808712 3 9 .651664 210.603886 185.434078 164.961598 1.07801995 1 065544675 4.01876095 3 .7267521 4 143522425 9.5166055 9 37223695 9.48219155 2 1 .8741842 5 20.41563636 21.79319338 92.60786375 99.3080825 88.6401875 N/A 0.1849921 0.411685025 0.51010B9 0.4956458 2 .632548575 2 .317925975 2.062019975 0 0190 0.0120 0.0120 0 0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 0.0120 PQ 1 657 2 98 .3 2 6 7 .4 327.9 >501 491.643 496.1706 <25 <25 <25 <25 <25 <25 36.3 2 5 .2 30.1 9 7 .6 127.8 9 8 .9 332.321 2 4 4 .5963 251.8495 4 9 0 .2051 494.7347 >501 4 7 .2 5497 57.65922 6 6 .7 7 0 6 7 2.00 2 .0 0 2.00 2.00 2.00 2.00 2.00 1000.00 1000.00 1000.00 1000.00 1000.00 1000.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2 .0 0 2 .0 0 2.00 100.00 100.00 100.00 m l 252322 131.385636 596.55581 534 720604 655.794326 >1002 983.285956 992.34126 <25000 <25000 <25000 <25000 <25000 <25000 72.665522 5 0 .441 822 60.17112 195.243738 255.649826 197.725206 664 64198 489.192588 503 699054 980 410204 989 469372 N/A 4725.4966 5765 9224 6677.067 I. 57662763 7.15866972 6.41664965 7.86953191 > 12.024 II. 11.9080951 <300 <300 087198626 0.60530186 0.72205344 2 34292486 3.06779791 2.37270247 7.97570376 5.87031106 604438665 11.7649224 11.8736325 N/A 56.7059592 69.1910688 80.124804 80.3% 7 9 .2% 7 4 .8% 84 6% 56.0% 7719.944%315 73.1% 54 6% 5 3 .4% 56.4% 51.5% 51.5% 5 0 .1% N/A 15.9% 12. 1% N/A 11. 2% 12.3% N/A 11.2% 12.9% 14.7% Page 3 of 3 Page 236 of 703 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: sOOl120a sOO1120b sOO1122a t0 1 0 1 2 2 S001211 1001215 S001207 H001214a&b t010123 tO10124 t010125 R010320 H010405ext H010405int H010404ext R010404ext R010405 R010402a&b HO10329 H010319a R010312 R010329a&b H010402a&b HO10222 RO10222 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 Sam ple Data File RUSH0032.D RUSH0033.D RUSH034.D RUSH0035.D RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0040.D RUSH0041.D RUSH0046.D RUSH0047.D RUSH0048.D RUSH0049.D RUSH0050.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.0 RUSH0060.D RUSH0061.D RUSH0062.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH0068.D RUSH0069.D RUSH0074.D RUSH0075.D RUSH0076.D RUSH0077.D RUSH0078.D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0082.D RUSH0083.D Sample D escription 1311-5070-S3 1311-5071-S3 1311-5072-S3 1311-5072MS-S3 1311-5091-S3 1311-5092-S3 1311-5093-S3 1311-5093MS-S3 1311-5103-S3 1311-5104-S3 1311-5105-S3 1311-5105MS-S3 1 3 11 -5 1 06-S 3 1311-5107-S3 1311-5108-S3 1311-5108MS-S3 1311-5136-S3 1311-5137-S3 1311-5138-S3 1311-5138MS-S3 1311-5139-S3 1311-5140-S3 1311-5141 -S3 1311-5141MS-S3 1311-5142-S3 1311-5143-S3 13 11-5144-S3 1311-5144MS-S3 1311-5175-S3 1311-5176-S3 1 3 1 1 - 5 17 7 -S 3 1311-5177MS-S3 1311-5178-S3 1311-5179-S3 1311-5180-S3 1311-5180MS-S3 1311-5214-S3 1311-5215-S3 1311-5216-S3 1311-5216MS-S3 Analytical Run Information*: Acceptable Quant Range: 25 - 1002ng/ml Calibration Curve r2: 0.9880787 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Rush Run ID: R010405 M easured C oncentration, ug/L 41.690375 35.16084 68.331228 268.971058 < 25 25.536054 <25 226.293398 < 25 < 25 < 25 221.075617 50.046567 61.22001 65.688394 266.885789 182.567883 190.956582 242.287857 422.825169 < 25 < 25 < 25 197.948699 < 25 < 25 < 25 199.992825 < 25 < 25 < 25 187.321981 <25 < 25 <25 191.566565 47.254966 57.659224 66.77067 243.807595 T h e o re tic a l M atrix Spike C o n c e n tra tio n , ug/L R e p lic a te Sample %RSD 200 200 - 200 9 . -200 200 200 200 200 200 200 36.31 N/A N/A 13.66 15.76 N/A N/A N/A N/A 17.06 M atrix Spike Recovery, % 100.32 113.15 110.54 100.60 90.27 98.97 100.00 93.66 95.78 88.52 D ilution Factor, Nx 10 100 100 100 2 2 2 2 100 100 100 100 100 100 100 100 10 10 10 10 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 100 100 100 100 3M Environmental Laboratory Cmc s/<r/6i Page 238 of 703 BACK TO MAIN Quality Control Sample Data S am ple Data File HILL0032.D HILL0033.D HILL0034.D HILL0035.D HILL0036.D HILL0037.D HILL0038.D HILL0039.D HILL0040.D HILL0041.D HILL0046.D HILL0047.D HILL0048.D HILL0049.D HILL0050.D HILL0051.D mucosa,p HILL0053.D HILL0054.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 H ILL0088.D HILL0089.D HILL0090.D HILL0091.D HILL0092.D Sample D escription 1311-4124-S2 1311-4125-S2 1 3 1 1 -4 126 -S 2 1311-4148-S2 1311-4149-S2 1311-4150-S2 1311-4124-S3 1311-4125-S3 1311-4126-S3 1311-4148-S3 1311-4149-S3 1311-4150-S3 1311-4124-S4 1311-4125-S4 1311-4148-S4 1311-4149-S4 ,1341-4150-S4* 1311-4124-S5 1 3 1 1- 4 1 2 5 -S 5 1311-4126-S5 1311-4148-S5 1311-4149-S5 1311-4150-S5 1311-4124-S6 1311-4125-S6 1311-4126-S6 1311-4126MS-S6 131-4148-S6 1311-4149-S6 1311-4150-S6 1311-4150MS-S6 1311-4124-S7 1311-4125-S7 1311-4126-S7 1311-4148-S7 1311-4149-S7 1311-4150-S7 1311-4124-S8 1311-4125-S8 1311-4126-S8 1311-4126M S-S8 1311-4148-S8 1311-4149-S8 1311-4150-S8 1311-4150MS-S8 Instrument: Hillary Run ID: H 010319a Measured C o n c e n tra tio n , ug/L < 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 78.0 213 6 < 2 .5 <2.5 <2.5 72.9 63.0 79.4 <2.5 <2.5 <2.5 2 3 5 .6 59.1 64.6 64.2 298.1 <2.5 <2.5 4.5 60.4 63.2 71.4 <2.5 2.5 <2.5 2 3 6 .3 58.6 62.8 36.4 296.8 Theoretical M atrix Spike C o n c e n tra tio n , ug/L R e p lic a te M atrix Spike Sample %RSD Recovery, % N/A 3.48 N/A 7.12 N/A 48.20 N/A 11.52 N/A 200 4 .90 200 N/A ' 117.78 116.99 8.86 N/A 200 26.99 207 1 1 8 .13 125.82 D ilution 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 Analytical Run Information*: Acceptable Quant Range: 2.5 - 1002ng/ml Calibration Curve i2: 0.9999964 Target Analyte: PFOS Internal Standard: THPFOS Point thrown out. Compared to the values obtained from other aliquots o f the same sample during this run (30.4,43.7, 79.4, 64.2, 71.4, and 36.4) the value obtained fo r the -S4 sample (212.6) is about three tim es higher. M ay be a bad injection. 3M Environmental Laboratory Page 239 of 703 BACK TO MAIN Quality Control Sample Data S a m p le D a ta F ile H IL U W 3 3 .P H IL L 0 0 3 .D H IL L 0 0 3 4 .P H IL L P 0 3 5 .P H IL L O Q 36.D H IL L 0 0 3 7 .P H IL L 0 0 3 B .P H IL L 003P .D H 1L L P 040.P M IU L 0 0 4 6 .P M L L 0 0 4 6 .P H IL L 0 0 4 7 .P h il l q o ib .d H IL L Q 049.t> H IL L P 0 5 0 .P H IL L 0 0 6 1 .D H IL L 0 0 5 3 .P H 1 L L 0053.P H IL L Q 8 5 4 .P H IL L 0 0 5 8 .D H IL L 0060. D H IL L 0 0 6 1 .D H IL L 0 0 6 3 .D H IL L 0 0 6 3 .D H IL L O Q 64.D H IL L 0 0 6 5 .D H IL L 0 0 6 6 .D H IL L 0 0 6 7 .D M IL L 0 0 6 8 .P W U .0 0 7 3 .D H IL L 0 0 7 4 .D S a m p le D e s c rip tio n 4 3 1 1-5431-S 1 4311 5 1 3 3 -S I 43-1T 5 1 3 3 -S 1 1311 5 1 3 3 M S S1 4 3 1 1 S 134-S 1 4311 6 136-S 1 4 3 1 1 - 6 1 3 6 -S-1 4.311-5136M S -S 14311 5137-S 1 1311 613 6 S1 4311 5 1 3 8 S1 4311 6130M S -S 14 3 1 1 .613Q .-S1 1311 6131 S1 1311 6 1 3 3 S1 1 3 1 1 -5 1 3 3 M S -S 1 1311 5 133 S1 1311. 5134 S1 1311 5135 S1 131-1-5 4 3 5 M S -S 1 4341-54-35-S 4 1311 6137 S1 1311 5 138 S1 1341 -5 4 3 8 M S -S 1 1311-5138-S 1 4 3 4 4 -5 4 4 0 -^ 4 1 3 1 1-6441-S 4 1341 -5 4 4 1 M S -S 1 1 3 4 1-6443-S 1 1311 5 1 4 3 .S1 1311-5444-S 1. H IL L 0 0 7 6 .D H IL L 0 0 7 7 .D W U .0 Q 7 5 .P 1 3 1 1 -5 4 4 6 -S4 43 4 4 -5 4 4 5 -5 4 1311-S 147-S 1 M IL L 0 0 8 0 .P H IL L 0 0 8 1 .D M J U 0 0 8 3 .D H IL L 00B 7.D H IL L 0 0 8 8 .D H 1L L 008P .D HILLO Q PO .D w u -o a a i.p H 1 1 1 0 0 8 3 ,0 H II_L0ftP3.D H U .LO O P4.D W U .Q 0 0 6 .D H IL L P P P fi.D H U .L 0 1 0 1 .D W U .U 1 0 2 .D M IL L 0 10 3 ,0 H IL L 0 1 0 4 .D H IL L 0 1 0 5 .D H IL L 0 1 0 6 .D H IL L 0 1 0 7 .D H IL L 0 1 0 8 .D H IL L 0 1 0 9 .D H IL L 0 1 1 0 .D H IL L 0 1 1 5 .D H IL L 0 1 1 6 .D H IL L 0 1 1 7 .D H IL L 0 1 1 8 .D H IL L 0 1 1 9 .D 1311 6148 S1 1311 -5 1 4 8 S1 1 3 4 -1 -5 4 5 0 -S41311-5460M S -S 1 43 4 4 -5 4 5 4 -5 4 1 3 1 1 -5 1 6 3 .5 1 4 3 4 4 -5 4 6 3 -5 4 U 1 1 -6 W M 3 -S 1 1 5 4 4 -5154-51 1 3 1 1 -6 1 6 6 S1 1 3 1 1 -6 1 5 6 5 1 1 3 1 1 6 1 6 6 M S S1 1 3 1 1 -6 157-S 1 1311 6168 S1 1341-5458-S 1 1 3 11-6158M S S1 1 3 1 1-5 1 6 0 -S 1 1 3 1 1-5 1 6 1 -S 1 1 3 1 1-5162-S 1 1311-5162M S -S 1 1 3 1 1-5 1 6 3 -S 1 1 3 1 1-5164-S 1 1311-5165-S 1 1 3 1 1-5165M S -S 1 1 3 1 1-5166-S 1 1 3 1 1-5167-S 1 1 3 1 1-5 1 6 8 -S 1 1 3 1 1-5168M S -S 1 Instrument: Hillary Run ID: H010329 T h e o re tic a l M a trix M easured S p ik e C o n c e n tra tio n , C o n c e n tra tio n , u g /L u g /L R e p lic a te S a m p le % R S D 383835366 4 5 3 -3 5 4 8 6 383608733 643615818 334470405 2 3 1 r8 0 7 3 3 3 3 4 5 *0 8 8 4 8 4 4 3 6 ,3 1 0 3 5 4 *^ 50 3 3 :3 6 6 1 ^ -5 *0 3 0 4 ,0 5 8 1 6 4 3 8 .3 4 0 3 1 3 3 3 ,7 0 4 8 7 8 3 7 ,0 8 4 0 1 4 3 3 7 ,3 5 3 0 3 5 4 3 3 ,4 7 7 3 1 8 4 3 6 ,4 4 8 4 6 8 4 3 5 ,3 0 8 3 8 3 344,4 7 3 5 8 4 8 0 ,8 0 3 4 0 7 7 2 ,0 8 3 1 4 1 7 3 ,3 4 5 3 0 8 3 8 0 ,4 4 3 3 0 6 4 5 3 .0 0 7 4 3 4 1 5 3 .0 6 8 6 3 3 4 5 1 ,8 8 8 3 6 ? 3 7 2 ,8 0 3 8 6 6 4 0 1 ,1 -3 3 8 4 3 8 1 ,0 8 7 1 3 3 8 3 .8 8 2 3 8 8 7 ,3 5 8 7 6 3 406 300 420 300 MA 300 400 300 543 300 6-32 200 003 200 036 200 WA4 M a trix S p ik e R eco very, % 1ip gj ^ 2 <|Q 40643 -|Q4 'f \Q4 i 10 41 4 3 7 .0 0 0 5 8 1 8 1 .3 4 8 3 8 3 1 5 3 ,8 1 4 0 6 3 3 7 6 ,6 3 3 4 7 4 4 6 8 ,3 0 8 1 3 5 4 7 8 .6 8 8 7 8 4 5 7 ,3 4 7 8 8 3 7 5 3 .8 4 0 3 8 7 3 5 3 ,6 4 3 6 3 1 3 6 0 ,5 0 4 -1 3 6 2 50,800634 184.3 7 7 1 3 3 5 18.487843 7 8 3 ,8 8 3 6 6 6 7 8 3 ,4 2 7 3 7 8 4 1 6 1 ,1 8 7 8 8 4 2 8 9 .0 0 2 1 6 4 2 5 8 .3 9 5 3 9 2 6 6 .0 3 3 3 9 4 4 8 0 .9 1 6 7 8 3 6 .2 4 7 6 4 9 6 .9 6 3 4 7 4 < 5.0 2 1 3 .5 0 8 1 1 2 7 9 .6 9 6 3 6 8 9 3 .2 2 8 9 8 6 9 4 .9 6 0 2 0 7 3 2 1 .3 7 1 6 8 4 200 200 200 200 200 200 200 200 02 2-30 4-70 21 5.88 95.84 9.36 4n? 9 11 1 .31 117 80 116.70 lft-4 38 107.44 106.75 113.21 D ilu tio n F acto r, Nx 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 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 3M Environmental Laboratory Page 240 of 703 BACK TO MAIN H IL L 0 1 2 0 .D H IL L 0 1 2 1 .D H IL L 0 1 2 2 .D H IL L 0 1 2 3 .D H IL L 0 1 2 4 .D H IL L 0 1 2 9 .D H IL L 0 1 3 0 .D H IL L 0 1 3 1 .D H IL L 0 1 3 2 .D H IL L 0 1 3 3 .D H IL L 0 1 3 4 .D H IL L 0 1 3 5 .D H IL L 0 1 3 6 .D H IL L 0 1 4 1 .0 H IL L 0 1 4 2 .D H IL L 0 1 4 3 .D H IL L 0 1 4 4 .P H 1L L 0145.D H IL L 0 1 4 6 .P H IL L 0 1 4 7 .P H IL L 0 1 4 8 .P H IL L 0 1 4 P .P H IL L 0 1 5 0 .P H IL L 0 1 5 5 .0 H IL L 0 1 5 6 .P H IL L 0 1 5 7 .P H JU .Q 158.P H IL L 0 1 5 P .P H IL L 0 1 6 0 .P H 1L L 0161.D H IL L 0 1 6 3 .P H IL L 9 1 6 1 .D H IL L 0 1 6 4 .D H IL L 0 1 6 5 .D H IL L 0 1 7 0 .D H IL L 0 1 7 1 .D H IL L 0 1 7 2 .D H IL L 0 1 7 3 .D H IL L 0 1 7 4 .D H IL L 0 1 7 5 .D H llu L 017fi.D H IL L 0 1 7 7 .D H IL L 0 1 7 8 .D H IL L 0 1 7 0 .D H IL L 0 1 8 1 .D H IL L 01B 6.D H tL L 01? ff.D H 1L L 0187.D H JU .Q 188.D H IL L 0 1 8 P .D H IL L 01P Q .P H 44.U 314,P H IL L 0 1 P 2 .D H IL L 0 1 P 3 .D H IL L 019B .D H IL L 01P 8.D H IL L 0 2 0 0 D H IU -0 3 9 1 ,D H IH .0 2 0 3 .D H IL L 0 2 0 .D H IL L 0 2 0 4 .D H IL L 0 2 0 5 .D H IL L 0 2 0 6 .D H IL L 0 2 0 7 .D 1 3 1 1 -5 1 69-S 1 1 3 1 1-5170-S 1 1 3 1 1-5171-S 1 1 3 1 1 -5 1 7 1 M S -S 1 1 3 1 1-5 1 7 2 -S 1 1 3 1 1-5173-S 1 1 3 1 1 -5 1 7 4 -S 1 1311-5174M S -S 1 1 3 1 1-5175-S 1 1 3 1 1 -5 1 76-S 1 1 3 1 1-5 1 7 7 -S 1 1 3 1 1 -5177M S -S 1 1 3 1 1-5178-S 1 1 311-5179-S 1 1 3 1 1-5180-S 1 1 311-518 0M S -S 1 1 3 1 1 -5181 S1 1 1 -6 1 8 2 S1 1311 -5 1 5 3 S1 1311..5 1 6 3 M S S1 1311 5184 S1 1 3 1 1 -6 1 8 6 S1 4 4 -6 1 8 6 S1 1311 5 1 8 6 M S S1 1 3 1 1 -6 1 8 7 S1 1311 -6 1 8 8 S1 1311. 6 1 8 0 S1 4 4 - 6 1 80M S -S 4 4 1 -5 1 0 0 S1 1311-6101 51 4 1 -6 1 0 2 51 4 -1 -6 192M S -S 41 3 1 1 -5 1 93-S 1 1 3 1 1-5194-S 1 1 311-5195-S 1 1 3 1 1 -5 1 95M S -S 1 1 311-5196-S 1 1 311-5197-S 1 1 3 1 1-5198-S 1 1 3 1 1-5198M S -S 1 1344 -6 1 0 0 51 1 3 1 .1 -6 2 0 0 S1 1344-6201 S1 1 3 1 1 -6 2 0 1 M S S1 1344-5202 51 1344 -6 2 0 3 S1 1 3 4 -1 -6 2 0 4 "S1 1 3 4 4 -6204 M S S1 1 344-6206 51 1 3 4 1 -6 2 0 6 S1 1 3 1 1 -6 2 0 7 S1 1 3 H -6 3 Q 7 M S S1 1311-6208 51 134-4-63Q O S1 1 3 1 1 6 2 1 0 S1 1311 S 2 1 0 M S S1 1 311-6212 51 1 3 4 4 -6 2 1 3 -S1 1 3 1 1 .6 2 1 3 M S S1 1 3 1 1-5214-S 1 1 3 1 1-5215-S 1 1 3 1 1-5 2 1 6 -S 1 1 3 1 1-5216M S -S 1 Analytical Run Information*: Acceptable Quant Range: 5 - 1O02ng/ml Calibration Curve r2: 0.9925463 Target Analyte: PFOS Internal Standard: THPFOS 3 4 4 .8 6 2 6 7 4 3 4 0 .7 5 9 6 6 6 3 6 5 .0 4 7 2 5 9 6 3 6 .3 7 1 3 5 6 2 0 3 ,7 9 7 9 3 9 1 8 7 .7 0 0 1 4 4 1 9 4 .5 1 0 2 7 6 4 2 2 .2 4 4 6 6 4 3 7 1 .3 2 3 1 9 6 3 7 1 .1 7 4 2 0 3 3 8 9 .7 0 8 7 3 9 6 4 5 .3 4 6 5 1 4 1 8 3 .2 6 6 6 5 8 1 7 8 .2 9 1 8 4 8 1 7 9 .6 0 0 5 0 7 3 8 7 .1 4 5 1 4 6 4 4 .0 3 6 0 6 0 ^ 5,0 < -6 *0 =-6*0 ^5*3 < 5*0 1 06,737034 6 ,6 5 7 0 7 1 = -6 6 ,3 0 4 6 4 1 4 0 5 *9 2 7 3 4 6 7.36P P 0P 7 ,3 1 2 1 9 0 <54> 4 6 4 *4 2 6 0 4 6 5 8 7 .3 5 3 9 8 2 3 7 5 .6 2 8 3 3 6 6 2 4 .6 5 1 5 3 9 9 4 7 .5 7 4 7 2 2 2 5 .4 0 0 5 6 4 1 6 .5 8 9 2 7 9 2 0 .4 7 5 8 0 2 2 3 6 ,9 7 5 4 3 7 ^5*4 *= 55 =-6*0 8 3 *0 8 0 1 1 8 < 6*0 < 5*0 =-6*0 < 5*0 < 5*0 =-6*0 < 5*0 0 8 *4 3 6 8 0 6 8 .2 7 0 8 0 0 6 *8 4 0 7 4 1 <5^ 1 5 3 ,0 0 0 3 6 4 4 3 ,3 7 0 7 6 1 -1 8 ,3 6 7 8 6 2 .1 3 5 ,2 6 0 8 0 2 8 .4 6 8 1 3 9 7 .309995 7 .7 07909 :J01.1 5 6 1 0 5 200 200 200 200 300 300 300 300 200 200 200 300 3.71 4.14 2.02 1.43 MA N /A 14.83 0*44 25.38 21.21 UlA f.j/A 300 300 300 200 7 iO M 7.52 135.66 113.87 127.82 103.77 MA 3.37 0*32 83*04 161.46 108.25 4-1.80 MA 4 0 .0 0 98.72 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 2 2 2 2 2 2 10 10 10 10 10 10 10 100 100 100 100 \ 3M Environmental Laboratory Page 241 of 703 BACK TO MAIN Quality Control Sam ple Data S am ple D ata File R U S H 0037.D R U S H 0038.D R U S H 0 0 3 9 .D R U S H 0040.D R U S H 0 0 4 1 .D R U S H 0042.D R U S H 0043.D R U S H 0048.D S am ple D escription 1311-5016-S1 1 3 1 1 -5 0 1 7-S1 1311-5018-S1 1311-5018MS-S1 1311-5070-S2 1311-5071-S2 1311-5072-S2 1311-5072M S -S 2 R U S M 0050.P U S H 00S 1.P R U & U 00& 3.P R U S H 0053.D R U S H 0 0 5 4 .D R U S H 0 0 5 5 .D R U S H 0056.D R U S H 0 0 5 7 .D R U S H 0062.D R U S H 0 O 6 3 .D R U S H 0064.D R U S H 0065.D R U S H 0 0 6 6 .D R U S H 0067.D R U S H 0068.D R U S H 0069.D R U S H 0070.D R U S H 0071.D R U S H 0076.D R U S H 0077.D R U S H 0078.D R S H 0079.D R U S H 0080.D R U S H 0081.D R U S H 0082.D R U S H 0083.D R U S H 0084.D R U S H 0085.D R U S H 0090.D R U S H 0091.D R U S H 0092.D R U S H 0093.D R U S H 0094.D R U S H 0095.D R U S H 0096.D R U S H 0 9 7 .D R U S H 0098.D R U S H 0099.D 4344.6 0 8 3 S3 1311 6083 S3 1311.6083M S S3 1311-5103-S2 1311-5104-S2 1311-5105-S2 1 3 1 1-510 5 M S -S 2 1311-5106-S2 1311-5107-S2 1311-5108-S2 1311-5108M S -S 2 1311-5127-S2 1311-5128-S2 1311-5129-S2 1311-5129M S -S 2 1311-5130-S2 1311-5132-S2 1311-5132M S -S 2 1311-5133-S2 1311-5134-S2 1311-5135-S2 1311-5135M S -S 2 1311-5136-S2 1311-5137-S2 1311-5138-S2 1311-5138M S -S 2 1311-5139-S2 1311-5140-S2 1311-5141-S2 1311-5141M S -S 2 1311-5142-S2 1311-5143-S2 1311-5144-S2 1311-5144M S -S 2 1311-5163-S2 1311-5164-S2 1311-5165-S2 131 1 -5 1 65M S -S 2 A n a lytica l Run Inform ation*: Acceptable Quant Range: 5 - 1002ng/ml C a lib ra tio n C u rve r2: 0.9 9 9 7 6 4 0 Target Analyte: PFOS Internal Standard: TH PFO S Instrument: Rush Run ID: R010402 (A) Theoretical M atrix M easured S p ik e C oncentration, C oncentration, u jj/L ug/L R eplicate S am ple %RSD 69.243301 69.879261 64.31529 236.736167 45C.789701 305.703229 3 39.490983 5 28,022186 119 098375 42 25468 28 725867 228 8^1515 121 844173 127 233095 133 630265 315.491169 67.811262 62.727361 84.309464 273.509217 < 5.0 < 5 .0 < 5 .0 2 1 1.049083 26.076048 26.69003 246.936174 1 0 7 .:13316 111.287815 106.223884 361.M 6659 289.673014 249.672867 276.604812 580.C 20253 105.277362 114.123143 103.239784 293.385505 491.927102 509.061312 513.037645 715.922726 < 5.0 < 5.0 < 5.0 204 .8 :2 4 1 6 2 4.53 200 2 0 .78 200 3M 3 300 4.63 200 1 5 .7 5 200 N/A 200 0.04 200 2.50 200 7.51 200 5.36 200 2.22 200 N/A 200 M atrix S pike R ecovery, % 8 6 .21 9 4 .2 7 100,66 90.93 94.60 105.52 110.12 1 2 7 .6 1 152.00 95.07 101.46 102.41 D ilution Factor, Nx 1000 1000 1000 1000 10 10 10 10 2 Contaminated 2 control 2 blanks 2 10 10 10 10 100 100 100 100 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 Sample Data Sam ple Data File RUSH120.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 RUSH0137.D RUSH0138.D RUSH0139.D RUSH0140.D RUSH0141.D RUSH0142.D RUSH0143.D RUSH0148.D RUSH0149.D RUSH0150.D RUSH0151.D RUSH0152.D RUSH0153.D RUSH0154.D RUSH0155.D RUSH0156.D RUSH01S7.D Sample D escription 1313-5166-S2 1311-5167-S2 1311-5168-S2 1311-5168MS-S2 1311-5169-S2 1311-5170-S2 1311-5171-S2 1311-5171MS-S2 1311-5172-S2 1311-5173-S2 1311-5174-S2 1311-5174MS-S2 1311-5175-S2 1311-5176-S2 1311-5177-S2 1311-5177MS-S2 1311-5178-S2 1311-5179-S2 1311-5180-S2 1311-5180MS-S2 1311-5199-S2 1311-5200-S2 1311 -5201-S2 1311-5201MS-S2 131-5202-S2 1311-5203-S2 1311-5204-S2 1311-5204MS-S2 1311-5205-S2 1311-5206-S2 Analytical Run Information*: Acceptable Quant Range: 10 - 1002ng/ml Calibration Curve r2: 0.9989973 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Rush Run ID: R010402 (b) M easured C oncentration, ug/L 42.932438 43.120798 42.621787 2 7 6 .7 0 0 8 6 5 160.750438 149.070084 165.740897 4 4 3 .4 9 0 2 5 6 380.66422 374.889478 3 7 9 .2 8 7 6 6 2 721.856858 174.993474 163.325091 174.345547 360.823329 74.086291 79.446466 70.91215 254.760727 < 10.0 10.0 < 10.0 170.997556 < 10.0 *: 10.0 < 10.0 200.243175 < 10.0 < 10.0 Theoretical M atrix Spike C oncentration, ug/L R e p lic a te Sample %RSD 0.59 200 5.40 200 0.80 200 3.84 200 5.77 200 N/A 200 N/A 200 N/A M atrix Spike Recovery, % 117.04 138.87 171.28 93.24 91.92 85.50 100.12 D ilution Factor, Nx 2 2 2 2 2 2 2 2 2 2 2 2 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 243 of 703 BACK TO MAIN Quality Control Sample Data Sam ple Data File HILL0031 .D MUX0 0 3 3 .0 H IL L W 3 3 .P HILLflQ34.P H IL L 0 0 5 .P HILLQ036.P HILL0037.P HIL1003S.P w u ooafco HILLQ040.P HIU.Q045.P HILL0Q46.P HILL0CM7.P HILL0048.P MU.LQ040.D HILL0P50.P HU.L0M1.P H1LLP052.P HILL0053.D HILLP054.P HILL0Q5P.P HILL0060.P HILLP061.P HILLP062.P HILLPP63.P HILLPP64.P HJLL006S.P HILL0Q66.P HILL0067.D H IL L 0 0 7 2 .D HILL0073.D HILL0074.D HILL0075.D H IL L 0 0 7 6 .D HILL0077.D HILL0078.D Sample D escription 4344-5043-S1 4311-5044-S1 4 5 4 4 -5 0 4 5-S1 43U -5045M S -S 1 4311-504 ft-S1 4 3 1 1 -5 0 5 0 - S1 43.n -50s a .s 1 4344-5054MS-S4 4 3 1 1 -5 0 7 ft-S1 4311-5Q80-S1 1311-5081-S1 4 3 1 1 -5 0 8 1M S.S1 4 3 1 1-5Q8S-S1 4344-5086-S4 1311-5Q87-S1 4311-5087MS S1 4 3 1 1-5001-S1 1311.5003-S1 .1311-5003.S1 4 3 1 1 -5003A4S-S1 4344-5434-S4 4341-5433-S1 4344-5433-S4 4311.5133MS S1 4311-5157-51 434,1-54 58-S1 1311 5150-S1. 4311 5150MS, S1 1311-5181 -S1 1311-5182-S1 1311-5183-S1 1311-5183MS-S1 1311-5199-S I 1311-5200-S1 1 3 1 1-5201-S1 1 3 1 1-5201M S-S1 Analytical Run Information*: Acceptable Quant Range: 10 - 1002ng/ml C a lib r a tio n C u r v e t2 : 0 .9 9 7 9 3 3 5 Target Analyte: PFOS Internal Standard: NONE Instrument: Hillary Run ID: H010405, external standard quant Measured Concentration, ug/L Theoretical Matrix Spike Concentration, ug/L R e p lic a te Sample %RSD 00.707034 55444873 103.405038 367.307805 43.130005 53,043033 38.586671 300,445138 06.758130 133,688674 03.303473 340.138057 54.84818 54.54481 54.656047 324.611003 40,300717 8.044223 3-183657 133.378137 433-354584 483.17750 408-700443 545.166673 55,410636 01.075774 80,143057 354.385364 30 Q1 200 47A2 200 4528 200 024 200 171 y; 200 005 200 200 27.424377 < 10.0 # D IV /0 ! <10.0 144.847675 200 <10.0 < 1 0 .0 <10.0 131.864428 N/A 200 Matrix Spike Recovery, % 1??.7n 1Q4.73 Quanted using internal standard, this data not used 43457 113 31 91 3 7 3 .Qp 107 19 72.42 65.93 D ilu tio n Factor, Nx 10 10 10 10 100 100 100 100 10 10 10 10 100 100 100 100 2 2 2 2 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 244 of 703 BACK TO MAIN Quality Control Sample Data S am ple Data File RUSH0032.D RUSH0033.D RUSH0034.D RUSH003S.D RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0040.D RUSH0041.D RUSH0046.D RUSH0047.D RUSH0048.D RUSH0049.D RUSH0050.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.D RUSH0060.D RUSH0061.D RUSH0062.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH0068.D RUSH0069.D RUSH0074.D RUSH0075.D RUSH0076.D RUSH0077.D RUSH0078.D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0082.D RUSH0083.D R U S H 0 0 8 8 .D RUSH0089.D RUSH0090.D RUSH0091.D RUSH0092.D Sample D escription 1311-4154-S2 1311-4155-S2 1311-4156-S2 1311-4178-S2 1311-4179-S2 1311-4180-S2 131-4154-S3 1311-4155-S3 1311-4156-S3 1311-4178-S3 1311-4179-S3 1311-4180-S3 1311-4154-S4 1311-4155-S4 1311-4156-S4 1311-4178-S4 1311-4179-S4 1311-4154-S5 1311-4155-S5 1311-4156-S5 1311-4178-S5 1311-4179-S5 1311-4180-S5 1311-4154-S6 1311-4155-S6 1311-4156-S6 1311-4156MS-S6 1311-4178-S6 1311-4179-S6 1311-4180-S6 1311-4180MS-S6 1311-4154-S7 1311-4155-S7 1311-4156-S7 1311-4178-S7 1311-4179-S7 1311-4180-S7 1311-4154-S8 1311-4155-S8 1311-4156-S8 1311-41 56M S -S 8 1311-4178-S8 1 3 1 1-4179-S 8 1311-4180-S8 1311-4180MS-SB Analytical Run Information*: Acceptable Quant Range: 1 0 - 1002ng/ml Calibration Curve r2: 0.9913280 Target Analyte: PFOS Internal Standard: NONE Instrument: Rush Run ID: R010404. external standard quant M easured C oncentration, ug/L < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 184.786805 < 10.0 < 10.0 < 10.0 256.265166 c 10.0 < 10.0 < 10.0 < 10.0 < 10.0 < 10.0 i 10.0 - 10.0 10.0 1 9 8 .8 8 0 5 0 2 : 10.0 < 10.0 * 10.0 155.579696 th e o re tic a l M atrix Spike C o n c e n tra tio n , ug/L R e p lic a te Sample %RSD N/A N/A N/A N/A N/A N/A N/A N/A N/A 200 N/A 200 N/A N/A N/A 200 N/A 200 M atrix Spike Recovery, % 92.39 128.13 99.44 77.79 D ilution 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 Quality Control Sample Data Sam ple Data File HILL0031.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 HILL0050.D HILL0051.D HILL0052.D HILL0053.D HILL0054.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 HILL0081.D HILL0082.D Sample D escription 1 3 1 1-4151-S 1 1 3 1 1-4152-S 1 1311-4153-S1 1311-4153MS-S1 1 3 1 1-4154 -S 1 1 3 1 1-4155 -S 1 1311-4156-S1 1311-4156MS-S1 1311-4157-S1 1 3 1 1-4158 -S 1 1311-415 9 -S 1 1311-4159MS-S1 1 3 1 1-4160 -S 1 1311-4161 -S 1 1 3 1 1-4162-S 1 1311-4162MS-S1 1 3 1 1-4163-S 1 1311-4164-S1 1311-4165-S1 1311-4165MS-S1 1311-4166-S1 1311-4167-S1 1 3 1 1-4168-S 1 1311-4168MS-S1 1311-4169-S1 1311-4170-S1 1311-4171 - S 1 1311-4171-MS-S1 1311-4172-S1 1311-4173-S1 1 3 1 1-4174-S 1 1311-4174MS-S1 1311-417 5 -S 1311-4176-S1 1 3 1 1-4177-S 1 1311-4177MS-S1 1311-417 8-S 1 1 3 1 1-4179-S 1 1311-418 0 -S 1 1311-4180MS-S1 Analytical Run Information*: Acceptable Q uant Range: 10 - 1002ng/ml Calibration Curve r2: 0.9979335 Target Analyte: PFOS Internal Standard: NONE Instrument: Hillary Run ID: H010404. external standard quant M easured C o n c e n tra tio n , ug/L < 10.0 < 10.0 < 10.0 168.305282 < 10.0 < 10.0 < 10.0 157.148327 < 10.0 < 10.0 < 10.0 173.055241 < 10.0 <10.0 <10.0 165.193594 <10.0 <10.0 <10.0 166.210776 < 10.0 < 10.0 < 10.0 164.639012 < 10.0 < 10.0 < 10.0 164.253095 < 10.0 < 10.0 < 10.0 165.168607 < 10.0 < 10.0 < 10.0 162.310247 < 10.0 < 10.0 < 10.0 153.354131 T h e o re tic a l M atrix Spike C o n c e n tra tio n , ug/L R e p lic a te Sample %RSD N/A 200 N/A 200 N/A 200 N/A 200 N/A 200 N/A 200 N/A 200 N/A 200 N/A 200 N/A 200 M atrix Spike Recovery, % 84.15 78.57 86.53 82.60 83.11 82.32 82.13 82.58 81.16 76.6B D ilution 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 3M Environmental Laboratory Page 246 of 703 BACK TO MAIN Quality Control Sample Data S a m p le D a ta F ile H IL L 0 0 3 1 .D H IL L 0 0 3 2 .D H IL L 0 0 3 3 .D H IL L 0 0 3 4 .D H IL L 0 0 3 5 .D H IL L 0 0 3 6 .D H IL L 0 0 3 7 .D H IL L 0 0 3 8 .D H L L 0 0 3 9 .D H IL L 0 0 4 0 .D H IL L 0 0 4 5 .D H IL L 0 0 4 6 .D H IL L 0 0 4 7 .D H IL L 0 0 4 8 .D H IL L 0 0 4 9 .D H IL L 0 0 5 0 .D H IL L 0 0 5 1 .D H IL L 0 0 5 2 .D H IL L 0 0 5 3 .D H IL L 0 0 5 4 .D H IL L 0 0 5 9 .D H IL L 0 0 6 0 .D H IL L 0 0 6 1 .D H IL L 0 0 6 2 .D H IL L 0 0 6 3 .D H IL L 0 0 6 4 .D H IL L 0 0 6 5 .D H IL L 0 0 6 6 .D H IL L 0 0 6 7 .D H IL L 0 0 7 3 .D H IL L 0 0 7 3 .D H IL L Q 0 7 4 .D H iL L 0 0 7 5 iD H IL L 0 0 7 6 .D WUOOWrO H IL L 0 0 7 8 .D S a m p le D e s c rip tio n 1 3 1 1-5043-S 1 1 3 1 1-5 0 4 4 -S 1 1 3 1 1 -5 0 4 5-S1 1 3 1 1-5045M S -S 1 1 3 1 1-5 0 4 9 -S 1 1311-5050-S 1 1 3 1 1-5051-S 1 1 3 1 1-5 0 5 1 M S -S 1 1 3 1 1-5 0 7 9 -S 1 1 3 1 1-5 0 8 0 -S 1 1311-5 0 8 1 -S 1 1 3 1 1 -5 0 8 1 M S -S 1 1 3 1 1-5 0 8 5 -S 1 1 3 1 1-5086-S 1 1 3 1 1-5 0 8 7 -S 1 1 3 1 1 -5087M S -S 1 1 3 1 1-5 0 9 1 -S 1 1 3 1 1-5 0 9 2 -S 1 1 3 1 1-5 0 9 3 -S 1 1 3 1 1-5093M S -S 1 1 311-5121-S 1 1 3 1 1-5122-S 1 1 3 1 1 -5 1 23-S 1 1 3 1 1-5 1 2 3 M S -S 1 1 3 1 1 -5 1 5 7 -S I 1 3 1 1-5158-S 1 1 3 1 1-5159-S 1 1311-5159M S -S 1 4 .3 44-S 484-S 1 4 4 4 4 -6 4 8 3 -8 4 4 4 4 4 -6 4 8 8 -8 4 1 3 1 1 5 1 8 3 M S 84 1311 5199-S 1 4 3 4 4 -5 3 0 0 -8 4 4 4 4 4 -6 3 0 4 -8 4 ,1444-5301 M S -8 4 Analytical Run Information*: Acceptable Quant Range: 5 - 1002ng/ml Calibration Curve r2: 0.9998940 Target Analyte: PFOS Internal S tandard: T H P FO S Instrument: Hillary Run ID: H010405. internal standard quant T h e o re tic a l M a trix M easu red S p ik e C o n c e n tra tio n , C o n c e n tra tio n , u g /L u g /L R e p lic a te S a m p le % R S D 9 1 .8 9 1 6 3 5 5 6 .7 6 5 1 7 1 1 0 2 .4 8 7 5 8 7 3 2 6 .6 2 2 5 7 9 4 1 .7 4 7 3 5 7 5 1 .7 4 1 3 0 9 3 8 .0 2 4 0 0 2 2 3 4 .6 9 0 7 2 2 9 6 .6 0 6 4 5 7 121.2 1 3 2 1 4 9 1 .0 1 2 5 0 7 3 0 5 .1 8 5 3 1 5 5 2 .0 7 9 3 3 3 5 1 .3 5 5 2 9 9 5 1 .6 7 6 9 8 1 2 5 6 .6 7 0 4 0 3 4 0 .6 9 2 0 7 3 1 2 .2 5 0 2 9 5 7 .04131 2 2 8 .1 1 2 5 6 4 4 3 7 .9 5 3 2 3 7 5 0 3 .5 3 0 2 4 8 4 2 3 .3 7 0 9 3 7 7 4 6 .0 7 0 8 7 5 6 .2 3 7 2 7 4 86 .0 8 4 0 1 8 7 .8 4 3 5 6 3 3 0 5 .6 4 6 2 4 5 2 0 ,1 6 6 1 6 9 5 ,7 8 2 3 5 9 28.59 200 16.18 200 15.61 200 0.70 200 90.59 200 9.39 200 23.15 200 105,6 3 5 1 6 4 200 44 *6rO WA 200 M a trix S p ik e R ecovery, % 163.31 117.35 152.59 128.34 114.06 373.04 152,62 2 t04 sludge samples will be quanted without the IS D ilu tio n Facto r, Nx 10 10 10 10 100 100 100 100 10 10 10 10 100 100 100 100 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 Quality Control Sample Data S a m p le D a ta F ile H IL L 0071 P H J U .0 6 3 3 .P H IU _ 0 0 3 3 .P H IL L 0 0 3 4 .D H IL L 0 0 5 .D H IL L 0 P 3 6 .P H IL L Q 037.D H J U 0 0 3 8 .P H IL L 003Q .D k U U 0 0 4 ftO H I L L 0 0 ,i 5 . P H I L L 0 0 /1 6 .D H IL IlO O -17.D H IL L 0 0 4 8 .P H IL L 0 Q 4 8 .D H IL L 005Q .C 1 W U O O frU i H IL L 0 0 5 3 .D H IL L 0 0 5 3 D H IL L 0 0 5 4 .D H IL L 0 0 5 P .P H IL L Q 0 6 0 .P H IL L 0 0 6 1 .P H IL L 0 0 6 3 .P H IL L P P fiT P H IH .0 0 6 4 .D H IL L P 0 6 5 .P H iLlaO O g .P H IU 0 0 6 7 .D H IL L 0 0 7 2 .D H IL L 0 0 7 3 .D H IL L 0 0 7 4 .D H IL L 0 0 7 5 .D H IL L 0 0 7 6 .D H IL L 0 0 7 7 .D H IL L 0 0 7 8 .D S a m p le D e s c rip tio n 4 3 1 4 -5 0 4 3-S 4 1311-5044 S1 1314-504 5 .S 1 4 -3 1 4 -5 0 4 5M -S -S 1 1 3 1 1 .5 0 4 0 S1 4 31-1 -5 0 5 0 -S 4 1 3 1 1 -5 0 5 1 S1 4 3 1 4 -5 0 5 4 M S -S I 4 3 1 4 -6 0 7 .0 -S 4 4 3 1 4 -5 0 8 0 -S 4 4 3 1 4 -5 0 8 1 -S i 43 1 4 -5 0 8 4 M S -S 1 4 314-5085-S 1. 4 3 1 4 -5 0 8 6 -S 1 4 3 1 4 -5 0 8 7 -S 4 4 3 1 4 -5 Q 8 7 M S -S 1 4 3 4 4 -5 0 0 4 -S 4 4 3 1 4 -5 0 0 3 -S 1 4 314-5Q 03-S 4. 1314-5003M S -S 1 4 3 1 1 -5 1 3 4 -S I 4 3 1 4 -5 1 3 3 -S 1 4 3 1 4-5133-S 4- 4 3t133M S -S 1 4 3 1 1 -5 1 5 7 -S i 4 3 1 1-5158-S 1 4 3 1 1 -5 1 5 0 -S I 4 3 4 1 -5 .1 5 0 M S .S 1 1 3 1 1-5181-S 1 1 3 1 1 -5 1 8 2 -S 1 1 3 1 1-5183-S 1 1 3 1 1 -5 1 8 3 M S -S 1 1 3 1 1 -5 199-S 1 1 3 1 1 -5 200-S 1 1 3 1 1 -5 2 0 1 -S 1 1311-5 2 0 1 M S -S 1 Analytical Run Information*: Acceptable Quant Range: 10 - I002ng/ml C a lib r a tio n C u r v e r2: 0 .9 9 7 9 3 3 5 Target Analyte: PFOS Internal Standard: NONE Instrument: Hillary Run ID: H010405. external standard quant M easured C o n c e n tra tio n , u g /L T h e o re tic a l M a trix S p ik e C o n c e n tra tio n , u g /L R e p lic a te S a m p le % R S D 0 0 .7 0 7 0 3 4 5 5 .4 4 1 8 7 7 4 0 3 .4 0 5 0 2 8 2 6 7 ,3 0 7 8 0 5 4 2 .1 3 0 0 0 5 5 3 .0 4 7 0 3 3 38r586674 2 0 0 .4 4 6 1 3 8 0 6 .7 5 8 1 3 0 1 2 2 .6 8 8 6 7 4 0 2 .3 0 7 1 7 3 2 4 0 .1 3 8 0 5 7 6 4 .8 4 8 1 8 5 4 .5 4 4 8 1 5 4 .6 5 6 0 4 7 2 3 4 .6 1 1 0 0 3 4 0 3 0 0 7 -1 7 3183557 432378427 4 2 2 .2 5 1 5 8 4 4 8 3 .1 7 7 5 0 4 0 8 .7 0 0 4 1 2 5 4 6 .1 6 6 6 7 2 5 5 .4 1 0 6 2 6 0 4 .0 7 5 7 7 4 8 0 ,1 4 3 0 5 7 354385364 2 7 .4 2 4 3 7 7 < 10.0 < 1 0 .0 1 4 4 .8 4 7 6 7 5 < *0.0 <* 0 .0 < ' 0.0 1 3 1 .8 6 4 4 2 8 20,01 300 17 02 300 45^0 200 031 200 121.'P 200 & 05 200 2 5 .54 200 # D IV /0 ! 200 N/A 200 M a trix S p ik e R eco very, % 133,70 104.73 Quanted using in te rn a l standard, this data not used 124.57 112.31 -1Q 14 277 np 127 io 7 2 .4 2 65 93 D ilu tio n F a c to r, Nx 10 10 10 10 100 100 100 100 10 10 10 10 100 100 100 100 2 2 2 2 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 248 of 703 BACK TO MAIN Quality Control Sample Data Sample Data File RUSH0032.D RUSH0033.D RUSH0034.D RUSH0035.D RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0040.D RUSH0041.D RUSH0046.D RUSH0047.D RUSH0048.D RUSH0049.D RUSH0050.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.D RUSH0060.D RUSH0061.D RUSH0062.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH0068.D RUSH0069.D RUSH0074.D RUSH0075.D RUSH0076.D RUSH0077.D RUSH0078.D R U S H 0079.D RUSH0084.D RUSH0085.D RUSH0086.D RUSH0087.D RUSH0088.D RUSH0089.D RUSH0090.D RUSH0091.D Sample Description 1311-5124-S1 13 1 1-5125-S1 1311-5126-S1 1311-5126MS-S1 1311-5127-S1 1311-5128-S1 1311-5129-S1 1311-5129MS-S1 1311-5130-S1 13 1 1-513 1 -S1 1311-513 2 -S 1 1311-5132MS-S1 1311-5133-S1 1311-5134-S1 1311-5135-S1 1311-5135MS-S1 1311-5136-S1 1311-5137-S1 1311-5138-S1 1311-5138MS-S1 13 11 -5139-S1 1311-5140-S1 1311-5141-S1 1311-5141MS-S1 1311-5142-S1 1311-5143-S1 1311-5144-S1 1311-5144MS-S1 1311-5145-S1 1311-5146-S1 1311-5147-S1 1311-5147MS-S1 1311-5148-S1 1311-5149-S1 1311-5150-S1 1311-5150MS-S1 1311-5151-S1 1311-5152-S1 1311-5153-S1 1311-5153MS-S1 1311-5154-S1 13 1 1-5155-S1 1311-5156-S1 1311-5156MS-S1 R010412 Instrument: Rush Run ID: R010412 Measured Concentration, ug/L 235.149546 235.642534 230.804348 493.847976 21.144501 <10.0 <10.0 221.257013 24.842763 18.057138 25.246348 254.1411 112.234056 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 343.243911 <10.0 <10.0 <10.0 220.445044 123.282427 90.083398 1 5 2 .5 0 7 8 8 8 423.934455 470.275971 4 8 1.768175 461.552835 867.494012 259.294489 273.244648 260.405148 559.64233 Theoretical Matrix Spike Concentration, ug/L Replicate Sample %RSD 200 200 200 200 200 200 200 200 200 200 200 1 .14 N /A 1 7 .7 8 1 0 .2 3 6 .6 1 0.8 4 6 .56 N /A 2 5 .6 1 2.1 5 2.9 3 Matrix Spike Recovery, % 1 3 1 .5 2 1 1 0 .6 3 1 1 4 .4 5 1 2 5 .4 3 1 2 2 .6 2 1 3 4 .8 5 1 2 3 .4 0 1 1 0 .2 2 1 3 5 .7 1 2 02.97 1 4 9 .6 2 Analytical Run Information*: Acceptable Quant Range: 1 0 - 1 002ng/ml Calibration Curve r2: 0.9999132 Target Analyte: PFOS Internal Standard: THPFOS > ' 3M Environmental Laboratory Page 249 of 703 BACK TO MAIN Quality Control Sample Data Sample Data File HILL0031.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 HILL0050.D HILL0051.D HILL0052.D HILL0053.D HILL0054.D HILL0059.D HILL0060.D HILL0061.D HILL0062.D HILL0063.D HILL0064.D HILL0065.D HILL0066.D Sample Description 1311-518 4 -S 1 1311-5185-S1 1 3 1 1-5 186-S 1 1 3 1 1-5 1 8 6 M S -S 1 1311-5187--S1 1311-5188-S1 1 3 1 1-5 189-S 1 1 3 1 1-5 1 8 9 M S -S 1 13 1 1-5 1 90-S1 1 3 11 -519 1 -S1 1311-5192-S1 1311-5192MS-S1 1311-5202-S1 1311-5203-S1 1311-5204-S1 1311-5204MS-S1 1311-5205-S1 1311-5206-S1 1311-5207-S1 1311-5207MS-S1 13 11-5208-S1 1311-5209-S1 1 3 1 1 -5 2 1 0-S1 1311-5210MS-S1 1 3 1 1 - 5 2 1 1-S1 1 3 1 1-5 2 1 2 -S 1 1311-5213-S1 1311-5213MS-S1 Analytical Run Information*: Acceptable Quant Range: 10 - 400.8ng/ml Calibration Curve r2: 0.9913025 Target Analyte: PFOS Internal Standard: THPFOS H010412 Instrument: Hillary Run ID: H010412 Measured Concentration, ug/L < 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 215.922611 Theoretical Matrix Spike Concentration, ug/L Replicate Sample %RSD 200 200 200 200 200 200 200 N /A N /A 1 8 .3 4 N /A N /A 1 4 .9 8 25 .5 1 Matrix Spike Recovery, % 6 2 .0 8 6 2 .9 1 1 0 2 .3 0 5 5 .4 5 5 9 .1 1 9 7 .1 9 95 .7 3 > 3M Environmental Laboratory Page 250 of 703 BACK TO MAIN Quality Control Sample Data S a m p le D ata File H IL L 0 0 3 2 .D H IL L 0 0 3 3 .D H IL L 0 0 3 4 .D H IL L 0 0 3 5 .D H IL L 0 0 3 6 .D H IL L 0 0 3 7 .D H IU .00 3 8 .D H IL L 0 0 3 9 .D H IL L 0 0 4 0 .D H IL L 0 0 4 5 .D H IL L 0 0 4 6 .D H ILL 0O 47 .D H IL L 0 0 4 8 .D H IL L 0 0 4 9 .D H IL L 0 0 5 0 .D H IL L 0 0 5 1 .D HI L I 0052.D H IL L 0 0 5 3 .D HILL0054.D H IL L 0 0 5 9 .D H IL L 0 0 6 0 .D HILL0061.D H IL L 0 0 6 2 .D HILL0O63.D HILL0064.D H IL L 0 0 6 6 .D HILL0066.D HILL0067.D HILL0068.D HILL0073.D HILL0074.D H IL L 0 0 7 5 .D HILL0076.D HILL0077.D HILL0078.D HILL0079.D HILL0080.D HILL0081.D HILL0082.D HILL0087.D HILL00B8.D HILL0089.D HILL0090.D HILL0091.D HILL0092.D H IL L 0 0 9 3 .D H ILL0094. D H1LL0O95.D H IL L 0 0 9 6 .D HILL0101.D H IL L 0 1 0 2 .D H IL L 0 1 0 3 .D H IL L 0 1 0 4 .D H IL L 0 1 0 5 .D H IL L 0 1 0 6 .D HILL0107.D HILLD108.D HILL0109D H IL L 0 1 1 0 .D H IL L 0 1 1 5 .D HILL0116.D HILL0117.D HILL0118.D H IL L 0 1 1 9 .D HILL0120.D H1LL0121.D HILL0122.D H IL L 0 1 2 3 .D HILL0124.D HILL0129.D H IL L 0 1 3 0 .D H IL L 0 1 3 1 .D H IL L 0 1 3 2 .D H IL L 0 1 3 3 .D HILL0134.D H IL L 0 1 3 5 .D H IL L 0 1 3 6 .D Sample D escription -5019-S3 -5020-S3 -5021-S3 -5021MS-S3 -5055-S3 -5056-S3 -5057-S3 -5 0 5 7 M S -S 3 -5091-S3 -5092-S3 -5093-S3 -5093MS-S3 -5127-S3 -5128-S3 -5129-S3 -51 29 M S -S 3 -5163-S3 -5164-S3 -5165-S3 -5 1 6 5 M S -S 3 -5199-S3 -520O-S3 -5201-S3 -52D1MS-S3 -5022-S3 -5023-S3 -5024-S3 -5 0 2 4 M S -S 3 -5058-S3 -5059-S3 -5060-S3 -5 0 6 0 M S -S 3 -5094-S3 -5095-S3 -5096-S3 -5096MS-S3 -5130-S3 -5132-S3 -5 1 3 2 M S -S 3 -5166-S3 -5167-S3 -5168-S3 -5 1 6 8 M S -S 3 -5202-S3 -5203-S3 -5204-S3 -5 2 0 4 M S -S 3 -5025-53 -5026-S3 -5027-S3 -50 27 M S -S 3 -5061-S3 -5062-53 -5063-S3 -5 0 6 3 M S -S 3 -5097-S3 -5098-S3 -5099-S3 -5 0 9 9 M S -S 3 -5133-S3 -5134-53 -5135-S3 -5 1 3 5 M S -S 3 -5169-53 -5170-53 -5171-53 -5171MS-S3 -5205-S3 -5206-53 -5207-S3 -5 2 0 7 M S -S 3 -5028-53 -5029-53 -5030-S3 -5 0 3 0 M S -S 3 -5064-53 -5065-S3 A n a ly tic a l R un In fo rm atio n *: A cceptable Q uant R ange: 5 - 10G2ng/ml Calibration Curve r2: 0.9978666 Target Analyte: PFOS internal Standard: THPFOS Instrument: Hillary Run ID: H010316 Theoretical M atrix Measured Spike C oncentration, C oncentration, ug IL ug/L R e p lic a te Sample %RSD < 5.0 < 5 .0 < 5.0 N/A 193.2 < 5.0 < 5 .0 < 5.0 198.3 10.0 27.8 < 5 .0 200 N/A 200 61.45 187.3 < 5.0 < 5 ,0 < 5.0 207.2 < 5.0 < 5.0 < 5 .0 199.1 <5.0 < 5.0 < 5.0 172.7 < 5.0 < 5,0 < 5.0 190.5 42.6 48.9 57.0 261.8 56.4 45.9 57.9 268.0 111.6 98.8 333.9 142.0 200 N/A 200 N/A 200 N/A 200 N/A 200 14.60 200 12.21 200 863 200 99.1 65.7 37 39 281.1 36.3 25.2 30.1 205.7 200 18.24 200 < 5.0 < 5 .0 < 5 .0 193.0 N/A 200 159.8 203.2 180.8 11.98 416.4 161.9 173.0 194.7 200 0 45 557.2 200 393.7 375.2 4.32 361.3 657.1 298.3 267.4 327.9 598.5 97.6 127.8 98.9 200 10.16 200 15.81 301.6 5.6 < 5 .0 6.0 200.4 461.1 285.5 200 542 200 M atrix Spike Recovery, % D ilu tio n Level, Nx 96.61 99.14 93 67 103 61 99 53 86.35 95 27 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 2 102 44 105 05 117.57 107.73 87.63 96 48 117.80 181.23 Low Interna! standard response 147.93 Low internal standard response 135 32 Low internal standard response 101.35 97.17 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 3M Environmental Laboratory Page 251 of 703 BACK TO MAIN Quality Control Sample Data S am ple Data F ile HILL036.D HILL0037.D HILL0038.D HILL0039.D HILL0040.D HILL0041.D HILL0042.D HILL0043.D HILL0044.D HILL0O45.D HILL0050.D HILL0051.D HILL0052.D HILL0053.D HILL0054.D HILL0055.D HILL0056.D HILL0057.D HILL0058.D HILL0059.D HILL0064.D H IL L 0 0 6 5 .D HILL0066.D H IL L 0 0 6 7 .D H IL L 0 0 6 8 .D H IL L 0 0 6 9 .D H IL L 0 0 7 0 .D H IL L 0 0 7 1 .D H IL L 0 0 7 2 .D H IL L 0 0 7 3 .D H IL L 0 0 7 8 .D H IL L 0 0 7 9 .D H IL L 0 0 8 0 .D H IL L 0 0 8 1 .D H IL 1 0 0 8 2 .D H IL L 0 0 8 3 .D H IL L 0 0 8 4 .D H L L 0 0 8 5 .D H IL L 0 0 8 6 .D HILL0087.D H ILL 0O 92 .D H1LL0093.D H IL L 0 0 9 4 .D H IU 0 0 9 5 .D H IL L 0 0 9 6 .D HILL0097.D HILLD098.D HILL0099.D H IL L 0 1 0 0 .D HILL0101.D HILL0106.D HILL0107.D WLL0108.D HILL0109.D HILL0110.D HILL0111.D H ILL0112.D H IL L 0 1 1 3 .D HILL0114.D H IL L 0 1 1 5 .D h i l l q i 3o .p HILL0121.D H IL L 0 1 2 2 .D H IL L 0 1 2 3 .D H IL L 0 1 2 4 .D H IL L 01 3F .P MU L013S.D un 1 nyj-r n H H U 136J H IL L 0 1 3 3 .D HILL0134.D H IL L 0 1 3 5 .D HILL0136.D H IL L 0 1 3 7 .D HILL0138.D HILL0139.D HILL0140.D Sample Description EOO-1 3 1 1 - 4 0 5 9 - S 7 E0 0 - 1 3 1 1 -4 0 6 0 -S 7 0 0-1 311-4064-S7 E00-1311-4065-S7 00-1311-4066-S7 0 0-1 311-4088-S7 E00-1311-4089-S7 E00-1311-4090-S7 0 0 -1 3 1 1-4094-S7 00-1311-4095-S7 0 0 -1 3 1 1-4096-S7 0 0-1311-4118-S7 0 0-1311-4119-S7 E00-1311-4120-S7 E00-1311-4004-S8 E00-1311-4005-S8 E00-1311-4006-S8 EOO-1311-40O6MS-S8 E00-1311-4028-S8 EOO-1311-4030-S8 E 0 0 -1311-4030M S -S 8 E00-1311-4034-S8 E00-1311-4035-S8 EOO-1311-4036-S8 EOO-1311-4036MS-S6 EOO-1311-4058-S8 E00-1311-4059-S8 E 0 0 -1 3 1 1-4060-S8 EOO-1311-4060MS-S8 E00-1311-4064-S8 E 0 0 -1 3 1 1-4065-S8 EOO-1311-4066-SB EOO-1311-4066MS-S8 EOO-1311-4088-S8 EOO-1311-4089-S8 EOO-1311-4090-S8 EOO-1311-4090MS-S8 EOO-1311-4094-S8 E00-1311-4095-S8 EOO-1311-409&-S8 EOO-1311-4096MS-S8 EOO-1311-4118-S8 EOO-1311 - 4 1 10-S8 E00-1311-4120-S8 EOO-1311-4120MS-SB E 0 0-13 11 -50 01 -S 1 E00-1311-5002-S1 EOO-1311-5003-S1 E0 O -13 11 -5 Q 0 3M S-S1 EOO-1311-5004-S1 EOO-1311-5005-S1 E00-1311-5006-S1 EOO-1311-5O06MS-S1 EOO-1311-5007-S1 E00-1311-5008-S1 EOO-1311-5009-S1 EOO-1311-5009MS-S1 EOO-1311-5010-S1 EO O-1311 - 5 0 1 1-S1 E 00-1311-5012-S1 E00-13 1t-S 01 3M S -S 4 EOO-1311-5013-S1 E 0 0-13 11 -50 14 -S 1 EOO-1311-5015-S1 EOO-1311 - 5 0 1 5M S-S 1 60 0 -1 3 1 1-fi017-S1 EOO-4311-501&-S1 EOO 1311 5018MS.S1 E 0 0 - 1 3 1 1-5 0 1 9-S1 EOO-1311-502O-S1 E 00-1311-5021-S1 EOO-1311-5021MS-S1 EOO-1311-5022-S1 E 0 0-13 11 -50 23 -S 1 E 00-13 11 -50 24 -S 1 EOO-1311-5024MS-S1 A n alytical R un In fo rm atio n *: Acceptable Quant Range: 5 - 501 ng/ml Calibration C urve r2: 0.9960079 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Hillary Run ID : H010311 Measured C oncentration, ug/L Theoretical Matrix Spike C oncentration, ug/L R e p lic a te Sample %RSD 25.2 24.5 < 5 .0 < 5 .0 < 5 .0 37.7 42.6 38.4 < 5.0 < 5 .0 < 5.0 2.12 N/A 0.67 N/A 29.5 28.6 28.9 < 5 .0 1.82 < 5 .0 < 5 .0 205.4 12.3 N/A 200 10.4 214.9 < 5 .0 < 5.0 < 5.0 205.9 29.8 11.5 25.7 241.8 < 5 .0 < 5.0 < 5 .0 213.6 40.2 41.4 37.5 256.5 < 5 .0 < 5.0 < 5 .0 198.4 < 5 .0 29.7 25.6 246.5 14.1 < 5 .0 < 5 .0 221.6 196.1 197.5 198.5 428.8 11.52 200 N/A 200 43 02 200 N/A 200 5.02 200 N/A 200 10.56 200 N/A 200 0.61 200 253.2 183.9 169.5 415.6 435.7 22.12 200 403.3 4.30 406.6 xo. 102.7 110.0 102.9 311.8 68W 642-8 6&W 021* 15.6 < 5 .0 < 5.0 207,0 186.8 193.1 200.3 437.0 394 200 4.65 200 N/A 200 3.49 200 M atrix Spike Recovery. % 102.69 102.21 102.93 106.02 106.70 109 51 IS <1 30 % 99.20 11045 110.02 115.14 123 02 > 501ng/ml 104.40 > 501ng/mi > 501ng/rrrt > 501ng/ml 134.44 > 501 ng/ml 103.84 110.33 Q-Test C alculation (N -3 ) -0.77001074 D ilu tion 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 2 2 2 2 2 2 2 10 10 10 10 10 10 to 10 100 100 100 100 100 100 100 100 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 252 of 703 BACK TO MAIN Quality Control Samle Data Sam ple Data File RUSH0031.D RUSH0032.D RUSH0033.D RUSH0034.D RUSH0035.D RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D R USHQ Q 40.P R U S H 0 Q 4 5 .D R U S H Q 0 4 6 .D RUSH0047.D RUSH0048.D RUSH0049D RUSH0050.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D R USH0O 5C.D RUSH0060.D RUSH0061.D RUSH0062.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH0068.D RUSH0073.D RUSH0074.D RUSH0075.D RUSH0076.D RUSH0077.D RUSH0078.D RUSH0079.D RUSHOOBO.D RUSH0081.D RUSH0082.D Sam ple D escription 1 3 1 1 - 4 1 2 1 -S1 1311-412 2 -S 1 1311-4123-S1 1311-4123MS-S1 1311-4124-S1 1311-4125-S1 1 3 1 1-4126-S1 1311-4126MS-S1 1 3 1 1-4127-S1 1 3 1 1-4129-S1 1311-4129MS-S1 1 3 1 1-4130-S1 1311-4131 -S1 1311-4132-S1 1311-4132MS-S1 1 3 1 1-4133-S1 1311-4134-S1 1311-4135-S1 1311-4135MS-S1 1311-4137-S 1 1311-4138-S1 1 3 1 1-4138M S-S1 1 3 1 1-413 9 -S 1 1311-4140-S1 1311-4141-S1 1311-4141MS-S1 1311-4142-S1 1311-4143-S1 1311-4144-S1 1311-4144MS-S1 1311-4145-S1 1 3 1 1-414 6 -S 1 1311-4147-St 1311-4147MS-S1 1311-4148-S1 1311-4149-S1 1311-4150-S1 1311-4150MS-S1 A n a ly tic a l R u n In fo rm a tio n *: Acceptable Quant Range: 2.5 - 250.5ng/ml C alibration Curve r2: 0,9982281 Target Analyte: PFOS Internal Standard: THPFOS In stru m e n t: R ush R un ID: R 010314 M easured C oncentrt on, ug/L T h e o re tic a l M atrix Spike C oncentration, ug/L R e p lic a te Sam ple %RSD < 2 .5 < 2 .5 < 2 .5 197.9 < 2 .5 < 2 .5 < 2 .5 199.4 37.0 i g p 27.3 231.6 24.3 21.9 25.0 232.9 22.5 23.3 23.7 225.7 *-2 -5 22.8 23.2 228.1 20,7 20.4 21.0 228.2 20.4 21.3 20.7 224.5 19.5 19.2 19.0 223.2 20.1 20.0 20.2 224,3 N/A 200 N/A 200 21.30 200 6.77 200 2.75 200 *"No internal Standard Detected 1.17 200 1.43 200 2.05 200 1.29 200 0.29 200 M atrix Spike Recovery, % 98.95 99.68 102.17 103.95 100.96 102.42 103.62 101.88 102.09 102,04 0 -T e s t C a lc u la tio n (N = 3) . 0.925233823 point thrown out. Q value was nearly 0.94, and the matrix spike passed, -4128 is an obvious outlier. D ilution Factor, Nx 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 3M Environmental Laboratory Page 253 of 703 BACK TO MAIN Quality Control Sample Data S am p le D ata File HILL0031.D HILL0032.D HILL0033.D H IL L 0 0 3 4 .D HILL0035.D H IL L 0 0 3 6 .D HILL0037.D HILL0038.D HILL0039.D HILL0040.D W LL0Q 4S.D W U .Q 047,D LW .L0046J) m uoo4aja HILL0050.D HILL0051.D HILL0052.D W LL00S3.D HILL0054.D HILL0059.D H IL L 0 0 6 0 .D HILL0061.D H IL L 0 0 6 2 .D H IL L 0 0 6 3 .D HILL0064.D H IL L 0 0 6 5 .D HILL0066.D HILL0067.D HILL0068.D H L L Q Q 7 3 .D H U .L0076.D MILL0076iP M ILL0077.P wu-ooze.p M ILL0070, D f j i i j_nng?.D H 1 L L 0 0 8 1 iP S am p le D escription E00-1311-5O62-S2 EOO-13 1 1 - 5 0 6 3 - S 2 EOO-13 1 1-5063M S-S2 EOO-13 11-5064-S2 E 0 0 -1 3 1 1 -5 0 6 5 -S 2 EOO-13 1 1-5066-S2 EOO-13 1 1-5066M S-S2 EOO-13 1 1-5067-S2 EOO-13 1 1-5068-S2 EOO-13 1 1-5069-S2 0 0 -1 3 1 1.5068M S -S 3 0 0 -4 .3 1 1 .SQ70-S3 EOO-1311 -5071 -S3 EOO-13 1 1 . S 0 7 3 .S3 0 0 4 0 4 4 -5073M S -S 3 EOO-13 1 1 - 5 0 9 1 -S 2 EOO-13 1 1-5092-S2 EOO-13 1 1-5093-S2 0 0 .1 3 1 1-SQ 93M S-S3 EOO-13 1 1-5094-S2 EOO-13 1 1-5095-S2 EOO-13 1 1-5096-S2 EOO-13 1 1-5096M S-S2 EOO-13 1 1-5097-S2 EOO-13 1 1-5098-S2 EOO-13 11-5099-S2 EOO-13 1 1-5099M S-S2 EOO-13 11-5100-S2 EOO-13 1 1 - 5 1 0 1 -S 2 EOO-13 1 1 - 5 1 0 2 -S 2 FOO 1311 5103M S S3 6 0 0 4 3 4 1 .5 1 0 3 S3 00-1311 5104 S3 00-1311.510 5 S3 0 0 -1 3 4 1.510SM S-S3 EOO-1311 5 1 0 6 S3 00-4-311.6407.S 3 EOO-1311 5 1 0 8 S3 EOO 1311 5 1 0 B M S S 3 - Instrum ent: Hillary Run ID: H010313 M easured Th eo retical M atrix S p ik e C o n centration, ug /L C o n centration, u g /L R eplicate Sam ple % RSD 66.5 53.4 252 7 114 7 120 2 188.2 415.8 438.9 417.8 333.4 5 6 8 ,3 3 0 4 4 ,5 4457 5 40630 33404 137.5 49.S33? 335-1 41.7 35.2 34.6 250.2 127/! 126/ 15.51 200 29.03 200 14.08 300 16.17 300 75.71 300 10.62 200 4.01 1 3 5 .5 3 5 3 .fi 3 3 4 .7 200 3 2 7 . 342.{* 6404. 6364 <^2 ( 706-4 4 4 8 7 -i 3004*4 3 0 4 5 -- 2.19 300 M* 300 Mi 337834 40354) 300 M atrix Spike Recovery, % 99.62 113.82 147,40 380.10 >501 ng/mL >501 ng/mL >501 ng/mL >501 ng/mL >501 ng/mL 100.70 ISTD<70% 107.79 109.06 134.13 330.61 3334U >501 n g /m l >501 ng/mL >501 ng/ml>501 ng/mL >501 ng/mL >501 ng/mL >501 ng/mL >501 ng/mL >501 n g /m l Q -Test C alculation (N = 3) 0.844627602 A n alytical Run Inform ation*: A cceptable Q uant Range: 5 - 501 ng/ml C alibration Curve r2: 0.9961319 Target Analyte: PFOS Internal Standard: THPFOS D ilution F a c to r, 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 Q u a lity C o n tro l S am ple Data S a m p le D ata File RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0O40.D RUSH0041.D ftllSM 0043-Q RUSH0O43.D RUSH0D44.D RUSH0045.D RUSMOOSOD RUSH0051.D RUSH0052.D R U S H 0 0 S 3 .D RUSH0054.D RUSHOOS5.D RUSH0056.D RUSH0057.D RUSH0058.D RUSH0059.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH0068.D RUSH0069.D RUSH0O70.D RUSH0071.D RUSH0072.D RUSH0073.D RUSH0078.D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0082.D RUSH0O83.D RUSH0084.D RSH0085.D RUSH0086.D RUSH0087.D RUSH0092.D RUSH0093.D RUSH0094.D RUSH0095.D RUSH0O96.D RUSH0O97.D RUSH0098.D RUSH0099.D RUSH0100.D RUSH0101.D RUSH0106.D RUSH0107.D RUSH0108.D RUSH0109.D RUSH0110.D RUSH0111.D R U S H 0112.D RUSH0113.D RUSH0114.D RUSH0115.D RUSH0120.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 RUSH0137.D RUSH0138.D RUSH0139.D RUSH0140D Sample D escriptio n 1 3 1 1-4 05 8-S4 1311-4059-S4 1311-4064-S4 1311-4065-S4 1311-4066-S4 1311-4088-S4 4m -4oao-s4^ 1311-4090-S4 1311-4094-S4 1311-4095-S4 n u ^ a a s ^ .: 1 3 1 1 - 4 1 18 -S4 1311-4119-S4 1311-4120-S4 1311-4004-S5 1311-4005-S5 1311-4006-S5 1311-4028-S5 1311-4030-S5 . 1311-4034-S5 1311-4035-S5 1311-4036-S5 1311-4058-S5 1311-4059-S5 1311-4060-S5 1311-4064-S5 1311-4065-S5 1311-4066-S5 1311-4088-S5 1311-4089-S5 1311-4090-S5 1311-4094-S5 1311-4095-S5 1311-4096-S5 1 3 1 1 - 4 1 18 -S5 1311-4119-S5 1311-4120-S5 1311-4004-S6 1311-4005-S6 1311-4006-S6 1311-4006MS-S6 1311-4028-S6 1311-4030-S6 1311-4030MS-S6 1311-4034-S6 1311-4035-S6 1311-4036-S6 1311-4036MS-S6 1311-4058-S6 1311-4059-S6 1311-4060-S6 1311-4060MS-S6 1311-4064-S6 1311-4065-S6 1 3 1 1 - 4 0 6 6 - S6 1311-4066MS-S6 1311-4088-S6 1311-40B9-S6 1311-4090-S6 1311-4090MS-S6 . 1311-4094-S6 1311-4095-S6 1311-4096-S6 1311-4096MS-S6 1311-4118-S6 1 3 1 1 - 4 1 19 -S6 1311-4120-S6 1311-4120MS-S6 1311-4004-S7 1311-40O5-S7 1311-4006-S7 1311-4028-S7 1311-403O-S7 1311-4034-S7 1311-4035-S7 1311-4036-S7 1311-4058-S7 A nalytical R un Information*: Acceptable Quant Range: 5 - 250.5ng/m l Calibration Curve t2: 0.9936833 Target Analyte: PFOS Internal Standard: THPFOS instrum ent: Rush R un ID: R010309 Theoretical M atrix M easured Spike C oncentration, C oncentration, ug/L ug/L R e p lic a te Sample %RSD 9.6 9.6 <5.0 <5.0 <5.0 76.8 <5.0 21.0 <5.0 94.0 4-3 044 N/A 80.61 129 33 12.3 17.8 15.9 <5.0 <5.0 <5.0 10,3 6.2 < 5 .0 <5.0 <5.0 27.1 27.1 32.9 <5.0 <5.0 <5.0 40.3 43.8 45.4 <5.0 <5.0 <5.0 18.9 24.1 26.3 <5.0 <5.0 <5.0 217.8 9.9 9.4 241.4 <5.0 <5.0 <5.0 226.5 29.6 28.0 27.2 208.2 <5.0 <5.0 <5.0 220.8 38.5 40.5 36.7 260.5 <5.0 <5.0 <5.0 211.0 29.6 28.5 25.9 262.6 <5.0 <5.0 < 5 .0 9.9 10.4 <5.0 8.9 <5,0 27.7 16.27 N/A 35.38 N/A 11.4 N/A 609 N/A 16.31 N/A 200 3.69 200 N/A 200 4.23 201 N/A 202 4 82 203 N/A 204 6 76 205 N/A 3.68 N/A D ilu tion M atrix Spike Factor, Recovery, % Nx 2 2 2 2 2 * No IS tddBd 2 2 2 2 2 'IS >70% 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 2 106.9 2 2 2 116,0 2 2 2 2 113,3 2 2 2 2 2 90.0 2 2 2 1093 2 2 2 2 110.2 2 2 2 103.4 2 2 2 2 2 115.5 2 2 2 2 2 2 2 2 2 '2 ?. 3M Environmental Laboratory Page 255 of 703 BACK TO MAIN Quality Control Sample Data S a m p le D ata File HILL0036.D HILL0037.D HIL10038.D HILL0039.D HILLOQ40.D HILL0041.D HILL0O42.D HILL0O43.D H IL L 0 0 4 4 .D HILL0045.D HILL0O50.D HILL0051.D HILL0O52.D HILL0053.D HILL0O54.D HILL0055.D H IL L 0 0 5 6 .D HILL0057.D HILL0058.D H IL L 0 0 5 9 .D HILL0O64.D HILL.0065.D H IL L 0 0 6 6 .D H ILL 0O 67 .D H IL L 0 0 6 8 .D H IL L 0 0 6 9 .D H IL L 0 0 7 0 .D HILL0071 .D H IL L 0 0 7 2 .D H IL L 0 0 7 3 .D H ILL 0O 78 .D H IL L 0 0 7 9 .D H IL L 0 0 8 0 .D H IL L 0 0 8 1 .D H IL L 0 0 8 2 .D H ILL 0O 83 .D H ILL 0O 84 .D H IL L 0 0 8 5 .D H ILL 0O 86 .D H IL L 0 0 8 7 .D H ILL 0O 92 .D H ILL 0O 93 .D H IL L 0 0 9 4 .D H ILL 0O 95 .D H ILL 0O 96 .D HILL0O97.D H ILL 0O 98 .D H IL L 0 0 9 9 .D H IL L 0 1 0 0 .D HILL0101.D H IL L 0 1 0 6 .D HILL0107.D H IL L 0 1 0 8 .D HILL0109.D H ILL0110.D HILL0111.D H IL L 0 1 1 2 .D H1LL0113.D HILL0114.D H IL L 0 1 1 5 .D H IL L 0 1 2 0 .D H IL L 0 1 2 1 .D H IL L 0 1 2 2 .D H IL L 0 1 2 3 .D H IL L 0 1 2 4 .D H IL L 0 1 2 5 .D H IL L 0 1 2 6 .D H IL L 0 1 2 7 .D H IL L 0 1 2 8 .D H IL L 0 1 3 3 .D H IL L 0 1 3 4 .D H IL L 0 1 3 5 .D H IL L 0 1 3 6 .D H IL L 0 1 3 7 .D H IL L 0 1 3 8 .D H IL L 0 1 3 9 .D H IL L 0 1 4 0 .D Sample D escription EOO-1311-4103-S1 EOO-1311-4104-S1 EOO-1311-4105-S1 E O O -1 31 1-4 10 5-S 1 -M S EOO-1311-4106-S1 E O O -1 3 1 1 -4 1 0 7 -S t EOO-1311-4108-S1 E O O -1 31 1-4 10 8-S 1 -M S EOO-1311 - 4 109-S1 EO O-1311 - 4 1 10-S1 EOO-131 M 1 1 1 -S 1 EO O-1311 - 4 1 1 1 - S 1 - M S EOO-1311 - 4 1 12-S1 EO O-1311 - 4 1 13-S1 EO O-1311 - 4 1 14-S1 EO O-1311 - 4 1 1 4 -S 1 -M S EO O-1311 - 4 1 15-S1 EOO-1311 - 4 1 16-S1 EO O-1311 - 4 1 17-S1 EO O-1311 -4 1 17 -S 1 -M S EOO-1311 - 4 1 18-S1 EO O-1311 - 4 1 1 9 - S I EOO-1311 - 4 120-S1 E O O -1 31 1-4 12 0-S 1 -M S EOO-1311-4004-S2 E00-1311-4005-S2 EOO-1311-4006-S2 EOO-1311-4028-S2 EOO-1311-4030-S2 EOO-1311-4034-S2 EOO-1311-4035-S2 EOO-1311-4036-S2 EOO-1311-4058-S2 EOO-1311-4059-S2 EOO-1311-4060-S2 EOO-1311-4064-S2 EOO-1311-4065-S2 EOO-1311-4066-S2 EOO-1311-4088-S2 EOO-1311-4089-S2 E0O-131.1-4O90-S2 EOO-1311-4094-S2 EOO-1311-4095-S2 EOO-1311-4096-S2 EOO-1311-4118-S2 EO O-1311 - 4 1 19 -S2 EOO-1311-4120-S2 EOO-1311-4004-S3 EOO-1311-4005-S3 EOO-1311-400B-S3 EOO-1311-4028-S3 EOO-1311-403O-S3 EOO-1311-4035-S3 EOO-1311-4036-S3 EOO-1311-4058-S3 E O O -1 31 1-4 05 9-S 3 EOO-1311-406O-S3 EOO-1311-4064-S3 EOO-1311-4065-S3 EOO-1311-4066-S3 EO O-131 1-4 0 8 6 -S 3 EOO-1311-4089-S3 EOO-1311-4090-S3 EOO-1311-4094-S3 EOO-1311-4095-S3 EOO-1311-4096-S3 E 00-1311-4118-S3 EO O-1311 - 4 1 19 -S3 EO O-1311 - 4 12 0-S3 E 0 0 -1 3 1 1-4004-S4 EOO-1311-4005-S4 EOO-1311-4006-S4 EOO-1311-402B-S4 EOO-1311-4030-S4 EOO-1311-4034-S4 E00-1311-4035-S4 EOO-1311-4036-S4 A n a lytica l Run Inform ation*: A cceptable Quant Range: 5 - 400.8ng/m l Calibration C urve r2: 0.9924853 T arget A nalyte: PFOS Internal Standard: THPFOS Instrument: Hillary Run ID: H010309 Itn o re tic a l M atrix Measured Spike C oncentration, C oncentration, ug/L ug/L R e p lic a te Sample %RSD 8.012285 6.1696 8.375534 15.73 190.967177 11 .5 34 11 3 2C0 11.512441 1 0 .7 8 9 9 8 5 3.75 195.20857 5.573715 5,956354 200 4.53 5.468121 190.080867 5.648499 200 5.788465 12.99 7.103971 196.371648 5.890369 6.081276 5.516164 188.305604 6.353969 200 4.93 200 6.139234 2.40 6.068331 187.872851 * 5.0 c 5.0 < 5.0 200 N/A 10 .5 40 60 4 10 .7 58 79 6 1.45 < 5 .0 < 5.0 < 5.0 N/A 9.632074 10 .8 82 82 3 13.580921 < 5 .0 17.76 < 5 .0 N/A < 5 .0 2 4 .5 6 5 4 4 7 2 2 .1 6 6 6 0 3 2 3 .3 1 4 4 3 3 514 < 5.0 < 5 .0 < 5 .0 N/A 15 .6 47 20 5 15.158642 17 .5 40 00 6 7.00 2 9 .0 4 1 6 2 9 < 5.0 N/A < 5.0 10 .3 90 45 5 10 .0 82 18 6 < 5 .0 13 < 5.0 3.728289 5.345841 11 .4 36 61 8 < 5.0 59.45 < 5 ,0 < 5.0 N/A 17 .1 40 26 2 2 2 .5 2 5 8 6 4 23 .1 12 19 1 < 5 .0 15.73 < 5 .0 N/A < 5 .0 8.254569 < 5 .0 97 66 45 .0 9 7 1 7 0 < 5 .0 < 5 .0 < 5 .0 N/A 12 .3 02 80 9 8.300946 < 5 .0 27.47 < 5 .0 < 5 .0 N/A M atrix Spike Recovery, % 91.30 92 21 9231 94 63 91.39 90 90 D ilu tion Factor, Nx 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 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 3M Environmental Laboratory Page 256 of 703 BACK TO MAIN Quality Control Sampla Data In s tru m e n t: R u sh R u n ID : r0 1 0 2 2 2 Q -Test D ilution C alc u la tio n (N -3 ) F a c to r, Nx 10 10 10 10 10 0.9883 10 10 10 1100 10 10 10 10 10 10 10 1100 10 1100 10 10 10 1100 10 10 1100 1100 10 10 10 0.9976 10 10 10 High internal standard response 10 10 A n a ly tic a l R un In fo rm a tio n *: Acceptable Quant Range: 5.0ppb-500.1ppb Calibration Curve r2: 0.9999393 Target Analyte: PFOS Internal Standard: THPFOS ` For more run info. See the Data Review Form Included in the Raw Data 3M Environmental Laboratory > Page 257 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Hillary Run ID: H010222 S a m p le D a ta F ile H ILL0037.D H ILL0038.D H ILL0039.D H ILL0040.D H ILL0041.D H ILL0042.D H ILL0043.D H ILL0044.D H ILL0045.D H ILL0046.D H ILL0051.D H ILL0052.D H ILL0053.D H ILL0054.D H ILL0055.D H ILL0056.D H ILL0057.D H ILL0058.D H ILL0059.D H ILL0060.D H ILL0065.D H ILL0O 66.D H 1 L L 0 0 6 7 .D H IU 00 68 .D H ILL0069.D H ILL0070.D H ILL0071.D H ILL0072.D H ILL 00 73 .D H ILL0074.D H ILL0079.D H ILL0080.D H ILL 00 81 .D H ILL0082.D H ILL0083.D H ILL0084.D H ILL 00 85 .D H ILL0086.D H ILL0087.D H ILL0088.D H ILL0093.D H ILL0094.D H ILL0095.D H ILL0096.D H ILL0097.D H ILL0098.D H ILL0099.D H ILL0100.D H ILL0101.D H ILL0102.D H ILL0107.D H ILL0108.D H ILL0109.D H ILL0110.D H ILL0111.D H ILL0112.D H ILL0113.D H IL L 0 1 14.D H ILL0115.D H ILL0116.D H ILL0121.D H ILL0122.D H ILL0123.D H 1LL0124.D H ILL0125.D H ILL0126.D H ILL0127.D H ILL0128.D S a m p le D e s c rip tio n 1 3 1 1 -4 0 0 1 -S1 1 3 1 1-4002-S1 1311-4003-S 1 1 3 1 1-4003M S-S1 1311-4004-S 1 1311-4005-S 1 1 3 1 1-4006-S1 13 11-4006M S-S1 1 3 1 1 -4 0 0 7 -S1 13 1 1-4008-S1 1311-4009-S 1 13 11-4009M S-S1 1311-4010-S 1 1 3 1 1 -4 0 1 1-S1 13 11 -40 12-S1 1 3 1 1-4012M S-S1 13 1 1-4013-S1 13 1 1-4014-S1 1 3 1 1 -4 0 1 5-S1 1311 -40 15M S-S1 13 11 -40 16-S1 13 11 -40 17-S1 1311-4018-S 1 1311-4018M S-S1 1311-4019-S 1 1311-4020-S 1 1311-4021-S 1 13 11 -40 21M S-S1 1311-4022-S 1 1311-4023-S 1 1311-4024-S 1 1 3 1 1-4024M S-S1 1311-402S-S1 1311-4026-S 1 1311-4027-S 1 1311-4027M S -S 1 1311-4028-S 1 1311-4029-S 1 13 1 1-4030-S1 1311-4030M S -S 1 13 1 1-4031-S1 13 1 1-4032-S1 1311-4033-S 1 13 11-4033M S-S1 1311-4034-S 1 1311-4035-S 1 1311-4036-S 1 1311-4036M S -S 1 1311-4037-S 1 1 3 1 1-4038-S1 13 1 1-4039-S1 13 11-4039M S-S1 1 3 1 1 -4 0 4 0-S1 13 11-4041-S1 1311-4042-S 1 13 1 1-4042M S-S1 1 3 1 1 -4 0 4 3-S1 1311-4044-S 1 13 11 -4045-S1 1311-4045M S -S 1 13 1 1-4046-S1 1311-4047-S 1 1 3 1 1-4048-S1 1311-4048M S-S1 1 3 1 1-4049-S1 1311-4050-S 1 1 3 1 1 -4 0 5 1 -S1 13 1 1 -4 0 5 1 M S-S1 M easured C on cen trati on, ug /L < 5 .0 < 5 .0 < 5.0 2 0 4 .7 < 5.0 < 5 .0 < 5 .0 2 0 4 .3 5 1 .2 5 5 .2 8 6 .0 256.1 5 2 .8 5 2 .4 5 0 .9 2 4 7 .2 51.1 5 2 .4 5 2 .6 251.1 51 .9 5 0 .2 5 1 .4 2 4 5 .8 4 9 .0 5 0 .7 5 0 .2 2 4 7 .5 S S .8 4 9 .3 5 2 .2 2 4 7 .3 5 2 .0 49 .7 5 2 .2 249.1 5 0 .5 5 3 .4 5 1 .0 2 4 8 .3 < 5.0 < 5 .0 < 5 .0 2 0 0 .9 < 5 .0 < 6 .0 < 5 .0 2 0 2 .3 3 6 .6 3 3 .0 2 8 .9 2 2 4 .0 1 1 .7 10.4 1 1 .3 2 1 0 .8 1 1 .5 9.9 1 0 ,2 2098 1 3 .6 1 1 .2 12.9 2 1 1 .8 9.5 8.7 10.4 2 0 9 .5 th e o re tic a l M a trix S p ike C o n ce n tra tio n , ug /L R e p lic a te S a m p le % RSD N/A 200 N/A 200 2970 200 1.92 200 1. 200 1.73 200 1.76 200 672 200 2.73 200 3.99 200 N/A 200 N/A 200 1175 200 5.83 200 7.95 200 979 200 876 200 M a trix S p ike R ecovery, % 102.35 102.15 85.05 98.17 99.29 97.19 98.67 97.54 98.42 98.65 100.45 101.16 97.98 9975 99.81 99.41 99.56 Analytical Run Inform ation*: A cce p ta b le Q u an t R ange: 5 .0 p p b -2 5 0 .5 p p b C a lib r a tio n C u rv e r2: 0 .9 9 8 3 5 6 6 T a rg e t A n alyte : PFO S Internal Standard: TH P FO S * f o r m o re run info . S e e th e D a ta R e v ie w F orm in c lu d e d in th e R a w D ata D ilu tio n F actor, Nx 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 10 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 S am ple Data File HILL0032.D HILL0033.D HILL0034.D HILL0035.D HILL0036.D HILL0037.D HILL0038.D HILL0039.D HILL0040.D HILL0041.D HILL0046.D HILL0047.D HILL0048.D HILL0049.D HILL0054.D HILL0056.D HILL0058.D HILL0060.D HILL0062.D HILL0064.D HILL0066.D HILL0068.D HILL0070.D HILL0072.D Sample D escription 1311-5207-S2 1311-5207MS-S2 1311-5208-S2 1311-5209-S2 1311-5210-S2 1311-5210MS-S2 1 3 1 1 -5 2 1 1-S2 1311-5212-S2 1311-5213-S2 1311-5213MS-S2 1311-5214-S2 1311-5215-S2 1311-5216-S2 1311-5216MS-S2 1311-4151 -S1 1311-4152-S1 1311-4153-S1 1311-4153MS-S1 1 31 1-4 15 4 -S I 1 3 1 1-4155-S 1 1311-4156-SI 1311-4156-MS-S1 1311-4157-SI 1311-4158-S1 Analytical Run Information*: Acceptable Quant Range: 2.5 - 1002ng/ml Calibration Curve r2: 0.9987251 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Hillary Run ID: H 010402 (A) M easured C o n ce n tra tio n , ug/L 2.852832 190.426303 9.070036 9.465038 7.399684 180.05532 16.467401 20.404356 19.825832 204.154139 105.301943 92.717039 82.480799 259.591125 < 2.5 < 2.5 < 2.5 98.223696 < 2.5 < 2.5 < 2.5 90.564759 < 2.5 <2.5 T h e o re tic a l M atrix Spike C o n c e n tra tio n , ug/L R e p lic a te Sample %RSD 200 12.68 200 11.25 200 12.23 200 N/A 200 N/A 200 N/A M atrix Spike Recovery, % 93.79 86.33 92.16 88.56 49.11 45.28 !S> 130% IS> 130% IS> 130% IS> 130% IS> 130% !S> 130% IS> 130% IS> 130% IS> 130% IS> 130% D ilution Factor, Nx 2 2 10 10 10 10 10 10 10 10 100 100 100 100 2 2 2 2 2 2 2 2 2 2 3M Environmental Laboratory Page 259 of 703 BACK TO MAIN Quality Control Sample Data Sam ple Data File RUSH0037.D RUSH0038.D RUSH0039.D RUSH0040.D RUSH0041.D RUSH0042.D RUSH0043.D RUSH0048.D RUSH0049.D RUSH0050.D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.D RUSH0056.D RUSH0057.D RUSH0062.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH0068.D RUSH0069.D RUSH0070.D RUSH0071.D RUSH0076.D RUSH0077.D RUSH0078.D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0082.D RUSH0083.D RUSH0084.D RUSH0085.D RUSH0090.D RUSH0091.D RUSH0092.D R U SH 0093.D RUSH0094.D RUSH0095.D RUSH0096.D RUSH0097.D RUSH0098.D RUSH0099.D Sample D escription 1311-5025-S1 1 3 1 1-5026-S 1 1311-5027-S1 1311-5027MS-S1 1 3 1 1-5028 -S 1 1311-5029-S1 1 3 1 1-5030 -S 1 1311-5030MS-S1 1 3 1 1-5031-S 1 1 3 1 1-5032 -S 1 1 3 1 1-5033-S 1 1311-5033MS-S1 1311-5034-S 1 3 1 1-5035-S 1 1311-5036-S1 1311-5036MS-S1 1311-5037-S1 1311-5038-1S 1311-5039-S1 1311-5039MS-S1 1 3 1 1-5040 -S 1 1311-5041-S1 1 3 1 1-5042-S 1 1311-5042MS-S1 1 3 1 1-5043 -S 1 1311-5044S1 1 3 1 1-5045 -S 1 1311-5045MS-S1 1311-5046-S1 1 3 1 1-5047 -S 1 1 3 1 1-5048-S 1 1311-5048MS-S1 1311-5049-S1 1311-5050-1S 1311-5051-S1 1311-5051MS-S1 1 3 1 1-5052 -S 1 1311-5053-S1 1 3 1 1-S054-S1 1311-5054MS-S1 1311-5055-S1 1 3 1 1-5056-S 1 1311-5057-S1 1311-5057MS-S1 1311-5058-S1 1 3 1 1-5059-S 1 1311-5060-S1 Analytical Run Information*: Acceptable Quant Range: 5 - 501ng/ml Calibration Curve r2; 0.9997025 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Rush Run ID: R010329a M easured C oncentration, ug/L 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 4 1 .7 7 10.29 5.71 227.32 31.83 34.15 32.79 T h e o re tic a l M atrix Spike C oncentration, ug/L R e p lic a te M atrix Spike Sample %RSD Recovery, % 5.50 200 27.35 201 2.86 202 3.59 203 N/A 204 27.21 205 28.62 206 8.16 207 1.56 208 11.34 209 101,93 210 3.54 136.22 - N/A 123.22 N/A N/A 121.02 N/A 128.85 N/A 139.74 105.53 D ilution Factor, Nx 10 10 10 10 10 10 10 10 100 100 100 100 100 100 100 100 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 Quality Control Sample Data S am ple Data File RUSH0120.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 RUSH0137.D RUSH0138.D RUSH0139.D RUSH0140.D RUSH0141.D RUSH0142.D RUSH0143.D RUSH0148.D RUSH0149.D RUSH0150.D R U S H 0 1 5 1 .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 R U SH 0176.D RUSH0177.D RUSH0178.D RUSH0179.D Sample D escription 1311-5060MS-S1 1311-5061 -S 1 1 3 1 1-5062-S 1 1311-5063-S1 1311-5063MS-S1 1 3 1 1-5064-S 1 1311-5065-S1 1311-5066-S1 1311-5066MS-S1 1 3 1 1-5067-S 1 1 3 1 1- 5068-S 1 1 3 1 1-5069-S 1 1311-5069MS-S1 1 3 1 1-5070-S 1 1311-5071-S1 1311-5072-S1 1311-5072MS-S1 1311-5073-S1 1311-5074-S1 1 3 1 1-5075-S 1 1311-5075MS-S1 1 3 1 1-5076-S 1 1 3 1 1- 5077-S 1 1 3 1 1-5 078-S 1 1311-5078MS-S1 1 3 1 1-5079-S 1 1311-5080-S1 1311-5081-S 1 1311-5081MS-S1 1 3 1 1-5082-S 1 1311-5083-S1 1 3 1 1-5084-S 1 1311-5084MS-S1 1 3 1 1-5085-S 1 1311-5086-S1 1311-5087-S1 1311-5087MS-S1 1 3 1 1 -5 0 8 8-S1 1311-5089-S1 1311-5090-S1 1311 -5091 -S1 1311-5092-S1 1 3 1 1-5093-S 1 1311-5093MS-S1 Analytical Run Information*: Acceptable Quant Range: 5,0 - 501ng/ml Calibration Curve t2: 0.9998900 Target Analyte: PFOS Internal Standard: THPFOS Instrument: Rush Run ID: R 010329b M easured C o n c e n tra tio n , ug/L < 5 .0 <5.0 < 5.0 > 501 > 501 > 501 > 501 > 501 >501 > 501 > 501 < 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 Theoretical M atrix Spike C o n c e n tra tio n , ug/L R e p lic a te Sample %RSD 2.93 200 3.84 200 4.30 200 3.99 200 N/A 200 13.95 200 N/A 200 2.72 200 N/A 200 4.37 97.90 200 M atrix Spike Recovery, % 142.34 125.78 146.66 125.08 1 0 3 .80 1 1 4 .18 N/A N/A N/A 110.71 5 / /s'/i D ilution Factor, Nx 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 2 2 2 2 > 3M Environmental Laboratory Page 261 of 703 BACK TO MAIN Q u a lity C o n tro l S a m ple Data S am ple Data File R U S H 0 0 3 0 .D RUSH0031.D RUSH0032.D BU S H O O .D RUSH0034.D RUSH0035.D RUSH0036.D R U S H 0 0 3 7 .D RUSH0038.D RUSH0039.D R U S H 0 0 4 4 .D RUSH0O45.D RUSH0O46.D RUSH0047.D R U S H 0 0 4 B .D p i lounnAQ n RUSH0050.D R U S H 0 0 5 1 .D RUSH0052.D RUSH0053.D RUSH0058.D RUSH0059.D RUSH0060.D BIISH0061.Q RUSH0062.D RUSH0063.D R U S H 0 0 6 4 .D RUSH0065.D R U S H 0 0 6 6 .D R U S H 0 0 6 7 .D R U S H 0 0 7 2 .D RUSH0073.D R U S H 0 0 7 4 .D RUSH0075.D RUSH0076.D RUSH0077.D R U S H 0 0 7 8 .D RUSH0O79.D RUSH0080.D B U S H 0 0 8 1 .D R U S H 0 0 8 6 .D R U S H 0 0 8 7 .D RUSH0088.D R U S H 0 0 8 9 .D R U S H 0 0 9 0 .D RUSH0091.D RUSH0092.D R U S H 00 93 .0 RUSH094.D R U S H 0 0 9 5 .D RUSH0100.D RUSH0101.D R U S H 0 1 0 2 .D RUSH0103.D RUSH0104.D RUSH0105.D R U S H 0 1 0 6 .D RUSH0107.D RUSH0108.D RUSH0109.D RUSH0114.D RUSH0115.D R U SH 0116.D RUSH0117.D R U S H 0 1 1 8 .D RUSH0119.D RUSH0120.D RUSH0121.D R U S H 0 1 2 2 .D R U S H 0 1 2 3 .D RUSH0128.D R U S H 0 1 2 9 .D R U S H 0 1 3 0 .D RUSH0131.D RUSH0132.D RUSH0133.D RUSH0134.D S im p le D escription 1 3 11 -50 88 -S 1 1 3 1 1-508 9-S1 1311-5090-S1 nn-snooM S -si 1 3 1 1- 5091-S1 1 3 1 1-509 2-S1 1311-5093-S1 1311-5093MS-S1 1 3 1 1- 5094-S1 1311*5095-81 1 3 1 1-509 6-S1 1311-5096MS-S1 1311-5097-S1 1 3 1 1-509 8-S1 1 3 11 -50 99 -S 1 13H 4009M S .S 1311-51Q0-S1 1 3 1 1-510 1-S1 1 3 11 -51 02 -S 1 1 3 1 1 -5 1 0 2 M S -S 1 1 3 11 -51 03 -S 1 1 3 1 1-510 4-S1 1311-5105-S1 1314 41 05 M S -S 1 13 11 -51 06 -S 1 1 3 1 1-510 7-S1 1311-5108-S1 1311-5108MS-S1 1 3 1 1 -5 1 0 9 -S 1 1 3 1 1 - 5 1 10-S1 1 3 1 1 - 5 1 1 1-S1 1 3 1 1 - 5 1 11MS-S 1 1 3 1 1 - 5 1 12-S1 1 3 1 1 - 5 1 13-S1 1 3 1 1- 511 4- S1 1 3 1 1 - 5 1 14 M S-S1 1 3 1 1 - 5 1 15-S1 1 3 1 1 - 5 1 16-S1 1 3 1 1- 511 7- S1 1311 5 1 17MS-S1 1 3 1 1 - 5 1 18-S1 1 3 1 1- 511 9- S1 1 3 11 -51 20 -S 1 1 3 1 1 -5 1 2 0 M S -S 1 1311-5019-S2 1311-5020-S2 1311-5021-S2 1311-5021MS-S2 1311-5022-S2 1311-5023-S2 1311-5024-S2 1311-5024MS-S2 1311-5025-S2 1311-5026-S2 1 3 1 1-5 02 7-S2 1311-5027MS-S2 1311-5028-S2 1311-5029-S2 1311-5030-S2 1311-5030MS-S2 1 3 1 1 -5 0 3 1 -S 2 1 3 1 1-5 0 3 2 -S 2 1 3 1 1-5 03 3-S2 1311-5033MS-S2 1311-5034-S2 1 3 1 1 -5 0 3 5 -S 2 1 3 1 1 -5 0 3 6 -S 2 1311-5035MS-S2 1 3 1 1 -5 0 5 5 -S 2 1 3 1 1- 5056-S2 1 3 1 1 -5 0 5 7 -S 2 1311-5057MS-S2 1 3 1 1-5 0 5 8 -S 2 1311-5059-S2 1311-5060-S2 1311-5060MS-S2 1311-5061-S2 A nalytical Run Information*: 0Acceptable Quant Ran e: 5 * 5Q1ng/ml Calibration Curve i2: 0.9992811 Target Analyte: PFOS Internal Standard: TH PFO S instrument: Rush R u n ID : R 0 1 0 3 1 2 M easured C oncentration, u g /L Theoretical M atrix Spike C oncentration, ug/L R e p lic a te Sample %RSD 239.0 268.9 269.9 5234 34.6 7.3 < 5 .0 203.3 49.0 54.8 46.2 263.8 4.27 30C 92 09 200 B 96 200 191.2 249.9 239.1 506.0 153.8 140.8 138.0 370.7 321.0 306.8 305.4 5024 180.1 176.0 170.2 407.9 13.4 < 5.0 < 5.0 205.6 62.4 61.1 66.1 13.77 aoa 5.82 200 2-77 206 2M 200 N/A 200 4.11 277.7 324.3 337.1 303.4 6054 200.5 177.7 204.6 460.9 5.2 < 5 .0 < 5.0 197.9 200 5.30 306 7.47 200 N/A 200 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 < 5 .0 < 5 .0 206.8 10.9 11.9 29.0 245.7 75.7 5.76 200 11.01 200 30.03 200 4.26 200 23 63 200 N/A 200 58 59 200 M atrix Spike Recovery, % 13606 < 501 ng/ml 101.67 108.84 133,46- < 501 ng/ml 116.34 444,36 <501 nm1 118.B6 102.81 105.79 163.36, <501 ne/irf 128.13 96 95 96.26 107.79 111.62 111.36 129.85 103 39 108 36 D ilution Factor, Nx 100 100 100 100 2 2 2 3 2 2 2 2 2 2 2 2 10 1100 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 2 2 2 2 2 2 2 2 2 2 2 2 22 2 2 2 2 2 2 22 2 2 2 22 2 2 3M Environmental Laboratory Page 262 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run ID: s001120a Sam ple Data File s00120_035 S00120_036 S00120 037 S00120 038 sD0120_039 S00120 043 S00120 044 S00120 046 S00120JM6 s00120_047 s00120_051 s00120_052 S00120_053 S00120_054 s00120^055 s00120_059 S00120^060 s00120_061 s00120,062 500120,063 s00120_067 sOO120,060 500120,069 s00120_070 S00120,071 s00120_075 s00120_076 s00120_077 500120,078 900120,079 S00120_083 900120,084 900120,085 Sample Description EOO-1311-1001 Ohr E00-1311-1002 Ohr EOO-1311-1003 Ohr EOO-1311-1004 Ohr EOO-1311-1005 Ohr EOO-1311-1006 Ohr E0O-1311-1OO7 Ohr EOO-1311-1008 Ohr EOO-1311-1009 Ohr EOO-1311-1010 24 hour, Omg/L, S1, C-1 EOO-1311-1011 24 hour. Omg/L, S1. C-1 EOO-1311-1012 24 hour, Omg/L, S1, C-1 EOO-1311-1012 24 hour, Omg/L, S1, C-1, MS EOO-1311-1013 24 hour, 0.10mg/L. S1, C-1 EOO-1311-1014 24 hour, 0.1 Omg/L. S1, C-1 EOO-1311-1015 24 hour. 0.1Omg/L. S t, C-1 EOO-1311-1015 24 hour, 0.1 Omg/L, S1, C-1, MS EOO-1311-1016 24 hour. 1.Omg/L, S1. C-1 EOO-1311-1017 24 hour, 1.Omg/L, S t, C-1 EOO-1311-1018 24 hour, 1.Omg/L, S1.C-1 EOO-1311-1018 24 hour, 1.Omg/L, S1.C-1 MS EOO-1311-1010 24 hour, Omg/L, S2, C-1 EOO-1311-1011 24 hour, Omg/L. S2. C-1 EOO-1311-1012 24 hour, Omg/L, S2, C-1 E00-1311-1012 24 hour, Omg/L. S2, C-1, MS EOO-1311-1013 24 hour, 0.1 Omg/L. S2, C-1 EOO-1311-1014 24 hour, 0.1Omg/L. S2, C-1 EOO-1311-1015 24 hour, 0.1 Omg/L. S2, C-1 EOO-1311-1015 24 hour, 0.1Omg/L, S2, C-1. MS EOO-1311-1016 24 hour, 1.Omg/L, S2, C-1 EOO-1311-1017 24 hour, 1.Omg/L, S2. C-1 EOO-1311-1018 24 hour, 1.Omg/L, S2. C-1 EOO-1311-1018 24 hour, lOmg/L, S2, C-1, MS Theoretical Matrix^ Measured Spike Concentration, Concentration, ug/L ug/L R e p lic a te Sample %RSD <24,75 <24.75 <24.75 <24.75 <24.75 <24.75 486.97 523.02 544.09 25.86 " Point thrown out <24.75 <24.75 217.61 200 <24.75 <24.75 <24.75 253.23 462.08 200 475.12 505.67 719.03 200 <24.75 <24.75 <24.75 248.01 200 <24.75 <24.75 <24.75 254.5 200 110.87 118.37 137.3 344.75 200 N/A N /A 5.58 N /A N/A 4.65 N /A N/A 11.15 M atrix Spike Recovery, % 108.81 126,62 106.68 124.01 127.25 103.73 A nalytical Run Inform ation*: Acceptable Quant Range: 24.75ppb-991.78ppb Calibration Curve ^0 .9 9 6 9 3 9 Target Analyte: PFOS Internal Standard: THPFOS *For more run info. See the Data Review Form included in the Raw Data Q > (\r c x 3UCr loS'A -P ur GiiesV ^ i x v t : o. i 8g Q-Test C a lc u la tio n (N = 3) Cx\ooo 3M Environmental Laboratory Page 263 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run ID: s001120b Sam ple Data File s00120_103 S00120JD4 S0012CM05 S0012CM06 800120.110 S 0 0 1 2 0 J 11 s00120_112 s00120,_113 s00120_114 800120J 18 s00120_119 S00120J20 s00120_121 s00120_122 s00120_126 S00120J27 s00120_128 S00120J29 S00120J30 S00120J34 S0120J35 s00120_136 S00120J37 s00120_138 s00120_142 s00120_143 s00120_144 s00120_145 S 0 0 1 2 0 J 46 s00120_150 s00120_151 s00120_152 s00120_153 S00120J54 S00120_158 S00120J59 Sam ple Description E00-1311-1019 24 hour, Omg/L, S1, C-2 E00-1311-1020 24 hour, Omg/L, S I, C-2 E00-1311-1021 24 hour, Omg/L, S1, C-2 E00-1311-1021 24 hour, Omg/L, S1, C-2, MS EOO-1311-1022 24 hour, 0.1 Omg/L, S1, C-2 E00-1311-1023 24 hour, 0.1 Omg/L, S I, C-2 EOO-1311-1024 24 hour, 0.1 Omg/L. S1, C-2 E00-1311-1024 24 hour, 0.10mg/L, S I, C-2, MS E00-1311-1025 24 hour, 1.Omg/L, S1, C-2 E00-1311-1026 24 hour, 1.Omg/L, S1.C-2 E00-1311-1027 24 hour. 1.Omg/L, S1, C-2 EOO-1311-102724 hour, 1.Omg/L, SI, C-2, MS EOO-1311-1028 24 hour, Omg/L, S1, C-3 EOO-1311-1029 24 hour, Omg/L, SI, C-3 EOO-1311-1030 24 hour, Omg/L, S1, C-3 EOO-1311-1030 24 hour, Omg/L, SI. C-3 MS EOO-1311-1031 24 hour, 0.1 Omg/L, SI, C-3 EOO-1311-1032 24 hour, 0.1 Omg/L, S1, C-3 EOO-1311-1033 24 hour, 0.1 Omg/L, S I, C-3 EOO-1311-1033 24 hour, 0.1Omg/L, S1, C-3 MS EOO-1311-1034 24 hour, 1.Omg/L, S1, C-3 EOO-1311-1035 24 hour, 1.Omg/L, S1, C-3 EOO-1311-1036 24 hour. 1.Omg/L, S I, C-3 EOO-1311-1036 24 hour, 1.Omg/L, 81, C-3 MS EOO-1311-1037 24 hour, Omg/L, S1, C-4 EOO-1311-1038 24 hour, Omg/L, S1, C-4 EOO-1311-1039 24 hour, Omg/L, S1, C-4 EOO-1311-1039 24 hour, Omg/L. S1, C-4 MS EOO-1311-1040 24 hour, 0.1 Omg/L, S1.C-*EOO-1311-1041 24 hour, 0.1 Omg/L, S I, C~< 600-1311-1042 24 hour, 0.1 Omg/L, S1.C-* EOO-1311-1042 24 hour, 0.1 Omg/L, S I, C-4 MS EOO-1311-1043 24 hour, 1.Omg/L, S1, C-4 EOO-1311-1044 24 hour, 1.Omg/L, S1, C-4 EOO-1311-1045 24 hour, 1.Omg/L, S1, C-4 EOO-1311-1045 24 hour, 1.Omg/L, S1, C-4 MS Theoretical Matrix M easured S p ik e Concentration, Concentration, R e p lic a te ug/L <24.75 u g /L Sam ple % R S D <24.75 N/A <24.75 340.34 <24.75 200 <24.75 N/A <24.75 374.07 200 457.51 475.62 2.92 484.59 790.19 200 29.19 <24.75 N/A <24.75 366.46 200 <24.75 <24.75 N/A <24.75 391.81 200 465.89 490.88 3.21 494.39 824.37 200 442.75 28.04 124.58 <24,75 376.04 <24.75 <24.75 200 N/A <24.75 389 200 417.87 455.03 5.94 469.4 466.25 200 Matrix Sp ike Recovery, % 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 1^:0.982880 Target Analyte: PFOS Internal Standard: TH PFO S *For more run info. See the Data Review Form included in the Raw Data 3M Environmental Laboratory Page 264 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run ID: s001122a Sam ple Data File s00122a_035 s00122a 036 s00122a_037 s00122aj)38 500122a 042 s00122a 043 s00122a_044 S00122a_045 s00122a_046 s00122a,,050 s00122a 051 s00122a_052 s00122a 053 s00122a_054 s00122a 058 s00122a_J)59 s00122a_060 S00122a_061 s00122a_062 s00122a_06B s00122a_067 s00122a 068 s00122aj>69 s00122a_070 s00122a_074 s00122a_075 s00122a,,076 S00122a_077 s00122a 078 s00122a_082 s00122a_083 s00122a_0B4 s00122a_085 s0 0 1 2 2 a_ 0 8 6 s00122a_090 s00122a_091 Sample Description E00-1311-1019 24 hour, Omg/L. S2, C-2 EOO-1311-1020 24 hour. Omg/L, S2. C-2 EOO-1311-1021 24 hour. 0mg/L. S2. C-2 EOO-1311-1021 24 hour. Omg/L, S2. C-2, MS EOO-1311-1022 24 hour. 0.1Omg/L, S2, C-2 EOO-1311-1023 24 hour, 0.1Omg/L, $2, C-2 EOO-1311-1024 24 hour, 0.1 Omg/L, S2, C-2 EOO-1311-1024 24 hour. 0.1 Omg/L. S2, C-2, MS EOO-1311-1025 24 hour, 1.Omg/L, S2. C-2 EOO-1311-1026 24 hour, 1.Omg/L, S2, C-2 EOO-1311-1027 24 hour, 1.Omg/L, S2, C-2 EOO-1311-1027 24 hour, 1.Omg/L, S2, C-2, MS EOO-1311-1028 24 hour. Omg/L, S2, C-3 EOO-1311-1029 24 hour, Omg/L. S2. C-3 EOO-1311-1030 24 hour, Omg/L, S2, C-3 EOO-1311-1030 24 hour, Omg/L, S2, C-3 MS EOO-1311-1031 24 hour, 0.1 Omg/L, S2. C-3 EOO-1311-1032 24 hour, 0.1Omg/L, S2, C-3 EOO-1311-1033 24 hour, 0.1 Omg/L, S2. C-3 EOO-1311-1033 24 hour, 0.1Omg/L, S2, C-3 MS EOO-1311-1034 24 hour, 1.Omg/L, S2, C-3 EOO-1311-1035 24 hour, 1.Omg/L, S2, C-3 EOO-1311-1036 24 hour. 1.Omg/L, S2, C-3 EOO-1311-1036 24 hour, 1.Omg/L, S2. C-3 MS E00-1311-1037 24 hour, Omg/L, S2, C-4 EOO-1311-1036 24 hour, Omg/L, S2, C-4 EOO-1311-1039 24 hour, Omg/L, S2, C-4 EOO-1311-1039 24 hour, Omg/L, S2, C-4 MS EOO-1311-1040 24 hour. 0.1 Omg/L, S2. C-4 EOO-1311-1041 24 hour, 0.10mg/L, S2. C-4 EOO-1311-1042 24 hour. 0.1Omg/L, S2, C-4 EOO-1311-1042 24 hour, 0.1Omg/L, S2, C-4 MS EOO-1311-1043 24 hour, 1.Omg/L, S2, C-4 EOO-1311-1044 24 hour, 1.Omg/L, S2, C-4 EOO-1311-1045 24 hour, 1.Omg/L, S2. C-4 EOO-1311-1045 24 hour, 1.Omg/L, S2, C-4 MS M easured Theoretical Matrix Spike Concentration, Concentration, Replicate ug/L ug/L Sample %RSD <24.75 <24.75 <24.75 489.95 <24.75 <24.75 <24.75 473.79 71.39 99.23 8802 540.69 <24.75 <24.75 <24.75 439.66 <24.75 <24,75 <24.75 459.97 261.99 201.55 133.08 625.5 <24.75 <24.75 <24.75 449.6 <24.75 <24.75 <24.75 439.78 25.99 N/A 200 N/A 200 16.25 200 N/A 200 N/A 200 32.43 200 N/A 200 N/A 200 84.89 69.38 30.68 496.84 200 M atrix Spike Recovery, % 244.98 236.90 226.34 219.83 229.99 246.21 224.80 219.89 233.08 A n alytical R u n Information*: Acceptable Quant Range: 24.75ppb-495.9ppb Calibration Curve r^O. 998460 Target Analyte: PFOS Internal Standard: THPFOS *For more run info. See the Data Review Form included in the Raw Data Q-Test C alculation (N = 3) -0.531145761 0.920373514 3M Environmental Laboratory Page 265 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Tucker Run ID: t010122 Sam ple Data File Sam ple Description t010l22_040 t010122_041 I010122J342 t010122_043 t010122_044 t010122_048 t010122_049 t010122J350 t010122_051 t010122_052 tOI0122.056 t010122_057 t010122_05B t010122_059 t010122_060 t010122_064 t010122_065 t010122_066 1010122^067 t010122_068 t010122_072 t010122.073 t010122_074 t010122,,075 t010122_076 t010122_080 t010122_081 t010122_082 t010122_083 t010122_084 t010122_088 t010122_089 t010122_090 t010122_091 EOO-1311-2001, Oug PFOS, control, 1/22/01 CMC EOO-1311-2002, Oug PFOS, control, 1/22/01 CMC EOO-1311-2003. Oug PFOS, control, 1/22/01 CMC E00-1311-2003ms, Oug PFOS, control,1/22/01 CMC EOO-1311-2004, 0.75ug PFOS, control, 1/22/31 CMC EOO-1311-2005,0.75ug PFOS, control,1/22/01 CMC EOO-1311-2006, 0.75ug PFOS, control, 1/22/01 CMC EOO-1311-2006ms, 0.75ug PFOS, control, 1/22/01 CMC EOO-1311-2007, 7.5ug PFOS, control. 1/22/01 CMC EOO-1311-2008, 7.5ug PFOS, control, 1/22/01CMC EOO-1311-2009,7.5ug PFOS, control,1/22/01 CMC EOO-1311-2009ms, 7.5ug PFOS, control,1/22/01 CMC EOO-1311-2010, Oug PFOS, Clay, 1/22/01 CMC EOO-1311-2011, Oug PFOS. Clay,1/22/01 CMC E00-1311-2012, Oug PFOS, Clay, 1/22/01 CMC EOO-1311-2012ms, Oug PFOS, Clay,1/22/01 CMC EOO-1311-2013, 0.75ug PFOS, Clay,1/22/01 CMC EOO-1311-2014, 0.75ug PFOS, Clay, 1/22/01 CMC EOO-1311-2015,0.75ug PFOS, Clay.1/22/01 CMC EOO-1311-2015ms, 0.75ug PFOS, Clay,1/22/01 CMC EOO-1311-2016, 7.5ug PFOS, Clay.1/22/01 CMC EOO-1311-2017, 7.5ug PFOS, Clay.1/22/01 CMC EOO-1311-2018, 7.5ug PFOS, Clay,1/22/01 CMC EOO-1311-2018ms, 7.5ug PFOS, Clay, 1/22/01 CMC EOO-1311-2019, Oug PFOS. Sediment, 1/22/0! CMC EOO-1311-2020, Oug PFOS, Sediment, 1/22/01 CMC EOO-1311-2021, Oug PFOS, Sediment, 1/22/01 CMC EOO-1311-2021 ms. Oug PFOS, Sediment, 1/22701 CMC EOO-1311-2022. 0.75ug PFOS, Sediment, 1/21701 CMC E00-1311-2023,0.75ug PFOS, Sediment, 1/22701 CMC EOO-1311-2024, 0.75ug PFOS. Sediment, 1/22/01 CMC E00-1311-2024ms, 0.75ug PFOS, Sediment, 1/22/01 CMC EOO-1311-2025,7.5ug PFOS, Sediment, 1/22/01 CMC EOO-1311-2026,7.5ug PFOS, Sediment, 1/22/31 CMC t010122_092 EOO-1311-2027,7.5ug PFOS, Sediment, 1/22/01 CMC t0 10122_ 09 6 E00-131 V2027m s, 7.5ug PFOS, Sediment, 1/22/01 CMC Measured Concentration, ug/L <25.0 <25.0 <25.0 194.28 95.92 96.85 95.39 331.94 802.01 587.71 671.3 757.91 <25.0 <25.0 <25.0 174.47 63.71 75.13 74.74 275.64 627.98 682.43 461.56 897.56 <25.0 <25.0 <25.0 192.1 109.78 89.72 88.54 250.93 568.24 608.75 625.2 930.32 Theoretical Matrix Spike C o n c e n tratio n , ug/L R e p lic a te Sam ple %RSD N/A 200 0.77 200 15.72 200 N/A 200 9.11 200 19.48 200 N/A 200 12.43 200 4.88 200 Matrix Spike Recovery, % 97.14 118.28 43.31 87.24 100.45 218.00 96.05 81.20 152.56 Analytical Run Information*: Acceptable Quant Range: 25ppb-1 OOOppb Calibration Curve 1^:0.996956 Target Analyte: PFOS Internal Standard: TH PFO S *For more run info. See the Data Review Form included in the Raw Data 3M Environmental Laboratory Page 266 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run IP: S001211 Sam ple Data File S001211.036 s001211.037 s001211.038 S001211.039 S001211.040 SO01211 . 0 4 4 s001211.045 s001211.046 s001211.047 S001211.048 s001211.052 s001211.053 S001211.054 S001211.055 8001211.056 8001211.060 S001211 061 5001211.062 S001211 063 S0O1211 .0 6 4 S001211 068 5001211.069 S001211.070 sOO1 2 1 1 .0 7 1 S01211 072 3001211.076 s001211.077 s 001211 078 S0012 1 1 .0 7 9 3001211.080 S001211 084 S001211 085 sOO1 2 1 1 .0 8 6 s001211.087 S001211.088 5001211.092 5001211.093 S01211 .09 4 s001211.095 S001211.096 3001211.100 S001211.101 5001211.102 S001211.103 5001211.104 S01211 .10 8 5001211.109 S001211.110 Sam ple Description 10x EOO-1311-3022-S1, O.Omg/L, 48hr, IM C Iay, 12/07/00 10x EOO-1311-3023-S1,O.Omg/L, 48hr, IM C Iay, 12/07/00 10x EOO-1311-3024-S1, O.Omg/L, 48hr, 1:1Clay, 12A7/0O 10x EOO-1311-3024ms-S1, O.O mL, 48hr, 1:1Clay, 12/07/00 10x EOO-1311-3025-S1 O.Omg/L, 4Bhr. 1:5 Clay, 12/07/00 10x EOO-1311-3026-S1 O.Omg/L, 48hr, 1:5 Clay, 12/07/00 10x EOO-1311-3027-S1 O.Omg/l, 48hr, 1:5 Clay, 12/07/00 10x EOO-1311-3027ms-S1 O.Omg/L, 48hr, 1:5 Clay, 12/07/00 10x EOO-1311-3028-S1 O.Omg/L, 48hr, 1:25 Clay, 12/07/OC 10x EOO-1311-3029-S1 O.OmL, 48hr, 1:25 Clay. 12/07/OC 10x EOO-1311-3030-S1 O.0mg/L, 48hr, 1:25 Clay, 12/07/OC lOx EOO-1311-3030ms-S1 O.Omg/L, 48hr, 1:25 Clay, 12/07W 10x E0O-1311-3058-S1, 0.5m g/L, 48hr, IM C Iay, 12/07/00 lOx EOO-1311-3056-S1,0.5mg/L, 48hr, 1:1Clay, 12/07/00 10x E0O-1311-3O6O-S1, 0.5m g/L, 48hr, IM C Iay, 12/07/00 10x EOO-1311-3060ms-S1,0.5mg/L, 48hr, IM C Iay, 12 /0 7 /tfl 10x EOO-1311-3061-S1,0.5mg/L, 48hr, 1:5Clay, 12/07/00 10x EOO-1311-3062-S1, 0.5m g/L, 48hr, 1:5Clay, 12/07/00 10x EOO-1311-3063-S1,0.5mg/L, 48hr, 1:5Clay, 12/07/00 10x EOO-1311-3063ms-S1, 0.5m g/L, 48hr, 1:5Clay, 12/07/C0 10x EOO-1311-3064-S1,0.5mg/L, 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3065-S1, .5mg/L, 48hr, t:2 5C lay. 12/07/00 10x EOO-1311-3066-S1,0.5mg/L, 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3066ms-S1,0.5mg/L, 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3085-S1,0.5mg/L, 36hr, 1:1Clay, 12/07/00 10x EOO-1311-3O86-S1,0.5mg/L, 36hr, 1:1Clay, 12/07/00 10x EOO-1311-3087-S1,0.5mg/L, 36hr, 1:1Clay, 12/07/00 10x EOO-1311-3087ms-S1, 0.5m g/L, 36hr, 1:1Clay, 12/07/03 10x EOO-1311-3088-S1, 0.5mg/L, 36hr, 1:5Clay, 12/07/00 10x EOO-1311-3089-S 1, 0.5m g/L. 36hr, 1:5Clay, 12/07/00 10x EOO-1311-3090-S1, 0.5m glL, 36hr, 1:5Clay, 12/07/00 lO x EOO-1311-3090ma-S1,0.5mg/L, 36hr, 1:5Clay, 12/07/00 10x EOO-1311-3091-S1, 0.5m g/L, 36hr, 1:25Clay, 12/07/00 10x EOO-1311-3092-S1,0.5mg/L, 36hr, 1:2SCIay, 12/07/00 10x EOO-1311-3093-S1, 0.5m g/L, 36hr, 1:25Clay, 12/07/00 10x EOO-1311 '3 0 9 3 m s -S 1 ,0.5m g/L, 36hr, l:2 5 C la y . 12/07/00 10x EOO-1311-3094-S1, D.5mg/L, 48hr, IM C Iay, 12/07/00 tO x EOO-1311-3095-S1,0.5mg/L, 48hr, IM C Iay, 12/07/00 10x EOO-1311-3096-S1, 0.5m g/L, 48hr, IM C Iay, 12/07/00 10x EOO-1311-3096ms-S1,0.5mgT., 48hr, IM C Iay , 12/07/OC 10x EOO-1311-3097-S1, 0.5mg/L, 48hr, 1:5Clay, 12/07/00 lO x EOO-1311-3098-S1, 0.5m g/l_ 48hr, 1:5Clay, 12/07/00 10x EOO-1311-3099-S1,0.5mg/L, 48hr, 1:5Clay, 12/07/00 10x EO O-1311-3099m s-S1,0.5mg/L, 48hr, 1:5Clay, 12/07/00 10x EOO-1311-3100-S1, 0.5m g/L, 4Bhr, 1:25Clay, 12/07/00 10x EOO-1311-3101-S1, 0.5mg/L, 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3102-S 1 .0.5m g/L, 48hr, 1:25Clay, 12/07/00 10x EOO-1311-3102ms-S1, 0.5mg/L, 48hr, 1:25Clay, 12/07/03 Measured Concentration, ug/L Theoretical Matrix S pike Concentration, ug/L R e p lic a te Sample %RSD <40.0 <40.0 <40.0 196.55 200 <40.0 <40.0 <40.0 185.82 200 <40.0 <40.0 <40.0 399.71 200 130.4 114,48 111.17 306.74 200 293.97 314.29 287.97 655.16 200 118.92 305.1 " Point Thrown out 128.68 309.9 200 131.97 138.13 44 .5 9 433.65 200 103.26 119.9 129.42 334.95 200 299.09 N/A N/A N/A 8.66 4.62 5.57 49 .8 8 11.27 313.39 3.94 289.84 497.01 200 . 59.14 62.46 8.29 69 .4 8 345.73 200 92.9 107.09 7.65 95.6 286.04 200 301.56 331.37 8.98 361.05 555.88 200 M atrix Spike Recovery, % 98 .2 8 92.91 199.86 97 .7 9 183.60 90.61 194,53 102.77 103.59 138,13 95 .2 2 97 .4 2 Analytical Run Information*: Acceptable Quant Range: 40.0ppb-1001.7ppb Calibration Curve ^0.992493 Target Analyte: PFOS Internal Standard: THPFOS *For more run info. See the Data Review Form included in the Raw Data Q-Test C a lc u la tio n (N s 3) 0.947577613 -0 .9 3 4 1 4 5 8 2 3M Environmental Laboratory Page 267 of 703 BACK TO MAIN Qualitv Control Samolo Data Instrument: Tucker Run ID: UJ01215 Sam ple Data File tOOl215 037 KX11215 038 (001215 039 tO01215 040 (001215 041 01215 045 01215 046 01215 047 (001215 04 01215 049 01215 053 01215 054 01215 055 01215 056 01215 057 01215 061 (001215 062 (001215 063 01215 064 (001215 065 01215 069 01215 070 (001215 071 01215 072 01215 073 W01215_77 01215 078 01215 079 01215 060 01215 061 01215 065 (001215 066 01215,097 01215 068 (001215_069 01215 093 01215,094 01215.095 01215,006 01215 097 01215,116 (001215_117 01215,118 01215 119 1001215_120 01215,124 t0012l5_12S 01215 126 01215,127 01215,128 01215,132 01216 133 (001215,134 01215,135 001215,136 01215 140 (001215,141 01215,142 (001215,143 001215 144 01215 148 01215,149 01215,150 01215 151 01215,152 01215,156 01215,157 01215,158 01215,162 01215,163 001215,164 001215 165 01215,166 01215,170 01215,171 01215 172 01215,173 01215,174 01215,17B 01215,179 Sam ple D escription 10x EOO-1311-3007 10* EOO-1311-3008 10* E00-1311-3009 10* EOO-1311-3009m 10* EOO-1311-3010 10* E00-1311-3011 10* EOO-1311-3012 10* EOO-1311-3012m 10x EOO-1311-3130 10* EOO-1311-3131 10* E00-1311-3132 10* EOO-1311-3132m 10* EOO-1311-3133 10* EOO-1311-3134 10* E00-1311-3135 10* EOO-1311-3135m 10x EOO-1311-3136 10* E00-1311-3137 10* EOO-1311-3138 10* EOO-1311-3138m 10* EOO-1311-3139 10* EOO-1311-3140 10x EOO-1311-3141 10* EOO-1311-3141m* 10* EOO-1311-3142 10* EOO-1311-3143 10* EOO-1311-3144 10* EOO-1311-3144ma 10x EOO-1311-3145 10* EOO-1311-3146 10* EOO-1311-3147 10x EOO-1311-3147ma 10* EOO-1311-3148 10* EOO-1311-3149 10* EOO-1311-3150 10* EOO-1311-3150m 10x E00-1311-3151 10* E00-1311-3152 10x EOO-1311-3153 10* EOO-1311-3153m* 10*600-1311-3154 10* EOO-1311-3155 10x600-1311-3156 10* EOO-1311-3156m 10* EOO-1311-3157 10* EOO-1311-3158 10* EOO-1311-3159 IO* EOO-1311-3159m 10* EOO-1311-3160 10* EOO-1311-3161 10* EOO-1311-3162 10* EOO-1311-3162m 10* EOO-1311-3163 10* EOO-1311-3164 10* EOO-1311-3165 10* EOO-1311-31eSms 10* EOO-1311-3166 10* EOO-1311-3167 1Qx E00-1311-3168 10* EOO-1311-3108m 10* EOO-1311-3169 10* EOO-1311-3170 10* EOO-1311-3171 10* EOO-1311-3171m 10* 00-1311-3172 10* EOO-1311-3173 10* EOO-1311-3174 10* EOO-1311-3174m* 10x EOO-1311-3184 10* EOO-1311-3185 10* EOO-1311-3188 10x EOO-1311-3186m 10x EOO-1311-3187 10* EOO-1311-3188 10* EOO-1311-3189 10* EOO-1311-3189m* 10* E00-1311-3190 10* EOO-1311-3191 10x E00-1311-3192 10* EOO-1311-3182m Theoretical M atrix M easured Spike C oncentration, C oncentration, R e p lic a te ug/L ug/L Sample %RSD <25.0 <25 0 <250 209 9 <25.0 <250 <25.0 189 67 96.66 92.97 87.04 263 27 396.95 233,83 271.06 449 46 32207 341.64 340.94 478.71 65.07 80.64 45 96 235.33 248.76 247 05 268.5 419.1 355.44 338.22 355 34 533.78 71.71 57.44 N/A 200 N/A 200 626 200 28 43 200 3.32 200 27.29 200 4.68 200 284 200 32 06 36.51 242.07 229 84 200 237.34 3.66 220.6 410.32 200 355 21 320.63 7.97 304.11 479 86 200 83.87 00.37 25.55 50.58 224.6 200 206.79 212.87 10.98 253.49 368 04 201 319.B4 318.04 9 06 371.72 537.50 202 68,64 60 37 37.76 30.48 207.13 19878 237.42 203 10.B8 196.59 361.74 304.44 20 368 92 346 68 963 44398 205 <25.0 <25.0 N/A <25.0 190.14 206 <25.0 <25.0 N/A <25.0 166 28 207 <25.0 <25.0 N/A <250 187.64 206 M atrix Spike Recovery, % 104 95 94.84 88.12 0919 67.89 94.68 75.30 89.22 102.78 B4B6 87 BB 87.01 57.00 B2.10 87.02 00 96 47.46 82.30 80.33 90.21 Analytical Run Information*: Acceptable Quant Range: 25.0ppb-1001.7ppb Calibration Curve ^ 0 .9 9 6 1 1 7 T arget A nalyte: PFOS Internal Standard: THPFOS ` F or m ore run info. See th e Data R eview Form included in the R aw Data Q -T e*t C alculation (N3) 0.405397727 -0.78328092 3M Environmental Laboratory Page 268 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Soup Run ID: s001207 Sample Data File s001207JJ36 s001207J>37 sQ01207_038 s0O1207_O39 S001207 040 S001207 044 s001207_04S 5001207^046 5001207,047 5001207,048 5001207,052 S001207,053 S001207 054 5001207,055 5001207,056 S001207,060 5001207,061 5001207,062 5001207,063 5001207,064 5001207,068 5001207,069 5001207,070 5001207,071 5001207,072 S001207,076 s001207,077 S001207,078 sO01207,079 5001207,080 s001207,084 S001207,085 5001207,104 s001207,105 s001207,106 5001207,110 5001207,111 S01207,112 s001207,113 5001207,114 5001207,118 s001207,119 5001207,120 sOO1207,121 5001207,122 S001207,126 5001207,127 s001207,128 s001207,129 s001207,130 5001207,134 s001207,135 SO01207,136 5001207,137 S001207,138 SO01207,142 5001207,143 SOO1207,144 5001207,145 S001207,146 S001207,150 S001207,151 S001207,152 5001207,153 5001207,154 S001207,158 5001207,159 5001207,160 Sample Description 10x EOO-1311-3001-S1. O.Omg/L, Ohr, No soil. 12/07/00 lOx EOO-1311-3002-S1, O.Omg/L, Ohr. No soil, 12/07/00 10x EOO-1311-3003-S1, O.Omg/L, Ohr, No soil. 12/07/00 10x EOO-1311-3003ms-S1 O.Omg/L, Ohr. No soil, 12/07/00 10x EOO-1311-3004-S1 O.Smg/L, Ohr, No so8, 12/07/00 10x EOO-1311-3005-S1. 0.5mg/L, Ohr. No soB, 12/07/00 10x EOO-1311-3006-S1,0.5mg/L, Ohr, No soil, 12/07/00 10x EOO-1311-3OO6ms-S1,0.5mg/L, Ohr, No so, 12/07/00 10x EOO-1311-3013-S1, O.mg/L, Ohr, 1:lday, 12/07/00 10x EOO-1311-3014-S1, O.Omg/L, Ohr, 1:1clay, 12/07/00 lOx EOO-1311-3015-S1. O.Omg/L. Ohr, 1:1day. 12>D7/00 10x EOO-1311-3015ms-S1,0.0mg/L, Ohr, 1:1day, 12/07/00 10x EOO-1311-3016-S1, O.Omg/L. Ohr, 1:5day, 12/07/00 10x EOO-1311-3017-S1, O.Omg/L, Ohr, 1:5day, 12/07/00 10x E00-1311-3018-SI, O.Omg/L, Ohr, 1:5day, 12/07/00 10x EOO-1311-3018ms-S1,0.0mg/L, Ohr. 1:5day, 12/07/00 10x EOO-1311-3019-S1,O.Omg/L. Ohr, 1:25clay, 12/07/00 10x EOO-1311-3020-S1,O.Omg/L, Ohr. 1:25day, 12707/00 10x EOO-1311-3021 S1,0.0mg/L, Ohr, 1:25day, 12/07/00 10x EOO-1311-3021ms-S1,O.Omg/L,Ohrl 1:25day, 12/07/00 10x EOO-1311-3031-S1,0.5mg/L, Ohr. 1:1day, 12/07/00 10x EOO-1311-3032-S1,0.5mg/L, Ohr, 1:1day. 12/07/00 lOx EOO-1311-3033-S1,0.5mg/L, Ohr. 1:1day, 12/07/00 10x EOO-1311-3033ms-S1,0.5mg/L, Ohr. 1:1day, 12/07/00 10x EOO-1311-3034-S1,0.5mg/L,Ohr, 1:5ciay, 12/07/00 10x EOO-1311-3035-S1,0.5mg/L,0hr, 1:5day, 12/07/00 10x EOO-1311-3036-S1,0.5mg/L,0hr, 1:5day. 12/07/00 10x EOO-1311-3036ms-S1,0.5mg/L,0hr, 1:5day, 12/07/00 10x EOO-1311-3037-S1.0.5mg/L.0hr, 1:25day, 12/07/00 10x EOO-1311-3038-S1,0.5mg/L,0hr, 1:25day, 12/07/00 10x EOO-1311-3039-S1,O.5mg/L,0hr, l:25day. 12/07/00 10x EOO-1311-3O39ms-S1,0.5mg/L,Ohr, 1:25clay, 12/07/00 10x EOO-1311-3040-S1,0.5mg/L,2hr, 1:1day. 12/07/00 10x EOO-1311-3041-S1,0.6mg/L,2hr, 1:1clay. 12/07/00 lOx EOO-1311-3042-S1,0.5mg/L,2hr, 1:1day, 12/07/00 10x EOO-1311-3042ms-S1,0.5mg/L,2hr, 1:1day, 12/07/00 10x EOO-1311-3043-S1,0.5mo/U,2hr, 1:5day. 12/07/00 10x 00-1311-3044-51,0.51^,2^, 1:5day, 12/07/00 10x EOO-1311-3045-S1,0.5mo/L,2hr, 1:5day, 12/07/00 10x EOO-1311-3045ms-S1,0.5mg/L,2hr, 1:5day, 12/07/00 10x EOO-1311-3046-S1,0.5mg/L,2hr, 1:25day, 12/07/00 10xE0O-1311-3O47-S1.0.5mg/L,2hr, 1:25day, 12/07/00 10x EOO-1311-3048-SI,O.5it)0/L,2hr, 1:25day, 12/07/00 10x EOO-1311-3048ms-S1,0.5mg/l,2hr, 1:25day, 12/07/00 10x EOO-1311-3049-S1,0.5mg/L,4hr, 1:1day, 12/07/00 10x EOO-1311-3050-S1,0.5mg/L,4hr. 1:1day, 12/07/00 lOx EOO-1311-30S1-S1,0.5mg/l.4hr, 1:1day, 12/07/00 10x EOO-1311-3051ms-S1,0.5mg/L,4hr, 1:1day, 12/07/00 10x EOO-1311-30S2-S1.0.5mg/L,4hr, 1:5day. 12/07/00 10x E0O-1311-3O53-S1,0.5mg/L,4hf, 1:5day, 12/07/00 10x EOO-1311-3054-S1,0.5mg/L,4hr, 1:5day, 12/07/00 10x EOO-1311-3054ms-S1,0.5mg/L,4hr, 1:5day, 12/07/00 10x EOO-1311-3055-S1,0.5mo/L.4hr. 1:25cWy. 12/07/00 10x EOO-l311-3056-S1,0.5mg/L,4hr, 1:25dy, 12/07/00 10x EOO-1311-3057-S1,0.5mg/L,4hr, 1:25day, 12707/00 10x EOO-1311-3057rrs-S1,0.5mg/L,4hr. 1:25day, 12/07/00 10x EOO-1311-3067-S1,0.5mg,16hr, 1:tday, 12/07/00 10x EOO-1311-3O68-S1,0.5mo/L,16nr, 1:1day, 12/07/00 10x EOO-1311-3069-S1,0.5mQ/L,16hr, 1:1day, 12/07/00 10x EOO-1311-3069ms-S1,0.5mg/L,16hr, 1:1day, 12/07/00 10x EOO-1311*3070-Sl,0.5mg/L.16hr, 1:5day, 12/07/00 10x EOO-1311-3071-Sl,0.5mg/L.16hr, 1:5day, 12/07/00 10x EOO-1311-3072-S1,0.5mg/L,16hr, 1:5clay. 12/07/00 10x EOO-131l-3072ms-S1,0.5mg/L,16hr, 1:5day, 12/07/00 10xEOO-1311-3073-81,0.5mg/L,16hr, 1:25day, 12/07/00 10x EOO-1311-3074-S1,0.5mg/L,16hr, 1:25day. 12/07/00 10x EOO-1311-3075-S1,0.5mg/L,16hr. 1:25day, 12/07/00 10x EOO-131l-3075ms-S1,0.5mQ/L.16hr,1:25clay, 12/07/00 Theoretical Matrix Measured Spike Concentration, Concentration, ug/L ug/L <25.0 <25.0 <25.0 243.94 <25.0 <25.0 <25.0 341.05 <25.0 <25.0 <25.0 463.23 <25.0 200 200 200 <25.0 <25.0 151.28 39B.29 449.17 <25.0 200 267.37 26.41 200 47.72 74.95 547.85 366 389.48 390.3 554.07 427.38 401.2 450.84 447.93 144.29 200 200 200 98.63 68.87 250.89 200 <25.0 155.7 140.92 351.48 200 317.1 318.56 326.3 515.02 200 113.88 88.39 92.13 431.57 200 126.4 113.16 136.92 333.48 326.15 201 326.21 319.46 525.54 202 119.29 99.92 166.04 438.97 203 140.62 136.17 152.02 373.61 204 330.98 321.53 346.78 518.38 205 Replicate Sample %RSD N/A N/A N/A N/A 6.49 48.96 3.61 6.82 36.55 7.05 1.54 14.03 9.49 1.20 26.47 5.72 3.83 Matrix Spike Recovery, % 121.97 170.53 231.62 75.64 133.69 238.45 81.89 1.45 91.01 105.28 94.36 169,72 07.79 102.02 134.45 108.62 83.71 A n alytical Run Inform ation*: Acceptable Quant Range: 25.0ppb-1001.7ppb Calibration Curve ^ 0 .9 9 6 0 2 6 Target Analyte: PFOS Internal Standard: THPFOS *F or m ore run info. See the Data Review Form included in the Raw Data Q-Test g3)Calculation (N -0.394590294 } ' 3M Environmental Laboratory Page 269 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Hillary Run ID: H001214a &b Sam ple Data File HII0037.D HIIOO30.D HII0039.D HII0040.D HH0041.D HHI045.D HI0046.D HH0047.D HII0048.D HIO049.D HI0053.D HI0054.D HII0055.D HHI0056.D HI0057.D HMI0061.D HII0062.D HHI0063.D HIO064.D HHI0065.D HIIO069.D HII0070.D HM0071.D Hi110072.D HHI0073.D HII0077.D HII0078.D HII0079.D HillOOBO.D HII0081.D HII0101.D HII0102.D HI0103.D HIK)104.D HII0105.D HMI0109.D HII0110.D HII0111.D HHI0112.D HIII0113.D HHI0117.D HII0118.D HI0119.D HII0120.D HII0121.D HII0125.D HII0126.D HI0127.D HII0128.D HI0129.D HII0133.D HI0134.D HH0135.D HNI0136.D HHI0137.D HNI0141.D HII0142.D HII0143.D HI0144.D HII0145.D Sample Description 1 3 1 1-3076-S1 1311-3077-S1 1311-3078-S1 1311-3078ms-S1 1311-3079-S1 1311-308Q-S1 1311-3081-S1 1311-3081-ms-S1 1311-3082-S1 1311-3083-S1 1311-3084-S1 1311-3084ms-S1 1311-3103-S1 1311-3104-S1 131.1-3105-S1 1311-3105ms-S1 1311-3106-S1 1311-3107-S1 1311-3108-S1 1311-3108ms-S1 1311-3109-S1 1311-3110-S1 1311-3111-S1 1311-3111ms-S1 1311-3112-S1 1311-3113-S1 1311-3114-S1 1311-3114ms-S1 1311-3115-S1 1311-3116-S1 E1311-3117-S1 E1311-3117-MS-S1 E 1 3 1 1 -3 1 18-S1 E 1 31 1 -3 1 19-S1 E1311-3120-S1 E1311-3120-MS-S1 E1311-3121-S1 1311-3122-S1 1311-3123-S1 1311 -3123-MS-S1 E1311-3124-S1 E1311-3125-S1 E1311-3126-S1 E1311-3126-MS-S1 E1311-3127-S1 E1311-3128-S1 E1311-3129-S1 E1311-3129-MS-S1 E1311-3175-S1 E1311-3176-S1 E1311-3177-S1 1 3 1 1-3177-MS-S1 E1311-3178-S1 E1311-3179-S1 E1311-3180-S1 E1311-3180-MS-S1 E1311-3181-S1 E 1 3 11-3182-S1 E1311-3183-S1 E1311-31B3-MS-S1 Measured Concentration, ug/L 125.100 105.408 34.090 275.722 116.696 1 1 0 .2 1 2 96.723 280.717 288.554 284.213 288.461 471.663 118.316 1 2 1 .8 8 6 87.387 284.067 451.551 442.987 447.692 647.955 402.850 428.582 425.083 611.097 78.065 85.862 59.321 289.160 247.502 268.700 331.41 448.22 365.63 <25.0 <25.0 183.42 <25.0 80.43 63.71 209.01 242.86 246.91 245.14 424.19 380.34 374.21 368.76 541.70 <25.0 <25.0 <25.0 241.96 <25.0 <25.0 <25.0 184.71 <25.0 <25.0 <25.0 188.81 Theoretical Matrix Spike Concentration, ug/L R e p lic a te M atrix Spike Sample %RSD Recovery, % 54.29 200 9.45 120.82 2 0 0 92.00 0 .8 6 2 0 0 91.60 17.37 200 0.96 98.34 200 3.33 100.13 200 18.33 93.01 200 15.44 104.92 2 0 0 58.40 N/A 2 0 0 91.71 16.41 2 0 0 72.65 0.83 200 1.55 200 89.53 86.47 N/A 201 120.38 N/A 2 0 2 91.44 N/A 203 93.01 Analytical Run Information*: Acceptable Quant Range: 25.0ppb-1001.7ppb(a and b) Calibration Curve 1^.9 998(8), 0.9998(b) Target Analyte: PFOS Internal Standard: THPFOS "For more run info. See the Data Review Form included in the Raw Data 3M Environmental Laboratory Page 270 of 703 BACK TO MAIN Quality Control Sample Data Sample Data File Sample Description t010123_002 t010123_003 t010123_004 t010123_005 tt)10123_006 t010123_010 t010123_011 t010123_012 t010123_013 1010123_014 t010123_018 t010123_019 t010123_020 t 0 10123_021 (010123_022 t010123_026 t010123_027 tt)10123_028 1010123^029 t010123_030 tt)10123_D34 t010123_035 t010123_036 (010123^037 t0 10123_038 (010123_042 (010123_043 (010123_044 I010123_045 t010123_046 t010123_050 t010123_051 t010123_052 t010123_053 (010123_054 10x E00-1311-3007-S2, Omg/L PFOS.no soil. 48h.1/03/01 CMC 10x EOO-1311-3008-S2, 0mg/L PFOS.no soil. 48h,1/03/01 CMC 10x E00-1311-3009-S2, Omg/L PFOS.no soil, 48h.1/03>1 OMC 10x EOO-1311-3009ms-S2, Omg/L PFOS.no soil, 48h, 1/03/01 CMC 10x E00-1311-301O-S2, 5mg/L PFOS.no soil, 48h,1/03/01 CMC 10x EOO-1311-3011-S2, 5mg/L PFOS.no soil, 48h, 1/03/01 CMC lOx E0O-1311-3012-S2, Omg/L PFOS.no soil, 4Bh, 1/03/01 CMC 10x E00-1311-3012ms-S2, Omg/L PFOS.no soil, 48h, 1/03/01 CMC 10x EDO-1311-3022-S2, Omg/L PFOS.1:1 day, 480,1/03/01 CMC 10x EOO-1311-3D23-S2, Omg/L PFOS, 1:1 day, 4Bh,1/03/01 CMC 10x EOO-1311-3024-S2, Omg/L PF0S,1:1 day, 480,1/03/01 CMC 10x EOO-1311-3024ms-S2, Om^L PFOS, 1:1 day. 48h.1/03,01 CMC 10x EOO-1311-3025-S2, Omg/L PFOS, 1:5 day, 480. 1/03/01 CMC 10x EOO-1311-3026-S2, Omg/L PFOS,1:5 day, 46h,1/03/01 CMC 10x EOO-1311-3027-S2, Omg/L PFOS,1:5 day, 480,1/03/01 CMC 10x EOO-1311-3027ms-S2, Omg/L PFOS, 1:5 day, 48h,1/03/D1 CMC 10x EOO-1311-3028-S2, Omg/L PFOS, 1:25 day, 48h, 1/03/0' CMC 10x EOO-1311-3029-S2, Omg/L PFOS, 1:25 day, 480,1/03/0' CMC 10x EOO-1311-3030-S2, Omg/L PFOS,1:25 day, 48h,1/03/0' CMC 10x EOO-1311-3030ms-S2. Omg/L PFOS, 1:25 day, 48h,1/02/0l CMC 10x EOO-1311-3094-S2, 5mg/L PFOS,1:1 day, 48h, 1/03/01 3MC 1Qx E00-1311-3095-S2, 5mg/L PFOS.1.1 day, 480,1/03/01 CMC tOx EOO-1311-3096-S2, 5mg/L PFOS, 1:1 day. 48h, 1/03/01 CMC 10x EOO-1311-3096ms-S2, 5mg/L PFOS,1:1 day, 480,1/03/1)1 CMC 10x E0CM311-3O97-S2, 5mg/L PFOS, 1:5 day, 48h. 1/03/01 CMC 10x EOO-1311-3098-S2, 5mg/L PFOS, 1:5 day, 48h, 1/03/01 CMC 10x EOO-1311-3098ms-S2, 5mg/L PFOS, 1:5 day, 48h, 1/03/01 CMC 10x EOO-1311-3100-S2, 5mg/L PFOS, 1:25 day, 480,1/03/01 CMC 10x EOO-1311-3101-S2, 5mg/L PFOS,1:25 day, 48h,1/03/01 CMC 10x EOO-1311-3102-S2. 5mg/L PFOS, 1:25 day, 480,1/03/01 CMC 10x EOO-1311-3102ms-S2, 5mg/L PFOS, 1:25 day, 48h,1/0301 CMC 10x EOO-1311-3166-S2, 5mg/L PFOS,1:1 Sed. 48h,1/03/01 CMC 10x EOO-1311-31668-S2, 5mg/L PFOS,1:1 Sed, 480,1/03/01 CMC 10x EOO-1311-3168-S2, 5mg/L PFOS,1:1 Sad, 480,1/03/01 CMC 10x EOO-1311-3168ms-S2, 5mg/L PFOS,1:1 Sad, 48h,1/03/01 CMC Analytical Run Information*: Acceptable Quant Range: 25.0ppb-1000ppb Calibration Curve ^0.997776 Target Analyte: PFOS Internal Standard: THPFOS *For more run info. See the Data Review Form included In the Raw Data Instrumant: Tucker Run ID: t010123 Theoretical Matrix Measured Spike Concentration, Concentration, ug/L ug/L <25.0 <25.0 <25.0 174.31 <25.0 <25.0 <25.0 194.29 <25.0 <25.0 <25.0 170.06 <25.0 <25.0 <25.0 129.49 <25.0 <25.0 <25.0 154.79 95.36 112.93 159.53 377.94 163.56 174.93 408.33 476.98 520.09 501.18 896.63 83.19 100.14 51.56 242.84 200 200 200 200 200 200 200 200 200 Replicate Sample %RSD N/A N/A N/A N/A N/A 27.05 4.75 4.33 31.49 Matrix Spike Recovery, % 87.16 97.15 85.03 64.75 77.40 109.21 116.70 197.73 95.64 Q-Test Calculation (N = 3) -0.651090994 3M Environmental Laboratory Page 271 of 703 BACK TO MAIN Quality Control Sample Data Instrument: Tucker Run ID: t010124 Sample Data File Sample Description tO I0124^003 t010124_004 1010124^005 t010124_006 1010124_007 t010124_011 t010124JD12 t010124_013 t010124_014 t010124_015 1010124J M 9 t010124_020 t0 1 0 1 2 4 _ 0 2 1 t010124_022 t010124_023 t010124J327 t010124_028 t010124_029 t010124_030 t0 1 0 1 2 4 _ 0 3 1 10x EOO-1311-3169-S2, 0.5m g/L PFOS, 1:5 Sed, 48h 1/03/01 CMC 10x EOO-1311-3170-S2, 0.5m g/L PFOS, 1:5 Sed, 48h 1/03/01 CMC 10x E 00-1311-3171-S 2, 0.5m g/L PFO S,1:5 Sed. 48h 1/03/01 CMC 10x EOO-1311-3171 ms~S2, 0.5m g/L PFO S,1:5 Sed, 4 8 h ,1/03/01 CMC tO x EOO-1311-3172-S2, 0.5m g/L P FO S ,1:25 Sed, 4811,1/03/01 CMC 10x EOO-1311-3173-S2, 0.5m g/L PFOS, 1:25 Sed, 48h, 1/03/01 CMC 10x EOO-1311-3174-S2, 0.5m g/L PFO S,1:25 Sed, 48h, 1/03/01 CMC 10x EOO-1311-3174m s-S2, 0.5m g/L PFO S,1:25 Sed, 48h,1/03/01 CM C 10x 00-1311-3184-S2, Omg/L PFO S,1:1 Sed, 4 0 h ,1/03/01 CMC 10x E00-1311 -3185-S2, Omg/L PFO S,1:1 Sed, 48h,1/D3/01 CMC 10x EOO-1311-3186-S2, Omg/L PFOS, 1:1 Sed, 4 8 h ,1/33/01 CMC 10x E00-1311-3186m s-S2, Omg/L PFOS,1:1 Sed, 48h, 1/03/01 CMC 10x EOO-1311-3187-S2, Omg/L PFOS, 1:5 Sed, 4Bh, 1/03/01 CMC 10x EOO-1311-3188-S2, Omg/L PFO S,1:5 Sed, 4 8 h ,1/03/01 CMC 10x EOO-1311-3189-S 2, Omg/L PFOS, 1:5 Sed, 4 8 h ,1/03/01 CMC 10x EOO-1311-3189m s-S2, Omg/L PFOS, 1:5 Sed, 4Bh, 1/03/01 CMC 10x EOO-1311-3190-S2, Omg/L PFOS, 1:25 Sed, 48h, 1/03/01 CMC 10x EOO-1311-3191-S2, Omg/L PFO S,1:25 Sed, 48h,1/03/01 CMC 10x EOO-1311-3192-S2, Omg/L PFOS, 1:25 Sed, 48h,1/03/01 CMC 10x EOO-1311-3192m s-S2, Omg/L P F O S ,1:25 Sed, 48 t,1/03/01 CMC Theoretical Matrix Measured Spike Concentration, Concentration, Replicate ug/L ug/L Sample %RSD 186.19 324.9 210.45 469.73 265.72 282.72 285.76 407,27 <40.0 <40.0 <40.0 161.33 <40.0 <40.0 <40.0 186.26 <40.0 <40.0 <40.0 188.01 30.80 200 3.08 200 N/A 200 N/A 200 N/A 200 Matrix Spike Recovery, % 129.64 60.76 80.67 93.13 94.01 Analytical Run Information*: Acceptable Quant Range: 40.0ppb-1000ppb Calibration Curve r^O.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 Quality Control Sample Data Instrument: Tucker Run ID: t010125 Sam ple Data File Sample Description t010125_040 t0 1 0 1 2 5 _ 0 4 t t010125_042 t010125_043 t010125_044 t010125_048 t010125_049 t010125_050 t010125_051 t010125_052 t010125_Q56 t010125_057 t010125_058 t010125_059 t010125_060 10x E00-1311-0016 10x EOO-1311-0017 10x EOO-1311-0010 10x E00-1311-0019 10x EOO-1311-0020 tOx E00-1311-0021 10x EOO-1311-0022 10x EOO-1311-0023 10x EOO-1311-0024 10x EOO-1311-0025 10x EOO-1311-0026 10x EOO-1311-0027 10x EOO-1311-0028 10x EOO-1311-0029 10x EOO-1311-0030 t010125_065 t010125_066 t010125_068 t010125_072 t010125_074 t010125_075 t010125_076 t010125_080 t010125_081 10x EOO-1311-0031 10x EOO-1311-0032 10x EOO-1311-0033 10x EOO-1311-0034 10x EOO-1311-0035 10x EOO-1311-0036 10x EOO-1311-0037 10x EOO-1311-0038 10x EOO-1311-0039 10x EOO-1311-0040 10x EOO-1311-0041 10x EOO-1311-0042 t010125_083 t010125_084 t010125_088 t010125j)89 t010125_090 10x EOO-1311-0043 10x EOO-1311-0044 10x EOO-1311-0045 10x EOO-1311-0046 10x EOO-1311-0047 10x EOO-1311-0048 t010125_091 10x EOO-1311-0049 t010125_092 10x EOO-1311-0050 t010125_096 10x EOO-1311-0051 t010125^097 10x EOO-1311-0052 t010125_D98 10x EOO-1311-0053 t010125_099 10x EOO-1311-0054 t010125_100 10 x E00-1311-0055 t010125_104 10x EOO-1311-0056 t010125_105 10x EOO-1311-0057 t010125_106 10x EOO-1311-0058 t010125_107 10x EOO-1311-0059 t010125_108 10x EOO-1311-0060 t010125_112 t0 l0 l2 5 _ 1 1 3 10x EOO-1311-0061 10x EOO-1311-0062 t010125_114 t010125_115 10x EOO-1311-0063 10x EOO-1311-0064 010125_110 t010125_120 10x EOO-1311-0065 10x EOO-1311-0066 t010125_121 10x EOO-1311-0067 t010125_122 10x EOO-1311-0068 t010125_123 10x EOO-1311-0069 t010125_124 10x EOO-1311-0070 t010125_128 10x EOO-1311-0071 1010125_129 t010125_130 10x EOO-1311-0072 10x EOO-1311-0073 t010125_131 10x EOO-1311-0074 t010125_132 10x EOO-1311-0075 Measured Concentration, ug/L <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 <40.0 615.66 534.11 623.15 511.02 599.06 539.37 602.7 543.28 615.46 566.96 561.3 582.06 560.81 629.91 548.47 570.84 614.54 549.94 635.77 539.81 402.35 417.47 359.31 380.97 609.1 603.9 540.32 680.88 543.97 617.2 549.02 605.04 529.29 613.74 535.27 547.43 326.1 457.52 586.47 412.39 473.07 399.6 428.08 471.39 418.75 theoretical M atrix Spike C o n ce n tra tio n , ug/L R e p lic a te M atrix Spike Sample %RSD Recovery, % N/A N/A N/A N/A 8.36 6.56 7.57 5.70 22.31 7.62 6.55 11.16 7.00 7.47 28.51 9.16 6.39 Analytical Run Information*: Acceptable Quant Range: 40ppb-1000ppb Calibration Curve r^O.998087 Target Analyte: PFOS Internal Standard: THPFOS For more run info. See the Data Review Form included in the F aw Data ^ 3M Environmental Laboratory Page 273 of 703 BACK TO MAIN Appendix F: Notes to File and 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 Environmental Laboratory N ote to F ile Project or Study Number: PFOS Adsorb/Desorb .. ........ ...... ' EOO-1311 Associated Study Number:__________________ In the "Suitable Container" section of this study the spiking concentration differs from the method but is stated correctly in the protocol. In this case the protocol takes precedence over the method. Recorded By: Ocnd Date S 3 4 lo 1 3M Environmental Laboratory Page 275 of 703 BACK TO MAIN 3M E nvironm ental Laboratory N ote to F ile Project or Study Number: PFOS Adsorb/Desorb .......... ............ ..... EOO-1311................. Associated Study Number: 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. I Recorded By dl ' lei^ OoAAk (1 Date ___ 0 / ____________________________ 3M Environmental Laboratory Page 276 of 703 BACK TO MAIN Rocord of Deviation /. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 s SOP Method Equipment Procedure Protocol Other: Document Number: ETS-8-110.0 Date(s) of occurrence: 11 Dec 00 to12 Mar 01 II. Description: Required Procedure/process: ETS-fl-110.0 section11.1states, "the average of two standard Curves will be plotted by linear regression (y = mx+bj, weighted 1/x, not forced through zero" Actual Procedure/process: Run s001217 was quantified using three curves. In addition, none o f the runs in this study were quantified using a linear or a weighted curve. quadratic, unweighted curve was used instead. ill. Actions Taken: (such as amendment issued, SO P revision, etc.) No additional action will be needed. Recorded By: IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. Date: zh h l Authorized By: (Study. D irecto r / P ro ject Lad) A Date: , W a f/Q ) 3MEnvironmental Laboratory Deviation No. _____________ (assigned by Study Director or Project Lead at the end of study or project) 3M Environmental Laboratory Page 277 of 703 BACK TO MAIN Record of Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 ^ SOP Method Equipment Procedure Protocol Other: Document Number: ETS-8-11. Date(s) o f occurrence: 11 Dec 00 tol2 Mar 01 II. Description: Required Procedure/process: ETS-8-110.0 sectionlO.2.1 states, " Matrix spikes are prepared for each sample set and analyzed to determine the matrix effect on the recovery efficiency." _ Section 10.2.3 states, "analyze the matrix spike and the matrix spike duplicate ( if prepared) in the same run as the original sample." Actual Procedure/process: Matrix spikes were not prepared for some sample sections, therefore, they were not analyzed. These matrix spikes were not required by method ETS-8-159 or ETS8-160. ill. Actions Taken: (such as amendm ent issued, SO P revision, etc.) A protocol amendment was drafted to address this issue. Recorded By: Date: s'h / t IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. Sufficient matrix spikes Were prepared to gauge the quality of the data. Authorized By: (S tu dyjD irector / ProtectM ead) Date: ~^7 3M Environmental Laboratory *W o f/o i / Deviation No. (assigned by Study Director or Project Lead at the end of study or project) 3M Environmental Laboratory Page 278 of 703 BACK TO MAIN Record of Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 ^ SOP Method Equipment Procedure Protocol Other: ' Document Number: ETS-8-155.0 Date(s) of occurrence: 11 Dec 00 tol2 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 sectionlO.2.1 states, " Matrix spikes are prepared for each sample set and analyzed to determine the matrix effect on the recovery efficiency.' Section 10.2.3 states, "analyze the matrix spike and the matrix spike duplicate ( if prepared) in the same run as the original sample." Actual Procedure/process: Matrix spikes were not prepared for some sample sections, therefore, they were not analyzed. These matrix spikes were not required by method ETS-8-159 or ETS8-160. iil. Actions Taken: (such as amendment issued, SO P revision, etc.) ETS-8-155 method has been revised so that matrix spikes may be prepared at the discretion Of the project lead. Recorded By: Date: k -J & fa / f IV. Impact on Study/P roject This deviation does not adversely affect the quality of the data. Sufficient matrix spikes Were prepared to gauge the quality of the data. Authorized By: (Study D irecto r / P r e c t/L e a d ) Date: / '-r 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) 3M Environmental Laboratory Page 279 of 703 BACK TO MAIN Record of Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 8. SOP Method Equipment Procedure Protocol Other: Document Number: TS-8-155.0 Date(s) o f occurrence: 11 Dec 00 to12 Mar 1 II. Description: Required Procedure/process: ETS-8-155.0 sectionl 1.1states, "the average of two standard Curves will be plotted by linear regression (y = mx+b), weighted 1/x, not forced through zero" Actual Procedure/process: Run t001215 was quantified using three curves. III. Actions Taken: (such as amendment issued, SO P revision, etc.) No additional action will be needed. Recorded By: ClAf' C&sJyKJ IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. Date: 7? /V Authorized By: (Study D irecto r / P r o je c t Lead) Dsaatie:.* 67 > 3M Environmental Laboratory Deviation No. _____________ (assigned by Study Director or Project Lead at the end of study or project) 3M Environm ental Laboratory Page 280 of 703 BACK TO MAIN Record of Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 53"SOP Method GEquipment Procedure Protocol Other: Document Number: ETS-8-155.0 j Date(s) of occurrence: 11 Dec 00 to! 2 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 section1Instates, "If the calibration curve does Not meet acceptance criteria performroutine maintenance or prepare a new standard curve (if necessary) and reanalyze" Actual Procedure/process: Some analytical runs contained one low curve point that failed acceptance criteria but was intentionally left in the calibration curve. The elimination of this Point would have resulted in successivejfailures of each next highest point in the curve. These Low points serve to anchor the quadratic curve and are needed to achieve an acceptable Calibration of the instrument. III. Actions Taken: (such as amendment issued, SO P revision, etc.) No additional action will be needed. Recorded By: jU & U '' IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. Date: 5 / `i f of 3M Environmental Laboratory Date:. / v f/6 / Deviation No. _____________ (assigned by Study Director or Project Lead at the end of study or project) 3M Environm ental Laboratory Page 281 of 703 BACK TO MAIN R ecord of D eviation /. Identification Study / Project No. Deviation Type: (Check onej PFOS Adsorb/Desorb/ E00-1311 SOP ^Method Equipment Procedure Protocol Other: .... Document Number: ETS-8-155.0 Date(s) of occurrence: 11 Dec tol2 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 sectionl6.4 states, "Print the integration summary, Integration method, and chromatogmms...and store in the study folder. Actual Procedure/process: Each acquisition sequence is set up similarly in that they begin with Solvent blank(s), and one set of standards prior to the samples bracketed by calibration curves. These samples serve to condition the column and warmup the instrument. These samples were Not processed along with the study samples and no chromatograms were printed out. This was Because they do not relate to the study in any way. III. Actions Taken: (such as amendment issued, SO P revision, etc.) No additional action will be needed. Recorded By: fx / j U - zV -- > IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. D ate: _2i_ 5|n|tn 3M Environmental Laboratory 3M Environm ental Laboratory Deviation No. ____________ (assigned by Study Director or Project Lead at the end of study or project) Page 282 of 703 BACK TO MAIN R ecord of D eviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ EOO-1311 SOP ^Method Equipment Procedure Protocol Other: Document Number: ETS-8-155.0 Date(s) of occurrence: 4/4/01,4/2/01, 4/12/001 II. Description: Required Procedure/process: ETS-8-155.0 section 14.4 states, "Continuing Calibration Verification (CCV) percent recoveries must be 30% of the standard concentration" Actual Procedure/process: In runs R010404, R010402(b), R010405, H010404, and R010412 The 5ng/ml CCV was outside the acceptable calibration range 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 Were used to demonstrate the continued acceptability of the calibration and the 5ng/ml Points were ignored. III. Actions Taken: (such as amendment issued, SO P revision, etc.) No action is needed. Recorded By: O .u n d u , IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. Date: p) / I i / a j 3M Environmental Laboratory 3M Environm ental 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 /. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 SOP $ Method Equipment Procedure Protocol Other: Document Number: TS-8-155.0 Date(s) o f 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 less than one half of the lowest standard used in the calibration curve.' Actual Procedure/process: Run rO10329b the area counts of the solvent blanks averaged 56% Ofthe area count of the lowest standard used in the curve. This amount of contamination is Not expected to have a significant effect on the sample quantitation. ill. Actions Taken: (such as amendment issued, SO P revision, etc.) No additional action will be needed. Recorded By: IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. D ate: 5! ic/o t 3M Environmental Laboratory Date:. . S// 7/oj Deviation No. _____________ (assigned by Study Director or Project Lead at the end of study or project) 3M Environm ental Laboratory Page 284 of 703 BACK TO MAIN Record of Deviation /. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 SOP '^Method Equipment Procedure Protocol Other: Document Number: TS-8-155.0 Date(s) of occurrence: 11 Dec 0 to12 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 section 11.2 states, "If the calibration curve does Not meet acceptance criteria performroutine maintenance or prepare a new standard curve (if necessary) and reanalyze.' Actual Procedure/process: High/low level standards were eliminated from curves to better fit The ranges appropriate to the data. Additionally calibration points that did not meet acceptance Criteria were thrown out of the curve. ill. Actions Taken: (such as amendment issued, SOP revision, etc.) The SOP will be revised to reflect these changes in the method. Recorded By: _____ O f ' n r L j 0 jir ) ( U \cu IV. impact on Study / Project This deviation does not adversely affect the quality of the data. Date: s~ 3M Environmental Laboratory 3M Environm ental Laboratory Date: . ^ // 7/0 / Deviation No. ____________ (assigned by Study Director or Project Lead at the end of study or project) * Page 285 of 703 BACK TO MAIN Record o f Deviation /. Identification Study / Project No. Deviation Type: (Check one) PFOS Adsorb/Desorb/ E00-1311 SOP 51Method Equipment Procedure Protocol ' Other: Document Number: ETS-8-155.0 Date(s) of occurrence: 11 Dec to12 Mar 01 II. Description: Required Procedure/process: ETS-8-155.0 section 10.1.2 states, "Analyze a method blank and A matrix blank prior to each calibration curve" Actual Procedure/process: There were several rims that did not analyze these blanks prior to the Calibration curve. These blanks were run alongside the samples being analyzed instead. Since The matrix and method blanks are to measure the contamination in the sample prep procedures And in the matrix solutions this is not expected to affect the results of the study. ill. Actions Taken: (such as am endment issued, SO P revision, etc.) No additional action will be needed. Recorded By: A k C ardU TK-J 57 IS ( / IV. Impact on Study / Project This deviation does not adversely affect the quality of the data. D ate: silfi J AuthorizedLBy- (Study,D irector /P r o je c t Lead) y y 7Date: ao / 3M Environmental Laboratory Deviation No. (assigned by Study Director or Project Lead at the end of study or project) 3M Environm ental Laboratory Page 286 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb .... ........... ...~~~... .... E00-1311 .......... .. Associated Study Number:__________________ 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 ofthe spreadsheets corresponds to the dilution factor that was acceptable. 3M Environm ental Laboratory Page 287 of 703 BACK TO MAIN 3M E n v i r o n m e n t a l La b o r a t o r y Note to File Project or Study Number: PFOS Adsorb/Desorb ....... BOO-1311........... '..... Associated Study Number:__________________ 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. 3M Environm ental Laboratory Page 288 of 703 BACK TO MAIN 3M E n v i r o n m e n t a l L a b o r a t o r y Note to File Project or Study Number: PFOS Adsorb/Desorb EOO-1311 Associated Study Number: Each acquisition sequence is set up similarly in that they begin with solvent blank(s), 2 high standards, solvent blank(s), 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 quantity the data or be scrutinized for meeting quality control standards. 3M Environm ental Laboratory Page 289 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb ............ .............................. EOO-1311 ... ...~ Associated Study Number: 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, 5ng/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. Recorded By: t-ncb i h r J j / h L J Date /.c7T7 3M Environm ental Laboratory Page 290 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb E00-131 Associated Study Number: 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 iluted sample and provided a consistent final sample volume of 1.00 mL. The diluters were calibrated to dispense a final volume of 1.OOrnL 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 samples that were not diluted the final sample volume was 1.OmL in all cases. 3M Environmental Laboratory Page 291 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File 1-------------------------------------Project or Study Number: PFOS Adsorb/Desorb E00-1311 Associated Study Number: 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 hut unrecorded steps were: ETS-8-160.1: Section 12.2.12 - "centrifuge until the aqueous layer appears clear" ETS-8-160.1: Section 12.3.7 - "add an equal amount of fresh CaCl2solution 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 Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb 00-1311 Associated Study Number: .............-..... ................- .................................... - 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 Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb .......... ..................... 00-31.......... "....... Associated Study Number:_________________ 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 Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb Eoo-in Associated Study Number: The 00002-104 calibration standards used in this study had a recorded THPFOS concentration of 250ppb, but the actual concentration was 249.3 lppb. 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. Recorded By: C o n e OocLfO Date h LV 3M Environmental Laboratory Page 295 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb ...... .. .. E0-1311 Associated Study Number:__________________ Two analytical methods were used in the analysis of samples in this study. The LC/MS/MS instrument (Soup) was run according to method ETS-8-110.0 and all others were run according to method ETS-8155.0. 3M Environmental Laboratory Page 296 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File Project or Study: PFOS Adsorb/Desorb Associated Study Number: E00-1311 Please note the following observation regarding significant figures: As a result of using two different software programs (HP ChemStation and Excel) to acquire, process and report analytical data, data containing three different amounts of significant figures can be found in the data packets. The chromatograms, batch report, and data imported into Excel are each unique. The imported data (i.e. area counts and concentrations) in Excel always has the highest number of significant figures. The electronic data systems carry more significant figures than are displayed. Unfortunately, the different types of software cannot be adjusted to display a consistent number of significant figures. However, by reporting all final concentrations with three significant figures, any differences in numbers of significant figures displayed in any of the raw data printouts is negated. Recorded By: Date S'/f/! 3M Environmental Laboratory Page 297 of 703 BACK TO MAIN 3M Environmental Laboratory Note to File Project or Study Number: PFOS Adsorb/Desorb EOO-1311 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 = 1suspected outlier - closest value | | maximum value - minimum value | The value of Q is compared to a critical value, Qc. Table of Q Critical values (80% confidence) N Qc 3 .781 4 .560 5 .451 6 .386 7 .344 If Q is larger than Qcthe outlier can be ciscarded with an 80% confidence. 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: Chromatograms 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\H010222.b\HILL0093.D Report Date: 20-Mar-2001 16:17 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Da<ta file D:\chem\Hillary.i\H010222.b\HILL0093.D Lab Smp Id Inj Date 23-FEB-2001 10:02 Operator KLT Inst ID: hillary.i Smp Info 1311-4031-SI Misc Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 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 * DF * 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) 4.92S 4.902 (1.000) 101S824 Compound Not Detected. 249.300 3M Environmental Laboratory Page 303 of 703 Data File: D:\chemSHillary.i\H010222.bSHILL0093.D BACK TO MAIN Page 2 Page 304 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0094.D Report Date: 20-Mar-2001 16:17 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file D:\chem\Hillary.i\H010222.b\HILL0094.D Lab Smp Id Inj Date 23-FEB-2001 10:13 Operator Smp Info KLT 1311-4032-SI Inst ID: hillary.i Misc Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type.- ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032 D Als bottle 55 Dil Factor 1 . 0 0 0 0 0 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 427 499 RT EXP RT REL RT RESPONSE CONCENTRATIONS ON-COLUMN FINAL (ng/mL) ( ug/L) 4.922 4.902 (1.000) 1079934 Compound Not Detected. 249.300 3M Environmental Laboratory Page 305 of 703 D ata F i le : D jSohem S H illary.iSH 010222.bSH ILL0094.D BACK TO MAIN Page 2 2 PFOS (U n d e te c te d ) Page 306 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0095.D Report Date: 20-Mar-2001 16:17 BACK TO MAIN Page 1 3M Environmental Laboratory EOO -1311 PFOS Adsorb/Desorb Data file : D :\chem\Hillary.i\H010222.b\HILL0095.D Lab Smp Id: Inj Date : 23-FEB-2001 10:24 Operator : KLT Inst ID: hillary.i Smp Info : 1311-4033-SI Mise Info : Comment : Method : D :\chem\Hillary.i\H010222.b\H010222t.m Meth Date : 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 56 Dii Factor: 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.929 4.902 (1.000) 1055100 Compound Not Detected. 249.300 3M Environmental Laboratory Page 307 of 703 Data File: D:\chem\Hi1lary.i\H010222,b\HILL0095.D BACK TO MAIN Page 2 Page 308 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0101.D Report Date: 20-Mar-2001 16:17 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Data file D:\chem\Hillary.i\H010222,b\HILL0101.D Lab Smp Id Inj Date 23-FEB-2001 11:31 Operator KLT Inst ID: hillary.i Smp Info 1311-4037-SI Mise Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 62 Dii 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.922 5.153 4.902 (1.000) 5.126 (1.047) 995964 876072 249.300 36.5776 36.6 3M Environmental Laboratory Page 309 of 703 Data File: D:\chernSHinary.i\H010222.bSHILL0101.D BACK TO MAIN Page 2 Page 310 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0102.D Report Date: 20-Mar-2001 16:17 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dafta file D:\chem\Hillary.i\H010222.b\HILL0102.D Lab Smp Id Inj Date 23-FEB-2001 11:42 Operator KLT Inst ID: hillary.i Smp Info 1311-4038-SI Misc Info Comment Method D:\chem\Hillary.i\H010222,b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 63 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATI ONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.922 5.153 4.902 (1.000) 5.126 (1.047) 992751 788043 249.300 33.0166 33.0 3M Environmental Laboratory Page 311 of 703 Data F ile : D :\c h em \H illa ry.i\H 010 222.b S H IL L 0102 .D BACK TO MAIN Page 2 Page 312 of 703 BACK TO MAIN R l p c r t ^ i ^ ^ M ^ o J f t i f 1 0 2 2 2 1A H IL L 0107 - W tIBU9LUUOMAU3 ^ /^ a 9 e 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dafca file D :\chem\Hillary.i\H010222.b\HILL0107.D Lab Smp Id Inj Date 23-FEB-2001 12:38 Operator KLT Inst ID: hillary.i Smp Info 1311-4039-SI Mise Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 64 Dii 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/raL) ( ug/L) 4.917 5.141 4.902 (1.000) 5.126 (1.046) 985052 683545 249.300 28.8722 28.9 D a t a g l i J t y ' g 'lg f H f H a r y . i \H 0 1 0 2 2 2 . b S H IL L 0 1 0 7 . D BACK TO MAIN JO)BJOqe~l mUdUUUOM AUB W Page 2 2 PFOS BACK TO MAIN Data ^l^giD^eJiiemXHillary. i\H010222 ,b\HILL0108 R,jej0qe-i eiuauuuoMAu^ ^/Page 1 Report Date: 20-Mar-2001 16:17 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daf-ta file D:\chem\Hillary.i\H010222.b\HILL0108.D Lab Smp Id Inj Date 23-FEB-2001 12:49 Operator KLT Inst ID: hillary.i Smp Info 1311-4039MS-S1 Misc Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 65 Dil Factor 1 . 0 0 0 0 0 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 427 499 CONCENTRATIONS ON-COLUMN RT EXP RT REL RT RESPONSE (ng/mL) FINAL ( ug/L) 4.914 5.138 4.902 (1.000) 5.126 (1.046) 844071 4577937 249.300 224.827 225 Dat| l ^ 11lara*isH010222.b\HILL0108.D BACK TO MAIN /IO}BJOqB~l IB)UaLUU0JIAU3 /\/ Page 2 BACK TO MAIN Data Elle : D g)tghem\Hillary.i\H010222 . bX H ILLO lO S^^gjQ ^ BJUQUJU0JIAU3 ^gP a9'e 1 ReportruDare: 2tP-Mar-2001 16:18 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Da*ta file D:\chem\Hillary.i\H010222,b\HILL0109.D Lab Smp Id Inj Date 23-FEB-2001 13 00 Operator KLT Inst ID: hillary.i Smp Info 1311-4040-SI Misc Info Comment Method D :\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 66 Dil Factor 1 . 0 0 0 0 0 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 427 499 CONCENTRATIONS ON-COLUMN RT EXP RT F.EL RT RESPONSE (ng/mL) FINAL ( ug/L) 4.909 5.140 4.902 (1.000) 5.126 (1.047) 990932 277725 249.300 11.7051 11.7 Data File: D :\chem\Hi11ary.iSH010222.bSHILLO109.D BACK TO MAIN Page 2 Page 318 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0110.D Report Date: 20-Mar-2001 16:18 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Da*ta file : D:\chem\Hillary.i\H010222.b\HILL0110.D Lab Smp Id: Inj Date : 23-FEB-2001 13 12 Operator : KLT Inst ID: hillary.i Smp Info : 1311-4041-SI Mise Info : Comment : Method : D :\chem\Hillary.i\H010222.b\H010222t.m Meth Date : 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 67 Dil Factor: 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.917 5.141 4.902 (1.000) 5.126 (1.046) 986341 246166 249.300 10.4312 10.4 3M Environm ental Laboratory Page 319 of 703 Data File: D:\chenSHi 11aryi\H01C>222,bSHILLC>L104D BACK TO MAIN Page 2 Page 320 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0111.D Report Date: 20-Mar-2001 16:13 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Da*ta file D:\chem\Hillary.i\H010222.b\HILL0111.D Lab Smp Id Inj Date 23-FEB-2001 13:23 Operator KLT Inst ID: hillary.i Smp Info 1311-4042-SI Mise Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 68 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.908 5.139 4.902 (I.000) 5.126 (1.047) 982392 265448 249.300 11.2875 11.3 3M Environm ental Laboratory Page 321 of 703 Data File: D:\chem\Hillary.iSH010222.bSHILLO:Lll.D BACK TO MAIN Page 2 Page 322 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0112.D Report Date: 20-Mar-2001 16:18 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Da*ta file D:\chem\Hillary.i\H010222,b\HILL0112.D Lab Smp Id Inj Date 23-FEB-2001 13:34 Operator KLT Inst ID: hillary.i Smp Info 1311-4042MS-S1 Mise Info Comment Method D :\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 69 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS RT EXP RT REL RT RESPONSE ON-COLUMN (ng/mL) FINAL ( ug/L) 4.915 5.146 4.902 (1.000) 5.126 (1.047) 873132 4439371 249.300 210.793 211 3M Environm ental Laboratory Page 323 of 703 Data File* D:\chem\Hillary,i\HO10222,b\HILL0:L12,D BACK TO MAIN Page 2 2 .2 - 2 .0 -' 1.8-: 1 .6 -j ~ 1.4-: < 1.2-i 1 1.0-; ~ 0 .8 > 0 6-: 0.4-: "'2i 4 .0 2 PFOS 9 .0 8.0- 7 .0 - ; 6 .0 - 1 5,0-' o ' h 4.0-: > 3 *<H 2 .0 -' Io n --------------------------------------- r 4 .9 1 5 1, 1- 4 .4 4 .8 M in 5 I2 Io n - 3 J 1 5^6 H . / -i---------- 1 A Erfofyffrfittal'hbortry Page 324 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0113.D Report Date: 20-Mar-2001 16:13 BACK TO MAIN Page 1 3M Environmental Laboratory- E00-1311 PFOS Adsorb/Desorb Data file D:\chem\Hillary.i\H010222.b\HILL0113.D Lab Smp Id Inj Date 23-FEB-2001 13:45 Operator KLT Inst ID: hillary.i Smp Info 1311-4043-SI Mise Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Als bottle 70 Cal File: HILL0032 D Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Target Version: 4.10 Compound Sublist: all.sub Processing Host W19401 Concentration Formula: Amt * E'F * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS RT EXP RT REL RT RESPONSE ON-COLUMN (ng/mL) FINAL ( ug/L) 4.914 5.145 4.902 (1.000) 5.126 (1.047) 984852 269994 249.300 11.4511 11.4 3M Environmental Laboratory Page 325 of 703 Data File; D:\ohem\Hillary,i\H010222.b\HILL0:L13.D BACK TO MAIN Page 2 Page 326 of 703 Data Pile: D:\chem\Hillary.i\H010222.b\HILL0114.D Report Date: 20-Mar-2001 16:13 BACK TO MAIN Page 1 3M Environmental Laboratory- E00--1311 PFOS Adsorb/Desorb Data file D:\chem\Hillary.i\H010222.b\HILL0114.D Lab Smp Id Inj Date 23-FEB-2001 13:56 Operator KLT Inst ID: hillary.i Smp Info 1311-4044-SI Mise Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t .m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 71 Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * EF * CpndVariable Cpnd Variable Local Compound Variable Compounds X THPFOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.925 5.149 4.902 (1.000) 5.126 (1.046) 999207 236262 249.300 9.88635 9.89 3M Environmental Laboratory Page 327 of 703 Data File; D ;SchenSHillaryiNH010222.b\H1LLO114,D BACK TO MAIN Page 2 2 PFOS Page 328 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0115.D Report Date: 20-Mar-2001 16:18 BACK TO MAIN Page 1 3M Environmental Laboratory E00--1311 PFOS Adsorb/Desorb Da*ta file D:\chem\Hillary.i\H010222.b\HILL0115.D Lab Smp Id Inj Date 23-FEB-2001 14:07 Operator KLT Inst ID: hillary.i Smp Info 1311-4045-SI Mise Info Comment Method D :\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle 72 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 4.922 5.146 4.902 (1.000) 5.126 (1.04S) 997394 242527 249.300 10.1649 10.2 3M Environmental Laboratory Page 329 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0L15.D BACK TO MAIN Page 2 Page 330 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0116.D Report Date: 20-Mar-2001 16:13 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file : D:\chem\Hillary.i\H010222,b\HILL0116.D Lab Smp Id: Inj Date : 23-FEB-2001 14:18 Operator : KLT Inst ID: hillary.i Smp Info : 1311-4045MS-SI Mise Info : Comment : Method : D:\chem\Hillary.i\H010222,b\H010222t.m Meth Date : 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date : 22-FEB-2001 22:42 Cal File: HILL0032.D Als bottle: 73 Dii Factor: 1 . 0 0 0 0 0 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 CONCENTRATIONS RT EXP RT REL RT RESPONSE ON-COLUMN (ng/mL) FINAL ( ug/L) 4.923 5.154 4.902 (1.000) 5.126 (1.047) 861434 4358791 249.300 209.780 210 3M Environmental Laboratory Page 331 of 703 Data File? D:\chem\Hi 1lary.iSH010222.b\HILL0116.L BACK TO MAIN Page 2 Page 332 of 703 Data File: D:\chem\Hillary.i\H010222.b\HILL0121.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\HILL0121.D Lab Smp Id Inj Date 23-FEB-2001 15:14 Operator Smp Info KLT 1311-4046-Sl Inst ID: hillary.i Mise Info Comment Method D:\chem\Hillary.i\H010222.b\H010222t.m Meth Date 13-Mar-2001 16:01 terrell Quant Type: ISTD Cal Date 22-FEB-2001 22:42 Als bottle 74 Cal File: HILL0032 .D Dil Factor 1 . 0 0 0 0 0 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 427 499 CONCENTRATIONS ON-COLUMN RT EXP RT REL RT RESPONSE (ng/mL) FINAL ( ug/L) 4.923 5.147 4.902 (1.000) 5.126 (1.046) 1017804 330798 249.300 13.5623 13.6 3M Environmental Laboratory Page 333 of 703 Data File: D:\chem\Hi 1lary.i\H010222.bSHILL0:L21.L BACK TO MAIN Page 2 Page 334 of 703 Data File: D:\chem\Rush.i\R01D222.b\RUSH0053.D Report Date: 09-Mar-2001 10:01 BACK TO MAIN Page 1 3M Environmental Laboratory Daa file D:\chem\Rush.i\R010222.b\RUSH0053.D Lab Smp Id Inj Date 23-FEB-2001 02:39 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4061-SI Mise 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 Cal File: RUSH0032.D Als bottle 26 Dii 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 427 499 CONCENTRATI ONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) S.555 5.512 (1.000) 713961 Compound Not Detected. 249.300 3M Environm ental Laboratory Page 335 of 703 Data Fi lei D:\chem\Rush.i\R010222.b\RUSH0053.D BACK TO MAIN Page 2 Page 336 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0054.D Report Date: 09-Mar-2001 10:01 BACK TO MAIN Page 1 3M Environmental 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-SI Mise 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 Cal File: RUSH0032.D Als bottle 27 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL . RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 427 5.559 5.512 (1.000) 722949 249.300 499 5.783 5.722 (1.040) 52969 2.96660 2.97 3M Environm ental Laboratory Page 337 of 703 Data Fi lei DiSohemSRush.i\R010222,bSRUSH0054.D BACK TO MAIN 4' 83 M ^ h v if$ ffh e n f ? Latfrato ry Page 338 of 703 Data File: D:\chem\Rush.i\R013222.b\RUSH0055.D Report Date: 09-Mar-2001 10:01 BACK TO MAIN Page 1 3M Environmental Laboratory- Data file D:\chem\Rush.i\R010222,b\RUSH0055.D Lab Smp Id Inj Date 23-FEB-2001 03:01 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4063-SI Mise 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 Cal File: RUSH0032 D Als bottle 28 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.560 5.512 (1.000) 717685 Compound Not Detected. 249.300 3M Environm ental Laboratory Page 339 of 703 Data File: D:\chem\Rush.i\R010222.bSRUSH0055.D BACK TO MAIN Page 2 1,8 1 .6 1 .4 in 1.2 S 1 *` 3 8- >- 0 . 6 0 .4 0 .2 - Io n 4 .8 5 .2 5 .6 6 .0 6 .4 __________H in _____________________ Page 340 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0065.D Report Date: 09-Mar-2001 10:01 BACK TO MAIN Page 1 3M Environmental Laboratory Da*ta file D:\chem\Rush.i\R010222.b\RUSH0065.D Lab Smp Id Inj Date 23-FEB-2001 04:53 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4067-SI Mise 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 Cal File: RUSH0032.D Als bottle 34 Dii Factor 1 . 0 0 0 0 0 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) 5.532 5.750 5.512 (1.000) 5.722 (1.039) 715149 708991 249.300 39.3413 39.3 3M Environm ental Laboratory Page 341 of 703 Data File; D :\chem\Rush.i\R010222,bSRUSH0065,D BACK TO MAIN Page 2 Page 342 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0066.D Report Date: 09-Mar-2001 10:01 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0066.D Lab Smp Id Inj Date 23-FEB-2001 05:04 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4068-SI Mise 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 Cal File: RUSH0032 D Als bottle 35 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.525 5.749 5.512 (1.000) 5.722 (1.041) 718563 738565 249.300 40.8065 40.8 3M Environm ental Laboratory Page 343 of 703 Data File; D:\chem\Rush.i\R010222.b\RUSH0066.D BACK TO MAIN Page 2 Page 344 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0067.D Report Date: 09-Mar-2001 10:01 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0067.D Lab Smp Id Inj Date 23-FEB-2001 05:16 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4069-SI Mise 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 Cal File: RUSH0032.D Als bottle 36 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.539 5.763 5.512 (1.000) 5.722 (1.040) 721833 483585 249.300 26.4888 26.5 3M Environm ental Laboratory Page 345 of 703 Data File: D:\chemSRush.i\R010222.b\RUSH0067..D BACK TO MAIN Page 2 1 .2 1 .0 - I o n ro r vs> Iis 0 *8 IO < 0 *6wX* > 0*4- __ J0*2- 1___ 1______________ 4' s3 M 5 h v i($ffn e r! Lafiofatory Page 346 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0068.D Report Date: 09-Mar-2001 10:01. 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 Mise 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 Cal File: RUSH0032.D Als bottle 37 Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4 . 1 0 Processing Host W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS ON-COLUMN RT EX P RT REL RT RESPONSE (ng/mL) FINAL ( ug/L) 5.539 5.763 5.512 (1.000) 5.722 (1.040) 626695 3383101 249.300 228.263 228 3M Environmental Laboratory Page 347 of 703 Data File: D:\chemSRushU\R010222.bSRUSH0068.D BACK TO MAIN Page 2 2 PFOS Page 348 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0069.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0069.D Lab Smp Id Inj Date 23-FEB-2001 05:38 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4070-SI Mise 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 Cal File: RUSH0032 D Als bottle 38 Dii Factor 1 . 0 0 0 0 0 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 427 499 CONCENTRATIONS RT EXP RT REL RT RESPONSE ON-COLUMN (ng/mL) FINAL ( ug/L) 5.541 5.758 5.512 (1.000) 5.722 (1.039) 723074 353028 249.300 19.2794 19.3 3M Environmental Laboratory Page 349 of 703 Data File: D:\chem\Rush.i\R010222.bSRUSHC'069 ,D BACK TO MAIN Page 350 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0070.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Daita file D:\chem\Rush.i\R010222.b\RUSH0070.D Lab Smp Id Inj Date 23-FEB-2001 05:49 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4071-SI Mise 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 Cal File: RUSH0032.D Als bottle 39 Dil Factor 1.00000 Integrator Falcon Target Version: 4.10 Compound Sublist: all.sub 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 RT EXP RT REL RT RESPONSE (ng/mL) FINAL { ug/L) 5.541 5.758 5.512 (1.000) 5.722 (1.039) 713569 401704 249.300 22.2391 22.2 3M Environmental Laboratory Page 351 of 703 Data File; DjSchemSRush.i\R010222.b\RUSH0070,D BACK TO MAIN page 2 Page 352 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0071.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0071.D Lab Smp Id Inj Date 23-FEB-2001 06:00 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4072-SI Mise 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 Cal File: RUSH0032.D Als bottle 40 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL. RT EXP RT REL RT RESPONSE (ng/mL) { ug/L) 5.539 5.756 5.512 (1.000) 5.722 (1.039) 710887 385139 249.300 21.3995 21.4 3M Environmental Laboratory Page 353 of 703 Data File? Dj\ohem\Rush.iSR010222.b\RUSH0071,D BACK TO MAIN Page 2 2 PFOS Page 354 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0072.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0072.D Lab Smp Id Inj Date 23-FEB-2001 06:11 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4072MS-S1 Mise 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 Cal File: RUSH0032.D Als bottle 41 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS . ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.539 5.756 5.512 (1.000) 5.722 (1.039) 626987 3324237 249.300 223.877 224 3M Environmental Laboratory Page 355 of 703 Data File: D:\chemSRush,iSR010222,b\RUSH0072..D BACK TO MAIN Page 2 Page 356 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0073.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory- Data file D:\chem\Rush.i\R0L0222.b\RUSH0073.D Lab Smp Id Inj Date 23-FEB-2001 06:23 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4073-SI Mise 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 Cal File: RUSH0032.D Als bottle 42 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.546 5.770 5.512 (1.000) 5.722 (1.040) 719422 366061 249.300 20.0945 20.1 3M Environmental Laboratory Page 357 of 703 Data File: D:\chemSRush.i\R010222.bSRUSH0073.D BACK TO MAIN Page 2 Page 358 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0074.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D :\chem\Rush.i\R010222.b\RUSH0074.D Lab Smp Id Inj Date 23-FEB-2001 06:34 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4074-SI Mise 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 Cal File: RUSH0032.D Als bottle 43 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.546 5.770 5.512 (1.000) 5.722 (1.040) 721925 377219 249.300 20.6367 20.6 3M Environmental Laboratory Page 359 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0074..D BACK TO MAIN Page 2 2 PFOS Page 360 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0079.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0079.D Lab Smp Id Inj Date 23-FEB-2001 07:30 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4075-SI Mise 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 Cal File: RUSH0032.D Als bottle 44 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.547 5.779 5.512 (1.000) 5.722 (1.042) 721016 356402 249.300 19.5198 19.5 3M Environmental Laboratory Page 361 of 703 Data File: D:\chem\Rush. i\R010222.b\RUSH0079..D BACK TO MAIN Page 2 1 .8 -i 1 .6 -i 1 .4 -j ~in 1.2 3 08-; 5- 0 .6 -j 0.4-; 0,2-' Ion 4.8 5.2 5.6 6.0 6.4 ________Min________________ 2 PFOS Page 362 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0080.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0080.D Lab Smp Id Inj Date 23-FEB-2001 07:41 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4075MS-S1 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 Cal File: RUSH0032.D Als bottle 45 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) { ug/L) S .541 5.772 5.512 (1.000) 5.722 (1.042) 530748 3329105 249.300 222.791 223 3M Environmental Laboratory Page 363 of 703 Data Filet DtSchemSRush.i\R010222,bSRUSH0080tD BACK TO MAIN 2 PFOS Page 364 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0081.D Report Date: 09-Mar-2001 10:02 BACK TO MAIN Page 1 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0081.D Lab Smp Id Inj Date 23-FEB-2001 07:52 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4076-SI Mise 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 Cal File: RUSH0032.D Als bottle 46 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.553 5.777 5.512 (1.000) 5.722 (1.040) 721345 400719. 249.300 21.9443 21.9 3M Environmental Laboratory Page 365 of 703 Data File; D;SchemSRush.iSR010222.b\RUSH0081,.D BACK TO MAIN Page 2 Page 366 of 703 Data File: D:\chem\Rush.i\R0l0222.b\RUSH0107.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Da<ta file D:\chem\Rush.i\R010222.b\RUSH0107.D Lab Smp Id Inj Date 23-FEB-2001 12:43 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4090-SI Mise 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 Cal File: RUSH0032.D Als bottle 64 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.510 5.734 5.512 (1.000) 5.722 (1.041) 676009 288064 249.300 16.8245 16.8 3M Environmental Laboratory Page 367 of 703 Data File} D:\chem\Rush,i\R010222.b\RUSH0107.D BACK TO MAIN Page 2 Page 368 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0108.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Da*ta file D:\chem\Rush.i\R010222.b\RUSH0108.D Lab Smp Id Inj Date 23 -FEB-2001 12:54 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-409 0MS-SI Mise 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 Cal File: RUSH0032.D Als bottle 65 Dii Factor 1 . 0 0 0 0 0 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 SG MASS 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.521 5.745 5.512 (1.000) 5.722 (1.041) 594782 3043722 249.300 215.511 216 3M Environm ental Laboratory Page 369 of 703 Data File D:\chem\Rush.i\R010222.b\RUSH0108.D BACK TO MAIN Page 2 Page 370 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0109.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN page l 3M Environmental Laboratory Data file D:\chem\Rush.i\R010222.b\RUSH0109.D Lab Smp Id Inj Date 23-FEB-2001 13:05 Operator KLT/MLA Inst ID: Rush.i Smp Info 1311-4091-SI Mise 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 Cal File: RUSH0032.D Als bottle 66 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.520 5.512 (1.000) 696138 Compound Not Detected. 249.300 3M Environm ental Laboratory Page 371 of 703 Data File: D:\chem\Rush,i\R010222.b\RUSH0109tD BACK TO MAIN Page 2 2 PFOS (Undetected) Page 372 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0110.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Da.lta file D:\chem\Rush.i\R010222 .b\RUSH0H0 .D Lab Smp Id Inj Date 23-FEB-2001 13:16 Operator KLT/MLA Inst ID: Rush.i Smp Info 1 3 1 1 - 4 0 9 2 -SI Mise Info Comment Method D:\chem\Rush.i\R010222.b\R010222t.m Meth Date 09-Mar-2001 09 15 terrell Quant Type: ISTD Cal Date 2 2 -FEB-2001 22 45 Cal File: RUSH0032.D Als bottle 67 Dii 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 427 499 RT EXP RT REL RT RESPONSE CONCENTRATIONS ON-COLUMN FINAL (ng/mL) { ug/L) 5.502 5.512 (1.000) 702240 Compound Not Detected. 249.300 3M Environm ental Laboratory Page 373 of 703 Data File: D:\chero\Rush.i\R010222.b\RUSH0110.D BACK TO MAIN Page 2 Page 374 of 703 Data File: D:\chem\Rush.i\R010222.b\RUSH0111.D Report Date: 09-Mar-2001 10:03 BACK TO MAIN Page 1 3M Environmental Laboratory Da*ta file D:\chem\Rush.i\R010222.b\RUSH0111.D Lab Smp Id Inj Date 23-FEB-2001 13:27 Operator KLT/MLA Inst ID : R u s h .i Smp Info 1 3 1 1 - 4 0 9 3 -SI Mise 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 Cal File: RUSH0032.D Als bottle 68 Dii 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) S.S04 5.512 (1.000) 713216 Compound Not Detected. 249.300 3M Environm ental Laboratory Page 375 of 703 Data File? D:\chem\Rush.i\R010222.b\RUSH0111.D BACK TO MAIN Page 2 Page 376 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0036.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Ddta file D :\Chem\Hillary\H010309,b\HILL0036.D Lab Smp Id 1311-4103-SI Inj Date 09-MAR-2001 22:29 Operator KLT Inst ID: hillary.i Smp Info Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312 .m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 14 Dii 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.034 5.265 5.009 (1.000) 5.233 (1.046) 1056178 234470 254.000 8.01228 8.01 3M Environm ental Laboratory Page 377 of 703 Data File: D:\Chem\HillargSH010309.bSHILlJX>36.D BACK TO MAIN Page 2 Page 378 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0037.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dafta file D:\Chem\Hillary\H0l0309.b\HILL0037.D Lab Smp Id 1311-4104-SI Inj Date 09-MAR-2001 22:40 Operator KLT Inst ID: hillary.i Smp Info Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031 D Als bottle 15 Dii Factor 1 . 0 0 0 0 0 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.037 5.268 5.009 (1.000) 5.233 (1.046) 1221819 215844 254.000 6.16960 6.17 3M Environmental Laboratory Page 379 of 703 Data Filet Dt\Chem\Hi11ary\H010309.bSHILL0037.D BACK TO MAIN Page 2 Page 380 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0038.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Da*ta file D:\Chem\Hillary\H010309.b\HILL0038.D Lab Smp Id 1311-4105-SI Inj Date 09-MAR-2001 22:51 Operator KLT Inst ID: hillary.i Smp Info Study Number EOO-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 16 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist : all.sub Target Version: 4 . 1 0 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.042 5.266 5.009 (1.000) 5.233 (1.044) 1028599 237536 254.000 8.37553 8.38 3M Environmental Laboratory Page 381 of 703 Data File Dj\Chem\Hi1lary\H010309.b\HILL0038.D BACK TO MAIN Page 2 Page 382 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0039.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Data file D:\Chem\Hillary\H010309.b\HILL0039.D Lab Smp Id 1311-4105MS-S1 Inj Date 09-MAR-2001 23:03 Operator KLT Inst ID: hillary.i Smp Info Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 17 Dil Factor 1 . 0 0 0 0 0 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 FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ug/mL) 5.029 5.260 5.009 (1.000) 5.233 (1.046) 874849 3963142 254.000 190.967 191 3M Environmental Laboratory Page 383 of 703 Data File: D:\Chem\H11arySH010309,b\HILL0039.D BACK TO MAIN Page 2 Page 384 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0040.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory . E00-1311 PFOS Adsorb/Desorb Dafta file : D:\Chem\Hillary\H010309.b\HILL0040.D Lab Smp Id: 1311-4106-SI Inj Date : 09-MAR-2001 23:14 Operator : KLT Inst ID: hillary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:10 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 Compounds * 1 THPFOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS ON-COLUMN PINAL RT EXP RT REL RT RESPONSE (ng/mL) (ug/mL) 5.036 5.260 5.009 (1.000) 5.233 (1.045) 1468017 452939 254.000 11.5341 11.5 3M Environmental Laboratory Page 385 of 703 Data File? D:\Chem\Hi 1lary\H010309.b\HILL0040,D BACK TO MAIN Page 2 2 PFOS Page 386 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0041.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dalta file : D :\Chem\Hillary\H010309.b\HILL0041.D Lab Smp Id: 1311-4107-SI Inj Date : 09-MAR-2001 23:25 Operator : KLT Inst ID: hillary.i Smp Info : Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 19 Dil Factor: 1 . 0 0 0 0 0 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 PINAL RT EXP RT REL RT RESPONSE (ng/mL) (ug/mL) 5.034 5.265 5.009 (1.000) 5.233 (1.046) 1055707 325164 254.000 11.5124 11.5 3M Environmental Laboratory Page 387 of 703 Data File: D:\Chem\Hi11 ary\H010309*b\HILL0041 .D BACK TO MAIN Page 2 Page 388 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0042.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Data file D :\Chem\Hillary\H010309.b\HILL0042.D Lab Smp Id 1311-4108-S1 Inj Date 09-MAR-2001 23:37 Operator KLT Inst ID: hillary.i Smp Info Study Number EOO-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031 D Al s bottle 2 0 Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4 . 1 0 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 EX P RT REL RT RESPONSE (ng/mli) (ug/mL) 5.026 5.250 5.009 (1.000) 5.233 (1.045) 1050237 304848 254.000 10.7900 10.8 3M Environmental Laboratory Page 389 of 703 Data File: D:\Chem\Hillary\H010309.bSHILL0042.D BACK TO MAIN Page 2 Page 390 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0043.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dalta file : D:\Chem\Hillary\H010309.b\HILL0043.D Lab Smp Id: 1311-4108MS-S1 Inj Date 09-MAR-2001 23:48 Operator : KLT Inst ID: hillary.i Smp Info : Study Number E00-1311 Mise Info : Comment : Method : D:\Chem\Hillary\H010309.b\H0103l2.m Meth Date : 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 21 Dii Factor: 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL (ng/mL) (ug/mL) 5.028 5.259 5.009 (1.000) 5.233 (1.046) 865040 4001498 254.000 195.209 195 3M Environmental Laboratory Page 391 of 703 Data File: D:\Chem\Hi1lary\H010309.b\HILL0043.D BACK TO MAIN Page 2 Page 392 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0044.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb U d L d J -X JL ti D :\Chem\Hillary\H010309.b\HILL0044.D Lab Smp Id 1311-4109-SI Inj Date 09-MAR-2001 23:59 Operator KLT Inst ID: hillary.i Smp Info Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 22 Dii Factor 1.00000 Intec_rrator 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.027 5.258 5.009 (1.000) 5.233 (1.046) 1073533 173898 254.000 5.57372 5.57 3M Environmental Laboratory Page 393 of 703 Data File} D:\ChemSHillarySH010309.b\HILL0044.D BACK TO MAIN Page 2 Page 394 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0045.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Dalta file D :\Chem\Hillary\H010309.b\HILL0045.D Lab Smp Id 1311-4110-SI Inj Date 10-MAR-2001 00:11 Operator KLT Inst ID hillary.i Smp Info Study Number E00-1311 Misc Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 23 Dil Factor 1 . 0 0 0 0 0 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.031 5.262 5.009 (1.000) 5.233 (1.046) 1045079 179135 254.000 5.95635 5.96 3M Environmental Laboratory Page 395 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0045.D BACK TO MAIN Page 2 Page 396 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0050.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Datta file : D :\Chem\Hillary\H010309.b\HILL0050.D Lab Smp Id: 1311-4111-SI Inj Date : 10-MAR-2001 01:08 Operator : KLT Inst ID: hillary.i Smp Info : Study Number E00-1311 Mise Info : Comment : Method : D:\Chem\Hillary\H010309.b\H010312.m Meth Date : 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date : 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle: 24 Dii 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.027 5.258 5.009 (1.000) 5.233 (1.046) 1036444 165195 254.000 5.46812 5.47 3M Environmental Laboratory Page 397 of 703 Data Filet D:\ChemSHi1lary\H010309,b\HILL0050.D BACK TO MAIN Page 2 Page 398 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0051.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page l 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Daf-ta file D :\Chem\Hillary\H010309.b\HILL0051.D Lab Smp Id 1311-4111MS-SI Inj Date 10-MAR-2001 01:19 Operator KLT Inst ID: hillary.i Smp Info Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 25 Dii 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 REL RT RESPONSE (ng/raL) (ug/mL) 5.028 5.259 5.009 (1.000) 5.233 (1.046) 869342 3920789 254.000 190.081 190 3M Environmental Laboratory Page 399 of 703 Data File: DtSChemSHiHary\H010309.bSHILL0051.D BACK TO MAIN Page 2 Page 400 of 703 Data File: D:\Chem\Hillary\H010309.b\HILL0052.D Report Date: 28-Mar-2001 09:00 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dafta file D:\Chem\Hillary\H010309.b\HILL0052.D Lab Smp Id 1311-4112-SI Inj Date 10-MAR-2001 01:30 Operator KLT Inst ID: hillary.i Smp Info Study Number E00-1311 Misc Info Comment Method D :\Chem\Hillary\H010309.b\H010312.m Meth Date 12-Mar-2001 11:10 anderson Quant Type: ISTD Cal Date 09-MAR-2001 21:32 Cal File: HILL0031.D Als bottle 26 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 REL RT RESPONSE (ng/mL) (ug/mL) 5.034 5.265 5.009 (1.000) 5.233 (1.046) 1043258 170915 254.000 5.64850 5.65 3M Environm ental Laboratory Page 401 of 703 Data File: D :\Chem\Hi11aryNH0 10 30 9 ,b\HILL0052.D BACK TO MAIN Page 2 Page 402 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0029.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dafta file : D:\chem\Rush.i\R010314.b\RUSH0029.D Lab Smp Id: Inj Date : 14-MAR-2001 23:57 Operator : KLT Inst ID: Rush.i Smp Info : TN-A 4802 MeOH Mise 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: 92 Dii 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 QUANT SIG MASS 427 CONCENTRATIONS RT EXP RT REL RT RESPONSE ON-COLUMN (ng/mL) FINAL ( ug/L) Compound Not Detected. 3M Environm ental Laboratory Page 403 of 703 BACK TO MAIN 2 PFOS Page 404 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0030.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Da*ta file D:\chem\Rush.i\R010314.b\RUSH0030.D Lab Smp Id Inj Date 15-MAR-2001 00:11 Operator KLT Inst ID: Rush.i Smp Info TN-A 4802 MeOH Mise 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 92 Dii Factor 1 . 0 0 0 0 0 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 QUANT SIG MASS 427 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) { ug/L) Compound Not Detected. 3M Environm ental Laboratory Page 405 of 703 Data File: D:\chem\Rush,iSR010314.b\RUSH0030.D BACK TO MAIN Page 2 Io n 4.8 5.2 5.6 6.0 6.4 ________ H in _____________________ Page 406 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0031.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\RUSH0031.D Lab Smp Id: Inj Date : 15-MAR-2001 00:26 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4121-SI Mise 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: 14 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.467 5.462 (1.000) 1425324 Compound Not Detected. 254.000 3M Environm ental Laboratory Page 407 of 703 Data File: D:\chemSRush.iSR010314.b\RUSH0031.D BACK TO MAIN Page 2 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 EOO-1311 PFOS Adsorb/Desorb DaMza file D:\chem\Rush.i\R0l0314.b\RUSH0032.D Lab Smp Id Inj Date 15-MAR-2001 00:40 Operator KLT Inst ID: Rush.i Smp Info 1311-4122-SI Mise Info Comment Method D :\chem\Rush.i\R0l0314.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 15 Dii 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) II w 5.466 5.462 (1.000) 1078944 Compound Not Detected. 254.000 3M Environm ental Laboratory Page 409 of 703 Data File; DjNchemNRush,i\R010314.bSRUSH0032.D BACK TO MAIN Page 2 Page 410 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0033.D Report Date: 20-Mar-2001 15:47 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Da^ta file D:\chem\Rush.i\R010314.b\RUSH0033.D Lab Smp Id Inj Date 15-MAR-2001 00:54 Operator KLT Inst ID: Rush.i Smp Info 1311-4123-SI Mise 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 16 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSB (ng/mL) ( ug/L) 5.466 5.462 (1.000) 1090803 Compound Not Detected. 254.000 3M Environm ental Laboratory Page 411 of 703 Data File} DSchem\Rush*iNR010314.bSRUSH0033.D BACK TO MAIN Page 2 Ion rfrirfftrfientttab'rtory Page 412 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0060.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\RUSH0060.D Lab Smp Id Inj Date 15-MAR-2001 07:22 Operator KLT Inst ID: Rush.i Smp Info 1311-4137-SI Mise 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 35 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.477 5.687 5.462 (1.000) 5.679 (1.038) 1099389 757619 254.000 22.8306 22.8 3M Environmental Laboratory Page 413 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0060.D BACK TO MAIN Page 2 Page 414 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0061.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Ddta file D :\chem\Rush.i\R010314,b\RUSH0061.D Lab Smp Id Inj Date 15-MAR-2001 07:36 Operator KLT Inst ID: Rush.i Smp Info 1311-4138-SI Mise 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 36 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATI ONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) { ug/L) 5.469 5.686 5.462 (1.000) 5.679 (1.040) 1083504 757822 254.000 23.2114 23.2 3M Environmental Laboratory Page 415 of 703 Data File; D:\chem\Rush.i\R010314.b\RUSH0061.D BACK TO MAIN Page 2 Page 416 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0062.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page l 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Ddta 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 Mise 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 37 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.470 5.687 5.462 (1.000) 5.679 (1.040) 947454 4939810 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 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 Ddta file D:\chem\Rush.i\R010314.b\RUSH0063.D Lab Smp Id Inj Date 15-MAR-2001 08:05 Operator KLT Inst ID: Rush.i Smp Info 1311-4139-SI 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 38 Dil Factor 1 . 0 0 0 0 0 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 427 499 CONCENTRATIONS ON-COLUMN RT EXP RT REL RT RESPONSE (ng/raL) FINAL ( ug/L) 5.469 5.687 5.462 (1.000) 5.679 (1.040) 1086262 684895 254.000 20.6690 20.7 3M Environmental Laboratory Page 419 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0063.D BACK TO MAIN Page 2 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 EOO-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-SI Mise 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 39 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/raL) ( ug/L) 5.469 5.686 5.462 (1.000) 5.679 (1.040) 1087521 677314 254.000 20.3860 20.4 3M Environmental Laboratory Page 421 of 703 Data File D ;\chem\Rush.i\R010314,b\RUSH0064.D BACK TO MAIN Page 2 2 PFOS 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 Datta file D :\chem\Rush.i\R010314.b\RUSH0065.D Lab Smp Id Inj Date 15-MAR-2001 08:34 Operator KLT Inst ID: Rush.i Smp Info 1311-4141-SI Mise 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 40 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.401 5.691 5.462 (1.000) 5.679 (1.038) 1075484 687097 254.000 20.9767 21.0 3M Environm ental Laboratory Page 423 of 703 Data File} DjSchemSRush.i\R010314,b\RUSH0065.D BACK TO MAIN Page 2 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 E00-1311 PFOS Adsorb/Desorb Delta file D :\chem\Rush.i\R010314.b\RUSH0066.D Lab Smp Id Inj Date 15-MAR-2001 08:48 Operator KLT Inst ID: Rush.i Smp Info 1311-4141MS-S1 Mise 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 41 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.473 5.684 5.462 (1.000) 5.679 (1.038) 915669 4776931 254.000 228.225 228 3M Environm ental Laboratory Page 425 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0066.D BACK TO MAIN Page 2 2 PFOS Page 426 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0067.D Report Date: 20-Mar-2001 15:48 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb D^ta file D:\chem\Rush.i\R010314.b\RUSH0067.D Lab Smp Id Inj Date 15-MAR-2001 09:02 Operator KLT Inst ID: Rush.i Smp Info 1311-4142-SI Mise 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 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4 . 1 0 Processing Host: W19401 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 REL RT RESPONSE (ng/mL) ( ug/L) 5.478 5.695 5.462 (1.000) 5.679 (1.040) 1079679 673507 254.000 20.4226 20.4 3M Environm ental Laboratory Page 427 of 703 Data File: D:\chem\Rush.i\R010314.b\RUSH0067.D BACK TO MAIN Page 2 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 l 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dcfcta file D:\chem\Rush.i\R010314.b\RUSH0068.D Lab Smp Id Inj Date 15-MAR-2001 09:17 Operator KLT Inst ID: Rush.i Smp Info 1311-4143-SI 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 43 Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.470 5.687 5.462 (1.000) 5.679 (1.040) 1108514 716747 254.000 21.2606 21.3 3M Environm ental Laboratory Page 429 of 703 Data File: D:\chem\Rush.i\R010314,bNRUSHC>068.D BACK TO MAIN Page 2 Page 430 of 703 Data File: D:\chem\Rush.i\R0l0314.b\RUSH0072.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\RUSH0072.D Lab Smp Id Inj Date 15-MAR-2001 10:14 Operator KLT Inst ID: Rush.i Smp Info TN-A 4802 MeOH Mise 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 93 Dii Factor 1 . 0 0 0 0 0 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 QUANT SIG MASS 427 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) Compound Not Detected. 3M Environm ental Laboratory Page 431 of 703 Data File: D:\chem\Rush,iSR010314.b\RUSH0072.D BACK TO MAIN Page 2 Page 432 of 703 Data File: D:\chem\Rush.i\R0l0314.b\RUSH0073.D Report Date: 20-Mar-2001 15:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dcita file D:\chem\Rush.i\R010314.b\RUSH0073.D Lab Smp Id Inj Date 15-MAR-2001 10 29 Operator KLT Inst ID: Rush.i Smp Info 1311-4144-SI 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 44 Cal File: RUSH0027.D Dil Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.483 5.700 5.462 (I.000) 5.679 (1.040) 1091080 688862 254.000 20.7003 20.7 3M Environm ental Laboratory Page 433 of 703 Lata File D:\chem\Rush.i\R010314,b\RUSH0073,D BACK TO MAIN Page 2 2 PFOS 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 EOO-1311 PFOS Adsorb/Desorb Dtta file D :\chem\Rush.i\R010314.b\RUSH0074.D Lab Smp Id Inj Date 15-MAR-2001 10:43 Operator KLT Inst ID: Rush.i Smp Info 1311-4144MS-S1 Mise 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 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.462 5.686 5.462 (1.000) 5.679 (1.041) 895662 4609795 254.000 224.468 224 3M Environmental Laboratory Page 435 of 703 Data File} D :\chem\Rush.i\R010314.b\RUSH0074.D BACK TO MAIN Page 2 2 PFOS Page 436 of 703 Data File: D:\chem\Rush.i\R0l0314.b\RUSH0075.D Report Date: 20-Mar-2001 15:49 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Da^a 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-SI Mise 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 46 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) ( ug/L) 5.467 5.684 5.462 (1.000) 5.679 (1.040) 1070260 640428 254.000 19.4900 19.5 3M Environmental Laboratory Page 437 of 703 BACK TO MAIN 2 PFOS 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 Dafta file : D:\chem\Rush.i\R0l0314.b\RUSH0076.D Lab Smp Id: Inj Date : 15-MAR-2001 11 12 Operator : KLT Inst ID: Rush.i Smp Info : 1311-4146-SI Mise 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: 47 Dii Factor: 1 . 0 0 0 0 0 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 SXG MASS 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) { ug/L) 5.459 5.676 5.462 (1.000) 5.679 (1.040) 1090781 644391 254.000 19.2107 19.2 3M Environmental Laboratory Page 439 of 703 Data File; D:\chem\Rush.i\R010314.b\RUSH0076.D BACK TO MAIN Page 2 Page 440 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0031.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dcf-ta file D:\Chem\Hillary\H010404.b\HILL0031.D Lab Smp Id 1311-4151-SI Inj Date 04-APR-2001 21:52 Operator CMC Inst ID: hillary.i Smp Info Omg/L PFOS Study Number E00-1311 Mise Info Comment Method D :\Chem\Hillary\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 41 Dii Factor 1 . 0 0 0 0 0 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 49 9 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSE (ng/mL ) (ng/mL) 5.108 5.092 0.016 1562301 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 441 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0031.D BACK TO MAIN Page 2 Page 442 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0032.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Da^a file D :\Chem\Hillary\H010404,b\HILL0032.D Lab Smp Id 1311-4152-SI Inj Date 04-APR-2001 22:07 Operator CMC Inst ID: hillary.i Smp Info Omg/L PFOS Study Number EOO-1311 Mise Info Comment Method D :\Chem\Hillary\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 42 Dii Factor 1 . 0 0 0 0 0 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) 5.111 5.092 0.019 1575594 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 443 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0032.D BACK TO MAIN 2 PFOS (U n d e te c te d ) Page 444 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0033.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Da^a file D:\Chem\Hillary\H010404.b\HILL0033.D Lab Smp Id 1311-4153-SI Inj Date 04-APR-2001 22:21 Operator CMC Inst ID: hillary.i Smp Info Omg/L PFOS Study Number E00-1311 Misc Info Comment Method D :\Chem\Hillary\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 43 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) 5.106 5.092 0.014 . 1560062 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 445 of 703 Data File: D:\Chem\Hillara\H010404.bSHILL0033.D BACK TO MAIN Page 2 3.0 Ion 2 .4 - yj, ~ 2.1- \ S. 1.8; W A 3 1.5- ^ > 1.2; W 0.9; 0.6; a, a3 M i?fiv i^ h e n f f'L a lx S fa to ry Page 446 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0034.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\H010404.b\HILL0034.D Lab Smp Id 1311-4153MS-S1 Inj Date 04-APR-2001 22:36 Operator CMC Inst ID: hillary.i Smp Info Omg/L PFOS Study Number E00-1311 Mise Info Comment Method D :\Chem\Hillary\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 44 Dii Factor 1 . 0 0 0 0 0 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) 5.105 5.315 5.092 5.309 0.013 0.006 1537278 3170996 254.000 168.305 254 168 3M Environmental Laboratory Page 447 of 703 Data F ile : D :\C h em \H illaryS H 010404.b\H ILL 003 4.D " BACK TO MAIN Page 2 Page 448 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0035.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN lP a g e 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dalta file : D:\Chem\Hillary\H010404.b\HILL0035.D Lab Smp Id: 1311-4154-SI Inj Date : 04-APR-2001 22:50 Operator : CMC Inst ID: hillary.i Smp Info : Omg/L PFOS Study Number E00-1311 Mise Info : Comment : Method : D :\Chem\Hillary\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: 45 Dii Factor: 1 . 0 0 0 0 0 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) 5.098 5.092 0.006 1599896 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 449 of 703 Data File: D;SChemSHillarySH010404.b\HILL0035.D BACK TO MAIN Page 2 Page 450 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0036.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Daf-ta file D:\Chem\Hillary\H010404.b\HILL0036.D Lab Strip Id 1311-4155-SI Inj Date 04-APR-2001 23:04 Operator CMC Inst ID: hillary.i Smp Info Omg/L PFOS Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\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 46 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/mli) (ng/mL) 5.099 5.092 0.007 1613917 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 451 of 703 Data File} D:\Chem\Hi1lary\H010404.b\HILL0036.D BACK TO MAIN Page 2 Page 452 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0037.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page l 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dsfta file D:\Chem\Hillary\H010404.b\HILL0037.D Lab Smp Id 1311-4156-SI Inj Date 04-APR-2001 23:19 Operator CMC Inst ID: hillary.i Smp Info Omg/L PFOS Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\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 47 Dii Factor 1 . 0 0 0 0 0 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 THPPOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS RT EXP RT DLT RT RESPONSE ON-COLUMN (ng/mL) FINAL (ng/mL) 5.093 5.092 0.001 1644662 Compound Not Detected 254.000 254 3M Environmental Laboratory Page 453 of 703 Data File: D:\Chem\Hi1lary\H010404.b\HILL0037.D BACK TO MAIN Page 2 Page 454 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0039.D Report Date: 09-Apr-2001 13:05 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dai-ta file D:\Chem\Hillary\H010404.b\HILL0039.D Lab Smp Id 1311-4157-SI Inj Date 04-APR-2001 23:48 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number E00-1311 Misc Info Comment Method D :\Chem\Hillary\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 49 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 CONCENTRATIONS QUANT SIG ON-COLUMN FINAL , MASS RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) 427 499 5.098 5.092 0.006 1587389 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 455 of 703 Data File: D:\ChemSHillary\H010404*b\HILL0039.D BACK TO MAIN Page 2 Page 456 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0040.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dstta file D:\Chem\Hillary\H010404.b\HILL0040.D Lab Smp Id 1311-4158-SI Inj Date 05-APR-2001 00:02 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\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 50 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4 . 1 0 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 DLT RT RESPONSE CONCENTRATIONS ON-COLUMN PINAL (ng/mL) (ng/mL) 5.098 5.092 0.006 1567309 Compound Not Detected. 254.000 254 3M Environm ental Laboratory Page 457 of 703 Data File: D:\ChemSHillary\H010404.b\HILL0040,D BACK TO MAIN Page 458 of 703 Data File: D:\Chem\Hillary\H0l0404.b\HILL0041.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dsfta file D:\Chem\Hillary\H0l0404.b\HILL0041.D Lab Smp Id 01003-07-03 Inj Date 05-APR-2001 00:16 Operator CMC Inst ID hillary.i Smp Info 5 ng/mL PFOS in MeOH Mise Info Comment Method D :\Chem\Hillary\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 3 Dii Factor 1 . 0 0 0 0 0 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) 5.105 5.315 5.092 5.309 0.013 0.006 1307B17 101216 254.000 2.67325 254 2.67 3M Environm ental Laboratory Page 459 of 703 Data File: D:\Chem\Hi1lary\H010404.bSHILL0041.D BACK TO MAIN Page 2 2,01,8-j 1.6-j l^o 1.2-: o 1.0-i 3 0.8-i 5- 0 .6 - i 0 ,4 -. 0.2-i 4 .4 4 2 PFOS Page 460 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0045.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Dta file : D:\Chem\Hillary\H010404.b\HILL0045.D Lab Smp Id: 1311-4159-SI Inj Date : 05-APR-2001 01:14 Operator : CMC Inst ID: hillary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Mise Info : Comment : Method : D:\Chem\Hillary\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: 51 Dii Factor: 1 . 0 0 0 0 0 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 CONCENTRATI ONS ON-COLUMN RT EXP RT DLT RT RESPONSE (ng/mL) FINAL (ng/mL) 5.098 5.315 5.092 5.309 0.006 0.006 1569488 202756 254.000 7.96638 254 7.97 3M Environm ental Laboratory Page 461 of 703 Data File: D:\ChemSHillarySH010404.b\HILL0045.D BACK TO MAIN Page 2 Page 462 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0046.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Ddta file D:\Chem\Hillary\H010404.b\HILL0046.D Lab Smp Id 1311-4159MS-S1 Inj Date 05-APR-2001 01:28 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\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 52 Dii Factor 1 . 0 0 0 0 0 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 RT EXP RT DLT RT RESPONSE ON-COLUMN (ng/mL) FINAL (ng/mL) 5.098 5.315 5.092 5.309 0.006 0.006 1521100 3255972 254.000 173.055 254 173 3M Environm ental Laboratory Page 463 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0046.D BACK TO MAIN Page 2 Page 464 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0047.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory <* E00-1311 PFOS Adsorb/Desorb Da^a file D:\Chem\Hillary\H010404.b\HILL0047.D Lab Smp Id 1311-4160-SI Inj Date 05-APR-2001 01:43 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number EOO-1311 Mise Info Comment Method D:\Chem\Hillary\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 53 Dii Factor 1 . 0 0 0 0 0 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 THPPOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) 5.105 5.315 5.092 5.309 0.013 0.006 1563690 80242 254.000 1.58149 254 1.58 3M Environm ental Laboratory Page 465 of 703 Data FileJ D:\Chem\HillarySH010404.b\HILL0047.D BACK TO MAIN Page 2 Page 466 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0048.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\HILL0048.D Lab Smp Id: 1311-4161-SI Inj Date : 05-APR-2001 01:57 Operator : CMC Inst ID: hillary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Misc Info : Comment : Method : D:\Chem\Hillary\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: 54 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 RT EXP RT DLT RT RESPONSE (ng/mL) FINAL (ng/mL) 5.098 5.092 0.006 1535494 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 467 of 703 Data File: D;\Chem\HiHary\H010404.b\HILL0048.D BACK TO MAIN Page 2 Page 468 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0049.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dta file : D:\Chem\Hillary\H010404.b\HILL0049.D Lab Smp Id: 1311-4162-SI Inj Date : 05-APR-2001 02:11 Operator : CMC Inst ID hillary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Mise Info : Comment : Method : D :\Chem\Hillary\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: 55 Dii 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) 5.093 5.092 0.001 1528194 Compound Not Detected. 254.000 254 3M Environmental Laboratory Page 469 of 703 Data File: D:\Chem\Hi1larySH010404.b\HILL<X>49,D BACK TO MAIN Page 2 Page 470 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0050.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\HILL0050.D Lab Smp Id 1311-4162MS-S1 Inj Date 05-APR-2001 02:26 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number E00-1311 Mise Info Comment Method D :\Chem\Hillary\H010404.b\H0l0404.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 56 Dii 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) 5.097 5.315 5.092 5.309 0.005 0.006 1514404 3115242 254.000 165.194 254 165 3M Environmental Laboratory Page 471 of 703 Data File: D :\Chem\Hi11ary\H010404.b\HILL0050.D BACK TO MAIN Page 2 Page 472 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0051.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Dta file D :\Chem\Hillary\H010404.b\HILL0051.D Lab Smp Id 1311-4163-SI Inj Date 05-APR-2001 02:40 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number E00-1311 Mise Info Comment Method D:\Chem\Hillary\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 57 Dii Factor 1 . 0 0 0 0 0 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) 5.097 5.314 5.092 5.309 0.005 0.005 1537963 76776 254.000 1.40113 254 1.40 3M Environmental Laboratory Page 473 of 703 Data File; D:\Chem\Hillary\H010404.b\HILL0051.D BACK TO MAIN Page 2 Page 474 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0052.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\HILL0052.D Lab Smp Id: 1311-4164-SI Inj Date : 05-APR-2001 02:55 Operator : CMC Inst ID: hillary.i Smp Info : 5mg/L PFOS Study Number E00-1311 Mise Info : Comment : Method : D :\Chem\Hillary\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: 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 Compounds 1 THPFOS 2 PFOS QUANT SIG MASS 427 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) 5.091 5.308 5.092 -0.001 5.309 -0.001 1529992 96528 254.000 2.42918 254 2.43 3M Environmental Laboratory Page 475 of 703 Data File: D:\ChemSHillary\H010404.bSHILL0052.D BACK TO MAIN Page 2 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 Laboratory Page 483 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0053.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Dta file D:\Chem\Hillary\H010404.b\HILL0053.D Lab Smp Id 1311-4165-SI Inj Date 05-APR-2001 03:09 Operator CMC Inst ID: hillary.i Smp Info 5mg/L PFOS Study Number EOO-1311 Mise Info Comment Method D:\Chem\Hillary\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 59 Dii Factor 1 . 0 0 0 0 0 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 CONCENTRATI ONS ON-COLUMN FINAL RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) 5.091 5.308 5.092 -0.001 5.309 -0.001 1541462 166651 254.000 6.08283 254 6.08 3M Environm ental Laboratory Page 477 of 703 Data Filet D:\Chern\Hillary\H010404.b\HILL0053.D BACK TO MAIN Page 2 2 PFOS Page 478 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0054.D Report Date: 09-Apr-2001 13:06 BACK TO MAIN Page 1 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb Dta 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: hillary.i Smp Info 5mg/L PFOS Study Number EOO-1311 Mise info Comment Method D:\Chem\Hillary\H010404.b\H010404.m Metti Date 09-Apr-2001 13:02 carlson Quant Type: ESTD Cal Date 04-APR-2001 20:41 Cal File: HILL0026.D Als bottle 60 Dii Factor 1 . 0 0 0 0 0 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 427 493 CONCENTRATIONS ON-COLUMN RT EXP RT DLT RT RESPONSE (ng/mL) FINAL (ng/mL) 5.098 5.308 5.092 0.006 5.309 -0.001 1500713 3133475 254.000 166.211 254 166 3M Environm ental Laboratory Page 479 of 703 Data File: D:\ChemSHillary\H010404.b\HILL0054.D BACK TO MAIN Page 2 Page 480 of 703 Data File: D:\Chem\Hillary\H010404.b\HILL0059.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\HILL0059.D Lab Smp Id: 1311-4166-SI Inj Date : 05-APR-2001 04:35 Operator : CMC Inst ID: hillary.i Smp Info : 5mg/L PFOS Study Number EOO-1311 Mise Info : Comment : Method : D:\Chem\Hillary\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: 61 Dii Factor: 1 . 0 0 0 0 0 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 FINAL RT EXP RT DLT RT RESPONSE (ng/mL) (ng/mL) S .098 5.308 5.092 0.006 5.309 -0.001 1687410 183857 254.000 6.98024 254 6.98 3M Environm ental Laboratory Page 481 of 703 Data File: D:\Chem\Hillary\H010404.bSHILL0059.D 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 Environm ental Laboratory Page 483 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Decatur.PRO\SampleDB\t010l23 Last modified: Wed Jan 24 07:48:32 2001 Method: C: \MASSLYNX\Decatur.PRO\MathDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Wed Jan 24 07:54:16 2001 Page 1 Compdund 1: PFOS(499) ^ # Name t010122 098 2 1010122"'099 3 t010122~"lOO 4 t010122-"lOl 5 t010122~ 102 6 t0 1 0 1 2 2 ""l03 7 t010122~ 104 a t010122~ 105 9 tQ10122_"106 10 t010122~ 107 11 t0l0122~`l06 12 tlO122 "l09 13 t010122~'n o 14 t010122~'111 15 t010122 "112 16 t0l0122"'113 17 t0l0122_" i n 18 t010122"[ll5 19 tQ10123"'OOI 20 t010123~ 21 t010123 003 22 tOl0123~'004 23 t01Q123~'005 24 t010123~"006 25 t010123~*007 26 t010123~'008 27 t010123~"009 28 t010123 'OlO 29 toi 0 1 2 3 ''011 30 t010123* 012 31 t010123"'013 32 t010123 014 33 t010123' 015 34 t010123__016 35 t010123"'017 36 t010l23"'018 37 t010l23~'019 38 t010l23_'020 39 t010l23^'021 40 tQ10l23_ 022 41 t010l23~"023 42 tOlQ123~'024 43 t010123~'025 44 tOl 0123~ 026 45 t010l23`027 46 t010l23"'028 47 t010l23~'029 48 tOlO 123~*030 49 t010123" 031 50 t010123" 032 51 t010l23_'033 52 to 101 2 3 ""034 53 t010123" 035 54 1010123~*036 55 t010l23~*037 56 t010l23~ 038 57 toi 01 2 3 "'039 56 t010l23 "0*0 59 t010l23~"041 60 t010123""042 61 t010l23_ 043 62 t010l23""044 63 t010!23 045 64 t010123~ 046 65 t010123~ 047 66 tQ10l23 048 67 t010123'"049 68 t010123 ~050 69 t010123 051 70 t010l23 052 71 tOl0123 ~053 72 t010l23 "054 73 t010l23 "055 74 to 10123*"056 75 t010123*"057 76 101012 3_~QS8 77 toi 0123""059 79 t010123 "060 79 t010l23 ~061 80 toi 01 2 3 '"062 81 101012 3*"063 82 toi 0 1 2 3 '"064 0 0 Sampielist Text 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 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 lOx E00-1311-3007-S2, Omg/L PFOS,no soil.. lOx EOO-1311-30O8-S2, Omg/L PFOS,no soil.. lOx EO0-1311-3009-S2, Omg/L PFOS,no soil.. lOx EOO-1311-3009ms-S2, Omg/L PFOS,no so.. lOx E00-1311-3010-S2, 5mg/L PFOS,no soil.. 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 E00-1311-3011-S2, 5mg/L PFOS,no soil.. lOx B00-1311-312-S2, Omg/L PFOS,no soil.. lOx EOO-1311-3012ma-S2, Omg/L PFOS,no so.. lOx E0O-1311-3O22-S2, Orag/L PFOS,1:1 cla.. lQx E00-1311-3023-S2, Omg/L PFOS,1:1 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 EOO-1311-3024-S2, Omg/L PFOS,1:1 cla.. lx E00-131l-3024ms-S2, Omg/L PFOS,1:1 c.. lOx EOO-1311-3025-S2, Omg/L PFOS,1:5 cla.. lOx E00-1311-3026-S2, Omg/L PFOS,1:5 cla.. lOx E00-13U-3027-S2, Omg/L 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-I311~3027ms-S2, Omg/L PFOS,1:5 c.. lOx EO0-1311-3028-S2, Omg/L PFOS,1:25 cl.. lOx E00-1311-3029-S2, Omg/L PFOS,1:25 cl.. lOx EOO-1311-303O-S2, Omg/L PFOS,l:25 cl.. lOx EOO-1311-3030ms-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 EO0-1311-3094-S2, 5mg/L PFOS,1:1 cla.. lOx E00-1311-3095-S2, 5rag/L PFOS,1:1 cla.. 1Ox EOO--1311--3096--S2, 5mg/L PFOS,1:1 cla.. 1Ox EO0-1311-3096ms-S2, 5mg/L PFOS,1:1 c.. lOx E00-1311-3097-S2, 5mg/L 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 1Ox E00-1311-3098-S2, 5mg/L PFOS,1:5 cla.. lOx E00-131l-3Q98ms-S2, 5rag/L PFOS,1:5 c.. lOx E00-1311-310-S2, 5mg/L PFOS,1:25 cl.. lOx E00-1311-3101-S2, 5mg/L PFOS,1:25 cl.. lOx E00-1311-3102-S2, 5mg/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 E00~1311-3102ras-S2, 5mg/L PFOS,1:25 .. lOx EOO-1311-3166-S2, 5rag/L PFOS,1:1 Sed. . lOx E00-1311-31668-S2, 5mg/L PFOS,1:1 Se.. lOx EOO-1311-3168-S2, 5rag/L PFOS,1:1 Sed.. lOx E00-131l-3l60ms-S2, 5mg/L PFOS,1:1 S.. 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 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 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 6.304 6.382 6.156 6.159 6.457 6.431 6.408 6.396 6.355 Area 149480 155378 144563 164749 166221 101623 212615 292832 353867 439196 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 130235 B 2227419 1351396 1295576 163488 155335 1338917 2 190122 3728466 3779124 3814147 134U00 166983 166594 4547300 873870 1003813 582014 1618471 1337470 171733 174436 154736 107657 179721 196874 231081 314548 396613 Response 0.000 0.000 0.000 346.252 399.780 436.052 499.891 689.623 841.868 1162.333 1595.061 1977.399 4519.670 8986.881 12406.422 17167.793 0.000 0.000 0.000 350.116 366.988 378.604 3271.735 382.904 4305.279 0.000 0.000 341.086 273.510 3615.037 341.722 255.127 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 451B.724 0.000 0.000 1916.324 2217.788 3017.B93 6774.423 3087.088 4505.026 0.000 0.000 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 0.000 210,235 380.367 456.559 546.187 754.734 988.034 Ppb Flags 0.00 bb 0.00 bb 0.00 bb 3.79 bb 6.92 bbX 9,03 bbX 12.76 bbX 23.83 bb 32.71 MM 51.40 bb 76.63 bb 98.92 bb 246.93 bb 506.27 bb 704.16 970.81 0.00 bb 0.00 bb 0.00 bb 4.02 bb 5.00 bb 5.69 bb 174.31 bb 5.93 bb 239.11 bb 0.00 bb 0.00 bb 3.49 bb 0.00 bb 194.29 bb 3.53 bb 0.00 bb' 252.97 bb 0.00 bb 0.00 bb 3.85 bb 170.06 MM 0.00 bb 0.64 bb 0.00 bb 236.44 bb 0.00 bb 0.00 bb 129.49 bb 5.56 bb 5.88 bb 3.15 bb 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 0.00 5.78 10.23 15.46 27.63 41.24 %Dev od Comment 177 81 -1-85 3 br CO l &( 5 -SfzJU" ' h d - h L r^ / / y -r4e-c ( / O ca t s i & i O < 'j-b-li U ^ - f a Se<^-i^csL.(ftC)e m c m -r -o | A K 'U & 4 i \ 3M Environm ental Laboratory Page 484 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: . C:\MASSLYNX\Decatur.PR0\SampleDB\t010123 Last modified: Wed Jan 24 07:48:32 2001 Method: C:\MASSLYNX\Deoatur.PR0\MethDB\PF0S - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Wed Jan 24 07:54:16 2001 Compound 1: PFOS(499) Name 83 t010123 065 84 t010123~ 066 85 t010123* 067 86 t010123' 068 87 t010123**069 88 tQ10123**070 89 t010123'*071 90 t010123**072 91 t010123**073 Samplelist Text 50 ppb FC Mix 00002-104-07 75 ppb FC Mix 00002-104-00 100 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 RT 6.303 6.374 6.300 6.340 6.150 6.163 6.156 6.164 6.141 Area 463216 623373 740153 1392032 2222555 3363541 4161343 137404 141494 Response 1186.763 1561.132 1995.565 4451.B28 9308.893 13449.481 180860..008080 0.000 ppb Flags 52.83 bb 74.65 bb 99.98 bb 242.90 bb 524.93 bb 764.42 bb 1031.66 bb 0.00 bb 0.00 bb %Dev 6 -0 -0 -3 5 2 3 Page 2 Quantitated and Printed by CMC on 24 Jan 01 Study # E00-1311 3M Environm ental Laboratory i(c3'"'' f<9t Page 485 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tuaker (LA052) Sample List: C:VMASSLYNX\Pecatur.PRO\SafflpleDB\t010123 Last modified: Wed Jan 24 07:48:32 2001 Method: C: \MASSLYNX\Decatur. PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Wed Jan 24 07:54:16 2001 Compound 2: I.S.(TH-PFOS)(427) * {fame 1 t010122 09B 2 t010122"099 3 t010122~100 4 t010122~101 5 t010122~102 6 t010122~103 7 t010122"l04 8 tO10122~X05 9 t010122~106 10 t010122~107 11 t010122"l08 12 t010122~109 13 t010122~110 14 t010122~ll1 IS t010122 112 16 t010122~113 17 t010122_114 18 t010122_115 19 t010123 001 20 t010123~002 21 t010123~003 22 t010123 0 04 23 t010123~005 24 t010123~006 25 t010123_007 26 t010123~008 27 t010123 009 28 t010123~010 29 t010123~011 30 tOlO123_012 31 tOl0123~0l3 32 t010123_014 33 t010123 015 34 t010123_016 35 t010123~017 36 t010123 018 37 t010123~019 38 t010123~020 39 t010123~021 40 t010123 022 41 t010123~023 42 t010123~024 43 tO10123~025 44 t010123~026 45 t010123 027 46 t010123~028 47 t010123 029 48 t010123~030 49 t010123 031 50 t010123~032 51 t Q l O m 033 52 t010123~034 53 t010123J)35 54 t010123 036 55 t010123 037 56 t010123~03B 57 t010123 039 58 t010123~04 0 59 t010123 041 60 t010123~042 61 t010123 043 62 t010123~Q4 4 63 t010123~045 64 t010123~046 65 t010123 047 66 t010123 048 67 t010123 049 6B t010123 050 69 t010123 051 70 t010123~052 71 t010123~053 72 t010123 054 73 t010123 055 74 t010123 056 75 t010123~057 76 tO10123^058 77 t010123~059 78 t010123~060 79 t010123~06l 80 t010123~062 81 t010123~063 82 t010123~064 Samplelist Text 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 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 lOx E00-1311-3007-S2, Omg/L PFOS,no soil.. lOx E00-1311-3008~S2, Omg/L PFOS,no soil.. lOx E00-1311-3009-S2, Omg/L PFOS,no soil.. lOx EOO-1311-3009ras-S2, Omg/L pFOS,no so.. lOx E00-1311-3010-S2, 5mg/L PFOS.no soil.. 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 10x E00-1311-3011-S2, 5mg/L PF0S.no soil.. lOx E00-1311-3012-S2, Omg/L PFOS.no soil.. lOx EO0-1311-3012ms-S2, Orag/L PFOS.no 3 0 .. lOx EOO-1311-3022-S2, Omg/L PFOS,1:1 cla.. lOx E00-1311-3023-S2, Omg/L PFOS,1:1 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 EOO-1311-3024-S2, Omg/L PFOS,1:1 cla.. lOx E00-1311-3024n\3-S2, Omg/L PF0S,1:1 c.. lOx EOO-1311-3025-S2, Omg/L PFOS,1:5 cla.. 10x-E0O-1311-3026-S2, Omg/L PFOS,1:5 cla,. lOx E00-1311-3027-S2, Omg/L 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 EOO-1311-3027ms-S2, Omg/L PFOS,1:5 e.. lOx EO0-1311-3028-S2, Omg/L PFOS,1:25 cl.. lOx E00-1311-3029~S2, Omg/L PFOS,1:25 cl.. IQx EOO-1311-3030-S2, Omg/L PFOS,1:25 cl.. lOx E00-131l-3030ms-S2, 0rag/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 EOO-1311-3094-S2, 5mg/L PFOS,1:1 cla.. lOx EOO-1311-3095"S2, 5mg/L PFOS,1:1 cla.. lOx EOO-1311-3096-S2, 5 n g / b P F O S , 1:1 cla.. lOx EOO-1311-3096ms-S2, 5mg/L PFOS,1:1 c.. lOx EO0-1311-3097-S2, 5mg/L 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 EO0-1311-3O98-S2, 5mg/L PFOS,1:5 cla.. lOx EOO-1311-3098ras-S2, 5rag/L PFOS,1:5 c.. lOx EO0-1311-3100-S2, 5mg/L PFOS,1:25 cl.. lOx E00-1311-3101-S2, 5mg/L PFOS,1:25 cl.. lOx EOO-1311-3102-S2, 5mg/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 EO0-1311-3102ras-S2, 5mg/L PFOS,1:25 .. lOx EOO-1311-3166-S2, 5mg/L PFOS,1:1 Sed.. lOx EOO-1311-31668-S2, 5mg/L PFOS,1:1 Se.. lOx EOO-1311-3168-S2, 5rag/L PFOS,1:1 Sed.. lOx EOO-1311-3168m3-S2, 5mg/L PFOS,1:1 S.. 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 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 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 6.98B 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 6.2B9 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 6.34 6 6.335 6.324 6.294 Area 691 560 661 118951 103945 104129 106331 106157 105084 94464 91385 87246 72111 56656 62640 49733 951 553 548 109593 103586 103996 83590 105510 72867 675 Q 108447 113341 79040 122235 118145 7902B 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 Response 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 49732.637 951.098 552.916 547.605 109593.180 103586.234 103995.594 83589.734 105510.461 72866.516 675.222 108447.039 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 110999.164 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 72219.969 127941.430 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 Flags 1.95 bb 1.58 bb 1.87 bb 336.00 bb 293.61 bb 294.13 bb 300.35 bb 299.85 bb 296.82 bb 266.83 bb 258.13 bb 246.44 bb 203.69 bb 160.03 bb 176.94 bb 140.48 bb 2.69 bb 1.56 bd 1.55 bb 309.56 bb 292.59 bb 293.75 bb 236.11 bb 298.03 bb 205.82 bb 1.91 bd 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 304.74 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 34B.35 bb 333.66 bb 304.51 bb 298.76 bb 294.30 bb 283.47 bb %Dev od Comment 34 17 18 20 20 19 7 3 -1 -19 -36 -29 -44 24 17 18 -6 19 -18 23 20 -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 Page 3 Quantitated and Printed by CMC on 24 Jan 01 Study # E00-1311 3M Environm ental Laboratory C M l iij-1 /a i Page 486 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Ddsorb Study, LC/MS Instrument: Tucket (LA052) Sample List: C: \MASSLYNX\Decatur. PRO\SampleDB\t010123 Last modified: Wed Jan 24 07:48:32 2001 Method: C:\MASSLYNX\Decatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Coda: Printed: Wed Jan 24 07:54:16 2001 Compound 2: X.S.(TH-PFOS)(427) 1 Hama 83 t010123 065 B4 t010123"'066 85 t010123 067 86 t010123~ 068 87 t010123_069 88 tO10123 070 89 t010123~"071 90 tO10123~"072 91 t010123~'073 Samplelist Text 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 RT 6.242 6.302 6.251 6.279 6.102 6.091 6.095 6.092 6.069 Area 97500 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 Flags 275.63 bb 281.98 bb 261.91 bb 220.81 bb 168.60 bb 176.60 bb 162.48 bb 4.24 bb 5.09 bb ftDev 10 13 5 -12 -33 -29 -35 Page 4 Quantitated and Printed by CMC on 24 Jan 01 Study # E00-1311 3M Environm ental Laboratory tmc Ilatti Page 487 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (IA052) Sample List: C: \MASSLYNX\Decatur.PR0\SampleDB\t010124 Last modified: Wed Jan 24 09:14:06 2001 Method: C:\MASSLYNX\Decatur.PRO \MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Thu Jan 25 07:47:21 2001 Page 1 Compound 1: PFOS(499) # Name t010123 057 / 2 tO 10123 "058 i 3 t O l 0123 "059 4 t0 l0 1 2 3 * "060 5 t010123*"061 6 t0 l0 1 2 3 " 0 62 7 t010123 "063 8 t 0 l 0 1 2 3 ~064 9 t0 1 0 1 2 3 "O 65 10 t0 1 0 1 2 3 "066 11 t O l 0123 067 12 t0 1 0 1 2 3 "068 13 t0 1 0 1 2 3 *069 14 1 0 1 0123' 070 15 t0 1 0 1 2 3 "071 16 t0 10123* ~072 l 17 t0 1 0 1 2 3 " 073 18 t 0 1 0 1 2 4 '"OOI 19 t010124* "002 20 t010124 "003 21 t0 1 0 1 2 4 004 22 t O l 0124 ~005 23 tO 10124 "006 24 t O l 0124 "007 25 t0 1 0 1 2 4 "000 26 t O l 0124""009 27 t O l 0124 "010 28 t0 l0 1 2 4 " o n 29 t 010124 "012 30 t010124 "013 31 t O 10124 "0 14 32 t010 1 2 4 "015 33 t0 1 0 1 2 4 ""0 1 6 34 t010124* " o i 7 35 t010124 "Ol 8 36 tO l0124 '019 37 t O l 0124 "020 38 t010124*"021 39 t0 1 0 1 2 4 "O22 40 t 010124 "023 41 t0 1 0 1 2 4 '~024 42 t010124~"025 43 t010124 "02 6 44 tO l0124~"027 45 t010124""02 8 46 tO l0124" 029 47 t010124""030 48 t0 1 0 1 2 4 ` 031 49 tO l0124~'032 50 tO 10124-'033 51 t0 1 0 1 2 4 " '034 52 t O l 0124" 03,5 53 t0 1 0 1 2 4 " 0 3 6 54 t0 1 0 1 2 4 ~ '0 3 7 55 t0 1 0 1 2 4 " "038 56 t0 1 0 1 2 4 ~ '039 57 t O l 0124" 04 0 58 t010124"'041 59 t010124~'042 60 t010124~ 043 61 t0 1 0 1 2 4 ~ 04 4 62 tD10124~j ) 4 5 63 t0 1 0 1 2 4 "04 6 64 t0 10124* "047 65 t0 1 0 1 2 4 `~048 66 t010124""049 67 t O l 0124'" o s o Samplelist Text MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 6 50 p p b FC Mix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC Mix 0 0 0 0 2 -1 0 4 -0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 ppb FC M ix 0 0 0 0 2 -1 0 4 -1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx E 0 0 -1 3 1 1 -3 1 6 9 -S 2 , 0.5m g/L PFOS,1:5 S .. lOx E 0 0 -1 3 1 1 -3 1 7 0 -S 2 , 0.5m g/L PFOS,1:5 S .. lO x EO0 - 1 3 1 1 - 3 1 7 1 - S 2 , 0 .5 m g /L P F O S ,1 :5 S . . lOx E O O -1311-3171iruj-S2, O.Smg/L PFOS, 1 : 5 . . lOx E O O -1311-3172-S2, 0.5m g/L PFOS,1:25 . . 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E O O -1311-3173-S2, 0.5m g/L PFOS,1:25 . . lOx E O O -1311-3174-S 2, O.Smg/L PFOS,1 :2 5 . . lOx E00 -1 3 1 1 -3 174ra3~S2, 0.5rag/L PFOS,1 : 2 .. lO x E 0 0 -1 3 U -3 1 8 4 -S 2 , Omg/L PFOS, 1 :1 S e d .. lO x E 0 0 - 1 3 1 1 - 3 1 8 5 - S 2 , Omg/L P F O S ,1 :1 S e d .. 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 0 0 -1 3 1 1 -3 1 8 6 -S 2 , Omg/L PFO S,1 :1 S e d .. lO x E 0 0 -1 3 1 1 - 3 1 8 6 ra s - S 2 , Omg/L P FO S ,1 :1 S . . lOx E 0 0 -1 3 1 X -3 1 8 7 -S 2 , Omg/L PFO S,1 :5 S e d .. lO x E O O -1 3 U -3 1 8 B -S 2 , Omg/L PFOS, 1 :5 S e d .. lO x E00 -1 3 1 1 - 3 1 0 9 - S 2 , Omg/L PFO S,1 :5 S e d .. 250 ppb FC Mix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lO x E O O -1 3 1 1 -3 1 0 9 ra s-S 2 , Omg/L P F O S ,1 :5 S . . lOx E O O -1311-31 9 0 -S 2 , Omg/L PFO S,1 :2 5 S e .. lO x E O O -1 3 1 1 -3 1 9 1 -S 2 , Omg/L P FO S,1 :2 5 S e .. lO x E O O -1 3 1 1 -3 1 9 2 -S 2 , Omg/L PFO S,1 :2 5 S e .. lOx EOO -1311 - 3 1 92m s-S 2, Omg/L P FO S,1 :2 5 . . 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 - 1 0 4 - 0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 9 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 1 750 p p b FC Mix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4740, A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 RT 6.382 6 .1 5 6 6.159 6.457 6,431 6.408 6 .3 9 6 6.355 6.303 6.374 6.300 6 .3 4 0 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 .4 0 9 6.328 6.317 6.507 6.290 6.580 6.216 6.420 6 .2 1 8 6.565 6 .3 8 6 6.361 6.218 6 .5 9 2 6.193 6.543 6.528 6.204 6.375 6.123 6.402 6.134 6.159 6.541 6 .0 8 6 6.363 6.111 6 .5 1 6 6.121 6.325 6.121 6 .3 6 0 6.110 6.553 Area 174436 154736 107657 179721 196874 231081 314548 396613 463216 623373 740153 1392032 2222555 3363541 4161343 137404 141494 329160 148405 2008353 297837a 2091729 3089729 2749532 1690139 211382 186560 2974252 2789063 3375943 174753 183066 1492375 185832 192377 189635 1332791 190604 202180 176278 1440653 166808 209975 1789138 201659 177442 202407 1351244 1589633 188064 173176 189146 107963 195139 170706 230314 325950 393053 426687 615435 678046 1475797 2194012 3224378 3953019 137693 185417 Response 0 .0 0 0 0 .0 0 0 2 1 8 .2 3 5 3 8 0 .3 6 7 4 5 6 .5 6 9 546. 187 754.734 988.034 1 1 8 6 .7 6 3 1561.132 1995.565 4 4 5 1 .8 2 8 9 3 0 8 .8 9 3 13449.481 10086.088 0 .0 0 0 0 .0 0 0 O.00Q 0 .0 0 0 3570.085 6104.627 4018.001 8604.097 5030.908 4 4 0 6 .OQ1 0 .0 0 0 0 .0 0 0 5340.462 5 3 9 5 .8 7 8 7580.041 331.804 3 5 1 .0 1 1 4495.674 0 .0 0 0 0.G0Q 378.275 3109.357 369.223 3 6 9 .2 6 6 3 4 4 .8 6 0 4 2 5 9 .8 4 9 0 .0 0 0 0.000 3571.515 4 0 8 .1 1 3 3 4 3 .8 7 2 372.116 . 3603.727 3 7 40003.... 200010006000 2 2 3 .5 9 5 4 4 2 .1 9 6 3 5 9 .2 0 5 5 0 4 .8 7 7 684.561 9 1 3 .3Q9 1007.082 1636.708 1616.410 4437.320 9228.069 13956.302 0.0001 6 7 7 1 . 4 2 2 0.000 ppb Flags 0.00 bb 0.00 bb 7.77 bb 1 6 .2 8 bbX 2 0 .2 8 bbX 2 4 .9 9 bbX 3 5 .9 6 bbX 48.27 bb 58.76 bb 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 .0 0 bb 0 .0 0 bb 186.19 bb 324.90 bb 210.45 bb 469.73 bb 265.72 bb 2 3 1 .5 6 bb Q .00 bb 0 .0 0 bb 282.72 bb 285.76 bb 407,27 bb 13.73 bb 14.78 bb 236.45 bb 0 ,0 0 bb 0 .Q0 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 106.26 bb 17.74 bb 14.36 bb 15.85 bb 188.01 bb 1 9 5 .5 5 MM 0.00 bb 0.00 bb 0.00 bb 8.05 bb 1 9 .5 3 bbX 1 5 .1 7 bbX 2 2 .8 2 bbX 3 2 .2 7 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 %Dev 551 306 150 44 21 18 5 2 -6 1 -0 3 -7 -5 -11 -22 681 203 128 29 11 -1 10 -18 -7 0 4 -5 od Comment l ) 3 - H 5\tlLrkS- <La U-u P /e - r 61bH Court*. J S KC-UJ [ i f C L ^ r t '-i- C/*1*- y - W 'o t 6S>* Quantitated and Printed by CMC on 25 Jan 01 Study # E00-1311 3M Environmental Laboratory M l l / j ' I jI Page 488 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C: \MASSLYNX\Deaatur.PRO\SampleDB\t010124 Last modified: Wed Jan 24 08:14:06 2001 Method: C: \MASSLYNX\Decatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Thu Jan 25 07:47:21 2001 C o a p m d 2: I.S. (TH-PFOS) (427) * Name 1 t0 1 0123 057 2 t O l 0123 "058 3 t010123 "059 4 t010123 060 5 t010123 061 6 t O l 0123 "062 7 t01 0 1 2 3 "063 8 t0 1 0 1 2 3 064 9 t010123 065 10 t 0 1 0 1 2 3 "066 11 t0 1 0 1 2 3 "067 12 t 0 1 0 1 2 3 "068 13 t0 1 0 1 2 3 "069 14 t0 1 0 1 2 3 "070 15 t0 1 0 1 2 3 "071 16 t0 1 0 1 2 3 ~072 17 t0 1 0 1 2 3 "073 10 t0 1 0 1 2 4 ~001 19 t O l 0124 "002 20 t0 1 0 1 2 4 003 21 1010124 " 004 22 t0 1 0 1 2 4 "005 23 t010124 "006 24 t0 1 0 1 2 4 007 25 t 010124 "008 26 t010124 "009 27 t0 1 0 1 2 4 "010 28 t010124 " o il 29 t 010124 ~012 30 t0 1 0 1 2 4 " 013 31 t0 1 0 1 2 4 "014 32 t O l 0124 "015 33 t0 1 0 1 2 4 ~016 34 t0 1 0 1 2 4 017 35 t O l 0124 "018 36 t0 1 0 1 2 4 ~019 37 t0 1 0 1 2 4 020 38 t O l 0124 " o 2 1 39 t0 1 0 1 2 4 022 40 t0 1 0 1 2 4 023 41 t0 1 0 1 2 4 "024 42 t0 1 0 1 2 4 " 025 43 t0 1 0 1 2 4 "026 44 6010124 027 45 t0 1 0 1 2 4 " 028 46 t0 1 0 1 2 4 "029 47 t0 1 0 1 2 4 ~030 48 t0 1 0 1 2 4 " 031 49 t0 1 0 1 2 4 "032 50 t 0 1 0 l 2 4 " 033 51 t 0 1 0 l 2 4 034 52 t0 1 0 1 2 4 " 035 53 t O l 0124 "036 54 tO10124 ~037 55 t0 1 0 1 2 4 ~038 56 t0 1 0 l2 4 ~039 57 t0 1 0 1 2 4 "04 0 58 t0 1 0 1 2 4 041 59 t0 1 0 1 2 4 042 60 t01 0 1 2 4 " 04 3 61 t-010124 044 62 t O l 0124 045 63 t O l 0124 046 64 t O l 0124 047 65 tO lO 124 ~04 8 66 t0 1 0 l2 4 ~04 9 67 t O l 0124 " 050 Samplelist Text MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 ppb FC M ix 0 0 0 0 2 -1 0 4 -0 4 . 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lO x EOO-1311 -3 1 6 9 -S 2 , 0.5m g/L PFOS,1:5 S .. lOx E 0-1 3 1 1 -3 1 7 0 -S 2 , O.Smg/L PFO S,1:5 S . . lOx E 0 0 -1 3 1 1 -3 1 7 1 -S 2 , 0.5m g/L PFO S,1 :5 S .. lOx E 00 -1 3 U -3 1 7 1 m 3 -S 2 , 0.5m g/L PFOS,1 : 5 .. lOx E 0 0 -1 3 1 1 -3 1 7 2 -S 2 , 0.5m g/L PFOS,1:25 . . 250 p p b FC Mix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E00 -1 3 1 1 -3 1 7 3 -S 2 , 0.5m g/L PFOS,1:25 . . lOx E 0 0 -1 3 1 1 -3 1 7 4 -S 2 , 0.5rag/L PFOS,1:25 . . lOx EOO-1311 -3 174ni3-S2, 0.5m g/L PFOS,1 : 2 .. lO x E 0 0 -1 3 1 1 -3 1 8 4 -S 2 , Omg/L P FO S,1 :1 S ed . . lO x EOO-1 3 1 1 -3 1 8 5 - S 2 , Omg/L P F O S ,1 :1 S e d .. 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 1 Ox EO O -1311 - 3 1 8 6 -S 2 , Omg/L P F O S ,1 :1 S e d .. lO x E 0 0 -1 3 1 1 -3 1 8 6 m s-S 2 , Omg/L P FO S,1 :1 S .. lO x EOO-1311 - 3 1 B 7-S 2, Omg/L P FO S,1 :5 S e d .. lO x E 0 0 -1 3 1 1 - 3 1 8 8 -S 2 , Omg/L P FO S,1 :5 S e d .. lO x E 0 -1 3 1 1 -3 1 8 9 -S 2 , Omg/L P F O S ,1 :5 S e d .. 2 5 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lO x EO O -1311 - 3 1 89m 3-S 2, Omg/L P F O S ,1 :5 S . . lO x E 0 0 -1 3 1 1 -3 1 9 0 -S 2 , Omg/L P FO S,1 :2 5 S e .. lO x EOO- 1 3 1 1 - 3 1 9 1 - S 2 , Omg/L P F O S ,l:2 S S e . . lO x E 0 0 -1 3 1 1 -3 1 9 2 -S 2 , Omg/L P FO S,1 :2 5 S e .. lO x E 0 0 - l3 1 1 - 3 1 9 2 m s - S 2 , Orag/L P F O S ,1 :2 5 . . 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 . 5 ppb FC Mix 00002-104-02 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 - 1 0 4 - 0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q , 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 RT 6.322 6 .0 9 5 6 .0 6 3 6.179 6 .3 4 6 6.335 6.324 6.294 6.242 6.302 6.251 6.279 6.102 6.091 6.095 6.092 6 .0 6 9 6.067 6.102 6 .3 3 8 6.075 6.144 6.073 6.301 6.038 6.420 6.157 6 .3 9 6 6 .1 4 5 6.280 6.131 6 .2 0 6 6.230 6.192 . 6.161 6.387 6.145 6.351 6.120 6.347 6.122 6 .4 08 6.192 6.277 6.122 6 .3 1 5 6.121 6 .3 3 8 6.239 6.131 6 .3 1 5 6 .0 3 9 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 .0 4 6 6.252 Area 595 2000 123326 118124 107803 105770 104192 100354 97580 99827 92725 78172 59689 62522 57521 1502 1802 846 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 110324 118808 114045 119036 107590 105922 94005 104869 83147 59439 57758 58925 1403 612 Response 5 9 5 .3 6 8 2000.157 123326.328 118123.727 107803.281 105770.016 104191.516 100354.180 97579.789 99027.031 92724.766 7B 171.930 59689.027 62521.754 57521.328 1502.362 1801.890 8 4 6 .3 0 2 1 7 5 9 .6 4 9 140637.594 121972.141 130147.320 88947.891 136631.984 95899.828 5 6 6 .2 2 7 1 4 5 6 .8 9 6 139231.969 129221.938 111343.148 131668.844 130088.313 82989.492 7 0 3 .9 6 3 125328.508 107159.664 129057.625 136879.719 127789.961 B 4 5 4 0 .3 5 2 1735.427 7 2 1 .5 2 8 125236.625 123531.180 129002.477 1 3 5 9 8 4 .18B 93739.367 106167.570 913.271 1535.103 5 2 1 .4 9 2 120713.117 110323.898 118807.953 114044.594 119036.070 107590.352 105921.656 94005.047 104869.109 8 3 1 4 6 .8 3 6 59438.539 57758.453 58924.914 1482.589 6 1 2 .2 0 5 . ppb Flags 1.61 bb 5.41 bb 333.59 bb 319.52 bb 291.60 bb 286.10 bb 281.83 bb 271.45 bb 263.95 bb 270.03 bb 250.82 bb 211.45 bb 161.46 bb 169.12 bb 155.59 bb 4 .06 bb 4.87 bb 2.29 bb 4.76 bb 380.42 bb 329.93 bb 352.04 bb 240,60 bb 369,58 bb 259.41 bb 1.53 bb 3.94 bb 376.62 bb 349.54 bb 301.18 bb 3 56.16 bb 351.88 bb 224.48 bb 1.90 bb %Dev 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 289.86 bb 349.10 bb 370.25 bb 345.67 bb 228.70 bb 4.69 bb 1.95 bb 338.76 bb 334.15 bb 340.95 bb 367.83 bb 253.56 bb 287.18 bb 2.47 bb 4.15 bb 1.41 bb 326.62 bb 298.42 b b 321.37 bb 308.49 bb 321.99 bb 291.03 bb 286.51 bb 254.28 bb 283.67 bb 224.91 bb 160.78 bb 156.23 bb 159.39 bb 4.01 bb 1 .66 bb 36 16 40 48 38 -9 36 34 40 47 1 15 31 19 29 23 29 16 15 2 13 -10 -36 -38 -36 Page 2 Quantitated and Printed by Q4C on 25 Jan 01 Study # E00-1311 3M Environmental Laboratory cmc f Page 489 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Decatur.PRD\SampleDB\t010125 Last modified: Thu Jan 25 10:45:39 2001 Method: C: \MASSLYWC\Decatur. PRO \MethDB\PFOS - THPFOS Last modified: Wad Jan 31 07:38:20 2001 Job Code: Printed: Wed Jan 31 07:42:18 2001 Compound 1: PFOS(499) # Name 1 t010X25 001 2 t010125~002 3 t0 1 0 1 2 5 003 4 t0 1 0 1 2 5 _ 0Q4 5 t010125~005 6 t010125~006 7 t010125~007 B t010125~008 9 t010125~009 10 tO lO 125 010 11 t0 1 0 1 2 5 _ 011 12 t 0 l0 1 2 5 ~ 0 1 2 13 t0 1 0 1 2 5 _ 013 14 t O 1 0 125~014 15 t0 1 0 1 2 5 ~ 0 1 S 16 t0 1 0 1 2 5 ~ 016 17 t0 1 0 1 2 5 ~ 0 1 7 18 t010125~01B 19 tO l0 1 2 5 ~ 019 20 t010125 020 21 t0 l0 1 2 5 ~ 0 2 1 22 t0 l0 1 2 5 022 23 t 0 l 0 1 2 5 023 24 t0 1 0 1 2 5 024 25 t010125~025 26 t010125~026 27 t0 1 0 1 2 5 027 28 t0 l0125~ 028 29 t010125 029 30 t01012S~030 31 t0 1 0 1 2 5 " 031 32 t0 1 0 1 2 5 032 33 t010125 033 34 t010125~034 35 t010125 035 36 t010125 036 37 t010125 037 38 t010125 038 39 1 0 10125 039 40 t010125~040 41 t0 l0 1 2 5 041 42 t0 1 0 1 2 5 042 43 tO10125~43 44 t0 1 0 1 2 5 ~ 0 4 4 45 t0 1 0 1 2 5 045 46 t010125~046 47 t0 1 0 1 2 5 047 48 t0 1 0 1 2 5 048 49 1010125 049 50 t010125~050 51 t0 1 0 1 2 5 _ 051 52 t010126 052 53 tO10125~053 54 tO10125^054 55 tO 10125 055 56 t010125" 056 57 t0 1 0 1 2 5 057 58 t010125 058 59 t0 10125~ 059 60 t010125 060 61 t0 1 0 1 2 5 _ 061 62 t01012S~ 062 63 t0 10125_063 64 t0 1 0 1 2 5 064 65 t010125~ 065 66 t010125~066 67 t01'0125 067 68 t010125 068 69 t010125~069 70 t010125~070 71 t0 10125 071 72 t01012S " 072 73 t O l 0125 073 74 t0 1 0 1 2 S ~ 074 75 tO 1012S~075 76 t010125 076 77 t0 1 0 1 2 5 ~ 0 7 7 78 t01012S~078 79 tO 10125_079 80 tO l0 1 2 5 ~ 0 8 0 81 t0 1 0 1 2 5 081 82 t0 1 0 1 2 5 ~ 0 8 2 Samplelist Text MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 1000 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 1 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 1 2 .5 ppb FC Mix 0 0 0 0 2 -1 0 4 -0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 p p b FC Mix 0 0 0 0 2 -1 0 4 -1 0 500 ppb FC Mix 0 0 0 0 2 -1 0 4 -1 1 7 5 0 p p b VC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 9 2 5 0 . p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 500 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 2 1 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx EOO-1311-0016 lOx EOO-1311-017 lOx E 00-1311-0018 lOx EOO -1311-0019 lOx EOO-1311-0020 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx E 00-1311-0021 lOx EOO-1311-0O22 lOx EOO-1311-0023 lOx E 00-1311-0024 lOx EOO-1311-0O25 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E00-1311-0O 26 lOx E 00-1311-0027 lOx EOO -1311-0028 lOx E 00-1311-0029 lOx EOO-1311-0030 25 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx E 00-1311-0031 lOx EOO-1311-0032 lOx EOO -1311-0033 lOx E00-L311-0034 lO x EOO-1311-0035 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx EOO-1311-0036 1 Ox EO O -1311 -0 0 3 7 1 Ox EO O -1311-0O 38 lOx EOO-1311-0039 lOx E0O -1311-0040 25 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx EOO-1311-0041 lOx EOO-1311-0042 lOx EOO-1311-0043 RT 6.450 6.241 6.119 6.542 6 .1 0 8 6.543 6.121 6.520 6 .1 5 6 6.388 6.111 6.292 6 .3 8 8 6.074 6.483 6.134 6.509 6 .3 9 8 6.265 6 .1 0 7 6.531 6.265 6.352 6 .1 4 6 6.349 6.121 6.302 6.110 6.458 6 .1 1 0 6 .1 5 6 6.341 6.050 6.520 6.543 6.050 6 .5 9 0 6.073 6 .4 1 0 6.121 6.500 6.169 6.675 6.170 6 .4 5 8 6 .0 4 9 6.567 6 .0 6 2 6.590 6.107 6.662 6.108 6 .4 9 2 6 .0 9 5 6 .6 2 6 6.144 6.612 6.072 6.135 6.170 6.445 6 .0 3 9 6 .4 6 0 6.025 6 .5 0 8 6.035 6.505 6 .0 3 5 6.532 6.674 6.108 6.315 6.012 6.458 6 .0 8 6 6.325 6 .0 9 6 6.205 6 .5 7 9 6.254 6.109 6.507 Area 831200 296143 5181707 5239732 251789 296161 190383 228073 209027 256076 321643 422644 508823 625655 696012 1607022 2477999 3324924 3625888 140546 175460 150713 168830 132405 181926 170151 223063 298612 400141 469182 604584 744175 1484003 2300138 3223153 3992950 178960 106658 168177 84602 162860 141596 180330 141421 1301101 125026 161718 104841 170430 138637 193349 134611 1353B55 139866 198325 139708 198474 146440 55629 145556 1369261 122300 151469 2808144 2511874 2834724 2425654 2748880 1418330 59950 138127 2531397 2761946 2545826 2807459 2632773 1501077 148933 174595 2612098 2687648 2610315 Response 831200.000 296143.250 5101707.000 5239732.000 251708.984 296161.125 190383.219 2 2 0 0 7 3 .4 3 8 209827.078 256076.359 3 2 1 6 4 2 .6 5 6 422643.563 5 0 8 8 2 3 .1 8 8 625654.688 696012.313 1607021.750 2477998.750 3324924.000 3 6 2 5 8 0 8 .2 5 0 140546.016 175459.922 150713.141 168829.969 1 3 2 4 0 4 .5 7 8 181925.563 170150.672 223063.438 298612.031 400141.438 469181.844 604584.250 744174.750 1404002.500 2300137.500 3223152.500 3992949.500 178960.375 106658.201 168176.719 84681.828 162860.281 141596.422 188329.828 141420.531 . 1301100.500 125026.102 161717.701 104841.234 170429.656 138637,172 193349.172 134610.734 1 3 5 3 B S S .250 139866.328 198324.719 139707.766 190473.656 146448.297 55628.688 145555.625 1369261.375 122300.242 151468.953 2808143.500 2511874.250 2834724.000 2425654.250 2748880.250 1418330.250 59950.008 138126.672 2531397.000 2761945.500 2545825.750 2807459.250 2632772.750 1501077.125 148933.156 174594.859 2612098.000 2687647.500 2610315.000 pp b Flags 125.20 bb 9.40 bb 1495.43 bb 1527.47 bb 0.05 bb 9.40 bb 0.00 bb 0.00 bb 0.00 bb 0.95 bb 14.79 bb 36.27 bb 54.76 bb 80.04 bb 95.4 0 bb 304,22 bb 525.01 bb 767,38 bb 862.44 bb 0.0 0 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0 .0 0 bbX 0 .0 0 bbX 0 .0 0 bbX 9 .9 2 bbX 31.47 bb 46.24 bb 7 5.46 bb 105.97 bb 274.84 bb 477.90 bb 736.43 bb 986.75 bb 0.00 bb 0 .0 0 bb 0.00 bb 0.00 bb 0 .0 0 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 244.20 bb 0,00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 247.80 bb 0.00 bb 0.00 bb 615.66 bb 534.11 bb 623.15 bb 511.02 bb 599.06 bb 259.33 bb 0.00 bb 0.00 bb 539.37 bb 602.70 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 4Dev 50 53 -100 -100 -91 -41 -9 10 7 -5 22 5 2 -14 -100 -100 -1 0 0 -60 -21 -8 1 6 10 -4 -2 -1 -7 -2 -1 4 12 od Comment . Page 1 Quantitated and Printed by CMC on 31 Jan 01 Study # E00-1311 . /ne )/?//o( 3M Environmental Laboratory Page 490 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C: \MASSLYNX\Decatur. PRD\SampleDB\t010125 Last modified: Thu Jan 25 10:45:39 2001 Method: C:\MASSLYNX\Decatur.PRO\MathDB\PFOS - THPFOS Last modified: Wed Jan 31 07:38:20 2001 Job Code: Printed: Wed Jan 31 07:42:18 2001 Compound 1: PFOS(499) Name 03 t0 1 0 1 2 5 083 84 t0 1 0 1 2 5 084 85 t O l 0125 085 86 t10125 086 07 t0 1 0 1 2 5 087 88 t O l 0125 088 89 t0 1 0 1 2 5 089 90 t010125~090 91 t0 1 0 1 2 5 091 92 t0 1 0 1 2 5 092 93 t0 1 0 1 2 5 093 94 t0 1 0 1 2 5 094 95 t0 1 0 1 2 5 _ 0 9 5 96 tO l0125 096 97 t0 1 0 1 2 5 097 98 t0 1 0 1 2 5 ~ 0 9 8 99 t01Q 125~Q 99 100 tO l0 1 2 5 ~ 1 00 101 t O l 0125 101 102 t O l 0125 102 103 t0 1 0 1 2 5 103 104 t0 1 0 1 2 5 104 105 t0 10125 105 106 t0 10125 106 107 t0 1 0 1 2 5 1Q7 108 t0 1 0 1 2 5 100 109 tO l0 1 2 5 _ 109 110 t 0 1 0 1 2 5 ~ l 10 111 t0 1 0 1 2 5 111 112 1 010125_112 113 t0 10125 113 114 tO l0 1 2 5 _ 114 115 t0 1 0 1 2 5 115 116 t0 10125 116 117 t010125 117 118 t0 l0 1 2 5 118 119 t 0 1 0 1 2 5 ~ l 19 120 t010125~120 121 t0 1 0 1 2 5 121 122 t01Q 125 122 123 t O l 0125 123 124 t0 1 0 1 2 5 124 125 t010125~125 126 t0 10125 126 127 t0 1 0 1 2 S " l27 12B t0 1 0 1 2 5 128 129 t O l 0125 129 130 tO l0125_130 131 t010125~131 132 t010125~132 133 .010125 13 3 134 t0 1 0 1 2 5 _ 1 3 4 135 tO l0125_135 136 t010125~136 137 t010125~137 138 t010125~13B 139 tO l0125~139 140 t0 1 0 1 2 5 ~14 0 111 t010125~141 142 t 0 1 0 1 2 5 ~ l 42 143 t0 1 0 1 2 5 ~ 143 144 t0 1 0 1 2 5 ~ 1 4 4 145 t010125~145 146 tO l0 1 2 5 ~ 1 4 6 147 t0 1 0 1 2 5 147 148 t010125~14 0 149 tO l0 1 2 5 ~ 14 9 150 t 0 1 0 1 2 5 " l5 0 151 t010125~151 Samplalist Text lO x E0O-1311-OO44 lOx E 00-1311-0045 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 00-1311-0046 lOx E 00-1311-0047 lOx EO O -1311-0048 lOx E 00-1311-0049 lO x EOO-1311-O50 25 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , TN-A^-474 0 , A l i q . 1 2 /0 4 /0 0 lOx E00-1311-0051 lOx E00-1311-0052 lOx E 00-1311-0053 lOx EOO -1311-0054 lOx E 00-1311-0055 2 5 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 00-1311-0056 lOx EOO-1311-0057 lOx E 00-1311-0058 lOx E 00-1311-0059 lO x EOO-1311-0060 250 ppb FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 00-1311-O 061 lOx E00-1311-OO62 lOx EOO-1311-0063 lOx EOO-1311-0064 lOx EOO-1311-0065 25 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E0O-1311-0066 lOx EOO-1311-0067 lOx E00-1311-OO68 lO x E00-1311-0069 lOx EOO-1311-0070 2 5 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 00-1311-0071 lOx EOO-1311-0072 lOx EOO -1311-0073 lOx E00-1311-0074 lOx EOO-1311-0075 250 ppb FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 pp b FC M ix 0 0 0 0 2 -1 0 4 - 0 6 50 pp b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 pp b FC M ix 0 0 0 0 2 -1 0 4 - 0 0 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 2 5 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 5 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 ppb FC M ix 0 0 0 0 2 -1 0 4 -1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 RT 6 .0 7 3 6.324 6.047 6.578 6 .0 3 6 6.313 6 .1 1 9 6 .2 9 9 6.098 6.17 6.050 6.373 6.059 6 .3 6 3 6.09 9 6.120 6 .1 8 0 . 6.331 6 .0 4 6 6 .4 4 8 6.051 6 .5 4 1 6 .4 9 3 6.048 6.340 6.071 6 .4 6 8 6.024 6.552 6.322 6.071 6 .5 0 7 6.061 6.535 6.503 6.058 6.528 6 .3 8 5 6.033 6.168 6 .0 5 0 6 .4 3 6 6.157 6.060 6.662 6.026 6.543 6 .1 5 6 6.073 6.263 6 .1 3 5 6 .5 7 6 6.070 6.581 6 .0 9 5 6 .4 5 0 6.181 6.326 6 .0 9 6 6.312 6 .2 4 0 6.530 6.109 6.424 6.039 6.528 6.040 6.556 6.674 Area 2858504 2564991 1595213 179278 113308 2646938 2804164 2570307 2879210 2533023 1333005 146205 70603 2005865 2065654 1033231 1920545 2784784 1582417 100976 126826 2766212 2534908 3035785 2548403 2813637 1387797 125005 174696 2567028 2770308 2493961 2B01319 2516190 1357075 103976 175921 2561146 1697580 2221049 2703580 2045583 1373129 131690 209049 2281647 1994915 2107328 2275225 2070675 1418906 189572 77809 X882 58 177973 191704 191084 235222 30832B 387661 479692 578191 780577 1380449 2466444 3197643 4125592 205462 71219 Response 2858584.250 2564990.500 1595213.250 179278.266 113308.227 2646937.500 2804164.000 2570386.500 2879210.250 2533023.250 1333005.000 146204.859 70683.414 2005864.625 2065653.500 1833230.750 1920544.625 2784784.000 1582416.750 180975.719 126826.359 2766211.500 2534908.000 3035785.000 2548402.500 2813637.000 1387796.500 125084.563 174695.734 2567027.750 2770308.000 2 4 9 3 9 6 0 .5 0 0 2801318.750 2516190.000 1357075.125 103975.977 175920.563 2561146.000 1697580.000 2221840.750 2703579.500 2045583.000 1373120.625 131689.594 209048.594 2281647.250 1994914.500 2107328.000 2275224.500 2070675.125 1410906.000 189572.422 77009.250 100257.766 177972.719 191784.063 191084.234 235222.219 308328.469 307661.406 479691.563 570191.375 780576.875 1380448.675 2466444.250 3197642.500 4125591.750 205461.656 71219.266 . . ppb Flags 629.91 bb 548.47 bb 301.38 bb 0 .0 0 bb Q.Q0 bb 570.84 bb 614.54 bb 549.94 bb 635.77 bb 539.81 bb 239.33 bb Q.Q bh 0 .0 0 bb 402.35 bb 417.47 bb 359.31 bb 380.97 bb 609.10 bb 298.31 bb 0.00 bb 0.00 bb 603.90 bb 540.32 bb 680.08 bb 543.97 bb 617.20 bb 252.15 bb 0.00 bb 0.00 bb 549.02 bb 605.04 bb 529.29 bb 613.74 bb 535.27 bb 244.95 bb 0.0 0 bb 0.00 bb 547.43 bb 326.10 bb 457.52 bb 586.47 bb 412.39 bb 248.71 bb 0.00 bb 0.00 bb 473.07 bb 399.60 bb 428.08 bb 471.39 bb 418.75 bb 259.46 bb 0.0 0 bb 0.00 bb 0.00 bb 0.00 bb 0 .0 0 bbX 0 .0 0 bbX 0 .0 0 bbX 1 1 .9 8 bbX 28-81 bb 40.49 bb 69.74 bb 114.00 bb 250.42 bb 5 2 1 .9 1 MM 728.76 bb 1034.37 bb 0.00 bb 0.0 0 bb %Dev 21 -4 19 1 -2 -1 4 -100 -100 -100 -52 -28 -3 -7 14 0 4 -3 3 od Comment Page 2 Quantitated and Printed by CMC on 31 Jan 01 Study # E00-1311 3M Environmental Laboratory C i'Vl L Page 491 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tualcer (LA052) Sample List: C:\MASSLYNX\Decatur.PRO\SampleDS\t010125 Last modified: Thu Jan 25 10:45:39 2001 Method: C: \MASSLYNX\Deoatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 31 07:38:20 2001 Job Code: Printed: Wed Jan 31 07:42:18 2001 I.S.(TH-PF0S)(427) 4 Marne 1 t0 1 0 1 2 5 001 2 t01012S 002 3 t010125~003 4 t0 1 0 1 2 5 004 5 t010125_005 6 t010125~006 7 t0 1 0 1 2 5 007 8 t010125~008 9 t010125_009 10 t01Q 12S " l0 11 t0 1 0 1 2 5 ~ 0 1 1 12 t0 1 0 1 2 5 _ 012 13 t0 10125~ 013 14 t0 1 0 1 2 5 014 15 t0 1 Q 1 2 5 _ 015 16 t0 1 0 1 2 5 ~ 0 1 6 17 t0 1 0 1 2 5 ~ 017 18 t0 1 0 1 2 5 010 19 t0 1 0 1 2 5 019 20 t0 1 0 1 2 5 " 020 21 t010125~ 021 22 t0 1 0 1 2 5 " 022 23 t010125_023 24 t 0 1 0 1 2 5 024 25 t0 1 0 1 2 5 025 26 t0 1 0 1 2 5 _ 026 27 t0 1 0 1 2 5 027 28 t010125~028 29 t0 10125 029 30 t010125~ 030 31 t O l 0125 031 32 t0 1 0 1 2 5 ~ 032 33 t O l 0125 033 34 t0 1 0 1 2 5 034 35 t010125_035 36 t010125~036 37 t0 1 0125 037 38 t0 1 0 1 2 5 03B 39 t010125~039 40 t0 1 0 1 2 5 _ 040 41 t 0 1 0 1 2 5 ~ 0 4 1 42 t010125_042 43 tO l0 1 2 5 ~ 0 4 3 44 t0 1 0 1 2 5 044 45 t0101 2 5 ~ 0 4 5 46 t010125 046 47 t0 1 0 1 2 5 047 48 t010125_048 49 t0 10125~ 049 50 t010125~ 050 51 t0 1 0 1 2 5 051 52 t010125~0S 2 53 tO l0125^053 54 t10125 054 55 t010125~ 055 56 t01Q125~056 57 tO l0 1 2 5 _ 057 58 t010125~058 59 1 0 1 0 1 2 5__059 60 t01G125~~Q60 61 t0 1 0 1 2 5 061 62 tO l0 1 2 5 _ 062 63 t 0 1 0 1 2 5 063 64 t0 1 0 1 2 5 ~ 0 6 4 65 t0 1 0 1 2 5 --065 66 t010125*"066 67 tO l0 1 2 5 ~ 067 68 t0 1 0 1 2 5 " 068 69 t0 1 0 1 2 S ~ 0 6 9 70 t010125~*070 71 t010125~ 071 72 t010125~072 73 t010125~073 74 t0 1 0 1 2 5 074 75 tOl0125~*075 76 t010125~076 77 t01012S~077 78 t010125~07B 79 t010125~ 079 80 t 010125 080 01 t O 10125 001 82 t O l 0125 082 Sasplelist Text MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 1000 ppb FC-M ix 0 0 0 0 2-104-13 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 2 5 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 pp b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 500 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 0 0 -1 3 1 1-0016 lOx EOO-1311-0017 lOx EOO-1311-O018 lOx EOO-1311-0019 lOx EOO -1311-0020 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx EOO -1311-0021 lOx EOO-1311-0022 lOx E 00-1311-O 023 lOx EOO-1311-O024 lOx EOO-1311-0025 . 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH Blank, TN-A-4740, Aliq. 12/04/00 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 10* E00-1311-0026 lO x EOO-1 3 1 1 -0 0 2 7 lOx EOO-1311-0028 lOx EOO -1311-0029 lOx EOO-1311-0030 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 00-1311-0031 lOx E 00-1311-0032 lOx EOO-1311-0033 lOx EOO-1311-0034 lOx EOO-1311-0035 250 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E00-1311-0O 36 lOx 00-13 1 1 -0 0 3 7 lOx E 00-1311-0038 lOx .EOO-1311-0039 lOx E 0 0 -1 3 11-0040 250 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lO x EOO--1311 --0041 lOx E0-1311-0042 . lOx EOO-1311-0043 RT 6.209 7 .1 3 2 6.071 6.325 6 .0 4 8 6.012 6.061 6.231 6 .0 9 6 6 .1 5 9 6 .0 6 3 6.135 6.328 6 .0 2 6 6 .2 3 0 6.073 6 .4 0 0 6.193 6.217 6.046 6 .4 1 0 6.120 6.292 6 .0 8 6 6 .1 4 5 6 .0 6 1 6 .1 0 9 6 .0 6 1 6 .2 0 6 6 ,0 6 2 6.035 6 .2 8 0 5 .9 9 0 6.399 6.362 5 .9 9 0 6 .0 0 0 6.169 6.025 6 .3 8 0 6.108 6.072 6:110 6.157 5 .9 5 2 5 .9 9 0 6.265 6.047 6.121 6 .0 4 0 6.179 6.035 6 .1 4 5 6.084 6.002 6 .0 1 2 5 .9 7 0 6 .1 0 9 6.144 5 .9 6 6 5 .9 7 7 6 .2 0 7 5 .9 6 3 6.204 5 .9 7 5 6 .3 0 3 6.000 6 .0 4 8 6.050 5 .9 5 2 6.133 6.037 6 .0 8 5 5.987 6.157 6.037 6 .0 4 9 6 .2 0 6 Arsa 5373 11729 70045 75600 2522 519 126675 117847 110679 112125 109100 107613 99745 102506 96942 82354 73659 62381 46986 1691 514 1019 503 110013 106158 109910 105112 101461 99250 97592 96662 84852 76758 76238 70176 53632 0 1428 603 118872 112733 110966 114288 109119 86705 1001 0 124529 122964 117237 117726 116042 9244 4 2050 712 113810 119408 252894 186886 185019 92634 1567 0 108803 119501 113016 119626 107200 103229 1198 1922 116049 108684 119125 108263 115063 89852 607 0 116893 106721 122748 Response 5372.524 11728.611 7 0 0 4 5 .3 3 6 7 5 6 0 0 .1 5 6 2522.483 5 1 9 .1 9 5 126675.086 117046.625 118679.031 112125.469 1 0 9 1 0 0 .3 9 8 107613.313 99744.711 102505.703 96941.961 82353.539 73659.094 62380.656 4 6 9 8 5 .8 5 2 1690.943 5 1 4 .2 2 2 1 0 1 9 .1 0 6 503.462 118013.289 106157.750 109909.656 105111.656 101460.953 99250.172 97591.688 9 6 6 6 2 .0 0 0 04852.133 76757.734 76237.547 70176.188 53631.707 1427.568 603.102 118872.305 112733.109 110965.875 114288.406 109118.742 8 6 7 0 5 .1 5 6 1080.741 . 124529.461 122964.258 117236.961 117725.922 116041.797 9 2 4 4 4 .0 8 6 Z 050.362 7 1 2 .3 3 6 113810.109 119407.734 252894.094 186885.938 185019.070 9 2 6 3 3 .82B 1567.286 100802.805 119501.391 113015.695 119626.469 1 0 7 1 9 9 .B44 103228.641 1198.204 1922.064 116048.961 108683.570 119124.578 108263.000 1 1 5 0 6 3 .2 5 8 89851.828 606.992 116893.242 106720.656 122748.484 ppb Flags 14.48 bb 31.62 bb 1B8.03 bb 203.00 bb 6.80 bb 1 .40 bb 341.49 bb 317.69 bb 319.93 bb 302.27 bb 294.11 bb 290.10 bb 260.89 bb 276.33 bb 261.33 bb 222.01 bb 198.57 bb 168.16 bb 126.66 bb 4.56 bb 1.39 bd 2.75 bb 1 .3 6 bb 318.14 bb 286.18 bb 296.29 bb 283.36 bb 273.52 bb 267.56 bb 263.09 bb 260.58 bb 228.74 bb 206.92 bb 205.52 bb 189.18 bb 144.58 bb %Dev od Comment -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 3.85 bb 1.63 bb 320.45 bb 303.90 bb 299.14 bb 308.10 bb 294.16 bb 233.74 bb 2.91 bb 28 22 20 23 18 -7 335.70 bb 331.49 bb 316.05 bb 317.36 bb 312.82 bb 249.21 bb 5.53 bb 1.92 bb 306.81 bb 321.90 bb 681.75 bb 503.80 bb 498.77 bb 249.72 bb 4.23 bb 34 33 26 27 25 -O 23 29 173 102 100 -0 293.31 bb 322.15 bb 304.61 bb 322.49 bb 288.99 bb 278.28 bb 3.23 bb 5.18 bb 312.84 bb 292.99 bb 321.13 bb 291.85 bb 310.19 bb 242.22 bb 1.64 bb 17 29 22 29 16 11 25 17 28 17 24 -3 315.12 bb 287.70 bb 330.90 bb 26 15 32 Page 3 Quantitated and Printed by CMC on 31 Jan 01 Study # E00-1311 3M Environmental Laboratory C M C (13l / I Page 492 of 703 BACK TO MAIN Q u a n t if y C om pound Sum m ary R e p o r t PROS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Deoatur.PRO\SampleDB\t010125 Last modified: Thu Jan 25 10:45:39 2001 Method: C: \MASSLYKX\Decatur. PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 31 07:38:20 2001 Job Code: Printed: Wed Jan 31 07:42:18 2001 Compound 2: I.S.(TH-PFOS)(427) Name 83 t0 1 0 1 2 5 083 84 tO lO 125 084 85 tO lO 125 085 86 t0 1 0 1 2 5 086 87 t0 1 0 1 2 5 087 88 t0 1 0 1 2 5 088 89 t0 1 0 1 2 5 089 90 t0 10125 090 91 t0 1 0 1 2 5 091 92 t0101 2 5 _ 0 9 2 93 t0 1 0125 093 94 t0 1 0 1 2 5 094 95 t0 1 0 1 2 5 095 96 t0 1 0125 096 97 t0 1 0 1 2 5 097 98 t0 1 0 1 2 5 098 99 t0 1 0 1 2 5 ~ 099 100 t0 1 0 1 2 5 100 101 t0 1 0 1 2 5 101 102 t0 1 0 1 2 5 102 103 t0 1 0 1 2 5 103 104 t0 1 0 1 2 5 104 105 t0 1 0 1 2 5 105 106 tO l0125 106 107 t0 1 0 1 2 5 107 108 t0 1 0 1 2 5 108 109 t0 1 0 1 2 5 109 110 t0 1 0 1 2 5 110 111 t O l 0125 111 112 t0 1 0 1 2 5 _ 112 113 t01012S 113 114 t0 1 0 1 2 5 114 115 t0 1 0125 115 116 t0 1 0 1 2 5 ~ 116 117 tO lO 125 117 118 t010125" l l 8 119 t0 1 0 1 2 5 119 120 t0 1 0125 120 121 t0 1 0 1 2 5 121 122 t0 1 0 1 2 5 122 123 t0 1 0 1 2 5 _ 123 124 t0 1 0 1 2 5 ~ 1 2 4 125 t0 1 0 1 2 5 125 126 t010125 126 127 t0 1 0125 127 128 t010125~128 129 t0 1 0 1 2 5 129 130 t010125~130 131 t0 1 0 1 2 5 131 132 t0 1 0 1 2 5 132 . 133 t0 1 0 1 2 5 133 134 t0 1 0 1 2 5 134 135 t010125~135 136 t01012S 136 137 t0 1 0 1 2 5 137 138 t0 1 0125 138 139 t0 1 0 1 2 5 139 140 t0 1 0 1 2 5 140 141 t0 1 0 1 2 5 141 142 t0 1 0 1 2 5 142 143 t010125_143 144 t0 1 0 1 2 5 144 145 t0 1 0 1 2 5 145 146 tO l0 1 2 5 _ 14 6 147 t0 10125_ 147 148 t0 10125 148 149 t0 1 0 1 2 5 149 150 t0 1 0 1 2 5 ISO 151 t0 1 0 1 2 5 151 Samplelist Text 10X E0Q-1311-0 44 10x E 00-1311-0045 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 10k E00-1311-004 6 10x-E 0O -1311-O O 47 lOx EOO-1311-0048 10X EO O -131 1 -0 0 4 9 1 Ox E 0 0 -1 3 1 1 -O 0 5 0 250 ppb FC Mix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx E 00-1311-0051 lOx EO0-1311-0052 lOx EO-1311-0053 lOx EOO-1311-0054 lOx E 00-1311-0055 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 lOx E 00-1311-0056 lOx E 00-1311-0057 lOx EOO-1311-0058 lOx EOO-1311-0059 lOx E 0 0 -1 3 11-0060 25Q p p b FC M ix 0 Q Q 2-104-10 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx E 00-1311-0061 lOx EO0-1311-O062 lOx E 00-1311-0063 lO x E 00-1311-0064 lOx E 00-1311-0065 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx E 00-1311-0066 lOx EO0-1311-OO67 lOx E 0 0 -1 3 11-0068 lOx E00-1311-OO69 lOx E0Q-1311-070 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 lOx EO-1311-0071 lOx E 0 0 -1 3 1 1-0072 lOx E 00-1311-0073 lOx EOO-1311-0074 lOx EOO-1311-0075 2 5 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH Blank, TN-A-4740, Aliq. 12/04/00 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 ,5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 1 750 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 RT 6.013 6.072 5 .9 9 9 5 .9 7 6 6.253 6.070 6.070 6 .0 4 9 6 .0 3 8 5.986 5.975 6.291 6 .0 3 9 5 .9 9 9 6.120 6.271 5 .9 9 8 6.376 5 .9 9 0 6.361 6 .1 6 8 5 .9 8 8 6.071 6.011 6.372 5.952 6,262 6.023 6.170 6.001 6.245 6 .2 0 3 5 ,9 0 6 6,383 6.313 5.985 5 .9 9 9 5 .9 6 6 6.351 6.000 6,000 6.084 5.965 6.267 5 .9 9 9 5.977 6 .2 0 3 6 .0 8 6 5.962 5.975 6.354 6.121 6.085 6.048 6.108 6.192 6.240 6 .0 6 1 6.159 5.979 6.288 5.979 5.953 5.988 Area 105324 116901 83072 O 1668 106186 103150 112295 96921 102624 71867 0 1056 68547 62273 68098 53704 104842 81701 695 2071 123699 114165 101409 109000 98029 81428 1436 0 99050 96206 112143 97979 115602 94374 1721 . 530 102207 207435 209218 222164 131563 80381 1806 1008 159566 128245 173139 176159 141078 77577 0 1240 0 118927 107193 110172 113811 115567 110021 97363 111684 94649 90408 67716 73708 55605 578 1101 Response 105324.102 116900.750 83072.023 1668.148 106186.273 103150.477 112295.242 9 6 9 2 1 .0 1 6 102624.383 71867.242 1055.913 68546.523 62273.418 68097.969 53704.141 1 0 4 8 4 2 .3 2 0 81701.250 6 9 5 .1 4 1 2071.462 123699.445 114164.625 101408.508 109000.344 98029.047 81428.047 1435.502 ' 9 9 0 4 9 .6 8 0 96205.742 112143.391 97978.953 115601.617 94374.211 1720.759 5 3 0 .4 1 6 102207.477 207435.234 2 0 9 2 1 B .3 5 9 222163.859 131562.906 88380.602 1 8 0 6 .3 1 6 1 0 8 8 .4 5 6 159665.938 1 2 8 2 4 4 .8 5 9 173139.297 176158.922 141078.141 77576.617 1240.172 118927.320 107192.914 110171.938 1 1 3 8 1 0 .5 7 0 115567.383 110021.266 97363.398 111684.203 94649.477 90407.883 67715.648 73708.352 55605.203 578.391 1101.073 ' ppb Flags 203.93 bb 315.14 bb 223.94 bb %Dev 14 26 -10 od Comment 4 .5 0 2 8 6 .2 6 2 7 8 .0 7 3 0 2 .7 2 2 6 1 .2 8 2 7 6 .6 5 193.74 bb bb bb bb bb bb bb 15 11 21 5 11 -23 2.85 bb 184.79 bb 167.88 bb 183.58 bb 144.77 bb 282,63 bb 220.25 bb 1.87 bb 5.58 bb 333.47 bb 307.76 bb 273.38 bb 293.84 bb 264.27 bb 219.51 bb 3.87 bb -26 -33 -27 -42 13 -12 33 23 9 18 6 -12 267.02 bb 259.35 bb 302.31 bb 264.13 bb 311.64 bb 254.41 bb 4.64 bb 1.43 bd 275.53 bb 559.20 bb 564.01 bb 598.91 bb 354.67 bb 238.26 bb 4.87 bb 2.93 bb 430,16 bb 345.72 bb 466.75 bb 474.89 bb 380.32 bb 209.13 bb 3.34 bb 320.60 bb 288.97 bb 297.00 bb 306.81 bb 311.54 bb 296.59 bb 262.47 bb 301.08 bb 255.15 bb 243.72 bb 182.55 bb 198.70 bb 149.90 bb 1.56 bb 2.97 bb 7 4 21 6 25 2 10 124 126 140 42 -5 72 38 87 90 52 -16 28 16 19 23 25 19 5 20 2 -3 -27 -21 -40 Page 4 Quantitated and Printed by Q4C on 31 Jan 01 Study # E00-1311 3M Environmental Laboratory C f/ n c /c! Page 493 of 703 BACK TO MAIN Quantify Compound Suionary Report PFOS Adsorb/Desorb E00-1311 Sample List: C:\MaSslynx\soup020199.pro\SainpleDB\s001120a Last modified: Thu Jan 11 07:00:06 2001 Method: C:\Maaslynx\soup020199.pro\MethDB\sOO1120 Last modified: Wed Nov 22 06:41:05 2000 Job Code: Printed: Thu J a n 11 07:03:22 2001 1 C om pound 1 : PFOS (4 9 9 > 9 9 ), fu n e X tt Name study no Samplelist Text 1 s0 0 1 2 0 ,, 0 0 1 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 2 s0 0 1 2 0 _ 0 0 2 EOO-1 3 1 1 9 9 1 .7 8 pp b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 -0 3 - 0 0 MLA 3 s00120_003 4 s00120_004 EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 -0 3 - 0 0 MLA E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 5 s0 0 1 2 0 _ 0 0 5 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 6 sQ 0120_006 EOO-1311 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 , A l i q . 1 1 - 0 3 - 0 0 MLA 7 s 0 0 1 2 0 _ 0 0 7 E 0 0 -1 3 1 1 2 . 4 7 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q - 1 1 -0 3 - 0 0 MLA 8 s0 0 1 2 0 ,, 0 0 8 EOO-1311 4 .9 5 pp b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 -0 3 - 0 0 MLA 9 S 00120_009 EOO-1 3 1 1 9 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q - 1 1 -0 3 - 0 0 MLA 10 sOO120_010 EOO-1311 2 4 .7 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q . 1 1 -0 3 - 0 0 MLA 11 s0012 0_ 0 11 EOO-1311 3 9 .6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q - 1 1 -0 3 - 0 0 MLA 12 s 0 0 1 2 0 _ 0 1 2 EOO-1311 4 9 .5 p p b PFOS 0 0 0 0 2 -8 6 - 0 7 A l i q - 1 1 - 0 3 - 0 0 MLA 13 s0 0 1 2 0 _ 0 1 3 EOO-1311 7 4 .2 6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 -0 3 - 0 0 MLA 14 s 0 0 1 2 0 _ 0 1 4 E 0 0 -1 3 1 1 9 9 .2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 - 0 3 - 0 0 MLA 15 S 00120_015 EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA 16 s 0 0 1 2 0 _ 0 1 6 EOO-1311 4 9 5 .9 p p b PFOS 0 0 0 0 2 -8 6 - 1 2 A l i q . 1 1 - 0 3 - 0 0 MLA 17 s 0 0 1 2 0 _ 0 1 7 EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 - 0 3 - 0 0 MLA 18 s0Q 120_018 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 / 1 6 / 0 0 19 s0Q 120_019 EOO -1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 / 1 6 / 0 0 20 s0 0 1 2 0 _ 0 2 0 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 21 s 0 0 1 2 0 _ 0 2 1 EOO-1311 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 , A l i q . 1 1 -0 3 - 0 0 MLA 22 S 00120_022 EOO-1311 2 . 4 7 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q - 1 1 -0 3 - 0 0 MLA 23 s0 0 1 2 0 _ 0 2 3 E 0 0 -1 3 1 1 4 .9 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 -0 3 - 0 0 MLA 24 s0 0 1 2 0 _ 0 2 4 EOO-1311 9 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 -0 3 - 0 0 MLA 25 s 0 0 1 2 0 _ 0 2 5 E 0 0 -1 3 1 1 2 4 .7 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q . 1 1 -0 3 - 0 0 MLA 26 s 0 0 1 2 0 _ 0 2 6 EOO-1311 3 9 .6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 - 0 3 - 0 0 MLA 27 sOO12 0_027 EOO-1311 4 9 .5 p p b PFOS 0 0 0 0 2 -8 6 - 0 7 A l i q , 1 1 - 0 3 - 0 0 MLA 28 s 0 0 1 2 0 _ 0 2 8 EOO-1311 7 4 .2 6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 -0 3 - 0 0 MLA 29 s0 0 1 2 0 _ 0 2 9 EOO-1311 9 9 .2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 -0 3 - 0 0 MLA 30 s 0 0 1 2 0 _ 0 3 0 E 0 0 -1 3 1 1 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA 31 s 0 0 1 2 0 _ 0 3 1 EOO-1311 4 9 5 .9 p p b PFOS 0 0 0 0 2 -8 6 - 1 2 A l i q . 1 1 - 0 3 - 0 0 MLA 32 s00120_Q 32 EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 - 0 3 - 0 0 MLA 33 s0 0 1 2 0 _ 0 3 3 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 34 s 0 0 1 2 0 _ 0 3 4 EOO-1311 MeOH B la p k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 35 S 0 0 1 2 0 ,,0 3 5 EOO-1311 E 0 0 -1 3 1 1 - 1 0 0 1 Ohr 36 s 0 0 1 2 0 ,, 0 3 6 E 0 0 -1 3 1 1 EOO -131 1 -1 0 0 2 Ohr 37 s 0 0 1 2 0 _ 0 3 7 E 0 0 -1 3 1 1 E 0 0 - 1 3 U - 1 0 0 3 O hr 38 sOO120_03 8 EOO-1311 E 0 0 -1 3 1 1 -1 0 O 4 Ohr 39 S00120_039 EOO-1311 EOO-131 1 -1 0 0 5 Ohr 40 s 0 0 1 2 0 _ 0 4 0 41 s0012 0_041 EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 42 s 0 0 1 2 0 ,, 0 4 2 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 43 S012CL.043 EOO-1311 E 0 0 -1 3 1 1 -1 O 0 6 Ohr 44 s 0 0 1 2 0 _ 0 4 4 EOO-1311 EOO -131 1 -1 0 0 7 Ohr 45 S00120_045 46 s 0 0 1 2 0 _ 0 4 6 EOO-1311 EOO-131 1 -1 0 0 8 Ohr EOO-1311 E 00-1311-10O 9 Ohr 47 s0 0 1 2 0 _ 0 4 7 E 0 0 -1 3 1 1 EO O -131 1 -1 0 1 0 24 h o u r , Omg/L, S i , C -l 48 S 00120_048 EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA 49 s0 0 1 2 0 _ 0 4 9 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 50 8 0 0 1 2 0 ,0 5 0 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 51 s00120,,051 EOO-1311 E0O -1311-1O 11 24 h o u r , Omg/L, S I , C -l S2 s00120_052 EOO-1311 EOO-131 1 -1 0 1 2 24 h o u r , Omg/L, S i, C - l 53 s0 0 1 2 0 _ 0 5 3 EOO-1311 EOO-131 1 -1 0 1 2 24 h o u r , Omg/L, S i , C - l , MS 54 500120^054 EOO-1311 E 0 0 -1 3 1 1 -1 O 1 3 24 h o u r , O .lO m g /L , S I , C - l 55 s0012 0_0 5 5 EOO-1311 E O O -1311-1014 24 h o u r , O .lO m g /L , S I , C - l 56 s 0 0 1 2 0 _ 0 5 6 E 0 0 -1 3 1 1 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA 57 s0 0 1 2 0 _ 0 5 7 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 58 s 0 0 1 2 0 ,, 0 5 8 59 S00120_059 60 s 00120,,060 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 EOO-1311-1015 24 hour, O.lOmg/L, SI, C-l EOO-1311 E O O -1311-1015 24 h o u r , O .lO m g /L , S I , C - l , MS 61 S0012QW061 E 0 0 -1 3 1 1 E 0 0 -1 3 1 1 -1 0 1 6 24 h o u r , 1 . Omg/L, S I , C - l 62 s 0 0 1 2 0 _ 0 62 EOO-1311 EOO-131 1 -1 0 1 7 24 h o u r , 1 . Omg/L, S I , C -l 63 S 00120_063 E 0 0 -1 3 1 1 E O O -1311-1018 24 h o u r , 1 . Omg/L, S I , C -l 64 s0 0 1 2 0 _ 0 6 4 EOO-1311 2 4 7 ,9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA 65 sOO120_065 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 66 s0 0 1 2 0 _ 0 6 6 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 67 s 0 0 1 2 0 ,, 0 6 7 E 0 0 -1 3 1 1 E 0 0 -1 3 1 1 -1 0 1 8 24 h o u r , 1 . Omg/L, S I , C - l MS 68 s 00120_068 EOO-1311 E O 0-1311-1010 24 h o u r, Omg/L, S2, C -l 69 s0 0 1 2 0 _ 0 6 9 E 0 0 -1 3 1 1 E O O -1311-1011 24 h o u r , Omg/L, S 2 , C -l 70 S 00120,,070 EOO-1311 E 0 0 -1 3 1 1 -1 0 1 2 24 h o u r , Omg/L, S 2, C -l 71 S00120_071 E 0 0 -1 3 1 1 E O 0 -1 3 1 1 -1 0 1 2 24 h o u r , Omg/L, S 2 , C - l , MS 72 s 0 0 1 2 0 _ 0 7 2 EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 0 3 - 0 0 MLA 73 s 0 0 1 2 0 _ 0 7 3 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 74 S00120_074 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 75 s0 0 1 2 0 _ 0 7 5 EOO-1311 E O G -1311-1013 24 h o u r , O .lO m g/L , S 2 , C - l 76 s 0 0 1 2 0 ,, 0 7 6 EOO-1311 E O O -1311-1014 24 h o u r , O .lO m g/L , S2 , C - l 77 S 00120,,077 E 0 0 -1 3 1 1 E O O -1311-1015 24 h o u r , O .lO m g/L , S 2, C -l 78 S 00120_078 EOO-1311 E O O -1311-1015 24 h o u r , O .lO m g /L , S 2 , C - l , MS 79 300120^079 E 0 0 -1 3 1 1 EOO -131 1 -1 0 1 6 24 h o u r , 1 . Omg/L, S 2 , C - l 80 s 0 0 1 2 0 _ 0 8 0 EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA 81 s 0 0 1 2 0 _ 0 8 1 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 82 500120^082 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 83 s0 0 1 2 0 _ 0 8 3 EOO-1311 E 0 0 -1 3 1 1 -1 0 1 7 24 h o u r , 1 . Omg/L, S 2, C -l 84 sOO12 0_0 84 EOO-1311 E 0 0 -1 3 1 1 - 1 0 1 8 24 h o u r , 1 . Omg/L, S 2 , C - l 85 s 0 0 1 2 0 ,, 0 8 5 EOO-1311 E 0 0 -1 3 1 1 -1 0 1 8 24 h o u r , 1 . Omg/L, S 2 , C - l , MS 86 s 0 0 1 2 0 ,, 0 8 6 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 87 s 0 0 1 2 0 ,, 0 8 7 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 / 1 6 / 0 0 88 s 0 0 120 _0 88 EOO-1311 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 , A l i q . 1 1 - 0 3 - 0 0 MLA 89 s0 0 1 2 0 _ 0 8 9 E 0 0 -1 3 1 1 2 . 4 7 ppb PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q . 1 1 - 0 3 - 0 0 MLA SOUP 020199: Quantitated and printed by CMC on 01/11/01 Pape 1 Type A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte B lank B lank A nalyte S tandard S tandard. S tandard S tan d ard S tan d ard S tandard S tandard S tandard S tandard S tandard S tan d ard A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte S tan d ard Std Cone 2 .4 7 4.95 9 .9 0 2 4 .7 5 3 9 .6 0 4 9 .5 0 7 4 .2 6 9 9 .2 0 2 4 7 .9 0 4 9 5 .9 0 9 9 1 .7 8 2 4 7 .9 0 2 4 7 .9 0 2 4 7 .9 0 2 4 7 .9 0 2 4 7 .9 0 2 4 7 .9 0 2 .4 7 RT 7 .1 4 1 7 .1 1 7 7 .1 1 8 7 .1 3 0 7 .1 1 8 7 .1 1 9 7 .1 1 7 7 .1 3 1 7 .1 3 1 7 .1 1 8 7 .1 1 8 7 .1 1 9 7 .1 1 7 7 .1 0 7 7 .1 0 5 7 .1 0 6 7 .1 0 7 7 .1 1 9 7 .1 1 8 7 .1 2 9 7 .1 1 7 7 .1 0 6 7 .1 1 8 7 .1 0 6 7 .1 1 7 7 .1 0 7 7 .1 0 6 7 .1 0 6 7 .1 0 6 7 .1 0 6 7 .1 0 6 7 .1 0 7 7 .1 3 0 7 .1 2 8 7 .1 3 1 7.142 7 .1 3 2 7 .1 3 3 7 .1 3 8 7 .1 3 1 7 .1 4 3 7 .1 4 4 7 .1 3 1 7 .1 4 3 7 .1 4 2 7 .1 3 3 7 .1 3 0 7 .1 3 0 7 .1 4 2 7 ,1 4 2 7 .1 4 1 7 .1 4 3 7 .1 3 1 7 .1 4 3 7 .1 4 2 7 .1 3 1 7 .1 3 0 7.118 7 .1 4 1 7 ,1 4 1 7 .1 4 4 7 .1 4 2 7 .1 4 0 7 .1 3 3 7 .1 3 2 7 .1 4 2 7 .1 3 1 7 .1 4 2 7 .1 4 1 7 .1 4 2 7 .1 4 1 7 .1 2 7 7 .1 5 4 7 .1 4 1 7.143 7 .1 3 0 7 .1 3 1 7 .1 2 9 7 .1 3 3 7 .1 1 9 7 .1 4 0 7 .1 2 8 7 .1 3 0 7 .1 3 2 7 .1 3 0 7 .1 2 7 7 .1 4 2 7 .1 2 0 7 .1 1 5 Area 259 30961 30002 213 148 691 1222 1468 1566 2745 3508 3899 5352 6795 12561 19155 28597 144 123 124 604 1095 1354 1454 2683 3390 3889 5282 6720 12653 19151 28429 207 133 110 161 119 2652 2598 12431 119 90 2578 19884 20845 21384 3116 12536 100 81 1084 540 11095 2562 2834 12793 133 149 2667 12420 19190 19557 20389 12905 160 89 25186 3033 1052 438 12229 13639 106 91 1425 1186 1470 12466 6830 13880 81 79 7145 7928 15596 109 81 625 1061 PPb *Dev Flag* Mod Co 0 .0 0 bb bbl bbl 0 .0 0 bb 0 .0 0 bb 0 .0 0 bb 0.00 -100 bb 0.00 -100 bb 0.00 -100 bb 17.72 -28 bb 34.55 -13 bb 43.26 -13 bb 76.26 3 bb 110.02 11 bb 257.10 4 bb 460.85 -7 bb 974.59 -2 bb 0 .0 0 bb 0 .0 0 bb 0 .0 0 bb 0 ,0 0 bb 0 ,0 0 -1 0 0 bbX 0 ,0 0 -100 bbX 0 .0 0 -100 bbX 16.35 -34 bb 31.91 -19 bb 43.05 -13 bb 74.65 1 bb 108.24 259.63 9 bb 5 bb 460.70 -7 bb 955.43 -4 bb 0 .0 0 bb 0 .0 0 0 .0 0 bb bb 0.00 bb 0 .0 0 bb 1 5 .6 8 bb 1 4 .5 0 bb 253.52 2 bb 0 .0 0 bb 0 .0 0 14.07 486.97 bb bb bb 523.02 bb 5 4 4 .0 9 bb 2 5 .8 6 bb 256.40 3 bb 0 .0 0 bb 0.00 bb 0 .0 0 0 .0 0 bb bb 2 1 7 .6 1 bb 13.72 bb 1 9 .6 6 bb 2 6 3 .5 0 6 bb 0 .0 0 0 .0 0 1 6 .0 1 bb bt> bb 253.23 bb 4 6 2 .0 8 475.12 bb bb 505.67 bb 2 6 6 .6 1 0.00 8 bb bb 0 .0 0 bb 719.03 bb 24.03 bb 0 .0 0 bb 0 .0 0 bb 248.01 bb 2 8 7 .2 5 16 bb 0 .0 0 bb 0 .0 0 hb 0 .0 0 bb 0.00 bb 0 .0 0 bb 254.50 bb 11Q.87 bh 294.14 19 bb 0 .0 0 bb 0 .0 0 bb 118.37 bb 137.30 bb 344.75 0.00 bb bb 0.Q hb 0.00 bb 0 .0 0 -100 bbX iV"vC \ / (( / o ( 3M Environmental Laboratory Page 494 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb EOO-13U Sample List: C:\Masslynx\soup020199.pro\SaropleDB\s001120a Last modified: Thru Jan 11 07:00:06 2001 Method: C:\Masslynx\soup020199.pro\MethD8\sO01120 Last modified: Wed Nov 22 06:41:05 2000 Job Code: Printed: Thu Jan 11 07:03:22 2001 i C o m p o u n d 1 : PFOS ( 4 9 9 > 9 9 ) ,, f u n e 1 Name 90 s00120_090 91 s 0 0 1 2 0 _ 0 9 1 92 s 0 0 1 2 0 _ 0 9 2 93 s00120_093 94 sQ 0120_094 95 s0 0 1 2 0 _ 0 9 5 96 s0 0 1 2 0 _ 0 9 6 97 s 0 0 1 2 0 _ 0 9 7 98 S0120_098 99 s00120_099 100 s00120_100 101 s 0 0 120 _10 1 102 s 0 0 1 2 0 _ 1 0 2 s tu d y no S a ra p le lis t T e x t EOO-1 3 1 1 4 .9 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 9 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1 3 1 1 2 4 .7 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q . 1 1 -0 3 - 0 0 MLA E 0 0 -1 3 1 1 3 9 .6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 - 0 3 - 0 0 MLA E 0 0 -1 3 1 1 4 9 .5 p p b PFOS 0 0 0 0 2 -8 6 - 0 7 A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 7 4 .2 6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 9 9 .2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 4 9 5 .9 p p b PFOS 0 0 0 0 2 -8 6 - 1 2 A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 EOO -1 3 1 1 MeQH B la n k , T N -A -4715, A l i q . 1 1 / 1 6 / 0 0 Page 2 Typ S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard A nalyte . A nalyte A nalyte S td Cone 4 .9 5 9 .9 0 2 4 .7 5 39.60 49.50 7 4 .2 6 99.20 2 4 7 .9 0 4 9 5 .9 0 9 9 1 .7 8 RT 7 .1 1 8 7 .1 1 6 7 .1 1 8 7 .1 1 7 7 .1 1 5 7 .1 1 7 7 .1 1 5 7 .1 2 9 7 .1 1 5 7 .1 1 8 7 .1 2 5 7 .1 2 6 7 .1 4 2 A rea 1382 1491 2749 3542 4013 5604 6903 13256 9804 29264 137 87 92 0 .0 0 0 .0 0 17.81 3 5 .3 0 4 5 .8 1 8 2 .0 8 112.60 2 7 8 .4 3 484.08 1 0 8 0 .6 5 0 .0 0 0 .0 0 0 .0 0 %Dev F la g s -100 bbX -100 bbX -28 bb -11 bb -7 bb 11 b b 14 b b 12 b b -2 bb 9 bb bb bb bb M od Co SOUP 020199: quantitated and printed by CMC on 01/11/01 3M Environmental Laboratory CJVXC i / U / o ( Page 495 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Ad3orb/Desorb EOO-1311 Sample List: C :\Masslynx\soup020199.pro\SampleDB\s001120a Last modified: Thu Jan 11 07:00:06 2001 Method: C:\Masslynx\soup020199.pro\MethDB\s001120 Last modified: Wed Nov 22 06:41:05 2000 Job Code: Printed: Thu Jan 11 07:03:22 2001 C om pound 2 : THPFOS (4 2 7 > 8 0 ), fu n e 2 * Name 1 sOO120_001 2 s00120_002 3 s00120_003 4 s00120_004 5 s00120_005 6 s00120_006 7 s00120_007 8 s00120_008 9 s00120_0Q9 10 S0012 0 _ 0 10 11 s0 0 1 2 0 _ 0 1 1 12 s0 0 1 2 0 _ 0 1 2 13 s0012Q _013 14 s0012 0 _ 0 14 15 S012 0_015 16 sO O 120_016 17 s0 0 1 2 0 _ 0 1 7 18 S012 0 _ 0 18 19 s 0 0 1 2 0 _ 0 1 9 20 s 0 0 1 2 0 _ 0 2 0 21 s00120_021 22 S0012 Q_022 23 s0 0 120_023 24 s0 0 1 2 0 _ 0 2 4 25 s 0 0 1 2 0 _ 0 2 5 26 s 0 0 1 2 0 _ 0 2 6 27 s0 0 1 2 0 ,,0 2 7 28 300 1 2 0 ,,0 2 8 29 s0 0 1 2 0 _ 0 2 9 30 S0012 0_030 31 sOO120_031 32 sOO120_032 33 s 0 0 1 2 0 _ 0 3 3 34 s0 0 1 2 0 _ 0 3 4 35 sOO120_0 35 36 s00120_Q 36 37 s0 0 1 2 0 _ 0 3 7 38 sOO120_03 8 39 s0 0 1 2 0 _ 0 3 9 40 s 0 0 1 2 0 J )4 0 41 s00120_041 42 s0 0 1 2 0 _ 0 4 2 43 s0012 0_043 44 s0 0 1 2 0 _ 0 4 4 45 S00120_045 46 s 0 0 1 2 0 _ 0 4 47 s0 0 1 2 0 _ 0 4 7 48 s 0 0 1 2 0 _ 0 4 8 49 S0012 0_049 50 S 00120_050 51 s0012 0_051 52 s 0 0 1 2 0 _ 0 5 2 53 s0012Q _053 54 s0 0 1 2 0 _ 0 5 4 55 s 0 0 1 2 0 _ 0 5 5 56 S012 0_0 56 57 S0012 0_057 58 s 0 0 1 2 0_058 59 s00120_059 60 S0012 0_0 60 61 s 00120,,061 62 s0 0 1 2 0 _ 0 6 2 63 s0 0 1 2 0 _ 0 6 3 64 s 0 0 1 2 0 _ 0 6 4 65 s 0 0 1 2 0_0 65 66 s 0 0 1 2 0 _ 0 6 6 67 s0 0 1 2 0 _ 0 67 68 s0 0 1 2 0 _ 0 6 8 69 s0 0 1 2 0 _ 0 6 9 70 s0 0 1 2 0 _ 0 7 0 71 s0 0 1 2 0 _ 0 7 1 72 s0 0 1 2 0 _ 0 7 2 73 s0 0 120_073 74 S00120_074 75 s00120_075 76 s00120_076 77 s0 0 1 2 0 _ 0 7 7 78 s 0 0 1 2 0 _ 0 7 8 79 s 0 0 1 2 0 _ 0 7 9 80 s 00120_080 81 s 0 0 12 0 _ 0 8 1 82 S012 0_082 83 s0012 0_083 84 S0012 0_084 85 S0120_085 86 S012 0_0 86 87 S0012 0_0 87 88 s00120_088 89 s0 0 1 2 0 _ 0 8 9 study no S a m p l e l i s t T e x t EOO-1311 MeOH B la n k , T N -A -471S , A l i a - 1 1 /1 6 /0 0 E 0 0 -1 3 1 1 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -471S , A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 EOO-1311 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 .4 7 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 4 .9 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 9 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 2 4 .7 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q , 1 1 -0 3 - 0 0 MLA EOO-1311 3 9 .6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 4 9 .5 pp b PFOS 0 0 0 0 2 -8 6 - 0 7 A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 7 4 .2 6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 9 9 .2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 4 9 5 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 2 A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 / 1 6 / 0 0 EOO-1311 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 2 . 4 7 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 4 .9 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 9 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 4 .7 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q . 1 1 -0 3 - 0 0 MLA E 0 0 -1 3 1 1 3 9 .6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 4 9 .5 p p b PFOS 0 0 0 0 2 -8 6 - 0 7 A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 7 4 .2 6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 9 9 .2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA E 0 0 -1 3 1 1 4 9 5 .9 p p b PFOS 0 0 0 0 2 -8 6 - 1 2 A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 -0 3 - 0 0 MLA E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 EOO-1311 EOO-131 1 -1 0 0 1 Ohr EOO-1311 EOO-1311 -1 0 0 2 Ohr EOO-1311 E 0 0 -1 3 1 1 -1 0 0 3 Ohr E00-1311 EOO-1311-1004 Ohr EOO-1311 EQ 0-131 1 -1 0 0 5 Ohr E 0 0 -1 3 1 1 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 00-1311 EOO-1311-1 0 0 6 Ohr E00-1311 E 00-1311-1007 Ohr EOO-1311 E O 0-1311-1008 Ohr E 00-1311 EOO-1311-1 0 0 9 Ohr E 00-1311 E 0 0 -1 3 1 1 -1 0 1 0 24 h o u r, Omg/L, S I, C -l EOO-1311 2 4 7 .9 pp b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 E 00-1 3 1 1 -1 0 1 1 24 h o u r, Omg/L, S I, C -l EOO-1311 E 0 0 -1 3 1 1 -1 0 1 2 24 h o u r, Omg/L, S I, C -l E 0 0 -1 3 1 1 EOO-131 1 -1 0 1 2 24 h o u r , Omg/L, S I , C - l , MS EOO-1311 E 0 0 -1 3 1 1 -1 0 1 3 24 h o u r, O .lO m g/L, S I, C -l EOO-1311 E 0 0 -1 3 11 -1 0 1 4 24 h o u r, O .lO m g/L, S I, C -l EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 E 0 0 -1 3 1 1 -1 0 1 5 24 h o u r , O .lO m g/L , S I , C - l EOO-1311 E Q 0 -1 3 1 1 -1 0 1 5 24 h o u r , O .lO m g /L , S I , C - l , MS E 00-1311 EQ O -1311-1016 24 h o u r , 1 . Omg/L, S I, C -l EOO-1311 E 0 0 -1 3 1 1 -1 0 1 7 24 h o u r , 1 . Omg/L, S I , C -l EOO-1311 E00-1 3 1 1 -1 0 1 8 24 h o u r, 1 . Omg/L, S I, C -l EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 0 0 -1 3 1 1 E O O -1311-1018 24 h o u r , 1 . Omg/L, S I , C - l MS EOO-1311 EO O -1311-1010 24 h o u r, Omg/L, S2, C -l EOO-1311 EG O -1311-1011 24 h o u r, Omg/L, S2, C -l E00-1311 E 0 0 -1 311-1012 24 h o u r, Omg/L, S2, C -l EOO-1311 EOO -131 1 -1 0 1 2 24 h o u r , Grog/L, S 2, C - l , MS EOO-1311 2 4 7 .9 pp b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 00-1311 EO O -1311-1013 24 h o u r , O .lO m g/L, S2, C -l EOO-1311 E 0 0 -1 3 1 1 -1 0 1 4 24 h o u r, O .lO m g/L, S2, C -l EOO-1311 E(1 0 -1 3 1 1 -1 0 1 5 24 h o u r , O .lO m g /L , S 2, C - l E 0 0 -1 3 1 1 E 00-1 3 1 1 - 1 0 1 5 24 h o u r , O .lO m g/L , S 2 , C - l , MS E 00-1311 E 0 0 -1 3 1 1 -1 0 1 6 24 h o u r , 1 . Omg/L, S 2, C - l EOO-1311 2 4 7 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 0 0 -1 3 1 1 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 E 00-1311 E 00-1 3 1 1 -1 0 1 7 24 h o u r , 1 . Omg/L, S 2, C -l E 0 0 -1 3 1 1 E 0 0 -1 3~1 1 -1 0 1 8 2~4 h o u r , 1 . Omg/L, S 2 , C -l EOO-1311 E O O -1311-1018 24 h o u r , 1 . Omg/L, S 2 , C - l , MS EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 , Aliq. 1 1 -0 3 - 0 0 MLA EOO-1311 2 . 4 7 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 , Aliq. 1 1 -0 3 - 0 0 MLA SOUP 020199: quantitated and printed by CMC on 01/11/01 3M Environmental Laboratory Type A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte Analyte A nalyte A nalyte Analyte Analyte Analyte Analyte Analyte A nalyte A nalyte Analyte A nalyte Blank Blank A nalyte S tandard S tandard S tandard S tandard S tandard S tan d ard S tandard S tandard S tandard S tandard S tandard A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte QC A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte A nalyte S tandard RT 6.938 6 .9 3 8 6.927 6 .9 2 6 6.952 6 .9 4 0 6 .9 3 8 6.927 6.939 6 .9 2 6 6 .9 2 6 6.926 6 .9 2 6 6.927 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 6 .9 2 5 6.927 6 .9 3 9 6.926 6 .9 3 8 6 .9 2 8 6 .9 2 7 6 .9 2 6 6.927 6.926 6 .9 2 6 6 .9 2 6 .246.10 6 .9 5 1 6 .9 5 1 6 .9 5 3 6.953 6.947 6 .9 5 1 2 4 6 .1 0 6.952 6 .9 5 1 6.962 6.953 6 .9 5 1 6 .9 5 1 2 4 6 .1 0 6 .9 4 8 6 .9 6 4 6.951 6 ,9 5 1 6.962 6.939 2 4 6 .1 0 6 .9 6 1 6.962 6 .9 6 5 6 .9 6 3 6.962 6.954 2 4 6 .1 0 6 .9 5 1 6.962 6 .9 4 9 6 .9 5 1 6 .9 6 2 6 .9 4 7 2 4 6 .1 0 6 .9 5 1 6.950 6.952 6.950 6.954 6 .9 3 9 6 .9 5 0 6.952 6 .9 3 8 .246 .1 0 6 .9 4 1 6 .9 3 5 Area 2930 2763 p p b %Dev Fie 257.53 2 4 2 .8 1 5 bb -1 bb 2812 3382 3449 3103 3256 2928 2648 2677 2711 2632 2507 2412 2 4 7 .1 7 297.23 303.13 2 7 2 .6 9 2 8 6 .2 0 257.37 2 3 2 .7 1 235.32 238.30 231.34 2 2 0 .3 1 211.97 0 bb 21 bb 23 bb 11 bb 16 bb 5 bb -5 bb -4 bb -3 bb -6 bb -10 bb -14 bb 2702 3155 3245 2865 3119 2791 2618 2621 2590 2611 2488 2506 2 3 7 .4 5 2 7 7 .2 8 285.19 251.77 2 7 4 .0 8 2 4 5 .2 5 2 3 0 .1 0 2 3 0 .3 4 2 2 7 .6 6 2 2 9 .4 3 218.68 220.25 -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 2 1 8 .7 6 24 bb 24 bb 25 bb 24 bb 23 b b -11 bb 3489 3477 3270 3377 3432 2527 306.60 305.55 2 8 7 .4 1 296.83 301.61 222.08 23 bb 22 bb 15 bb 19 bb 21 bb -10 bb 3519 3536 3401 3448 3526 2535 309.27 310.79 298.93 303.03 3 0 9 .9 1 2 2 2 .7 8 24 bb 24 bb 20 b b 21 bb 24 bb -9 bb 3578 3434 3445 3409 3431 2461 3 1 4 .4 4 301.76 302.81 299.65 301.57 216.30 26 bb 21 bb 21 bb 20 bb 21 bb -12 bb 3345 3773 7994 4614 4514 3079 294.00 331.60 702.58 4 0 5 .4 8 396.76 270.57 18 bb 33 bb 181 bb 62 bb 59 bb 10 bb 4S90 4334 4403 4276 4318 2941 403.42 380.88 386.94 375.79 379.46 2 5 8 .5 1 61 bb 52 bb 55 bb 50 b b 52 bb 5 bb 4117 4161 3976 361.83 365.66 3 4 9 .4 1 45 bb 46 bb 40 bb 2849 3166 250.36 278.28 2 bb 13 bb Civic I/(i/o( Page 496 of 703 BACK TO MAIN Q u a n tify C om pound S uranary R e p o rt PFOS A d s o r b / D es o r b E O O -1311 S a m p le L i s t : C :\M a s s ly n x \s o u p 0 2 0 1 9 9 .p ro \S a m p le D B \3 0 0 1 1 2 0 a L a s t m o d if ie d : T hu J a n 11 0 7 :0 0 :0 6 2001 M e th o d : C :\M a s s ly n x \s o u p 0 2 0 1 9 9 .p ro \M e th D B \s 0 0 1 1 2 0 L a s t m o d ifie d : wed N ov 22 0 6 :4 1 :0 5 2000 Job Code: P rin te d : Thu Jan 11 0 7 :0 3 :2 2 2001 t C om pound 2 : THPFOS { 4 2 7 > 8 0 ) , fu n e 2 tt Name 90 s0012Q _090 91 s0 0 1 2 0 _ 0 9 1 92 s0 0 1 2 0 _ 0 9 2 93 s 0 0 1 2 0 _ 0 9 3 94 s0 0 1 2 0 _ 0 9 4 95 s 0 0 1 2 0 _ 0 9 5 96 s0 0 1 2 0 _ 0 9 6 97 s 0 0 1 2 0 _ 0 9 7 98 s0012 0_098 99 S 00120_099 100 s0012 0_100 101 s00120_101 102 s00120_102 s tu d y no S a m p le lis t T e x t EOO-1 3 1 1 4 .9 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1 3 1 1 9 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 4 .7 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , Aliq. 1 1 -0 3 - 0 0 MLA EOO-1311 3 9 .6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 4 9 .5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 7 A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 7 4 .2 6 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 9 9 .2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 2 4 7 ,9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 4 9 5 .9 p p b PFOS 0 0 0 0 2 -8 6 - 1 2 A l i q . 1 1 - 0 3 - 0 0 MLA EOO-1311 9 9 1 .7 8 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 -0 3 - 0 0 MLA EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 /1 6 /0 0 EOO-1311 MeOH B la n k , T N -A -4 7 1 5 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B la n k , T N -A -4715, A l i q . 1 1 /1 6 /0 0 Page 4 Type S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard A nalyte A nalyte A nalyte S td Cone 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 2 4 6 .1 0 RT 6 .9 3 8 6.937 6 .9 3 8 6.937 6 ,9 3 6 6 .9 3 8 6 .9 3 6 6 .9 3 7 6 .9 3 7 6.925 A rea 3315 2979 3231 2840 2675 2716 2669 2377 2568 2460 PPb 291.36 261.80 283.98 2 4 9 .6 0 2 3 5 .1 1 238.73 234.57 2 0 8 .9 3 225.66 216.17 *D ev F la g s 18 bb 6 bb 15 bb 1 bb -4 bb -3 bb -5 bb -15 bb -8 bb -12 bb M od Co SOUP 0 2 0 1 9 9 : q u a n t i t a t e d a n d p r i n t e d b y CMC o n 0 1 / 1 1 / 0 1 3M Environmental Laboratory cM c i/a/oi Page 497 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Deoatur.PRO\SamplaDB\t010122 Last modified: Mon Jan 22 15:03:42 2001 Method: C: \MASSLYNX\Decatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: * Wed Jan 24 07:06:18 2001 Confound 1: PFOS{499) # Name 1 t0l0122J> 01 2 t010122~002 3 t01Q122~003 4 t010122~004 5 t010122~005 6 t010122~006 1 t010122~007 8 t01Q122~008 9 t010122~009 10 t010122~010 11 t 0 1 0 1 2 2 ~ 0 11 12 t0 1 0 1 2 2 ~ 0 1 2 13 t0 1 0 1 2 2 ~ 0 1 3 14 t0 1 0 1 2 2 ~ 0 1 4 15 t 0 1 0 1 2 2 ~ 0 l5 16 t010122~016 17 t010122~017 10 t0 10122~ 018 19 t010122~019 20 t010122"020 21 t0 1 0 1 2 2 ~ 0 2 1 22 t010122~ 022 23 t010122~023 24 t0 1 0 1 2 2 ~ 0 2 4 25 t010122~025 26 t010122~026 27 t010122~027 28 t010122~029 29 t010122~029 30 t010122~030 31 t010122~031 32 t010122~032 33 t O 10122^033 34 t0 1 0 1 2 2 ~ 0 3 4 35 t010122"035 36 t010122 036 37 t010122~037 38 t010122~038 39 t010122~039 40 t010122~0i*0 41 t010122~041 42 t010122~042 43 t010122~043 44 t0 1 0 1 2 2 '0 4 4 45 t010122~045 46 t010122~046 47 t010122" 047 40 t010122~048 49 t010122~049 50 t010122~050 51 t010122~"051 52 tO l0122^052 53 t010122~053 54 t o 1 0 122*~054 55 t0 1 0 1 2 2 '0 5 5 56 t0 1 0 1 2 2 J)S 6 57 t010122~057 58 t010122~058 59 t0 1 0 1 2 2 J> 5 9 60 t010122^060 61 t010122~ 061 62 t0 1 0 1 2 2 '0 6 2 63 t0 1 0 1 2 2 "0 6 3 64 t 0 1 0 1 2 2 ""064 65 t010122~ 065 66 tO 10122^066 67 t010122~ 067 68 tO 10122^068 69 t010122~ 069 70 t010122^070 71 t010122~ 071 72 t010122~072 73 t010122'o73 74 t0 1 0 1 2 2 '0 7 4 75 t010122~075 76 t010122" 076 77 t010122~077 78 tO 10122~078 79 t010122" 079 80 t010122~080 81 tO 10122^001 82 t O 1 0122^ 082 Samplelist Text MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 1 0 0 0 p p b PFOS 0 0 0 0 2 -1 0 4 - 1 3 1000 pp b PFOS 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q , 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 ppb FC M ix 0 0 0 0 2 -1 0 4 -0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 pp b FC M ix 0 0 0 0 2 -1 0 4 - 0 6 50 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 5 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 1 75 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 2 1000 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 0 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 1 2 .5 p p b FC M ix 0 0 0 0 2 -1 0 4 -0 2 5 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 3 10 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 4 25 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 5 40 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 6 50 pp b FC M ix 0 0 0 0 2 -1 0 4 - 0 7 75 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 8 100 p p b FC M ix 0 0 0 0 2 -1 0 4 - 0 9 25 0 p p b FC M ix 0 0 0 0 2 - 1 0 4 - 1 0 500 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 1 7 5 0 p p b FC M ix Q 0 Q 0 2 -IQ 4 -1 2 1000 pp b FC M ix 0 0 0 0 2 -1 0 4 - 1 3 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 E 0 0 - 1 3 1 1 - 2 0 0 1 , Oug PFOS, c o n t r o l , 1 / 2 2 / 0 1 . . EOO-131 1 -2 0 0 2 , Oug PFOS, c o n t r o l , 1 / 2 2 / 0 1 .. E O O -1 3 1 1 -2 0 0 3 , Oug PFOS, c o n t r o l , 1 / 2 2 / 0 1 . . E00 -1 3 1 1 -2 0 0 3 m s, Oug PFOS, c o n t r o l , 1 / 2 2 / . . E 0 0 -1 3 1 1 -2 0 0 4 , 0 . 75ug PFOS, c o n t r o l , 1 /2 2 .. 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 EOO-131 1 -2 0 0 5 , 0 . 75ug PFOS, c o n t r o l , 1 / 2 2 .. E 0 0 -1 3 1 1 -2 0 0 6 , 0 . 75ug PFOS, c o n t r o l , 1 /2 2 .. EOO-1311-2 0 0 6 m s, 0 .7 5 u g PFOS, c o n t r o l , 1 / . . EO O -1311-2007, 7 . 5ug PFOS, c o n t r o l , 1 / 2 2 / .. EO O -1311-2008, 7 . 5ug PFOS, c o n t r o l , 1 / 2 2 / .. 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 7 0 0 E O O -1311-2009, 7 . 5ug PFOS, c o n t r o l , 1 / 2 2 / .. EOO-131 l-2 0 0 9 n i3 , 7 .5 u g PFOS, c o n t r o l , 1 / 2 . . E O O -1 3 1 1 -2 0 1 0 , Oug PFOS, C l a y , 1 / 2 2 / 0 1 CMC E O O -1 3 1 1 -2 0 1 1 , Oug PFOS, C l a y , 1 / 2 2 / 0 1 CMC EO O -1311 - 2 0 1 2 , Oug PFOS, C l a y , 1 / 2 2 / 0 1 CMC 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 EOO -131 1 - 2 0 12m s, Oug PFOS, C l a y , 1 / 2 2 / 0 1 . . E 0 0 -1 3 1 1 -2 0 1 3 , 0 . 75ug PFOS, C la y ,1 /2 2 /0 1 .. EOO-131 1 -2 0 1 4 , 0 . 75ug PFOS, C la y ,1 / 2 2 / 0 1 .. EO O -1311-2015, 0 . 75ug PFOS, C la y ,1 /2 2 /0 1 .. EOO-131l-2 0 1 5 m s, 0 .7 5 u g PFOS, C la y ,1 / 2 2 / . . 250 p p b FC M ix 0 0 0 0 2 -1 0 4 -1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 /0 4 /0 0 EOO-1311 -2 0 1 6 , 7 .5 u g PFOS, C la y ,1 /2 2 /0 1 . . EQ0-131 1 -2 0 1 7 , 7 .5 u g PFOS, C la y ,1 /2 2 /0 1 . . EOO-1311 -2 0 1 8 , 7 .5 u g PFOS, C la y ,1 /2 2 /0 1 . . E O O -13ll-2018m a, 7 .5 u g PFOS, C la y ,1 /2 2 /0 .. E O O -1 3 1 1 -2 0 1 9 , Oug PFOS, S e d im e n t, 1 / 2 2 / 0 . 250 p p b FC M ix 0 0 0 0 2 -1 0 4 - 1 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 MeOH B la n k , T N -A -4 7 4 0 , A l i q . 1 2 / 0 4 / 0 0 E 0 0 - 1 3 1 1 - 2 0 2 0 , Oug PFOS, S e d i m e n t ,1 / 2 2 / 0 . . EOO -131 1 -2 0 2 1 , Oug PFOS, S e d i m e n t ,1 / 2 2 / 0 . . E 00-1 3 1 1 -2 0 2 1 m s, Oug PFOS, S e d im e n t,1 / 2 2 .. RT 6.471 6.518 6.494 6.302 6.27B 6.304 6.278 6.351 6.529 6 .6 0 3 6.467 6.565 6 .4 8 3 6.423 6.531 6.337 6.277 6.457 6 .5 5 6 6.423 6.507 6.217 6.266 6.242 6.241 6.212 6.292 6 .2 7 8 6.253 6.242 6.228 6.195 6.269 6.252 6.242 6 .2 8 9 6.192 6.278 6.240 6.241 6.241 6.204 6.205 6.336 6.472 6.412 6.459 6.542 6.325 6.338 6 .3 4 8 6.264 6 .3 8 6 6.433 6.241 6.508 6.446 6 .3 8 6 6.314 6.298 6 .4 1 0 6 .3 5 0 6 .2 0 6 6 .2 4 2 6.253 6.254 6.231 6 .3 3 6 6.579 6.423 6.312 6.361 6 .2 8 9 6.334 6 .4 0 3 6.251 6.576 6 .4 8 3 6 .5 6 8 6.409 6 .3 8 8 Area 0 1418177 5443742 4872953 666738 1B0374 163484 117782 135145 161293 196372 266693 338161 431890 513753 594508 1275366 2007741 2763803 3645079 131577 129156 112678 107071 127936 144180 174504 278880 388285 446576 570014 744606 1386363 2300090 3091049 3667595 119206 124131 117983 118400 120731 120322 1168B35 813735 1424150 135069 137576 813677 893031 1715684 5378311 4162893 1277079 136322 139432 4515612 4776306 159367 136483 132405 1319212 136755 138103 1229867 708722 80B319 814123 1843512 1423348 144495 139217 4604546 5217586 3567801 5013902 167395 1438406 144134 149923 173961 168416 1139314 Response 0 .0 0 0 19342.259 17296.491 0.000 0.000 0 .0 0 0 2 7 7 .5 0 6 3 4 2 .9 7 3 4 2 5 .4 2 9 539.114 820.039 1459.014 1810.543 1730.299 1936.961 4921.492 9491.826 13604.815 17205.562 0 .0 0 0 0 .0 0 0 0 .0 0 0 252.335 3 0 3 .0 8 1 3 4 4 .0 2 9 415.631 692.659 9 4 4 .4 5 5 1120.035 1520.355 2028.656 4 6 2 0 .5 6 8 8907.358 1 3 9 7 0 .4 1 6 18298.763 0 .0 0 0 0 .0 0 0 0 .0 0 0 2 6 9 .9 8 2 2 8 3 .1 7 0 275.218 3577.816 1879.330 4176.378 0 .0 0 0 0 .0 0 0 1 8 9 5 .4 9 6 1 8 7 0 .22B 5964.233 14195.194 10426.933 4483.933 0 .0 0 0 0.000 11893.660 13417.657 358.722 291.362 2 7 8 .8 9 8 4478.412 0.000 0 .0 0 0 3235.341 1324.360 1521.178 1514.413 4 9 8 6 .9 3 6 4035.575 0 .0 0 0 0 .0 0 0 11133.142 12089.190 8221.149 15883.856 3 4 8 .5 8 7 4448.547 0 .0 0 0 0 .0 0 0 3 6 6 .4 5 8 374.703 3540.157 ppb Flags Dev od Comment 0.00 bb 1092.32 bb 977.26 bb 0.00 bb 0 .0 0 bb 0.00 bb 2 .8 5 bb 6 .6 6 bb 11.46 bb 18.07 bb 34.41 bb 71.53 bb 92.39 bb 87.27 bb 99.26 bh 271.87 bb 534.29 bb 768.53 bb 972.14 bb 0.00 bb 0 .0 0 bb 0 .0 0 bb 1.39 bb 4 .3 4 bbX 6 .7 2 bbX 1 0 .8 9 bbX 2 7 .0 0 MM 4 1 .6 4 MM 5 1 -8 4 MM 7 5 .0 9 MM 1 0 4 .5 8 MM 254.51 bb 500.86 bb 789.27 bb 1033.68 bb 0.00 bb 0.00 bb 0.00 bb 2.42 bb 3.18 bb 2.72 bb 194.28 bb 95.92 bb 228.87 bb 0.00 bb 0.00 bb 96.85 bb 95.39 bb 331-94 bb 802.01 bb 587.71 bb 246-63 bb 0.00 bb 0.00 bb 671.30 bb 757.91 bb 7.58 bb 3.6 6 bb 2.93 bb 246.31 bb 0.00 bb 0.00 bb 174.47 bb 63,71 bb 75.13 bb 74.74 bb 275.64 bb 220.74 bb 0 .0 0 bb 0.00 bb 627.98 bb 682.43 bb 461.56 bb 897.56 bb 6.99 bb 244.58 bb 0.00 bb 0.00 bb 8.03 bb 8 .51 bb 192.10 bb 9 -2 167 129 81 38 79 85 16 -1 9 7 2 -3 74 34 9 8 4 4 0 5 2 0 5 3 -8 -l -1 -12 -2 b b b b b Page 1 Quantitated and Printed by CMC on 24 Jan 01 Study # E 0 0 -1 3 1 1 3M Environmental Laboratory r hn ( ( /z>i Page 498 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C: \MASSLYNX\Decatur.PRO\SampleDB\t010122 Last modified: Mon Jan 22 15:03:42 2001 Method: C: \MASSLYNX\Decatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Wed Jan 24 07:06:18 2001 Compound 1 : PFOS(49 9) # Name 03 t010122 083 84 t010122*'084 85 t010122* 085 06 t010122* 086 07 t0l0122~*087 88 t010122~*008 89 t010122~ 089 90 t010122~ 090 91 t010122~*091 92 t010122~*092 93 tOl0122* 093 94 t0l0122~ 094 95 t010122**095 96 t010122* 096 97 t010122*" 0 9 7 98 t010122~ 098 99 t010122~'099 100 tOl0122*' 1 0 0 101 t010122"'lOl 102 t010122**102 103 t010122~*103 104 t010122~*104 105 t010122"*105 106 t0l0122~*106 107 t010122**107 108 t010122**108 109 t010122**109 110 t010122**110 111 t010122*'ill 112 t010122**112 113 tOlO122* 113 114 t010122~"114 115 t010122**115 Samplelist Text B00-1311-2022, 0.75ug PFOS, Sediment,1/2.. E00-1311-2023, 0.75ug PFOS, Sediment,1/2. . 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 B00-1311-2024, 0.75ug PFOS, Sediment,1/2.. E00-1311-2024ms, 0.75ug PFOS , Sediment,1.. E00-1311-2025, 7.5ug PFOS, Sediment,1/22.. EOO-1311-2026, 7.5ug PFOS, Sediment,1/22.. EOO-1311-2027, 7.5ug PFOS, Sediment,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 EOO-13ll-2027ms, 7.5ug PFOS, Sediment,1/.. 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 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 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 6.486 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 417B0SO 4349355 1303467 148641 152985 5663187 1365566 149480 155378 144563 164749 166221 181623 212615 292832 353915 439196 583060 690084 1303673 2036643 3110621 3415199 185076 151445 Response 2118.433 1772.460 3983.564 0.000 0.000 1752.210 4558.469 10086.002 10795.713 11084.279 4507.499 0.000 0.000 16464.124 3642.340 0.000 0.000 0.000 346.252 399.780 436.052 499.891 689.623 841.984 1162.333 1595.061 1977.399 4519.670 8986.881 12414.655 17167.793 0.000 0.000 ' ppb Flags 109.78 bb 89.72 bb 217.73 bb 0.00 bb 0.00 bb 88.54 bb 250.93 bb 568.24 bb 608.75 MM 625.20 bb 252.60 bb 0.00 bb 0.00 bb 930.32 bb 198,01 bb 0.00 bb 0,00 bb 0,00 bb 6.85 bb 9.97 bbX 12.08 bbX 15.79 bbX 26.02 bb 35.60 MM 54.30 bb 79.42 bb 101.61 bb 240.69 bb 505.41 bb 700.94 MM 970.01 bb 0.00 bb 0.00 bb %Dev od Comment -13 b 1 299 142 58 7 -11 b 9 6 2 -1 1 -1 b -3 Page 2 Quantitated and Printed by CMC on 24 Jan 01 Study # E0 0-1311 3M Environmental Laboratory Ctnc i/j-y/) Page 499 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LA052) Sample List: C: \MASSLYHX\Decatur.PR0\SaapleDB\t010122 Last modified:. Mon Jan 22 15:03:42 2001 Method: C:\MASSLYNX\Decatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Wed Jan 24 07:06:18 2001 Compound 2: X.S.(TH-PFOS)<42?> f Name 1 t0l0122 _001 2 t010122""002 3 t010122""003 4 1010122'"004 5 t010122 "005 6 t010122 006 7 t010122`"007 0 t010122" 008 9 t010122*"009 10 t010122""OlO 11 t010122'" on 12 t010122 0 1 2 13 tOl0122 013 14 t010122_ 014 15 t010122*"015 16 tOl0122 016 17 tO10122"j)17 18 1010122 018 19 to 1 0 1 2 2 ""019 20 toio1 2 2 ""020 21 t010122`"021 22 t010122*"022 23 t010122 023 24 t010122""024 25 t010122""025 26 t01Q122~ 026 21 t010122" 027 28 1010122' 028 29 t010122`"029 30 t010122`"030 31 t010122 '031 32 to 1 0 1 2 2 ' 032 33 t010122~ 033 34 t010122*"034 35 t010122~'035 36 t010122 036 37 t010122~ 037 38 t010122~ 03B 39 t010122""039 40 t010122 " 0 40 41 t010122 041 42 toio 1 2 2 ' 042 43 t010122` 043 44 t010122_'044 45 t010122~'045 46 t010122~ 04 6 47 t010122~"047 48 t010122" 048 49 to 1 0 1 2 2 "'049 50 1010122""050 51 t010122~ 051 52 t010122 052 53 t010122~.053 54 tO1012Z~'054 55 1010122" 055 56 t010122""056 57 to 1 0 1 2 2 '~057 58 t010122*"058 59 1010122 ~059 60 toio 1 2 2 ""060 61 t010122""061 62 t010122 062 63 t010122* 063 64 t010122 "064 65 t010122' 065 66 to 1 0 1 2 2 ""O6 6 67 t010122" 067 68 to 1 0 1 2 2 ""068 69 tO10122 069 70 t010122 070 71 toio1 2 2 ' 071 72 t010122" 072 73 t010122* 073 74 tOIOI2 2 '"0?4 75 t010122~"075 76 t010122'*076 77 to 1 0 1 2 2 "*077 78 t010122~ 078 79 1010122" 079 80 tOl0 1 2 2 '"080 81 to 1 0 1 2 2 ""081 82 t010122~ 082 Samplelist Text MeOH Blank, TN-A-4740, Aliq 12/04/00 MeOH Blank, TN-A-4740, Aliq. 12/04/00 1000 ppb PFOS 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 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 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 00002-104-00 100 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 EOO-1311-2001, Oug PFOS, control,1/22/01.. EO0-1311-2002, Oug PFOS, control,1/22/01.. EOO-1311-2003, Oug PFOS, control,1/22/01.. E00-1311-2003m3, Oug PFOS, control,1/22/.. E00-1311-2004, 0.75ug PFOS, control,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 E00-1311-2005, 0.75ug PFOS, control,1/22.. 00-1311-2006, 0.75ug PFOS, control,1/22.. EOO-1311-2006ra3, 0,75ug PFOS , control,!/.. E00-1311-2007, 7.Sug PFOS, control,1/22/.. EOO-1311-2008, 7.5ug PFOS, control,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 EOO-- 1311-2009, 7.Sug PFOS, control,1/22/.. E00-1311-2009m3, 7.5ug PFOS, control,1/2.. E00-1311-2010, Oug PFOS, Clay,1/22/01 CMC EOO-1311-2011, Oug PFOS, Clay,1/22/01 CMC EOO-1311-2012, Oug PFOS, Clay,1/22/01 CMC 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 EOO-1311-2012ms, Oug PFOS, Clay,1/22/01 .. EOO-1311-2013, 0.75ug PFOS, Clay,1/22/01.. 00-1311-2014, 0.75ug PFOS, Clay,1/22/01.. EOO-1311-2015, 0.75ug PFOS, Clay,1/22/01.. EOO-131l-2015ms, 0.75ug 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 00-1311-2016, 7.Sug PFOS, Clay,1/22/01 .. 00-1311-2017, 7.5ug PFOS, Clay,1/22/01 .. 00-1311-2018, 7.5ug PFOS, Clay,1/22/01 .. 00-1311-2018ms, 7.5ug PFOS, Clay,1/22/0.. 00-1311-2019, Oug PFOS, Sediment,1/22/0.. 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 EOO-1311-2020, Oug PFOS, Sediment,1/22/0.. EOO-1311-2021, Oug PFOS, Sediment,1/22/0.. E00-1311-2021ms, Oug PFOS, Sediment,1/22.. RT 6.386 6.361 6.386 6.158 6.170 6.208 6.101 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 6.105 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 Area 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 1544 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 80036 623 547 110677 112367 80456 Response 3928.481 70360.727 70432.680 2936.239 1130.456 1051.464 106107.367 90510.055 94782.305 91062.211 81304.906 57943.418 59374.168 74228.898 76742.336 64785.551 52880.781 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 1544.154 1224.169 109637.445 106589.008 109296.547 81672.383 108247.570 05250.313 810.623 743.885 107317.102 119374.625 71915.523 94720.633 99011.055 71203.055 529.970 94916.367 08992.914 111065.523 117107.781 118685.422 73642.852 612.897 95033.773 133785.656 132844.172 13439S.797 92417.078 B8175.039 103397.250 107897.750 108494.609 78915.063 120052.766 80835.727 623.047 547.122 118677.195 112366.523 80456.438 ppb Flags Dev 11.28 bb 202.11 bb 202.32 bb 8.43 bb 3.25 bb 3.02 bb 304.80 bb 282.97 bb 272.27 bb 261.58 bb 233.55 bb 166.44 bb 170.55 bb 213.23 bb 220.45 bb 186.10 bb 151.90 bb 145.89 bb 152.14 bb 1.99 bb -19 -19 22 13 9 5 -7 -33 -32 -IS -12 -26 -39 -42 -39 2.17 bb 304.72 bb 303.14 bb 300.97 bb 301.51 bb 289.15 bb 295.24 bb 206.33 bb 269.24 bb 263.59 bb 215.47 bb 185.44 bb 158.89 bb 143.93 bb 2.09 bb 4.44 bb 3.52 bb 314.94 bb 306.18 bb 313.96 bb 234.61 bb 310.95 bb 244.88 bb 2.33 bb 2.14 bb 308.27 bb 342.91 bb 206.50 bb 272.09 bb 286.71 bb 204.53 bb 1.5.2 bb 272.65 bb 255.64 bb 319.04 bb 336.40 bb 340.93 bb 211.54 bb 1.76 bb 22 21 20 21 16 18 15 8 5 -14 -26 -36 -42 26 22 26 -6 24 -2 23 37 -17 9 15 -18 9 2 28 35 36 -15 272.99 bb 304.30 bb 381.60 bb 396.06 bb 265.47 bb 253.29 bb 9 54 53 54 6 1 297.01 bb 309.94 bb 311.66 bb 226.69 bb 344.86 bb 232.20 bb 1.79 bb 1.57 bb 340.90 bb 322.78 bb 231.11 bb 19 24 25 -9 38 -7 36 29 -8 Page 3 Quantitated and Printed by CMC on 24 Jan 01 Study # E00-1311 3M Environmental Laboratory a V )l Page 500 of 703 BACK TO MAIN Quantify Compound Summary Report PEOS Adsorb/Desorb Study, LC/MS Instrument: Tucker (LAO52) Sample List: C:\MASSLYNX\Deeatur.PRO\SampleDB\t010122 Last modified: Mon Jan 22 15:03:42 2001 Method: C:\MASSLYNX\Decatur.PRO\MethDB\PFOS - THPFOS Last modified: Wed Jan 24 06:53:49 2001 Job Code: Printed: Wed Jan 24 07:06:10 2001 Compound 2: I.S.(TH-PFOS)(427) * Name 83 t010122_ 083 84 t010122" 084 B5 t010122~ 085 86 t010122~'086 87 t010122~ 087 88 tQ10l22~'088 89 t010122~ 089 90 t010122~ 090 91 t010l22~ 091 92 t010122~ 092 93 t010122~' 0 9 3 94 t010122~'094 95 toi o1 2 2 "*095 96 t010l22" 096 97 t010l22~*097 90 tQl 0122~ 098 99 t010122_ 099 100 t010122_"lOO 101 t01Gl22~"lOl 102 t010l22~"102 103 t010l22~ 103 104 to 1 0 1 2 2 " 104 105 t010l22~"1 0 s 106 t010122""106 107 t01G122~ 107 108 1 0 1 0 1 2 2 " 108 109 t010122*"l09 110 t010122"" no 111 t010122""ill 112 t010122"" 1 1 2 113 t010122~" 1 1 3 114 t010122"'114 115 t010122"" 1 1 5 Samplelist Text E00-1311-2022, 0.75ug PFOS, Sediment,1/2.. EOO-1311-2023, 0.75ug PFOS, Sediment,1/2.. 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 EOO-1311-2024, 0.75ug PFOS, Sediment,1/2.. E00-1311-2024ras, 0.75ug PFOS , Sediment,!.. EO0-1311-2O25, 7.5ug PFOS, Sediment,1/22.. EOO-1311-2026, 7.5ug PFOS, Sediment,1/22.. E00-1311-2027, 7.5ug PFOS, Sediment,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 EOO-13ll-2027ms, 7.5ug PFOS, Sediment,1/.. 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 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 RT 6.180 6.102 6.240 7.101 6.168 6.193 6.325 6.230 6.302 6.193 6.216 6.386 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 Area 121124 122155 86155 0 24442 116050 88141 111262 96771 98097 71034 0 0 85993 93729 691 560 661 118951 103945 104129 106331 106157 105084 94464 91385 87246 72111 56656 62640 49733 951 553 Response 121123,969 122155,008 86155.375 ppb Flags 347.93 bb 350.90 bb 247.48 bb %Dev 39 40 -1 24442.334 116049.539 88141.375 111262.109 96771.055 98097.375 71033.633 70.21 bb 333.36 bb 253.19 bb 319.60 bb 277.90 bb 281.79 bb 204.05 bb 33 1 28 11 13 -18 85992.836 93728.602 690.849 560.268 660.914 118951.328 103945.063 104129.148 106330.531 106156.602 105003.742 94464.391 91385.258 87246.352 72111.070 56656.000 62640.102 49732.637 951.098 552.916 247.02 bb 269.24 bb 1.98 bb 1.61 bb 1.90 bb 341.69 bb 296.59 bb 299.12 bb 305.44 bb 304.94 bb 301.86 bb 271.35 bb 262.51 bb 250.62 bb 207.14 bb 162.75 bb 179.94 bb 142.86 bb 2.73 bb 1.59 bd -1 8 37 19 20 22 22 21 9 5 0 -17 -35 -28 -43 page 4 Quantitated and Printed by CMC on 24 Jan 01 Study # E00-1311 3M Environmental Laboratory Cmc ifd-q(oi Page 501 of 703 BACK TO MAIN Q u a n t if y C om pound S u iw o ary R e p o r t E 0 0 -1 3 1 1 PFOS A d s o r b / D e3 o r b S a m p le L i s t : C :\M a s s ly n x \s o u p 0 2 0 1 9 9 .p ro \S a m p X a D B \s 0 0 1 1 2 2 a L a s t m o d if ie d : Wed N ov 2 2 0 7 :2 3 :5 5 20 00 M e th o d : C :\M a s a ly n x \s o u p 0 2 0 1 9 9 .p ro \M e th D B \a 0 0 1 1 2 2 a L a s t m o d if ie d : Mon N ov 27 0 7 :4 2 :3 4 2000 Job Code: P rin te d : Mon Nov 27 0 7 :5 0 :4 1 t C o m p o u n d 1: PFOS (499>99), f u n c 1 2000 # Name study no Sample!ist Text 1 s00122a_J)01 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 2 sOO122a_002 EOO-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 s00122a_004 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 5 s00122a_005 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 6 s00122a_0Q6 EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 MLA 7 s00122a_007 EOO-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA 8 s00122a_008 EOO-1311 4.95 ppb PFOS 00002-86-03, Aliq. 11-03-00 MLA 9 s00122a_009 EOO-1311 9.9 ppb PFOS 00002-86-04, Aliq- 11-03-00 MLA 10 S00122a_010 EOO-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 11 s00122a_011 EOO-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA 12 s00122a_012 EOO-1311 49.5 ppb PFOS 00002-86-07 Aliq- 11-03-00 MLA 13 s0Q122a_013 EOO-1311 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA 14 s00122a_014 EOO-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA 15 s00122a_015 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 16 s00122a_016 EOO-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 17 s00122a_017 EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 18 s00122a_018 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 19 s00122a_019 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 20 s00122a_020 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 21 s00122a_021 EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 MLA 22 s00122a_022 EOO-1311 2.47ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA 23 s00122a_023 EOO-1311 4.95 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 EOO-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 26 s0Q122a_026 EOO-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA 27 s00122a_027 EOO-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA 28 s00122a_028 EOO-1311 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA 29 s00122a_029 E00-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA 30 sQ0122a_030 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 31 s00122a_031 EOO-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA 32 sOQ122a_032 EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA 33 s00122a_033 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 34 s00122a_034 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 35 s00122a_035 EOO-1311 E00-1311-1019 24 hour, Omg/L, S2, C-2 36 s00122a_036 EOO-1311 EQ0-13U-1020 24 hour, Omg/L, S2, C-2 37 s0Q122a_037 EOO-1311 E00-1311-1021 24 hour, Omg/L, S2, C-2 38 s00122a_038 EOO-1311 EOO-1311-1021 24 hour, Omg/L, S2, C-2, MS 39 s00122a_039 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 40 s00122a_04G E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 41 s00122a_041 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 42 sOO122a_042 EOO-1311 EOO-1311-1022 24 hour, O.lOmg/L, S2, C-2 43 s00122a_043 E00-1311 E00-13U-1023 24 hour, O.lOmg/L, S2, C-2 44 s00122a_044 EOO-1311 EOO-1311-1024 24 hour, O.lOmg/L, S2, C-2 45 sOO L22a_045 EOO-1311 00-1311-1024 24 hour, O.lOmg/L, S2, C-2, MS 46 s00122a_046 EOO-1311 EOO-1311-1025 24 hour, 1.Omg/L, S2, C-2 47 s00122a_047 _ EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 48 s00122a_048 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 49 s00122a_049 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 50 sQ0122a_050 EOO-1311 E00-1311-1026 24 hour, 1.Omg/L, S2, C-2 51 s00122a_051 EOO-1311 E00-13U-1O27 24 hour, 1. Omg/L, S2, C-2 52 s00122a_052 EOO-1311 E00-1311-1027 24 hour, 1.Omg/L, S2, C-2, MS 53 s00122a_053 EOO-1311 E00-1311-1028 24 hour, Omg/L, S2, C-3 54 sOO122a_054 EOO-1311 E00-1311-1029 24 hour, Omg/L, S2, C-3 55 s00122a_055 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 56 sQ0122a_056 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 57 sO0122a_057 58 s00122a_058 59 s00122a,,059 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 E00-1311-1030 24 hour, Omg/L, S2, C-3 EOO-1311 E00-1311-1030 24 hour, Omg/L, S2 , C-3 MS 60 sOO122a_060 EOO-1311 E00-1311-1031 24 hour, O.lOmg/L, S2, C-3 61 s00122a_061 EOO-1311 EO0-13U-1032 24 hour, O.lOmg/L, S2, C-3 62 s00122a_062 EOO-1311 EOO-1311-1033 24 hour, O.lOmg/L, S2, C-3 63 s00122a_Q63 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 64 s00122a_064 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 65 s00122a_Q6S EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 66 s00122a_066 EOO-1311 EOO-1311-1033 24 hour, O.lOmg/L, S2, C-3 MS 67 s00122a_067 E00-1'311 EOO-1311-1034 24 hour, 1. Omg/L, S2, C-3 68 s00122a_068 E00-1311 E00-1311-1035 24 hour, 1.Omg/L, S2, C-3 69 s00122a_069 EOO-1311 E00-1311-1036 24 hour, 1.Omg/L, S2, C-3 70 s00122a_070 EOO-1311 EOO-1311-1036 24 hour, 1.Omg/L, S2, C-3 MS 71 S00122a_071 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 72 s00122a_072 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 73 s00122a_073 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 74 s00122a_074 EOO-1311 E00-1311-1037 24 hour, Omg/L, S2, C-4 75 s00122a_07S EOO-1311 E00-1311-1038 24 hour, Omg/L, S2, C-4 76 s00122a_076 EOO-1311 E00-1311-1O39 24 hour, Omg/L, S2, C-4 77 s00122a_077 EOO-1311 E00-1311-1039 24 hour, 0mg/L, S2, C-4 MS 78 s00122a_078 EOO-1311 EOO-1311-104O 24 hour, O.lOmg/L, S2, C-4 79 s00122a_079 EOO-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 s00122a_081 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 82 s00122a_082 E00-1311 E00-1311-1041 24 hour, O.lOmg/L, S2, C-4 83 s00122a_083 EOO-1311 EOO-1311-1042 24 hour, O.lOmg/L, S2, C-4 84 sOO122a_084 EOO-1311 EOO-1311-1042 24 hour, O.lOmg/L, S2, C-4 MS 85 sQ0122a_08S EOO-1311 E00-1311-1O43 24 hour, 1.Omg/L, S2, C-4 86 s00122a_086 EOO-1311 E00-1311-1044 24 hour, 1.Omg/L, S2, C-4 87 s00122a_087 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA 88 s00122a_088 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 89 s00122a_089 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 SOUP 0 2 0 1 9 9 : q u a n t i t a t e d a n d p r i n t e d b y CMC o n 1 1 / 2 7 / 0 0 3M Environmental Laboratory Page 1 Type Analyte Analyte Analyte Analyte Analyte Analyte 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 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 Analyte Analyte QC Analyte Analyte B td Cone 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 7.118 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 7.118 7.127 7.141 7.118 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 rea 202 37418 36717 423 197 926 1416 1776 1900 3566 4431 4984 6826 8679 16310 24541 35819 263 198 186 855 1461 1741 1880 3444 4497 5027 7129 8453 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 L55 19173 1248 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 ppb VDev F l a g s M o d C o 0.00 bb bbl bbl 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 48.62 -2 bb 77.36 4 bb 107.79 9 bb 256.64 4 bb 565.92 14 bb bbl 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 bbxi 0,00 bb 0.00 bb 0.00 bb 0,00 bb 0,00 bb 328.62 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 Q .00 bb 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 143.43 bb 94.36 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 342.57 bb 15.18 bb 62.65 bb 234.87 -5 bb 0.00 bb 0.00 bb /c Page 502 of 703 BACK TO MAIN Q u a n t if y C om pound Sum m ary R e p o r t E O O -1 31 1 PFOS A d s o r b / D e s o r b S a m p le L i s t : L a s t m o d ifie d : M e th o d : L a s t m o d ifie d : Job Code: C :\M a s s ly n x \s o u p 0 2 0 1 9 9 .p ro \S a m p le P B \s 0 0 1 1 2 2 a Wed N ov 22 0 7 :2 3 :5 5 20 00 C : \M a s a ly n x \s o u p 0 2 0 1 9 9 .p ro \M e th D B \s 0 0 1 1 2 2 a Mon N ov 27 0 7 :4 2 :3 4 2000 P rin te d : Mon N ov 27 0 7 :5 0 :4 1 2000 I C om pound 1 : PFOS ( 4 9 9 > 9 9 ), fu n e 1 * Name 90 s00122a,,090 91 s00122a_091 92 s00122a,,Q92 93 s00122a,,093 94 s00122a_094 95 s00122a_095 96 s00122a_096 97 s00122a_Q97 98 s00122a_098 99 s00122a_099 100 s00122a_100 101 s00122a_101 102 s00122a_102 103 s00122a_103 104 s00122a_104 105 s00122a_105 106 s00122a_106 107 s00122a_107 108 s00122a_108 109 s00122a_109 110 S00122a,,110 s tu d y no S a m p le lis t T e x t EOO-1311 EOO-1311-1045 24 hour, 1.0mg/L, S2, C-4 E00-1311 EO0-1311-1045 24 hour, 1.0rag/L, S2, C-4 MS EOO-1311 247,9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 MLA 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 E00-1311 24,75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA EOO-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 EOO-1311 99.2 ppb PFOS 00002-86-09, Aliq. 11-03-00 MLA E00-1311 247.9 ppb PFOS 00002-86-10, Aliq, 11-03-00 MLA EOO-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA E00-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Page 2 Type Analyte Analyte QC Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte S td Cone 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 A rea 3002 20271 15179 140 149 164 803 1332 1713 1795 3284 4210 4728 6565 8022 15354 23 493 34251 241 189 150 p p b %Dev F la g s 19.14 bb 362.03 bb 231.29 -7 bb 0.00 bb 0.00 bb 0.00 bb 0,00 bb 0.00 -100 bbX 0.67 -86 bbX 1.84 -81 bbX 23.25 -6 bb 36.94 -7 bb 44.74 -10 bb 73.21 -1 bb 96.81 -2 bb 235.13 -5 bb 491.10 -1 bb bbxx 0.00 bb 0.00 bb 0.00 bb SOUP 0 2 0 1 9 9 : q u a n t i t a t e d a n d p r i n t e d b y CMC o n 1 1 / 2 7 / 0 0 3M Environmental Laboratory 1C U / J . 7 / 0 - L P Page 503 of 703 BACK TO MAIN Q u a n tify Com pound S unroary R e p o rt E 0 0 -1 3 1 1 PFOS A d s o r b / D e s o r b Sample List: C:\Masslynx\soup020199.pro\SarapleDB\s001122a L a s t m o d if ie d : Wed N o v 2 2 0 7 :2 3 :5 5 20 00 M e th o d : C :\M a s s ly n x \s o u p O 2 0 1 9 9 .p ro \M e th D B \a 0 0 1 1 2 2 a L a s t m o d if ie d : Mon N ov 27 0 7 :4 2 :3 4 20 00 Job Code: P rin te d : Mon N ov 27 0 7 :5 0 :4 1 2000 1 C om pound 2 : THPFOS { 4 2 7 > 8 0 ) , fu n e 2 * Name 1 s00122a_001 2 sOO122a_Q02 3 s00122a_003 4 s00122a_004 5 sOO122a_005 6 s00122a_006 7 s00122a_007 8 sQ0 1 2 2 a_ 0 0 8 9 s00122a_009 10 s00122a_010 11 s00122a_011 12 s00122a_012 13 s00122a_013 14 s00122a_014 15 sOO122a_015 16 s00122a_016 17 s00122a_017 18 sOO122a_018 19 s00122a_019 20 s00122a,,020 21 s00122a_021 22 s00122a_022 23 s00122a_023 24 s00122a_024 25 sOO122a_02 5 26 s00122a_026 27 s00122a_027 28 s00122a_028 29 s00122a_029 30 s00122a_030 31 s00122a_031 32 s00122a_Q32 33 sOO122a_033 34 s00122a_034 35 s00122a_035 36 s00122a_03 6 37 s00122a_037 38 s00122a_038 39 s00122a_039 40 s00122a_040 41 s00122a_041 42 s00122a_042 43 s00122a_043 44 S00122a_044 45 s00122a_045 46 s00122a_046 47 s00122a_047 48 s00122a_048 49 s00122a_049 50 s00122a_050 51 s00122a_051 52 S00122a_052 53 S00122a_053 54 a00122a_054 55 s00122a_055 56 s00122a_056 57 s00122a_057 58 s00122a_058 59 s O O 122a_059 60 s00122a_060 61 s0 0 1 2 2 a_ 0 6 1 62 s00122a_062 63 s00122a_063 64 s00122a_064 65 s00122a_065 66 s00122a_066 67 s00122a_067 68 s00122a_0 68 69 s00122a_069 70 s00122a_070 71 s00122a_071 72 s00122a_072 73 s00122a_073 74 s00122a_074 75 s00122a_075 76 s00122a_076 77 sOO122a_077 78 s00122a_078 79 s00122a_079 80 s00122a_080 81 s00122a_0.81 82 s00122a_082 83 s0Q122a_0 83 84 s00122a_084 85 s00122a_085 86 s00122a_0 86 87 sOO122a_087 88 sOO122a_08 8 89 s00122a_089 study no S a m p l e l i s t T e x t E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-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 EOO-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 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA E00-1311 39.6 ppb PFOS 00002-86-06, Aliq. 11-03-00 MLA EOO-1311 49.5 ppb PFOS 00002-86-07 Aliq. 11-03-00 MLA EOO-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 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA EOO-1311 495.9 ppb PFOS 00002-86-12 A l i q . 11-03-00 MLA EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq.11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq.11/16/00 ` EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-03-00 MLA EOO-1311 2.4?ppb PFOS 00002-86-02, Aliq. 11-03-00 MLA EOO-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 EOO-1311 24.75 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA 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 EOO-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 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA E00-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA EOO-1311 991.78 ppb PFOS 00002-86-13, aliq. 11-03-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 M60H Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 E00-1311-1019 24 hour, Orag/L, S2, C-2 EOO-1311 E00-1311-1020 24 hour, Omg/L, S2, C-2 EOO-1311 EOO-1311-1021 24 hour, Omg/L, S2, C-2 E00-1311 E00-1311-1021 24 hour, Omg/L, S2, C-2, MS E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 EOO-1311-1022 24 hour, 0.10mg/L, S2, C-2 E00-1311 E00-1311-1023 24 hour, O.lOmg/L, S2, C-2 E00-1311 EO0-1311-1024 24 hour, O.lOmg/L, S2, C-2 EOO-1311 EOO-1311-1024 24 hour, O.lOmg/L, S2, C-2, MS EOO-1311 EOO-1311-1025 24 hour, 1.Omg/L, S2, C-2 EOO-1311 247.9 ppb PFOS 00002-86-10, 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 EOO-1311 EOO-1311-1026 24 hour, 1.Omg/L, S2, C-2 E00-1311 E00-1311-1027 24 hour, l.Orag/L, S2, C-2 EOO-1311 E00-1311-1027 24 hour, 1.Omg/L, S2', C-2, MS EOO-1311 EOO-1311-1028 24 hour, Omg/L, S2, C-3 E00-1311 EOO-1311-1029 24 hour, Omg/L, S2, C-3 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 E00-1311-1Q30 24 hour, Omg/L, S2, C-3 EOO-1311 E O 0-1311-1030 24 hour, Omg/L, S 2 , C-3 MS EOO-1311 EQO-1311-1031 24 hour, O.lOmg/L, S2, C-3 EOO-1311 EOO-1311-1032 24 hour, O.lOmg/L, S2, C-3 EOO-1311 E O 0-1311-1033 24 hour, O.lOmg/L, S2, C-3 E00-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 EOO-1311-1033 24 hour, O.lOmg/L, S2, C-3 MS EOO-1311 E00-1311-1034 24 hour, 1.Omg/L, S2, C-3 EOO-1311 EOO-1311-1035 24 hour, 1.Omg/L, S2, C-3 E00-1311 E00-1311-1036 24 hour, 1.Omg/L, S2, C-3 EOO-1311 E00-1311-1036 24 hour, 1.Omg/L, S2, C-3 MS EOO-1311 247.9 ppb PFOS 00002-86-10, 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 EOO-1311 E00-1311-1037 24 hour, 0mg/L, S2, C-4 E00-1311 EOO-1311-1038 24 hour, Omg/L, S2, C-4 E00-1311 EOO-1311-1039 24 hour, Omg/L, S2, C-4 EOO-1311 E00-1311-1Q3 9 24 hour, Omg/L, S2, C-4 MS E00-1311 E00-1311-1040 24 hour, O.lOmg/L, S2, C-4 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 E00-1311-1041 24 hour, 0-10mg/L, S2, C-4 EOO-1311 E00-1311-1042 24 hour, O.lOmg/L, S2, C-4 E00-1311 EOO-1311-1042 24 hour, .10mg/L, S2, C-4 MS EOO-1311 E00-1311-1043 24 hour. 1.Omg/L, S2, C-4 EOO-1311 E00-1311-1044 24 hour, 1.Omg/L, S2, C-4 EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 SOUP 0 2 0 1 9 9 : q u a n t i t a t e d a n d p r i n t e d b y CMC o n 1 1 / 2 7 / 0 0 3M Environmental Laboratory Pag* 3 Type Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte Blank BlankAnalyte 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 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 8 td Cone 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 A rea 3051 3040 PPb %Dev F la g s M od Co 217.69 -12 bb 216.91 -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 -2 6 bb -26 bb -24 bb -30 bb -13 bb 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 -23 bb -23 bb -23 bb -10 bb 2598 2577 2600 2635 2502 3063 185.34 183.88 185.49 187.99 178.55 218.57 -26 bb -2 6 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 . C Jn C lt ip i/ Page 504 of 703 BACK TO MAIN Q u a n t if y Com pound Sum m ary R e p o r t E O O -1311 PPOS A d s o r b / D e s o r b S a m p le L is t ? L a s t m o d ifie d : M e th o d : L a s t m o d ifie d : Job Code: C :\M a S 3 ly n x \s o u p 0 2 0 1 9 9 .p ro \S a m p le D B \s 0 0 1 1 2 2 a Wed N o v 22 0 7 :2 3 :5 5 2000 C :\M a s s ly n x \s o u p 0 2 0 1 9 9 . p r o \M e th D B \s 0 O l122a Mon N ov 27 0 7 :4 2 :3 4 2000 P rin te d : Mon N ov 27 0 7 :5 0 :4 1 2000 t C om pound 2 : THPFOS (4 2 7 > 8 0 ), fu n e 2 # Name 90 s00122a_090 91 s00122a_091 92 s00122a_092 93 sOO122a_093 94 s00122a_Q94 95 s00122a_095 96 s00122a_09 6 97 s00122a_097 98 s00122a,,098 99 s00122a_099 100 sOO122a_100 101 s00122a_101 102 s00122a_102 103 s00122a_103 104 s00122a_104 105 s00122a_105 106 s00122a_106 107 s00122a_107 108 s00122a_108 109 sOO122a_109 110 sOO122a_110 s tu d y no S a m p le lis t T e x t EOO-1311 EOO-1311-1045 24 hour, 1.0mg/L, S2, C-4 E00-1311 E00-1311-1045 24 hour, 1.0mg/L, S2, C-4 MS EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA E0-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-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 EOO-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 ppb PFOS 00002-86-05, Aliq. 11-03-00 MLA EOO-1311 39.6 ppb PFOS 00002-86 -06, Aliq. 11-03-00 MLA EOO-1311 49.5 ppb PFOS 00002-86 -07 Aliq. 11-03-00 MLA EOO-1311 74.26 ppb PFOS 00002-86-08, Aliq. 11-03-00 MLA EOO-1311 99.2 ppb PFOS 00002-86 -09, Aliq. 11-03-00 MLA EOO-1311 247.9 ppb PFOS 00002-86-10, Aliq. 11-03-00 MLA EOO-1311 495.9 ppb PFOS 00002-86-12 Aliq. 11-03-00 MLA EOO-1311 991.78 ppb PFOS 00002- 86-13, aliq. 11-03-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Page 4 Type Analyte Analyte QC Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte S td Cone 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 246.10 RT 6.944 6.949 6.935 6.938 6.939 6.941 6.945 6.942 6.934 6.937 6.942 6.938 6.936 6.938 6.949 A rea 2748 2591 3076 p p b \Dev F l a g s 196.05 -22 bb 184.90 -26 bb 219-46 -11 bb Mod Co 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 0 2 0 1 9 9 : q u a n t i t a t e d a n d p r i n t e d b y CMC o n 1 1 / 2 7 / 0 0 3M Environmental Laboratory C m c h I j / o Page 505 of 703 BACK TO MAIN 3M Environmental Laboratory Inj Date Batch SampType File Sample Name 2/22/01 20:53 D:\chem\R ush.i\R 010222.b SAMPLE RUSH0022.D 00002-104-01 2/22/01 21:04 D:\chem\R ush.i\R 010222.b CALIB 1 RUSH0023.D 00002-104-02 2/22/01 21:16 0:tchem \Rush.itf?010222.b C ALB 2 RUSH0024.D 00002-104-03 2/22/01 21:27 D:Vchem\Rush.i\R010222.b CALIB 3 RUSHD025.D 00002-104-04 2/22/01 21:38 D:\chem\R ush.i\R 010222.b C ALIB 4 RUSH0026.D 00002-104-05 2/22/01 21:49 D:\chem\R ush.i\R 010222.b CALIB 5 RUSH0027.D 00002-104-06 2 0 2 /0 1 22:00 D:\chem \R ush.i\R 0 ! 0222. CALIB 6 RUSHQ028.D 00002-104-07 2/22/01 22:11 D:\chem\R ush.i\R 010222.b CALIB 7 R U SH 0029D 00002-104-08 2/22/01 22:22 D:\chem\R ush.i\R 010222.b CALIB 8 RUSH0030.D 00002-104-09 2/22/01 22:34 D:\chem\R ush.t\R010222.b CALIB 9 RUSH0031.D 00002-104-10 2/22/01 22:45 D IchemVRush i\R010222.b CALIB 10 RUSH0032.D 00002-104-11 2/22/01 22:56 D:\chem\R ush.i\R 010222.b SAMPLE RUSH0033.D 00002-104-12 2/22/01 23:07 D:\chem\R ush.i\R 010222.b SAMPLE RUSH0034.D 00002-104-13 2/23/01 1:32 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0047.D 00002-104-03 2/23/01 1:43 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0O48.D 00002-104-10 2/23/01 4:08 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0061.D 00002-104-03 2/23/01 4:20 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0062.D 00002-104-10 2/23/01 6:45 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0075.D 00002-104-03 2/23/01 6:56 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0076.D 00002-104-10 2/23/01 9:21 D:\cJiem\Rush.i\R010222.b CCALIB 1 RUSH0089.D 00002-104-03 2/23/01 9:33 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0090.D 00002-104-10 2/23/01 11:58 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0103.D 00002-104-03 2/23/01 12:09 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0104.D 00002-104-10 2/23/01 14:35 D:\chem\Rush.iVR010222.b CCALIB 1 RUSH0117.D 00002-104-03 2/23/01 14:46 D:\chem\R ush.R010222.b CCALIB 1 RUSH0118.D 00002-104-10 2/23/01 16:49 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0129.D 00002-104-03 2/23/01 17:00 D:\chem\R ush.i\R 010222.b CCALIB 1 RUSH0130.D 00002-104-10 2/23/01 17:34 D:\chem \Rush.i\R010222i> SAMPLE RUSH0133.D 00002-104-01 2/23/01 17:45 D:\chem\Rush.i\R01Q222.b CALIB 1 RUSH0134.D 00002-104-02 2/23/01 17:56 D:\chem\Rush.iAR010222.b CALIB 2 RUSH0135.D 00002-104-03 2/23/01 18:07 D:\chem\R ush.i\R 010222.b CALIB 3 RUSH0136.D 00002-104-04 2/23/01 18:18 D:\chem\R ush.i\R 010222.b CALIB 4 RUSH0137.D 00002-104-05 2/23/01 18:29 D:\chem\R ush.i\R 010222.b CALIB 5 RUSH0138.D 00002-104-06 2/23/01 18:41 D:\chem\R ush.i\R 010222.b CALIB 6 RUSH0139.D 00002-104-07 2/23/01 16:52 D:\chem\R ush.i\R 010222.b CALIB 7 RUSH0140.D 00002-104-08 2/23/01 19:03 D:\chem\R ush.i\R 010222.b CALIB_8 RUSH0141.D 00002-104-09 2/23/01 19:14 D:1chem\Rush.t\R010222.b CALIB 9 RUSH0142.D 00002-104-10 2/23/01 19:25 D:\chem\R ush.i\R 010222.b CALIB 10 RUSH0143.D 00002-104-11 2/23/01 19:36 D:\chem\R ush.i\R 010222.b SAMPLE RUSH0144.D 00002-104-12 2/23/01 19:48 D:\chem\R ush.i\R 010222.b SAMPLE RUSH0145.D 00002-104-13 Miac Info Compound Name did not m eet accuracy requirement Cal std 2 (L O O ) Cal std 3 Cal std 4 Cal std 5 Cal std 6 Cal std 7 Cal std 8 Cal std 9 Cal std 10 excluded to better fit data excluded to better fit data did not m eet accuracy requirement Cal std 12 (LOQ) Cal std 13 Cal std 14 Cal std 15 Cal std 18 Cal std 17 Cal std 18 Cal std 19 Cal std 20 excluded to better fit data excluded to better fit data 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 Area 5.553 5.561 5.558 5.554 5.545 5.54 5.539 5.552 5.567 5.56 5.551 5.549 5.555 5.561 5.567 5.555 5.547 5.545 5.539 5.54 686380 684164 689138 679632 671308 684907 678783 674589 668747 644602 619576 595985 576693 713865 652248 716157 659416 723145 654913 557797 5.532 5.507 5.51 5.537 5.536 5.509 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 average std deviation %CV 649228 714024 640235 748169 662645 729420 637769 718171 728159 734029 723187 711239 704611 706699 702051 685302 646270 610214 573864 562318 672484 45783 6.8% Amount Compound Name ng/m L RT Area Amount ng/mL % Dev 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 00 0.0 PFOS 5.785 56147 0.0 X PFOS 5.775 93148 5.0 0.0% PFOS 5.778 188431 10.0 0.0% PFOS 5.769 401765 25.0 0.0% PFOS 5.764 664873 40.1 0.3% PFOS 5.756 858165 50.2 0.4% PFOS 5.776 1276020 74.8 0.3% PFOS 5.764 1657895 99.5 0.5% PFOS 5.777 3779794 249.9 0.0% PFOS 5.775 6785120 500.1 0.0% PFOS 5.773 9501199 776.5 X PFOS 0 0 0.0 X PFOS 5.779 94822 5.3 5.9% PFOS 5.785 3852487 251.6 0.6% PFOS 5.78 93043 5.2 3.6% PFOS 5.771 3867395 249.7 0.1% PFOS 5.769 92534 5.1 2.1% PFOS 5.763 3872492 251.9 0.7% PFOS 5.771 94512 6.7 34 .6 % check sta ndard >30% due to low TH PFO S response PFOS 5.763 3834036 251.5 0.6% PFOS 5.731 91142 5.1 1.8% PFOS 5.741 3727210 247.7 0.9% PFOS 5.768 94563 5.0 0.9% PFOS 5.76 3860610 247.9 0.9% PFOS 5.733 94353 5.2 3.2% PFOS 5.728 3687433 245.8 1.7% PFOS 00 0.0 PFOS 5.735 50380 2.8 X PFOS 5.729 89391 5.0 0.3% PFOS 5.716 185120 10.5 4.7% PFOS 5.727 385518 22.1 11.5% PFOS 5.719 629059 36.4 8.9% PFOS 5.729 832703 48.3 3.5% PFOS 57 26 1248636 73.2 2.4% PFOS 5.73 1612642 98.2 1.8% PFOS 5.728 3713608 250.5 0.2% PFOS 5.722 6606557 499.8 0.0% PFOS 5.725 9143085 776.4 X PFOS 5.722 11261687 1017.6 X C(QTD)> cn oO) *o4i *OOvJ| 3M Environmental Laboratory "0 CCQD CD UOl O Ovl CO 2/22/01 23:41 D:\chem\Rush.i\R010222.b SAMPLE RUSH0037.D 1311-4052-S1 2/22/01 23:52 D:\chem\Rush.i\R010222.b SAMPLE RUSH0038.D 1311-4053-S1 2/23/01 0:03 D:\chem\Rush.i\R01Q222.b SAMPLE RUSH0039.D 1311-4054-S1 2/23/01 0:14 D:\chem\Rush.i\R010222.b SAMPLE RUSH0040.D 1311-4054MS-S1 2/23/01 0:25 D:\ctiem\Rusfvi\R010222.b SAMPLE RUSH0041.D 1311-4055-S1 2/23/01 0:36 D:\chem\Rush.i\R010222.b SAMPLE RUSH0042.D 1311-4056-S1 2/23/01 0:47 D:\chem\Rush.i\R010222.b SAMPLE RUSH0043.D 1311-4057-S1 2/23/01 0:59 D:\chem\Rush.i\R010222.b SAMPLE RUSH0044.D 1311-4057MS-S1 2/23/01 1:10 D:\chem\Rush.i\R010222.b SAMPLE RUSH0045.D 1311-4058-S1 2/23/01 1:21 D:\chem\Rush.i\R010222.b SAMPLE RUSH0046.D 1311-4059-S1 2/23/01 2:17 D:\chem\Rush.i\R010222.b SAMPLE RUSH0051.D 1311-4060-S1 2/23/01 2:28 D:\chem\Rush.i\R010222.b SAMPLE RUSH0052.D 1311-4060MS-S1 2/23/01 2:39 D:\chem\Rush.i\R010222.b SAMPLE RUSH0053.D 1311-4061-SI 2/23/01 2:50 D:\chem\Rushi\R010222.b SAMPLE RUSH0054.D 1311-4062-SI 2/23/01 3:01 D:\chsm\Rush.i\R010222.b SAMPLE RUSH0055.D 1311-4063-S1 2/23/01 3:13 D:\chem\Rush.i\R010222.b SAMPLE RUSH0056.D 1311-4063MS-S1 2/23/01 3:24 D:\chem\Rush.i\R010222.b SAMPLE RUSH0057.D 1311*4064-S1 2/23/01 3:35 D:\chem\Rush.i\R010222.b SAMPLE RUSH0058.0 1311-4065-S1 2/23/01 3:46 O:\chem\Rush.i\R010222.b SAMPLE RUSH0059.D 1311-4066-S1 2/23/01 3:57 D:\chem\Rush.i\R010222.b SAMPLE RUSH0060.D 1311-4066MS-S1 2/23/01 4:53 D:\chem\Rush.j\R010222 b SAMPLE RUSH0065.D 1311-4067-S1 2/23/01 5:04 D:\chem\Rush.i\R010222.b SAMPLE RUSH0066D 1311-4068-S1 2/23/01 5:16 D:\chem\Rush-i\R010222.b SAMPLE RUSH0067.D 1311-4069-S1 2/23/01 5:27 D:\chem\Rush.i\R010222.b SAMPLE RUSH0068.D 1311-4069MS-S1 2/23/01 5:38 D:\chem\Rush.i\R010222.b SAMPLE RUSH0069.D 1311-4070-S1 2/23/01 5:49 D:\chem\Rush.i\R010222.b SAMPLE RUSH0070.D 1311-4071-S1 2/23/01 6:00 D:\chem\RushJ\R010222.b SAMPLE RUSH0071.0 1311-4072-S1 2/23/01 6:11 D:\chem\Rush.i\R010222.b SAMPLE RUSH0072.D 1311-4072MS-S1 2/23/01 6:23 D:\chem\Rush-i\R010222.b SAMPLE RUSH0073.D 1311-4073-S1 2/23/01 6:34 D:\chem\Rush.i\R010222.b SAMPLE RUSH0074.0 1311-4074-S1 2/23/01 7:30 D:\chem\Rush.i\R010222-b SAMPLE RUSH0079.D 1311-4075-S1 2/23/01 7:41 D:\chem\Rush.i\R010222-b SAMPLE RUSH0080.0 1311-4075MS-S1 2/23/01 7:52 D:\chem\Rush.i\R010222.b SAMPLE RUSH0081.D 1311-4075-S1 2/23/01 8:03 D:\chem\Rush.i\R010222.b SAMPLE RUSH0082.0 1311-4077-S1 2/23/01 8:14 D:\chem\Rush.i\R010222.b SAMPLE RUSH0083.D 1311-4078-S1 2/23/01 8:25 D:\chem\Rush.i\R010222.b SAMPLE RUSH0084.D 1311-4078MS-S1 2/23/01 8:37 D:\cbem\Rush.i\R010222.b SAMPLE RUSH0085.0 1311-4079-S1 2/23/01 8:48 D:\cfiem1Rush.i\R010222.b SAMPLE RUSH0O86.O 1311-4060^1 2/23/01 8:59 D:\chem\Rush.f\R010222.b SAMPLE RUSH0087.D 1311-4081-SI 2/23/01 9:10 D:\cbem\Rush.i\R010222.b SAMPLE RUSH0086.D 1311-4081MS-S1 2/23/01 10:06 D:\chem\Rush.i\R010222.b SAMPLE RUSH0093.D 1311-4082-S1 2/23/01 10:17 D:\chem\Rush.i\R010222.b SAMPLE RUSH0094.D 1311*4063-S1 2/23/01 10:28 D:\chem\Rush.i\R010222.b SAMPLE RUSH0095.D 1311-4084-S1 2/23/01 10:40 O:\chem\Rush.ilRG10222.b SAMPLE RUSH0096.D 1311-4034MS-S1 2/23/01 10:51 D:\chem\Rush.i\R010222.b SAMPLE RUSH0097.D 1311-4085-S1 2/23/01 11:02 D:\chem\Rush.i\R010222.b SAMPLE RUSH0098.D 1311-4086-S1 2/23/01 11:13 D:\chem\Rush.i\R010222.b SAMPLE RUSH0099.D 1311-4087-S1 2/23/01 11:24 D:\diem\Rush.i\R010222.b SAMPLE RUSH0100.D 1311-4087MS-S1 2/23/01 11:35 D:\eJiem\Rush.i\R010222-b SAMPLE RUSH0101.D 1311-4088-S1 2/23/01 11:47 D:te/iemlRusft.ftR010222.b SAMPLE RUSH0102.D 1311-4089-S1 2/23/01 12:43 D:\chem\Rash.i\R010222.b SAMPLE RUSH0107.D 1311-4090-S1 2/23/01 12:54 D:\chem\Rush.i\R010222.b SAMPLE RUSH0108.D 1311-4090MS-S1 2/23/01 13:05 D:\chem\Rush.i\R010222.b SAMPLE RUSH0109.D 1311-4091-SI 2/23/01 13:16 D:\chem\Rush.i\R010222.b SAMPLE RUSH0110.D 1311-4092-S1 2/23/01 13:27 D:\chem\Rush.i\R010222.b SAMPLE RUSH0111.D 1311-4093-S1 2/23/01 13:39 D:tobem1Rush./1R010222.b SAMPLE R U S H D 1 1 2 .D 1311-4093MS-S1 2/23/01 13:50 D:\chem\Rush.i\R010222.b SAMPLE RUSH0113.D 1311-4094-S1 2/23/01 14:01 D:\chem\Rush.i\R010222.b SAMPLE RUSH0114.D 1311-4095-S1 2/23/01 14:12 D:\chem\Rush.i\R010222.b SAMPLE RUSH0115.D 1311-4096-S1 2/23/01 14:23 D:\chem\Rush.i\R010222.b SAMPLE RUSH0116.D 1311-4096MS-S1 2/23/01 15:19 D:\chsm\Rush.i\R010222.b SAMPLE RUSH0121.D 1311-4097-S1 2/23/01 15:30 D.WwmWush.f\R010222.b SAMPLE RUSH0122.D 1311-4098-S1 2/23/01 15:42 D:\cbem\Rush.i\R010222.b SAMPLE RUSH0123.D 1311-4099-S1 2/23/01 15:53 D:\chem\Rush.i\R010222.b SAMPLE RUSH0124.D 1311-4099MS-S1 2/23/01 16:04 D:\chem\Rush.i\R010222.b SAMPLE RUSH0125.D 1311-4100-S1 2/23/01 16:15 D:\chem\Rush.i\R010222.b SAMPLE RUSH0126.D 1311-4101-S1 2/23/01 16:26 D:\chem\Rush.i\R010222.b SAMPLE RUSH0127.D 1311-4102-SI 2/23/01 16:38 0:kchem\Rush.\R010222.b SAMPLE RUSH0128.D 1311-4102MS-S1 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 BACK TO MAIN 5.561 5.565 5.567 5.567 5.559 5.56 5.565 .5.567 5.566 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 5.541 5.54 5.54 5.547 5.547 5.548 5.541 5.554 5.545 5.551 5.539 5.537 5.543 5.528 5.526 5.527 5.526 5.513 5.509 5.504 5.506 5.505 5.51 5.516 5.502 5.511 5.521 5.521 5.503 5.505 5.525 5.531 5.547 5.533 5.54 5.523 5.529 5.526 5.52 5.515 5.515 5.518 5.51 738374 729081 748027 648640 720097 718694 713613 650599 698677 697037 712727 623982 713961 722949 717685 626622 693953 703230 683158 601504 715149 718563 721833 626695 723074 713569 710887 626987 719422 721925 721016 630748 721345 713442 714470 627930 716587 708783 767134 625739 711663 705320 711370 617162 702007 701896 704199 616234 683319 678063 676009 594782 696138 702240 713216 617233 706887 708135 705249 619647 727274 722539 724280 611327 714433 712362 699621 606960 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 249.3 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 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 5.763 5.763 5.758 5.759 5.757 5.757 5.771 5.771 5.779 5.772 5.778 5.769 5.775 5.756 5.761 5.767 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 5.764 5.747 5.753 5.757 5.751 5.739 5.74 5.735 5.734 210932 1863B7 214795 3273596 t 62434 159201 404553 3223948 199972 184162 188818 3147881 0 52969 0 3039824 0 0 0 2944564 708991 738565 483585 3383101 353028 401704 385139 3324237 366061 377219 356402 3329105 400719 384833 391323 3308122 327587 324602 608553 3277776 359433 317521 322509 3238116 275759 289371 598587 3378059 296195 292811 288064 3043722 0 0 0 2959566 0 0 0 2957005 379845 387610 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 0.0 0.0 0.0 205.5 39.3 40.8 26.5 228.3 19.3 22.2 21.4 223.9 20.1 20.6 19.5 222.8 21.9 21.3 21.6 222.3 18.1 18.1 31.4 221.0 19.9 17.8 17.9 221.4 15.5 16.3 33.7 232.1 17.1 17.1 16.8 215.5 0.0 0.0 0.0 201.0 0.0 0.0 0.0 200.7 20.6 21.2 31.3 233.1 14.8 15.5 14.0 212.8 3M Environmental Laboratory 2/22/01 20:42 D:\chem\Rush.i\R010222.b 2/22/01 23:18 D:\chem\Rush.i\R010222.b 2/22/01 2329 D:\chem\Rush.i\R010222.b 2/23/01 1:54 D:\chem\Rush.i\R010222.b 2/23/01 2:06 D:\chem\Rush.i\R010222.b 2/23/01 4:31 D:\chem\Rush.i\R010222.b 2/23/01 4:42 D:\chem\Rush.i\R010222.b 2/23/01 7:07 D:\chem\Rush.ftR010222.b 2/23/01 7:18 D:\chem\Rush.i\R010222.b 2/23/01 9:44 D:\chem\Rush.iVR010222.b 2/23/01 9:55 D:\chem\Rush.i\R010222.b 2/23/01 12:20 D:\chem\Rush.i\R010222.b 2/23/01 12:32 D:\chem\Rush.i\R010222.b 2/23/01 14:57 D:\chem\RushJ\R010222.b 2/23/01 15:08 D:\chem\Rush.i\R010222.b 2/23/01 17:11 D:\chem\Rush.i\R010222.b 2/23/01 17:22 D:\chem\Rush.i\R010222b 2/23/01 19:59 D:\ehem\Rush.i\R010222.b 2/23/01 20:10 DAd>em\Rush.i\R010222.b Sa m p l e sample SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0021.D TN-A 4755 MeOH RUSH0035.D TN-A 4755 MsOH RUSH0036.D TN-A 4755 MeOH RUSH0049.D TN-A 4755 MeOH RUSH0050.D TN-A 4755 MeOH RUSH0063.D TN-A 4755 MeOH RUSH0064.D TN-A 4755 MeOH RUSH0077.D TN-A 4755 MeOH RUSH0078.D TN-A 4755 MeOH RUSH0091.D TN-A 4755 MeOH RUSH0092.D TN-A 4755 MeOH RUSH0105.D TN-A 4755 MeOH RUSH0106.D TN-A 4755 MeOH RUSH0119.D TN-A 4755 MeOH RUSH0120.D TN-A 4755 MeOH RUSH0131.D TN-A 4755 MeOH RUSH0132.D TN-A 4755 MeOH RUSH0146.O TN-A 4755 MeOH RUSH0147.D TN-A 4755 MeOH THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS CQ"Q0) CD 0OO0l O o-vj CO BACK TO MAIN 0 00 PFOS 5.802 13952 0.0 0 00 PFOS 5.794 23163 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 00 0.0 0 00 PFOS 5.733 25813 0.0 0 00 PFOS 5.735 18305 0.0 3M Environmental Laboratory Sam ple B atch H010402.b, analyzed o n H illa ry 04-02-01. PFOS A dsorb/D esorb samples. M atrix: Soil/Sig/Sed. Standard curve range used fo r calibration o f sam ples: 5-1002 ng/m L Batch m ethod: H010402b.m Inj D ate B a tc h 4/3/01 3:14 D:\Chem\Hillary\H010402.b 4/3/01 3:28 D:\Chem\Hillary\H010402.b 4/3/01 3:43 D:\Chem\Hiilary\H010402.b 4/3/01 3:57 D:\Chem\Hillary\H010402.b 4/3/01 4:11 D:\Chem\HUIary\H010402.b 4/3/01 4:26 D:\Chem\Hiltary\H010402.b 4/3/01 4:40 D:\Cbem\Hillary1H010402.b 4/3/01 4:54 D:\Chem\Hillary\H010402.b 4/3/01 5:09 D:\Chem\Hilao'\H010402.b 4/3/01 5:23 D:\Chem\Hiliary\H010402b 4/3/01 5:38 D:\Chem\Hillary\H010402.b 4/3/01 5:52 D:\Chem\Hillary\H010402.b 4/3/01 6:06 D:\CherrAHillary\H010402.b 4/3/01 23:24 D:\Chem\Hiilary\H010402.b 4/3/01 23:39 D:\Chem\Hiilary\H010402.b 4/3/01 23:53 D:\Chem\Hillary\H010402.b 4/4/01 0:07 D:\Chem\HiHary\H010402.b 4/4/01 0:22 D:\Chem\Hillary\H010402.b 4/4/01 0:36 D:\Chem\Hillary\H010402.b 4/4/01 0:50 D:\Chem\Hillary\H010402.b 4 /4/011:05 D:\Chem\HiHary\H010402.b 4/4/01 1:19 D:\Chem\Hillary\H010402.b 4/4/01 1:34 D:\Chem\Hillary\H010402.b 4/4/01 1:48 D:\Chem\Hillary\H010402.b 4/4/01 2:02 D:\Chem\HiKarylH010402.b 4/4/01 2:17 D:\Chem\Hillary\H010402.b SampType SAMPLE C A LIB J CALiB 2 C A L IB _ 3 CAUB 4 SAMPLE CAL1B_5 CALIBJ CAUB_7 C A L IB _ 8 SAMPLE CAUB 9 CAUB 10 SAMPLE C A LIB J 1 C ALIBJ2 C A LIB J3 CALIB 14 SAMPLE C A LIB J5 CALJB_16 CALIB 17 CAUB 18 SAMPLE CALJBJ9 C A L IB _ 2 0 File HILL0077.D HILL0078.D HILL0079.D H IL L 0 0 8 0 .D H IL L 0 0 6 1 .0 HILL0082.D HILLO083.D HILL0084.D HILL0085.D HILL0086.D HiLL0087.D HILL0088 0 HILL0089.D H IL L 0 1 6 1 .D HILL0162.D H IL L 0 1 6 3 .D HiLL0164.D HILL0165D H IL L 0 1 6 6 .D HILL0167.D H /L L 0 1 6 8 .D HILL0169.D HILL0170.D HILL0171.D HJLL0172.D HILL0173.D Sample Nam e O ng/mL PFOS in MeOH 2.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 10 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 ng/m L PFOS in MeOH 250.5 ng/m L PFOS in MeOH 400.6 ng/m L PFOS in MeOH 501 ng/mL PFOS in MeOH 1002 ng/mL PFOS in MeOH O ng/mL PFOS in MeOH 2.5 ng/mL PFOS in MeOH 5 ng/mL P FO S in MeOH 10 ng/mL PFOS in MeOH 25 ng/mL PFOS in MeOH 40 ng/mL PFOS in MeOH 50.1 ng/m L PFOS in MeOH 75.1 ng/mL PFOS in MeOH 100.2 ng/m L PFOS in MeOH 250.5 ng/m L PFOS in MeOH 400.8 ng/m L PFOS in MeOH 501 ng/mL PFOS in MeOH 501 ng/mL PFOS in MeOH 0 03 3 r\ AO CX X U) 0 Q" O) CO CD OOl CO o --* o CO BACK TO MAIN H010402b.xls Mise InfC om pound Na RT Area Amount THPFOS 5.106 1211876 254 THPFOS 5.105 1169631 254 THPFOS 5.108 1115864 254 THPFOS 5.097 1128520 254 THPFOS 5.105 1132730 254 THPFOS 5.104 1144180 254 THPFOS 5.112 1088719 254 THPFOS 5.105 1050910 254 THPFOS 5.107 1034615 254 THPFOS 5 .1 0 5 969248 254 THPFOS 5.105 988215 254 THPFOS 5.106 1060823 254 THPFOS 5.107 928336 254 THPFOS 5.105 1337731 254 THPFOS 5.1 1311179 254 THPFOS 5.097 1236112 254 THPFOS 5.101 1272114 254 THPFOS 5.097 1284745 254 THPFOS 5.1 1303887 254 THPFOS 5.096 1207553 254 THPFOS 5.099 1208046 254 THPFOS 5.101 1167221 254 THPFOS 5.09 1093910 254 THPFOS 5.091 1097069 254 THPFOS 5.091 1175367 254 THPFOS 5.104 1023103 254 Averaae: 1143911.69 Std Dev: 110106.958 %RSP: 9.6% Compound NanRT Area Amount PFOS 000 PFOS 5.322 76308 3.396026 PFOS 5.325 108804 5.067026 PFOS 5.321 209068 9.618429 PFOS 5.322 565907 26,00359 PFOS 5.329 929336 42.42639 PFOS 5.336 1114128 53.58744 PFOS 5.322 1636985 82.09443 PFOS 5.331 2152918 110.3641 PFOS 5.329 4767587 269.8584 PFOS 5 329 7513403 430.2713 PFOS 5.33 9712588 527.3099 PFOS 5.331 15484980 1041.642 PFOS 0 00 PFOS 5.31 76978 3.057897 PFOS 5.307 107847 4.535542 PFOS 5.311 208869 8.524792 PFOS 5.308 560714 22.70129 PFOS 5.31 928989 37.17265 PFOS 5.306 1099646 47.62208 PFOS 5.309 1590311 69.17022 PFOS 5.318 2147218 97.2829 PFOS 5.307 4811322 239.8238 PFOS 5.309 7530799 385.2073 PFOS 5.309 9910075 481.6606 PFOS 5.321 15786129 951.0902 1487085 +30%: 800738 -30%: 101% 96% 104% 106% 107% 109% 110% 108% 107% 105% 104% 91% 85% 91% 93% 95% 92% 97% 96% 96% 96% 95% page 1 of 3 Page 510 of 703 3M Environmental Laboratory In] Date Batch 4/3/01 2:45 D:\Chem\Hillary\H010402. b 4/3/01 2:59 D:\Chem \Hillary\H0l0402lb 4/3/01 6:21 D:\Chem\Hillafy\H010402.b 4 /3/016:35 D:\Chem\Hillary\H010402.b 4/3/01 7:04 D:\Chem\Hilfary\H0l0402.b 4/3/01 7:33 D:\Chem\HiIlary\H0l0402.b 4/3/01 8:02 D:\Chem\Hillary\H0l0402.b 4/3/01 8:30 D:\Chem\Hillary\HOl0402.b 4/3/01 8:59 D:\Chem \Hilla;y\H0l0402.b 4/3/01 9:28 D:\Chem\Hillary\H010402.b 4/3/01 9:57 D:\Chem\Hillary\H0l0402.b 4/3/01 10:26 D:\Chem\Hillary\H010402.b 4/3/01 10:55 D:VChem\HiHaiy\H010402.b 4/3/01 11:52 D:\Chem\Hillary\HQ10402.b 4/3/01 12:07 D:VChwrtHllaiyNH010402.b 4/3/01 12:35 D:\Chem\Hiltary\H010402.b 4/3/01 13:04 D:\Chem\Hillary\H0l0402.b 4/3/01 13:33 D:\Chem\Hillary\H010402.b 4/3/01 14:02 D:\Chem\Hillary\H010402.b 4/3/01 14:31 D:\Chem\Hillary\H010402.b 4/3/01 15:00 D:\Chem\Hillary\H010402.b 4/3/01 15:28 D:\Chem\Hillary\H010402 b 4/3/01 15:57 D:\Chem\Hillary\H010402.b 4/3/01 16:26 D:\Chem\HiUary\H010402.b 4/3/01 17:24 D:\Chem\Hillary\H010402.b 4/3/01 17:38 D:\Chem\HtUary\HQ10402.b 4/3/01 18:07 D:\Chem\HilIaiy\H010402.b 4/3/01 18:36 D:\Chem\Hillary\H010402.b 4/3/01 19:05 D:\Chem\Hillafy\H010402.b 4/3/01 19:33 D:\Chem\Hillary\H010402.b 4/3/01 20:02 D:\Cherri\Hillary\H010402.b 4/3/01 20:31 D:\Chem\Hillafy\H010402.b 4/3/01 21:00 D:\Chem\Hiilary\H0l0402.b 4/3/0121:29 D:\Chem\Hillary\H010402 b 4/3/01 21:58 D\Chem\Hillary\H010402.b 4/3/01 22:55 D:\Chem\Hillary\H0l0402.b 4/3/01 23:10 D:\Chem\Hillary\H010402.b 4/4/01 2:31 D:\Chem\Hillary\H010402.b 4/4/01 2:45 D:\Chem\Hillary\H010402.b 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 SAMPLE SAMPLE SAMPLE File H IL L 0 0 7 5 .D H IL L 0 0 7 6 .D H IL L 0 0 9 0 .D H IL L 0 0 9 1 .D H IL L 0 0 9 3 .D HILLQ095.D H IL L 0 0 9 7 .D H IL L 0 0 9 9 .D H IL L 0 1 0 1 .D H IL L 0 1 0 3 .D H IL L 0 1 0 5 .D H IL L 0 1 0 7 .D H IL L 0 1 0 9 .D H IL L 0 1 1 3 .D H IL L 0 1 1 4 .D H IL L 0 1 1 6 .D H IL L 0 1 1 8 .D H IL L 0 1 2 0 .D H IL L 0 1 2 2 .D H IL L 0 1 2 4 .D HILL0126D HILLQ128.D H IL L 0 1 3 0 .D H IL L 0 1 3 2 .D H IL L 0 1 3 6 .D H IL L 0 1 3 7 .D H IL L 0 1 3 9 .D H IL L 0 1 4 1 .D H IL L 0 1 4 3 .D H IL L 0 1 4 5 .D H IL L 0 1 4 7 .D H IL L 0 1 4 9 .D H IL L 0 1 5 1 .D H IL L 0 1 5 3 .D HILL0155.D H IL L 0 1 5 9 .D HILL0160.D HILL0174.D HILL0175.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 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 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 TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH BACK TO MAIN H0l0402b.xls fC o m p o u n d Na 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 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 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 00 00 00 00 00 00 00 00 00 00 00 0Q 00 0Q 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 C om pound NarrRT 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 Area Amount 000 000 5.425 36059 0 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 000 page 2 o f3 co 5 m 3 s VSJ' =3 CD ST r- 0o)* o S o Q Inj Date Batch 4/3/01 6:49 D:\Chem\Hillary\H010402-b 4/3/01 7:18 D:\Chem\Hillary\H010402.b 4/3/01 7:47 D:\Chem\Hiliary\H010402.b 4/3/01 8:16 D:\Chem\Hillary\H010402.b 4/3/01 8:45 D:\Chem\Hillary\H010402.b 4/3/01 9:14 D:\Chem\Hiltary\H010402.b 4/3/01 9.42 0.\Chem\Hillary\H010402.b 4/3/01 10:11 D:\Chem\Hillary\H010402.b 4/3/01 10:40 D:\Chem\Hillary\H010402.b 4/3/0111:09 D:\Chem\HMIary\H010402.b 4/3/01 11:23 D:\Chem\HiHary\H010402.b 4/3/01 11:38 D:\Chem\Hillary\H010402.b 4/3/01 12:21 D:\Chem\Hillafy\H010402.b 4/3/0112:50 D:\Chem\Hillary\H010402.b 4/3/0113:19 D:\Chem\HiIlary\H010402-b 4/3/01 13:48 D:\Chem\Hillary\H010402.b 4/3/01 14:17 D:\Chem\Hiltary\H010402.b 4/3/01 14:45 D:\Chem\HillaryVH010402.b 4/3/0115:14 D:\Chem\Hillary\H010402.b 4 /3/0115:43 D:\Chem\Hiliary\H010402.b 4/3/0116:12 D:\Chem\Hillary\H010402.b 4/3/01 16:40 D:\Chem\Hillary\H010402.b 4/3/01 16:55 D:\Chem\Hillary\H010402.b 4 /3/0117:09 D:\Chem\Hillary\H010402.b 4/3/01 17:52 D:\Chem\Hillary\H010402.b 4/3/01 18:21 D:\Chem\Hillary\H010402.b 4/3/01 18:50 D:\Chem\HiUary\H010402.b 4/3/01 19:19 D:\Chem\Hillary\H010402.b 4/3/01 19:48 D:\Chem\Hillaiy\H010402.b 4/3/01 20:17 D:\Chem\Hiilary\H010402.b 4/3/01 20:46 D:\Chem\Hillary\H010402.b 4/3/01 21:14 D:\Chem\Hiilary\H010402.b 4/3/01 21:43 D:\Cbem\Hillary\H010402.b 4/3/01 22:12 D:\Chem\Hillary\H010402.b 4/3/01 22:27 D:\Chem\HiilaryUH010402.b 4/3/01 22:41 D:\Chem\HiHary\H010402.b 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 H IL L 0 0 9 2 .D H IL L 0 0 9 4 .D H IL L 0 0 9 6 .D H IL L 0 0 9 8 .D H IL L 0 1 0 0 .D H IL L 0 1 0 2 .D HILL0104.0 H IL L 0 1 0 6 .D H IL L 0 1 0 8 .D H IL L 0 1 1 0 .D H IL L 0 1 1 1 .D H IL L 0 1 1 2 .D H IL L 0 1 1 5 .D H IL L 0 1 1 7 .D H IL L 0 1 1 9 .D H IL L 0 1 2 1 .D H IL L 0 1 2 3 .D HILL0125.D H IL L 0 1 2 7 .D H IL L 0 1 2 9 .D H IL L 0 1 3 1 .O H IL L 0 1 3 3 .D H IL L 0 1 3 4 .D HILL0135.D HILL0136.D H IL L 0 1 4 0 .D HILL0142.D H IL L 0 1 4 4 .D H IL L 0 1 4 6 .D HILL0148.D HILLQ150.D HILL0152.D HILL0154.D HILL0156.D H IL L 0 1 5 7 .D H L L 0 1 5 8 .D Sample Nam e 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5m g/l PFOS Study Num ber E00-1311 5 ng/m l PFOS in MeOH 250.5 ng/m L PFOS in MeOH 5m g/l PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/l PFOS Study Num ber EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5ng/mL PFOS in MeOH 250.5 ng/m L PFOS in MeOH 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Num ber EOO-1311 5mg/L PFOS Study Number EOO-1311 5 ng/mL PFOS in MeOH 250 5 ng/mL PFOS in MeOH "U Q) (O CD Ol O O CO BACK TO MAIN HQ10402b.xls ifC om pound Na RT Area Amount C om pound NatrRT Area Amount THPFOS 5.106 1643844 254 ISTD>130% PFOS 5.33 209598 6.621818 THPFOS 5.112 1594154 254 ISTD>130% PFOS 5.329 3430184 114.2188 THPFOS 5.106 1605329 254 ISTD>130% PFOS 5.323 73592 2.392023 THPFOS 5.097 1598522 254 ISTD>130% PFOS 5.314 58689 1.919775 THPFOS 5.103 1558836 254 ISTD>130% PFOS 5.321 63584 2.130585 THPFOS 5.105 1574536 254 ISTD>130% PFOS 5.322 3247504 109.3654 THPFOS 5.105 1563077 254 1STD>130% PFOS 5.329 72816 2.430454 THPFOS 5.098 1582850 254 ISTD>130% PFOS 5.322 99365 3.268414 THPFOS 5.098 1574580 254 ISTD>130% PFOS 5.323 173732 5.731799 THPFOS 5.099 1545068 254 ISTD>130% PFOS 5.323 3282444 112.7346 THPFOS 5.105 1418003 254 PFOS 5.322 111688 4.096216 THPFOS 5.105 1327511 254 PFOS 5.322 4689629 190.655 THPFOS 5.087 1772997 254 ISTD>130% PFOS 5.319 178548 5.232697 THPFOS 5.091 1580363 254 ISTD>130% PFOS 5.309 143612 4.72336 THPFOS 5.09 1599960 254 ISTD>130% PFOS 5.314 73070 2.383101 THPFOS 5.098 1583275 254 ISTD>130% PFOS 5.322 3194485 106.9281 THPFOS 5.093 1507671 254 ISTD>130% PFOS 5.31 74289 2.569598 THPFOS 5.1 1613223 254 !STD>130% PFOS 5.317 73272 2.370152 THPFOS 5.099 1542538 254 ISTD>130% PFOS 5.316 125073 4.216276 THPFOS 5.098 1558630 254 tSTD>130% PFOS 5.316 3322158 113.1153 THPFOS 5.097 1638237 254 ISTD>130% PFOS 5.314 132485 4,20529 THPFOS 5.104 1636599 254 ISTD>130% PFOS 5.314 188089 5.969764 THPFOS 5.103 1485841 254 PFOS 5.313 102882 3.603134 THPFOS 5.112 1395726 254 PFOS 5.322 4803174 185,5252 THPFOS 5.093 1654266 2 54 ISTD>130% PFOS 5.31 189555 5.95208 THPFOS 5.099 1604691 254 ISTD>130% PFOS 5.316 3364843 111.2337 THPFOS 5.1 1567626 254 ISTD>130% PFOS 5.317 70689 2.353252 THPFOS 5.098 1657152 254 (STQ>13Q% PFOS 5.315 150169 4.710199 THPFOS 5.098 1628130 254 ISTD>130% PFOS 5.308 256726 8.187031 THPFOS 5.105 1586581 254 ISTD>130% PFOS 5.315 3420939 114.4608 THPFOS 5.106 1594869 254 ISTD>130% PFOS 5.316 197132 6.41957 THPFOS 5.105 1613975 254 ISTD>130% PFOS 5.315 178892 5.757917 THPFOS THPFOS 5.104 5.098 1647163 1616736 254 ISTD>130% PFOS 254 !STD>130% PFOS 5.314 88721 2.807077 5.308 3291692 107,9254 THPFOS 5.097 1495313 254 ISTD>130% PFOS 5.308 111995 3.895974 THPFOS 5.099 1408690 254 PFOS 5.309 4791463 183.2822 82% 76% 72% 74% 78% 73% page 3 of 3 3M Environmental Laboratory Sample Batch R010404.b, analyzed on H illary 04-04-01. PFOS Adsorb/Desorb samples. M atrix: Soil/SIg/Sed. Standard curve range used fo r calibration o f sam ples: 10-1002 ng/mL Batch m ethod: R010404.m {External Standard Quant) Inj Date Batch 4/4/01 17:33 D:\Chem\Rush\R010404.b 4/4/01 17:48 D:\Chem\Rush\R010404.b 4/4/01 18:02 D:\Chem\Rush\R010404.b 4/4/01 18:16 D:\Chem\Rush\R010404.b 4/4/01 18:31 D:Chem\Rush\R010404.b 4/4/01 18:45 D \Chem\Rush\R010404.b 4/4/01 18:59 D:\Chem\Rush\R010404.b 4/4/01 19:14 D:\Chem\Rush\R010404.b 4/4/01 19:28 D:\Chem\Rush\R010404.b 4/4/01 19:43 D:\Chem\Rush\R010404.b 4/4/01 19:57 D:\Chem\Rush\R010404.b 4/4/01 20:11 0:'Chem\Rush\R010404.b 4/4/01 20:26 D:\Chem\Rush\R010404.b 4/5/01 14:08 D:\Chem\Rush\R010404.b 4/5/01 14:22 D:\Chem\Rush\R010404.b 4/5/01 14:36 D:\Chem\Rush\R010404.b 4/5/01 14:51 D:\Chem\Rush\R0104O4.b 4/5/01 15:05 D:\Chem\Rush\R010404.b 4/5/01 15:19 D:\Chem\Rush\R01Q404.b 4/5/01 15:34 D:\Chem\Rush\R010404.b 4/5/01 15:48 D:\Chem\Rush\R010404.b 4/5/01 16:03 D:\ChemiRusrtlR010404.b 4/5/01 16:17 D:\Chem\Rush\R010404.b 4/5/01 16:31 D:\Chem\Rush\R010404.b 4/5/01 16:46 D:\Chem\Rush\R010404.b 4/5/01 17:00 D:\Chem\Rush\R010404.b SampType SAMPLE CALIB_1 CALIB_2 CALIB_3 CALIB.4 SAMPLE CALIB_S CALIB_6 C A U B .7 CALIB.8 SAMPLE CAUB_9 CALIB_10 SAMPLE CALIB_11 CALIB_12 CAUBJ3 C ALIBJ4 SAMPLE CAUB_15 CALIB_16 CAUB_17 CAUB.18 SAMPLE CALIB_19 CALIB_20 File RUSH0017.D RUSH0018.D RUSH0019.D RUSH0020.D RUSH0021.D RUSH0022.D RUSH0023.D RUSH0024.D RUSH0025.D RUSH0026.D RUSH0027.D RUSH028.D RUSH0029.D RUSH0098.D RUSH0099.D RUSH0100.D RUSH0101.D RUSH0102.D RUSH0103.D RUSH0104.D RUSH0105.D RUSHQ1D6.D RUSH0107.D RUSH0108.D RUSH0109.D RUSH0110.D Sample Name O ng/mL PFOS in MeOH 2.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 10 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 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 400.8 ng/mL PFOS in MeOH S01 ng/mL PFOS in MeOH 1002 ng/mL PFOS in MeOH O ng/mL PFOS in MeOH 2.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 10 ng/mL PFOS in MeOH 2 5 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 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/mL PFOS in MeOH "D __ f'1 o '- " V In j Date Batch 4/4/01 17:05 D:\Chem\R ush\R010404.b 4/4/01 17:19 D:\Chem\Rush\R010404.b 4/4/01 20:40 D:\Chem\Rush\R01O404.b r>> 4/4/01 20:54 D:\Chem\Rush\R010404.b 4/5/01 0:01 D:\Chem\Rush\R010404.b 4/5/01 0:15 D:\Chem\Rush\R010404.b 4/5/01 3:22 O:\Chem\Rush\R010404.b r> 4/5/01 3:37 D:'Chem\Rush\R010404.b 4/5/01 6:54 D:\Chem\Rush\R010404.b 4/5/01 7:08 D:\Chem\Rush\RQ10404.b f. 4/5/01 D:\Chem\Rush\R010404.b 4/5/01 D:\Chem\Rush\R010404 b 4/5/01 D:\Chem\Rush\R010404.b 3 4/5/01 D:\Chem\Rush\R010404.b 4/5/01 D:SChem\Ru$h\R010404.b 4/5/01 D:\Chem\Rush\R010404.b 7 4/5/01 D:\Chem\Rush\R010404.b SampType SAMPLE SAMPLE 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 RUSH0045.D RUSH0058.D RUSH0059.D RUSH0072.D RUSH0073.D RUSH0086.D RUSH0087.D RUSH0095.D RUSH0096.D RUSH0097.D RUSH0111.D RUSH0112.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 Page 512 of 703 BACK TO MAIN R 0 10404 external std quant.xls M ise tnfC om p o un d N aR T Area THPFOS 5.582 THPFOS 5.579 THPFOS 5.591 THPFOS 5.595 THPFOS 5.589 THPFOS 5.587 THPFOS 5.58 THPFOS 5.588 THPFOS 5.596 THPFOS 5.589 THPFOS 5.585 THPFOS 5.588 THPFOS 5.581 THPFOS 5.574 THPFOS 5.579 THPFOS 5.581 THPFOS 5.567 THPFOS 5.573 THPFOS 5.585 THPFOS 5.578 THPFOS 5.577 THPFOS THPFOS THPFOS 5.565 5.568 5.569 THPFOS 5.564 THPFOS 5,561 Am ount 583312 254 598272 254 619609 254 603517 254 600229 254 607817 254 612230 254 620258 254 614982 254 641474 254 615846 254 625062 254 640512 254 567197 254 573134 254 587603 254 566302 254 567276 254 550302 254 571777 254 568082 254 565114 254 573872 254 560676 254 557017 254 575273 254 A ve ra ae : 591028.6538 Std D ev: 26847.71188 % RSD: 4.5% M ise In fC om po un d NaRT 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 Am ount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Com pound N aiftT 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 re a Am ount 0 00 5.789 170517 0 5.801 218580 0.060813 5.805 300075 5.9Q1514 5.792 567394 25.29359 5.79 825934 44.38921 5.79 998865 57.34862 5.799 1408399 88.63623 5.799 1740059 114.5899 5.792 3758226 284.3931 5.788 5347186 432.4344 5.798 6357305 533.1193 5.784 11034302 1065.901 0 00 5.782 147436 0 5.784 189460 O 5.777 258280 2.90194 5.783 519265 21.77576 5.788 736331 37.73328 5.781 897827 49.75867 5.787 1258308 77.07207 5.768 1578440 101.8738 5.771 3350422 248.4373 5.772 4782617 378.3862 5,767 5638078 460.9056 5.764 9804784 915 2275 768337 +30%: 413720 -30%: 1% 59% 101% 111% 114% 118% 114% 114% 108% 106% 106% 0% 29% 87% 94% 99% 103% 102% 99% 94% 92% 91% C om pound NarRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A re a 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Am ount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 page 1 o f2 Page 513 of 703 3M Environmental Laboratory in j Date Batch 4/4/0121:09 D:\Chem\Rush\R010404.b 4/4/01 21:23 D:\Chem\Rush\R010404.b 4/4/01 21:37 D:\Chem\Rush\R010404.b 4/4/01 21:52 D:\Chem\Rush\R010404.b 4/4/01 22:06 D:\Chem\Rush\R010404.b 4/4/01 22:20 D:\Chem\Rush\R010404.b 4/4/01 22:35 D:\Chem\Rush\R010404.b 4/4/01 22:49 D:\Cheffi\Rush\R010404.b 4/5/01 23:03 D:\Chem\Rush\R010404.b 4/5/01 23:18 D:\Chem\Rush\R010404.b 4/5/01 23:32 D:\Chem\Rush\R010404.b 4/5/01 23:47 D:\Chem\Rush\R010404.b 4/5/01 0:30 D:\Chem\Rush\R010404.b 4/5/01 0:44 D:\Chem\Rush\R010404.b 4/5/01 0:58 D:\Chem\Rush\R010404.b 4/5/01 1:13 D:\Chem\Rush\R010404.b 4/5/01 1:27 D:\Chem\Rush\R010404.b 4/5/01 1:42 D:\Chem\Rush\R010404.b 4/5/01 1:56 D:\Chem\Rush\R010404.b 4/5/01 2:10 D:\Chem\Rush\R010404.b 4/5/01 2:25 D:\Chem\Rush\R010404.b 4/5/01 2:39 D:\Chem\Rush\R010404.b 4/5/01 2:53 D:\Chem\Rush\R010404.b 4/5/01 3:08 D:\Chem\Rush\R010404.b 4/5/01 3:51 D:\Chem\Rush\R010404.b 4/5/01 4.06 D:\Chem\Rush\R010404.b 4/5/01 4:20 D:\Chem\Rush\R010404.b 4/5/01 4:34 D:\Chem\Rush\R010404.b 4/5/01 4:49 D:\Chem\Rush\R010404.b 4/5/01 5:03 D:\Chem\Rush\R010404.b 4/5/01 5:17 D:\Chem\Rush\R010404.b 4/5/01 5:42 D:\Chem\Rush\R010404.b 4/5/01 5:56 D:\Chem\Rusb\R010404.b 4/5/01 6:11 D:\Chem\Rush\R010404.b 4/5/01 6:25 D:\Chem\Rush\R010404.b 4/5/01 6:39 D:\Chem\Rush\R010404.b 4/5/01 7:23 DXhem\Rush\R010404.b 4/5/01 7:37 D:\Chem\Rush\R010404.b 4/5/01 7:51 D:\Chem\Rush\R010404.b 4/5/01 8:06 D:\Chem\Rush\R010404.b 4/5/01 8:20 D:\Chem\Rush\R010404.b 4/5/01 8:34 D:\Chem\Rush\R010404.b 4/5/01 8:49 D:\Chem\Rush\R010404.b 4/5/01 9:03 D:\Chem\Rush\R010404.b 4/5/01 9:18 D:\ChemtRush\R01Q404.b 4/S/01 9:32 D:\Chem\Rush\R010404.b 4/5/01 9:46 D:\Chem\Rush\R010404.b 4/5/01 10:01 DXhemVRush\RQ1Q404.b 4/5/01 10:44 D:\Chem\Rush\R010404.b 4/5/01 10:58 D:VChem\Rush\R010404.b 4/5/01 11:13 D:\Chem\Rush\R010404.b 4/5/01 11:27 D:\Chem\Rush\R010404.b 4/5/01 11:42 D:\Chem\Rush\R010404.b 4/5/01 11:56 D:\Chem\Rush\R010404.b 4/5/01 12:10 D:\Chem\Rush\R010404.b SampType File SAMPLE RUSH0032.D SAMPLE RUSH0O33.D SAMPLE RUSH0034.D SAMPLE RUSH0035.D SAMPLE RUSH0036.D SAMPLE RUSH0037.D SAMPLE RUSHQ038.D SAMPLE RUSH0039.D SAMPLE RUSH0040.0 SAMPLE RUSH0041.D SAMPLE RUSH0042.D SAMPLE RUSH0043.D SAMPLE RUSH0046.D SAMPLE RUSH0O47.D SAMPLE RUSH0048.D SAMPLE RUSH0049.D SAMPLE RUSH0050.0 SAMPLE RUSH0051.D SAMPLE RUSH0052.D SAMPLE RUSH0053D SAMPLE RUSHQ054.D SAMPLE RUSH0055.D SAMPLE RUSH0056.D SAMPLE RUSH0057.D SAMPLE RUSH0060D SAMPLE RUSHOO01.D SAMPLE RUSH0062.D SAMPLE RUSH0063.D SAMPLE RUSH0064.D SAMPLE RUSH0065.D SAMPLE RUSH0066.D SAMPLE RUSH0067.D SAMPLE RUSH0068.D SAMPLE RUSH0069D SAMPLE RUSH0070.D SAMPLE RUSH0071.D SAMPLE RUSH0074.D SAMPLE RUSH0075.D SAMPLE RUSH0076.D SAMPLE RUSH0077.D SAMPLE RUSH0078.D SAMPLE RUSH0079.D SAMPLE RUSH0080.D SAMPLE RUSH0081.D SAMPLE RUSH0082.D SAMPLE RUSH0083.D SAMPLE RUSH0084.D SAMPLE RUSH0085.D SAMPLE RUSH0088.D SAMPLE RUSH0089.D SAMPLE RUSH0090.D SAMPLE RUSH0091.D SAMPLE RUSH0092.0 SAMPLE RUSH0093.D SAMPLE RUSH0094D Sample Name Study Number EOO-1311 Study Number E00-1311 Study Number EOO-1311 Study Number E00-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number E00-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 5 ng/ml PFOS in MeOH 250.5 ng/mL PFOS in MeOH Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH Study Number E00-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number E00-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 5 ng/ml PFOS in MeOH 250.5 ng/mL PFOS in MeOH Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 5 ng/mL PFOS in MeOH 2 5 0 .5 ng/m l PFOS in MeOH Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 Study Number EOO-1311 5 ng/m l PFOS in MeOH 250 .5 ng/mL PFOS in MeOH BACK TO MAIN R0104Q4 external std quantxls Mise InfCom pound NaRT Area THPFOS 5.589 THPFOS 5.589 THPFOS 5.574 THPFOS 5.596 THPFOS 5 .5 8 THPFOS 5 .5 7 4 THPFOS 5.581 THPFOS 5.578 THPFOS 5 .5 7 9 THPFOS 5.575 THPFOS 5.575 THPFOS 5.582 THPFOS 5 .5 7 THPFOS 5 .5 8 THPFOS 5.808 THPFOS 5.586 THPFOS 5,565 THPFOS 5.587 THPFOS 5.578 THPFOS 5 .5 7 8 THPFOS 5.588 THPFOS 5.594 THPFOS 5.589 THPFOS 5.589 THPFOS 5.579 THPFOS 5.581 THPFOS 5.564 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 THPFOS 5.594 THPFOS 5.603 THPFOS 5.597 THPFOS 5.585 THPFOS 5.582 THPFOS 5.589 THPFOS 5.5B4 THPFOS 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 1033666 254 7.84276 254 797188 254 753794 254 795069 254 817236 254 868427 254 566116 254 559850 254 862542 254 787133 254 934664 254 863820 254 1126734 254 942383 254 906043 254 976478 254 1316674 254 899797 254 619700 254 583040 254 904765 254 896633 254 902426 254 896486 254 913892 254 958949 254 747595 254 953521 254 921327 254 956257 254 621485 254 591317 254 672912 254 921483 254 914616 254 929161 254 924096 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 644837 254 iSTD>130% IS T D > 1 30% ISTD>130% ISTD>130% \STD>130% ISTD130% ISTD>130% ISTD>130% ISTD>130% tSTD>130% ISTD>130% ISTD>130% ISTD>130% 1STD>130% 1STD>130% iSTD>130% 1STD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% 1STD130% ISTD>130% ISTD>130% !STD>130% iSTD>130% ISTD>130% ISTD>130% iSTD>130% 1STD>130% !STD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% ISTD>130% Com pound NanRT Area Amount PFOS 0 00 PFOS 0 00 PFOS 0 0Q PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 5.785 3653083 275.043 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 5.792 3610058 271.2329 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 5.778 2604047 184.7868 PFOS 5.845 267284 3.547403 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 5.801 3590033 269.4627 PFOS 5.792 3440014 256.2652 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 5.794 3481787 259.9287 PFOS 5.777 2772166 198.8805 PFOS 0 00 PFOS 0 00 PFOS 0 00 PFOS 6.785 2250127 155.5797 PFOS 0 00 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 3M Environmental Laboratory BACK TO MAIN Sample Batch H010329.b, analyzed on Hillary 03-29-01. PFOS Adsorb/Desorb samples. Matrix: Soil/SIg/Sed. Standard curve range used fo r calibration of samples: 5-1002 ng/mL (2.5 ng/mL std not included due to the higher sample concentration range). Batch method: H010329.m Inj Date Batch SampType 3/29/01 17:54 D:\Chem\HillaSAMPLE 3/29/01 18:09 D:\Chem\HillCAUB_1 3/29/01 18:23 D:\Chem\HillCALIBj1 3/29/01 18:38 D:\ChemtHHICAUB_2 3/29/01 18:52 D:\Chem\HillCALIB_3 3/29/01 19:06 D:\Chem\HiliaSAMPLE 3/29/01 19:21 D:\Chem\HillCALIB_4 3/29/01 19:35 D:\Chem\HillCALIB_5 3/29/01 19:49 D:\Chem\HillCALIB_6 3/29/01 20:04 D:\Chem\HiUCAUB_7 3/29/01 20:18 D:\Chem\HHICALIB_8 3/29/01 20:33 D:\Chem\HillCALIB_9 3/29/01 20:47 D:\Chem\HillCALIB_10 3/31/01 16:58 D:\Chem\HillaSAMPLE 3/31/01 17:13 D:\Chem\HillCALIB_11 3/31/01 17:27 D:\Chem\HillCALIB_11 3/31/01 17:41 D:\Chem \HillCALIB_l2 3/31/01 17:56 D:\Chem\HiH CALIB_13 3/31/01 18:10 D:\Chem\HillaSAMPLE 3/31/01 18:25 D:\Chem\HilICALIB_14 3/31/01 18:39 D:\Chem\Hill CAUB_15 3/31/01 18:53 D:\Chem\HillCALIB_16 3/31/01 19:08 D:\Chem \HillCALIB_l7 3/31/01 19:22 D:\Chem\HillCALIB_18 3/31/01 19:36 D:\Chem\HillCALIB_19 3/31/01 19:51 D:\Chem\HillCAUB_20 File Sample Name Mise InfCompouncRT Area Amount H ILL0016.D O ng/mL PFOS in THPF0S 5.098 960831 254 H1LL0017.D 2.5 ng/mL PFOS i THPFOS 5.098 970141 254 HILL0018.D 5 ng/mL PFOS in THPFOS 5.098 1088770 254 HILL0019.D 10 ng/mL PFOS i THPFOS 5.088 954633 254 HILL0020.D 25 ng/mL PFOS in THPFOS 5.093 962518 254 HILL0021.D 4 0 ng/mL PFOS in THPFOS 5.092 969520 254 HILL0022.D 50.1 ng/mL PFOS THPFOS 5.098 976505 254 HILL0023.D 75.1 ng/mL PFOS THPFOS 5.093 967966 254 HILL0024.D 100.2 ng/mL PFO THPFOS 5.094 957847 254 HILL0025.D 250.5 ng/mL PFO THPFOS 0 00 HILL0026.D 400.8 ng/mL PFO THPFOS 5.091 969149 254 HILL0027.D 501 ng/mL PFOS THPFOS 5.092 973244 254 HILL0028.D 1002 ng/mL PFOS THPFOS 5.093 1000466 254 H ILL0212.D 0 ng/m L PFOS in THPFOS 5.07 842487 254 HILL0213.D 2.5 ng/mL PFOS i THPFOS 5.077 835488 254 HILL0214.D 5 ng/mL PFOS in THPFOS 5.078 850162 254 HILL0215.D 10 ng/mL PFOS i THPFOS 5.07 814436 254 H1LL0216.D 25 ng/mL PFOS in THPFOS 5.071 813666 254 HILL0217.D 4 0 ng/mL PFOS in HILL0218.D 50.1 ng/mL PFOS THPFOS THPFOS 5.07 5.076 800797 805652 254 254 H1LL0219.D 75.1 ng/mL PFOS THPFOS 5.07 799837 254 HILL0220.D 100.2 ng/mL PFO THPFOS 5.071 789834 254 HILL0221.D 250.5 ng/mL PFO THPFOS 5.073 812044 254 HILL0222.D 400.8 ng/mL PFO THPFOS 5.079 775631 254 HILL0223.D 501 ng/mL PFOS THPFOS 5.07 783605 254 HILL0224.D 1002 ng/mL PFOS THPFOS 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 Area Amount 000 5.323 68338 0.677157 5.315 154846 3.650955 5.312 209554 6.883663 5.324 550443 22.60741 5.316 874302 37.47291 5.315 1094742 47.43103 5.317 1620491 72.81732 5.318 2093623 96.65124 000 5.316 7386300 370.5128 5.316 8910984 454.6583 5.31 17048775 934.463 000 5.308 60341 0.858561 5.302 109759 2.805341 5.301 179020 7.088001 5.295 495753 24.4548 5.294 779905 40.69347 5.294 981753 52.01963 5.294 1483559 81.31145 5.295 1929027 108.8196 5.29 4679248 272.5867 5.303 6867611 437.8109 5.288 8368086 541.0708 5.294 15279147 1050.288 73.0% 68.8% 90.4% 9 3 .7 % 94.7% 97.0% 96.5% 0.0% Sample level in Vial too low 92.4% 90.8% 93.3% 56.1% 70.9% 97.8% 102.2% 103.8% 108.3% 108.6% 68.0% 109.2% 108.0% 104.8% Average: 857280.5 Std Dev: 196200.6 %RSD: 22.9% 1114465 +30%: 600096 -30%: Page 514 of 703 CMC ' ( V sb 5 ' Co S' $ 3 =3 3 <D 5T 0) Cr O 3 S' Inj Date Batch SampType 3/29/01 17:26 D:\Chem\HillaSAMPLE 3/29/01 17:40 D:\Chem\HillaSAMPLE 3/29/01 21:01 D:\Chem\HillaSAMPLE 3/29/01 21:16 D:\Chem\HillaSAMPLE 3/29/01 21:30 D:\Chem\HillaSAMPLE 3/30/01 0:23 D:\Chem\HillaSAMPLE 3/30/01 0:37 OACfwmriiliaSAMPLE 3/30/01 3:44 D:\Chem\HitlaSAMPLE 3/30/01 3:59 O:\Chem\HillaSAMPLE 3/30/01 7:06 D:\Chem\HillaSAMPLE 3/30/01 7:20 D:\Chem\HillaSAMPLE 3/30/01 10:28 D:\ChemVHillaSAMPLE 3/30/01 10:43 D:\Chem\HillaSAMPLE 3/30/01 13:50 D:\Chem\HillaSAMPLE 3/30/01 14:05 D:\Chem\HillaSAMPLE 3/30/01 17:12 D:\ChemVHitIaSAMPLE 3/30/01 17:27 D:\ChemWilIaSAMPLE 3/30/01 20:34 D:\Chem\HiIlaSAMPLE 3/30/01 20:48 D:\Chem\HillaSAMPLE 3/31/01 23:27 O:\Chem\HillaSAMPLE 3/31/01 23:41 D:\Chem\HillaSAMPLE 3/31/01 2:48 D:\Chem\HillaSAMPLE 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:\Chem\HillaSAMPLE 3/31/01 10:00 D:\Chem\HillaSAMPLE 3/31/01 13:08 O:\Chem\HillaSAMPLE 3/31/01 13:22 D:\Chem\HillaSAMPLE 3/31/01 16:30 D:\Chem\HillaSAMPLE 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 Mise InfCompouncRT HILL0014.D TN-A 4802 MeOH THPFOS HILL0015.D TN-A 4802 MeOH THPFOS HILL0029.D TN-A 4802 MeOH THPFOS HILL0030.D TN -A 4802 MeOH THPFOS HILL0031.D TN-A 4802 MeOH THPFOS HILL0043.D TN-A 4802 MeOH THPFOS H1LL0044.D TN-A 4802 MeOH THPFOS HILL0057.D TN-A 4802 MeOH THPFOS HILL0058.D TN-A 4802 MeOH THPFOS HILL0071-D TN-A 4802 MeOH THPFOS HILL0072.D TN-A 4802 MeOH THPFOS HILL0085.D TN-A 4802 MeOH THPFOS HILL0086.D TN -A 4802 MeOH THPFOS HILL0099.D TN-A 4802 MeOH THPFOS HILL0100.0 TN-A 4802 MeOH THPFOS HILL0113.D TN-A 4802 MeOH THPFOS HILL0114.D TN-A 4802 MeOH THPFOS HILL0127.D TN-A 4802 MeOH THPFOS HILL0128.D TN-A 4802 MeOH THPFOS HILL0139.D TN-A 4802 MeOH THPFOS HILL0140.D TN-A 4802 MeOH THPFOS HILL0153.D TN-A 4802 MeOH THPFOS HILL0154.D TN-A 4802 MeOH THPFOS HILL0168.0 TN-A 4602 MeOH THPFOS HILL0169.D TN-A 4802 MeOH THPFOS HILL0182.D TN-A 4802 MeOH THPFOS HILL0183.D TN-A 4802 MeOH THPFOS HILL0196.D TN-A 4802 MeOH THPFOS HILL0197.D TN-A 4802 MeOH THPFOS HILL0210.D TN-A 4802 MeOH THPFOS HILL0211.D TN-A 4802 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 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 QT)3 (Q CD Ol Ul O o CO Owe ^l3(o{ BACK TO MAIN CompounRT Area Amount PFOS 5.392 13019 0 PFOS 000 PFOS 5.386 23896 0 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 0 00 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 000 PFOS 0 00 PFOS 000 PFOS 000 PFOS 00 0 CO m s 3' CD =3 S' rQ) Oo* Q) o "U IQU) CD CJl o> nu--+ oc-voi Inj Oate Batch SampType 3/29/01 21:45 D:\Chem\HillaSAMPLE 3/29/01 21:59 D:\Chem\HillaSAMPLE 3/29/01 22:13 O:\Chem\HillaSAMPLE 3/29/01 22:28 D:\Chem\HillaSAMPLE 3/29/01 22:42 D:\Chem\HillaSAMPLE 3/29/01 22:56 D:\Chem\HiiiaSAMPLE 3/30/01 23:11 D:\Chem\HiliaSAMPLE 3/30/01 23:25 D:\Chem\HillaSAMPLE 3/30/01 23:40 D:\Chem\HillaSAMPLE 3/30/01 23:54 D:\ChemVHillaSAMPLE 3/30/01 0:08 D:\Chem\HillaSAMPLE 3/30/01 0:52 D:\Chem\HillaSAMPLE 3/30/01 1:06 D:\Chem\HillaSAMPLE 3/30/01 1:20 D:\Chem\HillaSAMPLE 3/30/01 1:35 D:\Chem\HiilaSAMPLE 3/30/01 1:49 D:\Chem\HillaSAMPLE 3/30/01 2:04 D:\Chem\HillaSAMPLE 3/30/01 2:18 D:\Chem\HillaSAMPLE 3/30/01 2:32 D:\Chem\HiIlaSAMPLE 3/30/01 2:47 D:\Chem\HiilaSAMPLE 3/30/01 3:01 D:\Chem\HillaSAMPLE 3/30/01 3:16 D:\Chem\HillaSAMPLE 3/30/01 3:30 D:\Chem\HillaSAMPLE 3/30/01 4:13 D:\Chem\HiliaSAMPLE 3/30/01 4:28 O:\Chem\HillaSAMPLE 3/30/01 4:42 D:\Chem\HilIaSAMPLE 3/30/01 4:56 D:\Chem\HillaSAMPLE 3/30/01 5:11 D:\Chem\HillaSAMPLE 3/30/01 5:25 D:\Chem\HiliaSAMPLE 3/30/01 5:40 D:\Chem\HiilaSAMPLE 3/30/01 5:54 D:\Chem\HillaSAMPLE 3/30/01 6:08 D:\Chem\HillaSAMPLE 3/30/01 6:23 D:\Chem\HillaSAMPLE 3/30/01 6:37 O:\Chem\HillaSAMPLE 3/30/01 6:51 O:\Chem\HiltaSAMPLE 3/30/01 7:35 D:\Chem\HillaSAMPLE 3/30/01 7:49 D:\Chem\HiliaSAMPLE 3/30/01 8:03 D:\Chem\HiilaSAMPLE 3/30/01 8:18 D:\ChemVHillaSAMPLE 3/30/01 8:32 D:\Chem\HillaSAMPLE 3/30/01 8:46 D:\Chem\HiliaSAMPLE 3/30/01 9:01 D:\Chem\HillaSAMPLE 3/30/01 9:15 D:\Chem\HillaSAMPLE 3/30/01 9:30 D:\Chem\HiliaSAMPLE 3/30/01 9:45 D:\Chem\HillaSAMPLE 3/30/01 9:59 O:\Chem\HillaSAMPLE 3/30/01 10:14 D:\Chem\HillaSAMPLE 3/30/01 10:57 D:\Chem\HillaSAMPLE 3/30/01 11:12 D:\Chem\HillaSAMPLE 3/30/01 11:26 D:\Chem\HillaSAMPLE 3/30/01 11:41 D:\Chem\HillaSAMPLE 3/30/01 11:55 D:\Chem\HillaSAMPLE 3/30/01 12:09 D:\Chem\HillaSAMPLE 3/30/01 12:24 D:\Chem\HillaSAMPLE 3/30/01 12:38 D:\Chem\HillaSAMPLE 3/30/01 12:53 D:\Chem\HillaSAMPLE File Sampfe Name Mise InfCompouncR* HILL0032D 10mg/mL PFOS Study NumTHPFOS HILL0033.D 10mg/mL PFOS Study NumTHPFOS HILL0034.D 10mg/mL PFOS Study NumTHPFOS HILL0035.D 10mg/ml PFOS Study NumTHPFOS HILL0036D 50mg/mL PFOS Study NumTHPFOS HILL0037.D 50mg/mL PFOS Study NumTHPFOS HILL0038.D 50mg/mL PFOS Study NumTHPFOS HILL0039.D 50mg/mL PFOS Study NumTHPFOS HILL0040.D Omg/mL PFOS Study NumbTHPFOS H1LL0041.D 5 ng/mL PFOS in MeOH THPFOS HILL0042.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0045D Omg/mL PFOS Study NumbTHPFOS HILL0046.D Omg/mL PFOS Study NumbTHPFOS HILL0047.D Omg/mL PFOS Study NumbTHPFOS HILL0048.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0049.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0050.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0051 D 0.5mg/mL PFOS Study NuriTHPFOS HILL0052.D 2mg/mL PFOS Study NumbTHPFOS HILL0053.0 2mg/mL PFOS Study NumbTHPFOS HILL0054.D 2mg/mL PFOS Study NumbTHPFOS HILL0055.D 5 ng/mL PFOS in MeOH THPFOS HILL0056.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0059.D 2mg/mL PFOS Study NumbTHPFOS HILL0060.D 5mg/mL PFOS Study NumbTHPFOS HILL0061 D 5mg/mL PFOS Study NumbTHPFOS HILL0062.D 5mg/mL PFOS Study NumbTHPFOS HILL0063.D 5mg/mL PFOS Study NumbTHPFOS HILL0064.D 10mg/mL PFOS Study NumTHPFOS HILL0065.D 10mg/mL PFOS Study NumTHPFOS HILL0066.D 10mg/mL PFOS Study NumTHPFOS HILL0067.D 10mg/mL PFOS Study NumTHPFOS HILL0068.D 50mg/mL PFOS Study NumTHPFOS HILL0069.D 5 ng/mL PFOS in MeOH THPFOS HILL0070.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0073.D 50mg/mL PFOS Study NumTHPFOS HILL0074.D 50mg/mL PFOS Study NumTHPFOS HILL0075.D 50mg/mL PFOS Study NumTHPFOS HILL0076.D Omg/mL PFOS Study NumbTHPFOS HILL0077.D Omg/mL PFOS Study NumbTHPFOS HILL0078.D Omg/mL PFOS Study NumbTHPFOS HILL0079.D Omg/mL PFOS Study NumbTHPFOS HILL0080.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0081.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0082.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0083.D 5 ng/mL PFOS in MeOH THPFOS HLL0084.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0087.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0088.D 2mg/mL PFOS Study NumbTHPFOS HILL0089D 2mg/mL PFOS Study NumbTHPFOS HILL0090.D 2mg/mL PFOS Study NumbTHPFOS HILL0091.D 2mg/mL PFOS Study NumbTHPFOS HILL0092.D 5mg/mL PFOS Study NumbTHPFOS HILL0093.D 5mg/mL PFOS Study NumbTHPFOS HILLX94.D 5mg/mL PFOS Study NumbTHPFOS HILL0095.D 5mg/mL PFOS Study NumbTHPFOS BACK TO MAIN Area Amount 5.092 941565 254 5.092 955051 254 5.091 947677 254 5.093 777892 254 5.085 1089404 254 5.083 1090640 254 5.084 1030788 254 5.077 1073111 254 5.085 918338 254 5.085 1091788 254 000 5.091 893965 254 5.086 871748 254 5.092 746435 254 5.092 887622 254 5.085 872024 254 5.083 867832 254 5.091 727915 254 5.083 854851 254 5.083 857430 254 5.09 854499 254 000 000 5.084 749219 254 5.084 876417 254 5.077 906862 254 5.085 901113 254 5.084 766376 254 5.086 913312 254 5.086 973798 254 5.079 911827 254 5.083 781459 254 5.088 979507 254 000 000 5.079 967155 254 5.084 990636 254 5.077 924192 254 5.076 868541 254 5.084 862422 254 5.085 848676 254 5.083 712693 254 5.077 830763 254 5.084 838359 254 5.087 817463 254 000 000 5.083 723549 254 5.086 829574 254 5.08 810539 254 5.078 813653 254 5.077 698202 254 5.072 870788 254 5.077 833403 254 5.078 865160 254 5.078 732175 254 -ISTP*7Q% . . . - IS T D < 7 0 % IS T D < 7 0 % .. . IS T P *7 0 % -IS T P * 7 0 % ISTP*7Q% IS T D 7 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 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area A m ount 5.317 7685289 399.8253 5.316 8722101 453.3549 5.315 7434958 382.6097 5.31 9661038 643.6158 5.302 5246893 224.4704 5.308 5197203 221.9073 5.308 4771646 215.0835 5.301 9471261 436.3103 5.309 540709 23.3661 5.302 162150 3.734831 000 5.315 126502 3.424213 5.31 88651 1.66155 5.316 3303886 204.9582 5.316 620867 28.34021 5.309 520023 23.70488 5.307 582795 27.08401 5.308 3691790 237.353 5.307 2353605 123.4773 5.307 2593339 136.4485 5.314 2562398 135.2093 000 000 5.308 5345747 344.4726 5.308 1620046 80.90241 5.301 1503995 72.09314 5.309 1497426 72.24531 5.301 4532655 280.4432 5.303 3057247 152.0074 5.31 3260951 152.0686 5.303 3051917 151.9884 5.307 5989063 372.804 5.312 2234423 101.1328 00 0 00 0 5.296 1999273 91.09713 5.301 1896764 83.9824 5.294 5706884 293.9526 5.307 199968 7.359762 000 00 0 5.3 3185982 207.1555 5.295 2350237 127.0906 5.309 1735740 91.24829 5.311 2751710 152.9141 000 00 0 5.314 5581843 375.5325 5.303 7796382 468.2081 5.297 7782923 479.6898 529 5 7488962 457.3479 5.301 9920061 752.9404 5.297 4681978 252.8436 5.294 4589661 259.5041 5.302 4617034 250.8006 5.302 7091269 484.3771 74.7% 0.0% Sam ple level !n V ial to o lo w 0.0% Sam ple level In Vial to o low 0.0% Sam ple level In V ial to o low 0.0% Sam ple level in Vial to o low 0.0% Sam ple level in V ial to o low 0.0% Sam ple level in Vial to o low 0.0% Sam ple level in V ial to o low Cm c 1 (3 | o ' p c 3 k S' ' (5 3M Environmental Laboratory 3/30/01 13:07 D:\Chem\HillaSAMPLE 3/30/01 13:21 D:\Chem\HillaSAMPLE 3/30/01*13:36 D:\Chem\HillaSAMPLE 3/30/01 14:19 D:\Chem\HillaSAMPLE 3/30/01 14:34 D:\Chem\HillaSAMPLE 3/30/01 14:48 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\HiliaSAMPLE 3/30/01 15:46 D:\Chem\HillaSAMPLE 3/30/01 16:00 D:\ChemVHillaSAMPLE 3/30/01 16:15 O:\Chem\HillaSAMPLE 3/30/01 16:29 D:\Chem\HillaSAMPLE 3/30/01 16:43 D:\Chem\HillaSAMPLE 3/30/01 16:58 D:\Chem\HillaSAMPLE 3/30/01 17:41 D:\Chem\HillaSAMPLE 3/30/01 17:56 D:\Chem\HillaSAMPLE 3/30/01 16:10 D:\Chem\HiliaSAMPLE 3/30/01 18:24 D:\Chem\HillaSAMPLE 3/30/01 18:39 D:\Chem\HillaSAMPLE 3/30/01 18:53 D:\Chem\HillaSAMPLE 3/30/01 19:08 D:\Chem\HilfaSAMPLE 3/30/01 19:22 D:\Chem\HillaSAMPLE 3/30/01 19:36 D:\Chem\HillaSAMPLE 3/30/01 19:51 D:\Chem\HillaSAMPLE 3/30/01 20:05 0 AChemVHillaSAMPLE 3/30/01 20:20 D:\Chem\HillaSAMPLE 3/30/01 21:03 D:\Chem\HiIlaSAMPLE 3/30/01 21:17 D:\Chem\HillaSAMPLE 3/30/01 21:32 O:\Chem\HillaSAMPLE 3/30/01 21:46 D:\Chem\HillaSAMPLE 3/30/01 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\HillaSAMPLE 3/31/01 23:12 D:\Chem\HillaSAMPLE 3/31/01 23:56 D:\Chem\HillaSAMPLE 3/31/01 0:10 O:\Chem\HillaSAMPLE 3/31/01 0:24 D:\Chem\HillaSAMPLE 3/31/01 0:39 D:\Chem\HillaSAMPLE 3/31/01 0:53 D:\Chem\HillaSAMPLE 3/31/01 1.08 D:\Chem\HiliaSAMPLE 3/31/01 1:22 D:\Chem\HillaSAMPLE 3/31/01 1:36 D:\Chem\HillaSAMPLE 3/31/01 1:51 D:\Chem\HillaSAMPLE 3/31/01 2:05 D:\Chem\HillaSAMPLE 3/31/01 2:20 D:\Chem\HilIaSAMPLE 3/31/01 2:34 D:\Chem\HillaSAMPLE 3/31/01 3:17 D:\Chem\HillaSAMPLE 3/31/01 3:32 D:\Chem\HillaSAMPLE 3/31/01 3:46 D:\Chem\HillaSAMPLE 3/31/01 4:00 D:\Chem\HillaSAMPLE 3/31/01 4:15 D:\Chem\HillaSAMPLE 3/31/01 4:29 D:\Chem\HillaSAMPLE 3/31/01 4:44 D:\Chem\HillaSAMPLE 3/31/01 4:58 DAChemtHiilaSAMPLE 3/31/01 5:12 D:\Chem\HillaSAMPLE 3/31/01 5:27 DACherrAHillaSAMPLE HILL0096 D 10mg/mLPFOS Study NumTHPFOS HILL0097.D 5 ng/mL PFOS in MeOH THPFOS HILL0098.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0101.D 10mg/ml PFOS Study NumTHPFOS HILL0102.D 10mg/mL PFOS Study NumTHPFOS HILL0103.D 10mg/mL PFOS Study NumTHPFOS HILL0104.D 50mg/mL PFOS Study NumTHPFOS HILL0105.D 50mg/mL PFOS Study NumTHPFOS HILL0106.D 50mg/mL PFOS Study NumTHPFOS HILL0107.D 50mg/mL PFOS Study NumTHPFOS HILL0108.D Omg/mL PFOS Study NumbTHPFOS HILL0109.D Omg/mL PFOS Study NumbTHPFOS H1LL0110.D Omg/mL PFOS Study NumbTHPFOS HILL0111 .D 5 ng/mL PFOS in MeOH THPFOS HILL0112 D 250.5 ng/mL PFOS in MeOTHPFOS HILL0115.D Omg/mL PFOS Study NumbTHPFOS HILL0116.D 0.5mg/mL PFOS Study NuriTHPFOS H1LL0117.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0118.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0119.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0120.D 2mg/mL PFOS Study NumbTHPFOS HILL0121.D 2mg/mL PFOS Study NumbTHPFOS HILL0122.D 2mg/mL PFOS Study NumbTHPFOS HILL0123.D 2mg/mL PFOS Study NumbTHPFOS HILL0124.D 5mg/mL PFOS Study NumbTHPFOS HILLQ125.D 5 ng/mL PFOS in MeOH THPFOS HILL0126.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0129.D 5mg/mL PFOS Study NumbTHPFOS HILL0130.D 5mg/mL PFOS Study NumbTHPFOS HILL0131.D 5mg/mL PFOS Study NumbTHPFOS HILL0132.D 10mg/mL PFOS Study NumTHPFOS HILL0133.D 10mg/mL PFOS Study NumTHPFOS HILL0134.D 10mg/mL PFOS Study NumTHPFOS HILL0135.0 10mg/mL PFOS Study NumTHPFOS HILL0136.D 50mg/mL PFOS Study NumTHPFOS HILL0137.D 5 ng/mL PFOS in MeOH THPFOS HILL0138.0 250.5 ng/mL PFOS in MeOTHPFOS HILL0141.D 50mg/mL PFOS Study NumTHPFOS HILL0142.D 50mg/mL PFOS Study NumTHPFOS HILL0143.D 50mg/mL PFOS Study NumTHPFOS HILL0144.D Omg/mL PFOS Study NumbTHPFOS HILL0145.D Omg/mL PFOS Study NumbTHPFOS HILL0146.D Omg/mL PFOS Study NumbTHPFOS HILL0147.D Omg/mL PFOS Study NumbTHPFOS HILL0148.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0149.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0150.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0151.D 5 ng/mL PFOS in MeOH THPFOS HILL0152.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0155.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0156.0 2mg/mL PFOS Study NumbTHPFOS HILL0157.D 2mg/mL PFOS Study NumbTHPFOS HILL0158. D 2mg/mL PFOS Study NumbTHPFOS HILL0159.D 2mg/mL PFOS Study NumbTHPFOS HILL0160.D 5mg/mL PFOS Study NumbTHPFOS HILL0161.D 5mg/mL PFOS Study NumbTHPFOS HILLQ162.0 5mg/mL PFOS Study NumbTHPFOS HILL0163.D 5mg/mL PFOS Study NumbTHPFOS HILL0164.D 10mg/mL PFOS Study NumTHPFOS 507 5.07 5.07 5.075 5.07 5.07 5.083 5.076 5.081 5.071 5.079 5.084 5.063 5.079 5.071 5.084 5.085 5.077 5.085 5.079 5.084 5.077 5.071 5.077 5.078 5.085 5.076 5.078 5.077 5.075 5.07 5.069 5.078 5.077 5.077 5.077 5.084 5.078 5.077 5.077 5.07 5.07 0 0 0 0 5.059 5.077 5.07 5.063 5.057 0 5.055 5.055 5.062 5.07 5.069 5.07 5.071 871278 1031178 935555 877270 893385 742701 907624 931206 919670 796555 849151 829076 621979 913364 935372 706581 624542 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 1127307 1057386 1222595 1394294 0 1405167 1264058 1123797 117X21 1140248 892226 1049855 Page 517 of 703 CmC BACK TO MAIN 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 254 PFOS 254 . PFOS 254 sm*430% PFOS 254 sm*430% PFOS 0 ISTD<70% PFOS 0 ISTPr70% PFOS 0 lSTD*-70% PFOS 0 ISTP'70% PFOS 254 sm*430% PFOS 254 sm*430% PFOS 254 . PFOS 254 ISTP*13Q% PFOS 254 sm*430% PFOS 0 STP*7Q% PFOS 254 sm>430% PFOS 254 1STO* 130% PFOS 254 sm*430% PFOS 254 sm*430% PFOS 254 sm*430% PFOS 254 . PFOS 254 - PFOS 5.294 8976434 519.4978 5.287 165503 4.265778 5.287 4930244 247.4028 5.292 12899537 783 9937 5.294 13256112 792.4273 5.287 15131931 1161.188 5.307 5518080 289.0022 5.308 5108086 258.3954 5.298 5181946 266.0334 5.296 7665976 480.9168 5.311 742763 36.24765 5.301 183483 6.963474 5.307 107928 2.972255 5.303 119662 2.959401 5.288 4919934 246.8948 5.308 3248594 213.5081 5.302 1502753 79.69637 5.294 1724356 93.22899 5.302 1736346 94.96021 5.303 4688064 321.3717 5.308 5634498 344.8627 5.295 5717625 340.7597 5.295 5974646 365.0473 5.301 8405232 636.3714 5.302 3725697 203.7979 5.309 122088 3.167352 5.307 4879273 250.0647 5.309 3516962 187.7001 5.294 3677170 194.5103 5.299 6262922 422.2447 5.294 6519410 371.3232 5.3 6622791 371.1742 5.302 6587808 389.7087 5.301 8780758 645.3465 5.301 3555043 183.2667 5.301 121133 2.821811 5 308 4866574 245.2477 5.295 3499027 178.2918 5.288 3507729 179.6005 5.294 6226527 387.1451 5.294 607465 14.93697 5.294 161015 1.850082 5.283 102458 0 5.294 2813295 0 5.288 123415 0 5.286 245088 0 5.283 154022 2.107086 5.301 104248 1.253723 5.294 4570480 199.7993 5.294 2934417 106.7379 5.288 298977 6.657971 5.295 308066 0 5.286 261303 5.394641 5.286 3012214 105.9273 5.294 256463 7.269909 5.301 268126 7.312199 5.293 138591 2.540176 5.294 3214850 164.426 5.295 12043940 587 354 85.3% 98.8% 59.2% 98.6% 63.3% 99.8% 56.4% 97.9% 25.1% 79.8% A l s i cm ^ Page 518 of 703 3M Environmental Laboratory 3/31/01 5:41 D:\Chem\HillaSAMPLE 3/31/01 5:56 D:\Chem\HillaSAMPLE 3/31/01 6:10 D:\Chem\HillaSAMPLE 3/31/01 6:53 D:\Chem\HillaSAMPLE 3/31/01 7:08 D:\Chem\HillaSAMPLE 3/31/01 7:22 D:\Chem\HillaSAMPLE 3/31/01 7:36 D:\Chem\HitlaSAMPLE 3/31/01 7:51 D:\Chem\HillaSAMPLE 3/31/01 8:05 DAChem\Hi!laSAMPLE 3/31/01 8:20 D:\Chem\HillaSAMPLE 3/31/01 8:34 D:\Chem\HillaSAMPLE 3/31/01 8:48 D:\Chem\HillaSAMPLE 3/31/01 9:03 D:\Chem\HillaSAMPLE 3/31/01 9:17 D:\Chem\HiilaSAMPLE 3/31/01 9:32 O:\Chem\HUIaSAMPLE 3/31/01 10:15 D:\Chem\HillaSAMPLE 3/31/01 10:29 D:\Chem\HillaSAMPLE 3/31/01 10:44 D:\Chem\HillaSAMPLE 3/31/01 10:58 D:\Chem\HillaSAMPLE 3/31/01 11:13 D:\Chem\HillaSAMPLE 3/31/01 11:27 D:\Chem\HillaSAMPLE 3/31/01 11:41 D:\Chem\HillaSAMPLE 3/31/01 11:56 D:\Chem\HitlaSAMPLE 3/31/01 12:10 D:\Chem\HillaSAMPLE 3/31/01 12:25 D:\Chem\HillaSAMPLE 3/31/01 12:39 D:\Chem\HillaSAMPLE 3/31/01 12:53 D:\Chem\HillaSAMPLE 3/31/01 13:37 D:\Chem\HillaSAMPLE 3/31/01 13:51 D:\Chem\HillaSAMPLE 3/31/01 14:05 D:\Chem\HillaSAMPLE 3/31/01 14:20 D:\Chem\HiIlaSAMPLE 3/31/01 14:34 D:\Chem\HillaSAMPLE 3/31/01 14:49 D:\Chem\HillaSAMPLE 3/31/01 15.03 D:\Chem\HiHs6AMPLE 3/31/01 15:17 D:\Chem\HillaSAMPLE 3/31/01 15:32 D:\Chem\HillaSAMPLE 3/31/01 15:46 D:\Chem\HillaSAMPLE 3/31/01 16:01 O:\Chem\HillaSAMPLE 3/31/01 16:15 D:\Chem\HillaSAMPLE HILL0165.D 10mg/mL PFOS Study NumTHPFOS HILL0166.D 5 ng/mL PFOS in MeOH THPFOS HILL0167.D 250.5 ng/mL' PFOS in MeOTHPFOS HILL0170.D 10mg/mL PFOS Study NumTHPFOS HILL0171.D 10mg/mL PFOS Study NumTHPFOS HILL0172.D 50mg/mL PFOS Study NumTHPFOS HILL0173.D 50mg/mL PFOS Study NumTHPFOS HILL0174.D 50mg/mL PFOS Study NumTHPFOS HILL0175.D 50mg/mL PFOS Study NumTHPFOS HILL0176.D Omg/mL PFOS Study NumBTHPFOS HILL0177.D Omg/mL PFOS Study NumbTHPFOS HILL0178.D Omg/mL PFOS Study NumS'HPFOS H1LL0179.0 Omg/mL PFOS Study NumbTHPFOS HILL0180.D 5 ng/mL PFOS in MeOH THPFOS HU.L0181.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0184D 0.5mg/mL PFOS Study NuriTHPFOS HILL0185.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0186.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0187.D 0.5mg/mL PFOS Study NuriTHPFOS HILL0188.D 2mg/mL PFOS Study NumbTHPFOS HILL0189.D 2mg/mL PFOS Study NumbTHPFOS HILL0190.D 2mg/mL PFOS Study NumbTHPFOS HILL0191.D 2mg/mL PFOS Study NumbTHPFOS HILL0192.D 5mg/mL PFOS Study NumbTHPFOS HILL0193D 5mg/mL PFOS Study NumbTHPFOS HILL0194.D 5 ng/mL PFOS in MeOH THPFOS HILL0195.D 250.5 ng/mL PFOS in MeOTHPFOS HILL0198.D 5mg/mL PFOS Study NumbTHPFOS HILL0199.D 5mg/mL PFOS Study NumbTHPFOS HILL0200.D 10mg/mL PFOS Study NumTHPFOS HILL0201.D 10mg/mL PFOS Study NumTHPFOS HILL0202.D 10mg/mL PFOS Study NumTHPFOS HILL0203.0 10mg/mL PFOS Study NumTHPFOS HILL0204.D 50mg/mL PFOS Study NumTHPFOS HILL0205.D 50mg/mL PFOS Study NumTHPFOS HILL0206.D 50mg/mL PFOS Study NumTHPFOS HILL0207.D 50mg/mL PFOS Study NumTHPFOS HILL020S.D 5 ng/mL PFOS in MeOH THPFOS HILL0209.D 250.5 ng/mL PFOS in MeOTHPFOS 5.07 5.077 5.078 5.078 5.062 5.077 5.073 5.078 5.078 5.07 0 5.077 5.07 5.077 5.077 0 0 5.071 0 0 0 5.056 5.056 5.057 5.072 5.055 5.062 5.07 5.074 5.077 5.071 5.077 5.077 5.077 5.084 5.077 5.078 5.077 5.07 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 938013 1005094 1020410 970721 844704 937393 900666 BACK TO MAIN 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 ISTORI 30% PFOS 0 ISTP-7Q/ PFOS 254 ISTPM3Q% PFOS 254 ISTORI 3Q% PFOS 254 JSTO*130% PFOS 254 ISTPM30% PFOS 0 1STD*70% PFOS 0 tSTPr7Q% PFOS 254 <STP~130% PFOS 0 <STP'70% PFOS 0 1STD*'7Q% PFOS 0 iSTP*'70% PFOS 254 ISTORI 30% PFOS 254 1SI-CM30% PFOS 254 ISTP*130% PFOS 254 <STP~13Q% PFOS 254 ISTORI 30% PFOS 254 ISTP~>130% PFOS 254 <STP^130% PFOS 254 - PFOS 254 1STP>130% PFOS 254 ISTORI 3Q% PFOS 254 ISTP~130% PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 5.294 7942166 375.6283 5.301 113187 1.95061 5.302 4685914 227.378 5.302 11897888 624.6515 5.294 13471666 947.5747 5.294 547258 25.40056 5.297 371026 16.58928 5.302 502489 20.4758 5.309 3544102 236.9754 000 5.3 15403 0 000 5.294 2562313 83.98912 000 5.301 4581504 169.9125 5.296 106080 0 5.296 88413 0 000 5.294 2763394 0 5.294 243781 0 5.288 191714 0 5.287 184484 2.736832 5.288 2856662 98.17581 5.288 314686 8.279809 5.289 267523 6.849741 0 00 5.286 4563196 169.0775 5.294 1B8759 4.143137 5.298 3245571 157.0094 5.301 335088 9.90566 5.302 525297 17.37075 5.301 550957 18.36785 5.301 3645184 178.2599 5.294 256482 8.468139 5.301 233790 7.309995 5.309 231102 7.707909 5.302 3674257 201.1561 5.295 112408 2.468054 5.294 4662409 242.609 39.0% 90.8% 0.0% 67.8% 0.0% 67.5% 49.4% 96.8% One 4 i 3 ? f ^ 56^> 3M Environmental Laboratory BACK TO MAIN Batch Sample List; Curve and Calibration Checks Acquistion Jnstrument/Sequence: HiHary/H010319(a) D ate/A nalystof Reprocessing: 0 2 A p r 0 1 / M L A Batch Method: R010319a.m "" Quantitation Range: 2.5 to 1002 ng/m L Inj Date Batch SampType File Sam ple Name Mise. Info. Com pound Name RT Area A m ount Com pound Name RT Area A m ount Theoretical 3/19/2001 20:05 3/19/2001 20:19 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 22:00 3/19/2001 22:14 3/19/2001 22:28 3/19/2001 22:43 3/20/2001 2:04 3/20/2001 2:18 3/20/2001 5:11 3/20/2001 5:25 3/20/2001 8:32 3/20/2001 8:47 3/20/2001 11:25 3/20/2001 11:39 3/20/2001 14:18 3/20/2001 14:32 C :\C H E M \H il la ry .i\ H 0 1 0 3 1 9 -a .b C:\CHEM\Hiiiary.i\H0103l9-a.b C :\C H E M \H il la ry .t\H 0 1 0 3 1 9 -a .b C:\CHEM\Hillary.i\H010319-a.b C:\CHEMVHillary.i\H010319-a.b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9 - a .b C : \ C H E M \H il la ry .f\H 0 1 0 3 1 9 -a .b C :\CHEM\Hillary\ i\H 010319-a. b C :\C H E M \H il la r y .i\ H 0 1 0 31 9 -a .b C :\C H E M \H il la ry .i\ H 0 1 0 3 1 9 -a .b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9 - a .b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9-a .b C:\CHEM\Htllary.i\H010319-a.b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9 - a .b C : \C H E M \H il la ry .i\ H 0 1 0 3 1 9 -a .b C : \C H E M \H il la ry .i\ H 0 1 0 3 1 9 -a .b C:\CHEM\Hillary.i\H010319-a. b C :\C H E M \H il la ry .t\H 0 1 0 3 1 9 -a .b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9 - a .b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9-a .b C :\C H E M \H illary .i\H 01 0 3l9 -a .b C :\C H E M \H il la r y .i\ H 0 1 0 3 1 9 - a .b C A LIB J CALIB_2 CALIB_3 C A LIB J CALIB 5 CALIB_6 CALIB_7 CALIB_8 CALIB_9 C A LIB J 0 C A LIB J 1 CALIB_12 C C A L IB J CCALIB_1 C C A L IB J CCALIB_1 CCAUBJ CCALIB_1 C C A L IB J C C A L IB J C C A L IB J C C A L IB J HILL0017.D HILL0018.D HILL0019.D HILL0020.D HILL0021.D HILL0022.D HILL0023.D HILL0024.D HILL0025.D HILL0026.D HILL027.D HLL0028.D HILL0042.D HILL0043.D HILL0055.D H1LL0056.D H H L 0 6 9 .D HILL0070.D HILL0081.D HILL0082.D H1LL0093.D HILL0094.D 2.5 ng/mL PFOS in MeOH 5 ng/mL PFOS in MeOH 10 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 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/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 P F O S 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 01003-07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-13 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 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 A verage Area: S td Dev: %RSD: 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 897103 6 7 4 2 4 .5 8% 952704 958659 946379 954921 955330 958316 961545 961218 963600 945005 937041 930802 869312 865137 854600 852353 828170 821673 792949 787755 795135 793444 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 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 63092 108976 207712 553295 871355 1084605 1595162 2149447 5065486 7558280 9061046 15880052 107823 4962586 104397 4950256 111868 4958647 108119 4876204 111428 4914110 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 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% t0To)D CD cn to o --t i Uo> 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Desorb BACK TO MAIN 3M Environmental Laboratory Batch Sample List: Samples Only Acquistion Instrument/Sequence: HiUary/H010319(a) Date/Analyst o f Reprocessing: Q2 A p r 01 / M LA Batch Method: R010319a.m Quantitation Range: 2.5 to 1002 ng/m L In] Date 3/19/2001 23:40 3/19/2001 23:54 3/20/2001 0:09 3/20/2001 0:23 3/20/2001 0:38 3/20/2001 0:52 3/20/2001 1:06 3/20/2001 1:21 3/20/2Q01 1:35 3/20/2001 1:49 3/20/2001 3:01 3/20/2001 3:16 3/20/2001 3:30 3/20/2001 3:44 3/20/2001 3:59 3/20/2001 4:13 3/20/2001 4:28 3/20/2001 4:42 3/20/2001 4:56 3/20/2001 6:08 3/20/2001 6:23 3/20/2001 6:37 3/20/2001 6:51 3/20/2001 7:06 3/20/2001 7:20 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 10:56 3/20/2001 11:11 3/20/2001 12:23 3/20/2001 12:37 3/20/2001 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 B a tc h C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hiliary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C :\C H E M \H illa ry.i\H 0 1 0 3 1 9 -a .b C :\C H E M \H illa ry.i\H 0 1 0 3 1 9-a.b C :\C H E M \H illa iy .i\H 0 1 0 3 1 9 -a .b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hiflary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C :\C H E M \H illa ry .i\H 0 1 0 3 l9 -a .b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\HilIary.iVH010319-a.b C:\CHEM\Hiilary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.iVH010319-a.b C:\CHEM\Hillary.i\H010319-a.b C :\C H E M \H ilta ry .i\H 0 1 0 3 l9 -a .b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hiflary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\HilIary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C :\C H E M \H illa ry .t\H 0 1 0 3 l9 -a .b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C :\C H E M \H illa ry ,i\H 0 10319-a.b C:\CHEM\HiIlary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b C :\C H E M \H illa ry.i\H 0 1 0 3 1 9 -a .b C:\CHEM\Hillary.i\H010319-a.b C:\CHEM\Hillary.i\H010319-a.b S am pT ype File Sample Name SAMPLE HILLO032.D 1311-4124-S2 SAMPLE HILLO033.D 1311-4125-S2 SAMPLE HILL0034.D 1311-4126-S2 SAMPLE HILLO035.D 1311-4148-S2 SAMPLE HILL0036.D 131-4149-S2 SAMPLE HILL0037.D 1311-4150-S2 SAMPLE HILLO038.D 1311-4124-S3 SAMPLE HILL0039.D 1311-4124-S3 SAMPLE HILL0040.D 1311-4126-S3 SAMPLE HILL0041.D 1311-4148-S3 SAMPLE HILL0046.D 1311-4149-S3 SAMPLE HILLO047.D 1311-4150-S3 SAMPLE HILL0048.D 1311-4124-S4 SAMPLE HILLO049.D 1311-4125-S4 SAMPLE HILL0050.D 1311-4148-S4 SAMPLE HILL0051.D 1311-4149-S4 SAMPLE HILL0052.D 1311-4150-S4 SAMPLE H1LL0053.D 1311-4124-S5 SAMPLE HILL0054.D 1311-4125-S5 SAMPLE HILL0059.D 1311-4126-S5 SAMPLE HILLD060.D 1311-4148-S5 SAMPLE HILLQ061.D 1311-4149-S5 SAMPLE HILL0062.D 1311-4150-S5 SAMPLE HILL0063.D 1311-4124-S6 SAMPLE HILL0064.D 1311-4125-S6 SAMPLE HILL0065.D 1311-4126-S6 SAMPLE HILL0066.D 1311-4126MS-S6 SAMPLE HILL0067.D 1311-4148-S6 SAMPLE HILL0068.D 1311-4149-S6 SAMPLE HILL0073.D 1311-4150-S6 SAMPLE HILL0074.D 1311-4150MS-S6 SAMPLE HILL0075.D 1311-4124-S7 SAMPLE HILL0076.D 1311-4125-S7 SAMPLE HILL0077.D 1311-4126-S7 SAMPLE HILL0078.D 1311-4148-S7 SAMPLE HILL0079.D 1311-4149-S7 SAMPLE HILL0080.D 1311-4150-S7 SAMPLE HILL0085.D 1311-4124-S8 SAMPLE HILL0086.D 1311-4125-S8 SAMPLE H1LLO087.D 1311-4126-S8 SAMPLE HILL0088.D 1311-4126MS-S8 SAMPLE HILL0089.D 1311-4148-S8 SAMPLE HILL0090.D 1311-4149-S8 SAMPLE HILL0091.D 1311-4150-S8 SAMPLE HILL0092.D 1311-4150MS-S8 C om pound Name 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 4.97 4.97 4.97 4.97 4.97 4.97 4.97 4.98 4.97 4.98 4.97 4.98 4.98 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 5.20 5.20 5,25 5.20 5,20 5.19 5.20 5.20 5.21 5.20 5.20 5.20 5.21 5.21 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 Am ount 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 78 0 212.6 1.4 0.0 1.4 72.9 63.0 79.4 1.6 1.1 1.0 235.6 59.1 64.6 64.2 298.1 2.4 1.6 4.5 60.4 63.2 71.4 1.8 2.5 1.5 236.3 58.6 62.8 36.4 296.8 3M Environmental laboratory E00-1311 PFOS Adsorb/Desorb Page 520 of 703 3M Environmental Laboratory BACK TO MAIN Batch Sample List: Methanol Blanks Acquistion Instrument/Sequence: Hillary/H010319(a) Date/Analyst of Reprocessing: 02 Apr 01 / MLA Batch Method: R010319a.m Quantitation Range: 2.5 to 1002 ng/mL Inj Date Batch SampType File Sample Name 3/19/2001 19:22 C:\CHEM\Hiilary.i\H010319-a.b SAMPLE HILL0014.D TN-A 4802 MeOH 3/19/2001 19:36 C:\CHEM\Hillary.i\H010319-a.b SAMPLE H1LL0015.D TN-A 4802 MeOH 3/19/2001 22:57 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0029.D TN-A 4802 MeOH 3/19/2001 23:11 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0030.D TN-A 4802 MeOH 3/19/2001 23:26 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0031.D TN-A 4802 MeOH 3/20/2001 2:33 C:\CHEM\Hiliary.i\H010319-a.b SAMPLE HILL0044.D TN-A 4802 MeOH 3/20/2001 2:47 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0045.D TN-A 4802 MeOH 3/20/2001 5:40 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0057.D TN-A 4802 MeOH 3/20/2001 5:54 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0058.D TN-A 4802 MeOH 3/20/2001 9:01 C:\CHEM\Hillary.l\H010319-a.b SAMPLE HILL0071.D TN-A 4802 MeOH 3/20/2001 9:15 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0072.D TN-A 4802 MeOH 3/20/2001 11:54 C:\CHEM\Hillary.l\H010319-a.b SAMPLE HILL0083.D TN-A 4802 MeOH 3/20/2001 12:08 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0084.D TN-A 4802 MeOH 3/20/2001 14:47 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0095.D TN-A 4802 MeOH 3/20/2001 15:01 C:\CHEM\Hillary.i\H010319-a.b SAMPLE HILL0096.D TN-A 4802 MeOH Compound Name RT Area Amount Compound Name RT Area Amount THPFOS 00 0 PFOS 5.22 14278 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 5.21 27267 0 THPFOS 00 0 PFOS 5.25 11603 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 THPFOS 00 0 PFOS 0.00 0 0 Page 521 of 703 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Page-6-M BACK TO MAIN 3M Environmental Laboratory Batch S am ple List: Curve and C alibration Checks A cq u 'isBon In stnJm ent/S equence: R u s h / R010312__________________________ D a te /A n a lyst o f R e processing: 27-28 M a r 01 / M LA _________________________ B atch M e thod: R 0 10312.m __________________________________________________ Q uantitation Range: 5 to 501 ng/m L, Q u a d ra tic fit, In te rn a l S ta ndard Q u a n t Inj Date Batch SampType File Sample Name .-1tja1*ISAA* A AAA A*9 3/13/200"! 12:59 3/13/2001 13:10 3/13/2001 13:21 3/13/2001 13:33 3/13/2001 13:44 3/13/2001 13:55 3/13/2001 14:07 3/13/2001 14:18 3/13/2001 14:29 3/13/2001 14:41 3/13/2001 17:08 3/13/2001 17:19 3/13/2001 19:47 3/13/2001 19:58 3/13/2001 22:26 3/13/2001 22:37 3/14/2001 1:05 3/14/2001 1:16 3/14/2001 3:44 3/14/2001 3:55 3/14/2001 6:23 3/14/2001 6:34 3/14/2001 9:02 3/14/2001 9:14 3/14/2001 11:07 3/14/2001 11:18 C :\C H E M \R ush.i\R 0l0312.b C :\CHEM \Rush.i\R010312. b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \RushJ\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C :\C H E M \R u sh .i\R 0 1 0 3 12.b C :\C H E M V R ush.i\R 010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C :\C H EM \R ush.i\R 0l0312.b C :\C H E M \R u sh ,i\R010312 .b C :\CHEM\Rush .i\R010312.b C:\CHEM \Rush.i\R010312.b C:\CHEM \Rush.i\R010312.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2.b C:\CHEM \Rush.t\R010312.b C:\CHEM \Rush.i\R010312.b C :\C H EM \R ushJ\R 0103f2-b C:\CHEM \Rush.i\R010312.b CALIB 1 RUSH0018.D CALIB 2 RUSH0019.D CALIB 3 RUSH0020.D CALIB 4 RUSH0021.D CALIB 5 RLISH0022.D CALIB 6 RUSH0023.D CALIB 7 RUSH0024.D CALIB 8 RUSH0025.D CALIB 9 RUSH0026.D CALIB 10 RUSH0027.D SAMPLE RUSH0040.D SAMPLE RUSH0041.D SAMPLE RUSH0054.D SAMPLE RUSH0055.D SAM PLE RUSH0068.D SAMPLE RUSH0069.D SAM PLE RUSH0082.D SAMPLE RUSH0083.D SAMPLE RUSH0096.D SAMPLE RUSH0097.D SAM PLE RUSH0110.D SAMPLE RUSH0111.D SAM PLE RUSH0124.D SAM PLE RUSH0125.D SAMPLE RUSH0135.D SAMPLE RUSH0136.D 5 ng/m L PFOS in M eOH 10 ng/mL PFOS in MeOH 25 ng/m L PFO S in M eOH 4 0 ng/mL PFOS in MeOH 50.1 ng/mL PFO S in M eO H 75.1 ng/mL PFOS in M eO H 100.2 ng/mL PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eO H 400.8 ng/mL PFO S in M eOH 501 ng/mL PFO S in M eO H 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eOH 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eO H 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFOS in M eO H 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eOH 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eO H 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eO H 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFOS in M eOH 5 ng/m L PFOS in M eOH 2 5 0 .5 ng/mL PFO S in M eOH C ACHEMVRuati.i\KQ 10312.t l 3/14/2001 12:15 C :\C H E M \R ush.i\R 010312. b C A LIB 11 R U S H 0141.D 5 ng/m L PFOS in M eO H 3/14/2001 12:26 C :\C H E M \R ush.i\R 010312.b C A LIB 12 R U SH 0142.D 1 0 ng/m L PFOS in M eOH 3/14/2001 12:38 C:VCHEM \Rush.i\R010312.b C A LIB 13 R U S H 0143.D 25 ng/m L PFOS in M eO H 3/14/2001 12:49 C :\C H E M \R u sh .i\R 0 l0 3 1 2 .b C A LIB 14 R U S H 0144.D 4 0 ng/m L PFOS in M eO H 3/14/2001 13:01 C :\C H E M \R ush.i\R 010312.b C A LIB 15 R U S H 0145.D 5 0 .1 ng/m L PFO S in M eO H 3/14/2001 13:12 C :\C H E M \R u s h .i\R 0 1 0 3 1 2 1> C A LIB 16 R U S H 0146.D 75.1 ng/m L PFOS in M eOH 3/14/2001 13:23 C :\C H EM \R ush.i\R 010312.b C ALIB_17 RUSH0147.D 100.2 ng/mL PFOS in MeOH 3/14/2001 13:35 C :\C H E M \R u sh .i\R 0 l0 3 1 2 .b C A LIB 18 R U S H 0148.D 2 5 0 .5 ng/mL PFO S in M eO H 3/14/2001 13:46 C :\C H E M \R ush.i\R 0l0312.b CALIB_19 RUSH0149.D 400.8 ng/mL PFOS in MeOH 3/14/2001 13:57 C:\CH EM \R ush.i\R 010312.b CALIB_20 RUSH0150.D 501 ng/m L PFOS in M eOH ** Lirtad 00 calibration point* ara not uaad in tha calibration calculation*. Mise Info 01003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 Com pound Name 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 0.32 5 .5 2 5.52 5.51 5 .5 2 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 5.46 5.47 5.46 5.47 5.47 5.47 5.47 Area Amount Compound Name 1175891 1179538 1182564 1170614 1181798 1181055 1158213 1161020 1178672 1183842 1100680 1104166 1077492 1087960 1078955 1102376 1038142 1024757 1028519 1029337 1016043 1006141 1011902 990965 995988 995410 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 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 Area A m o un t Theoretical 5 .7 3 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 .6 7 5 .6 7 5.68 5 .6 8 5.68 5.68 5 .6 9 5.69 204920 357143 891797 1351707 1672821 2422605 3017918 6654469 9884645 11780946 199857 6579760 203470 6288787 191641 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 4.0 264.3 4.0 264.9 70.1% 81.1% 98.7% 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% THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.46 5.46 5.46 5.46 5.46 5.46 5.47 5.46 5.46 5.46 Average: Std Dev: %RSD: 1010117 999012 1013523 1000910 1019495 1013642 1007297 1010097 995285 1019903 1070314 73154 7% 254 254 254 254 254 254 254 254 254 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS OC IS Ro9* (/- X% i w ^ i ) 5.68 5.68 5.68 5.68 5.68 5.68 5.69 5.67 5 .6 7 5 .6 7 184884 324179 787488 1203328 1495911 2154462 2739039 5867202 8617452 10475418 3.8 8.9 25.5 41.7 52.0 78.6 103.6 250.2 409.9 510.6 76.3% 89.0% 102.1% 104.2% 103.9% 104.6% 103.4% 99.9% 102.3% 101.9% 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Page 3 of 5 Page 522 of 703 BACK TO MAIN Batch Sample List: Samples Only Acquistion Instrument/Sequence: R ush / R010312 ______ Date/Analyst of Reprocessing; 27-28 M ar 01 / M LA Batch Method: R 01 0 3 l2 .m _______________________________________________ Quantitation Range: 5 to 501 ng/mL, Q u a d ra tic fit, In te rn a l Standard Quant. tnj Date 3/13/2001 15:15 3/13 /2 0 0 1 5:26 3/13/2001 15:37 3/13/2001 16:00 3/13/2001 16:11 3/13/2001 16:23 3/13/2001 16:34 3/13/2001 16:45 3/13/2001 16:57 3/13/2001 17:54 3/13/2001 18:05 3/13/2001 18:16 3/13/2001 18:28 3/13/2001 18:39 Batch C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b File RUSH0030.D RUSH0031.D RUSH0032.D C :\C H E M \R u s h .i\R Q 1 0 3 1 2 .b C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :V C H E M \R u s h .i \R 0 1 0 3 1 2 .b C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\ C H E M \R u s h .l\R 0 1 0 3 1 2 .b CACH EMIRush. i\R 010312.b C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\C H E M \R u sh .i\R 0 1 Q 3 1 2 .b C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\C H E M \R u s h .i\R 0 1 0312.b C :\C H E M \R u sh .i\R 0 1 0 3 l2 .b RUSH0034.D RUSH0035.D RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0044.D RUSH0045.D RUSH0046.D RUSH0047.D RUSH0048.D Sample Name 1311-5088-S1 1311-5089 1311-5090 1311-5091 1311-5092 1311-5093 1 3 1 1-50 93M S 1311-5094 1311-5095 1311-5096 1311-5096MS 1311-5097 1311-5098 1311-5099 Compound Name THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT 5.51 5,51 5.50 5,51 5.51 5.51 5.50 5.51 5.50 5.51 5.51 5.51 5.51 5.50 Area 1385664 1477514 1191529 Amount 254 254 254 Compound Name PFOS PFOS PFOS 1269217 1192069 1150399 1021896 1149765 1187956 1190238 1010278 1151402 1115232 1102724 254 254 254 254 254 254 254 254 254 254 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS RT 5.73 5.72 5.72 5.73 5.72 5.72 5.72 5.72 5 .7 2 5.72 5.73 5.72 5.72 5.71 Area 9084269 9108410 7368006 Amount 289.8 268.9 269.9 1291151 334372 177340 4988076 1598564 1827571 1567771 6130982 5335559 6471149 6167800 34.6 7.3 2.8 203.3 49.0 54.8 46.2 263.8 191.2 249.9 239.1 3/13/2001 19:02 C:\CHEM\Rush.i\R010312.b RUSH0050.D 1311-5100 THPFOS 5.50 1062217 254 PFOS 5.71 4081880 3/13/2001 19:13 C:\CHEM\Rush.i\R010312.b RUSH0051.D 1311-5101 THPFOS 5.49 1091409 254 PFOS 5.71 3885669 3/13/2001 19:24 C:\CHEM\Rush.t\R010312.b RUSH0052.D 1311-5102 THPFOS 5.49 1089550 254 PFOS 5.71 3812838 3/13/2001 19:36 C:\CHEM\Rush.i\R010312.b RUSH0053.D 1311-5102MS THPFOS 5.49 954668 254 PFOS 5.71 7634048 3/13/2001 20:32 C:\CHEM\Rush.i\R010312.b RUSH0058.D 1311-5103 THPFOS 5.49 1117174 254 PFOS 5.70 7957940 3/13/2001 20:44 C:\CHEM\Rush.i\R010312.b RUSH0059.D 1311-5104 THPFOS 5.50 1116604 254 PFOS 5.71 7667501 3/13/2001 20:55 C:VCHEM\Rush.i\R010312.b RUSH0060.D 1311-5105 THPFOS 5.48 1086708 254 PFOS 5.69 7435595 OrtOfiiOOl 24tO?-------0 * 0 1C M tftu a h .WW f lM a . b-----RU6 H006frB------ 13 H -5105MG------------- Ti IPFOS--------------------------943407------- 964--------------- PFQ6---------------6rW------4066669 3/13/2001 21:18 C:\CHEM\Rush.i\R010312.b RUSH0062.D 1311-5106 THPFOS 5.49 1197459 254 PFOS 5.71 5272348 3/13/2001 21:29 C:\CHEM\Ru9h.i\R010312.b RUSH0063.D 1311-5107 THPFOS 5.49 1180945 254 PFOS 5.69 5098549 3/13/2001 21:41 C:\CHEM\Rush.i\R010312.b RUSH0064.D 1311-5108 THPFOS 5.49 1203215 254 PFOS 5.70 5046570 3/13/2001 21:62 C:\CHEM\Rush.i\R010312.b RUSH0065.D 1311-5108MS THPFOS 5.48 1052179 254 PFOS 5.70 9075493 3/13/2001 22:03 C:\CHEM\Rush.i\R010312.b RUSH0066.D 1311-5109 THPFOS 5.49 1065391 254 PFOS 5 .7 0 478603 3/13/2001 22:15 C:\CHEM\Rush.i\R010312.b RUSH0067.D 1311-5110 THPFOS 5.48 1166374 254 PFOS 5.69 154573 3/13/2001 23:11 C:VCHEM\Rush.i\R010312.b RUSH0072.D 1311-5111 THPFOS 5.48 1179002 254 PFOS 0 .0 0 0 3/13/2001 23:23 C:\CHEM\Rush.i\R010312.b RUSH0073 D 1311-5111 MS THPFOS 5.48 956166 254 PFOS 5.69 4711542 3/13/2001 23:34 C:\CHEM\Rush.i\R010312.b RUSH0O74.D 1311-5112 THPFOS 5.48 1126349 254 PFOS 5.69 1945796 3/13/2001 23:45 C:\CHEM\Rush.i\R010312.b RUSH0075.D 1311-5113 THPFOS 5,48 1133593 254 PFOS 5.69 1923182 3/13/2001 23:57 C:\CHEM\Rush.i\R010312.b RUSH0076.D 1311-5114 THPFOS 5.48 1050097 254 PFOS 5.69 1911701 3/14/2001 0:08 C:\CHEM\Rush.i\R010312.b RUSH0077.D 1311-5114MS THPFOS 5.48 913903 254 PFOS 5.69 5785268 3/14/2001 0:20 C:\CHEM\Rush.i\R010312.b RUSH0078.D 1311-5115 THPFOS 5.47 1051071 254 PFOS 5.68 7556059 3/14/2001 0:31 C:\CHEM\Rush.i\R010312.b RUSH0079.D 1311-5116 THPFOS 5.48 1005648 254 PFOS 5.69 7453080 3/14/2001 0:42 C :\C H E M \R u s h .i\R 0 1 03 1 2 .b RUSH0080.D R U 3 1 10081.D 1311-5117 1311-5111M 3 THPFOS 5.47 1064613 254 PFOS 5.68 7243851 3/14/2001 1:50 C:\CHEM\Rush.i\R010312.b RUSH0086.D 1311-5118 THPFOS 5.48 1069400 254 PFOS 5.69 5158635 3/14/2001 2:02 C:\CHEM\Rush.i\R010312.b RUSH0087.D 1311-5119 THPFOS 5.48 1071246 254 PFOS 5.69 4662505 3/14/2001 2:13 C:\CHEM\Rush.i\R010312.b RUSH0088.D 1311-5120 THPFOS 5.47 1053796 254 PFOS 5 6 8 5171543 3/14/2001 2:25 C:\CHEM\Rush.AR010312.b RUSH0089.D 1311-5120MS THPFOS 5.47 906343 254 PFOS 5.68 8600968 3/14/2001 2:36 C:\CHEM\Rush.i\R010312.b RUSH0090.D 1311-5019-S2 THPFOS 5.47 1068914 254 PFOS 5.68 237607 3/14/2001 2:47 C:\CHEM\Rush.i\R010312.b RUSH0091.D 1311-5020 THPFOS 5.47 1035621 254 PFOS 0 .0 0 0 3/14/2001 2:59 C:\CHEM\Rush.i\R01Q312.b RUSHQQ9Z.D 1311-5021 THPFOS 5.46 1058784 254 PFOS 0 .0 0 0 3/14/2001 3:10 C:\CHEM\Rush.i\R010312.b RUSH0093.D 1311-5021MS THPFOS 5.46 908983 254 PFOS 5.67 4336124 3/14/2001 3:21 C:\CHEM\Rush.iAR010312.b RUSH0094.D 1311-5022 THPFOS 5.48 1047722 254 PFOS 5 .6 9 413339 3/14/2001 3:33 C:\CHEM\Rush.i\R010312.b RUSH0095.D 1311-5023 THPFOS 5.47 1044074 254 PFOS 5 .6 8 390331 3/14/2001 4:29 C:\CHEM\Rush.i\R010312.b RUSH0100.D 1311-5024 THPFOS 5.47 1027244 254 PFOS 5 .6 9 420991 3/14/2001 4:41 CACHE M\R ush.iNR010312 .b RUSH0101.D 1311-5024MS THPFOS 5.47 900913 254 PFOS 5.68 4492622 3/14/2001 4:52 3/14/2001 5:04 3/14/2001 5:15 C :\ C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\C H E M 1 R u sh .i\R 0 1 0 3 1 2 .b C :\C H EM \R ush.t\R 010312.b RUSH0102.D RUSH0103.D RUSH0104.D 1311-5025 1311-5026 1311-5027 THPFOS THPFOS THPFOS 5.46 5.47 5.46 1034605 1024646 1017504 254 254 254 PFOS PFOS PFOS 5.68 5.68 5.68 862953 889216 730970 3/14/2001 5:26 C:\CHEM\Rush.i\R010312.b RUSH01Q5.D 1311-5027MS THPFOS 5.48 879952 254 PFOS 5.69 4918144 3/14/2001 5:38 C:\CHEM\Rush.i\R010312.b RUSH0106.D 1311-5028 ' THPFOS 5.49 997963 254 PFOS 5 .7 0 1564024 3/14/2001 5:49 C:\CHEM\Rush.i\R010312.b RUSH0107.D 1311-5029 THPFOS 5.48 1030844 254 PFOS 5 .6 9 970831 3/14/2001 6:00 C:\CHEM\RuSh.i\R010312.b RUSH0108.D 1311-5030 THPFOS 5.47 1022445 254 PFOS 5 .6 9 1650112 3/14/2001 6:12 C:\CHEM\Rush.i\R010312.b RUS H 0109. D 1311-5030MS THPFOS 5.48 879426 254 PFOS 5.70 5622153 3/14/2001 7:08 C:VCHEM\Rush.i\R010312.b R U SH 0114.D 1311-5031 THPFOS 5.46 1025535 254 PFOS 5.68 1856615 3/14/2001 7:20 C:\CHEM\Rush.i\R010312.b RUSH0115.D 1311-5032 THPFOS 5.47 1025203 254 PFOS 5.68 1884859 3/14/2001 7:31 C:\CHEM\Rush.i\R010312.b RUSH0116.D 1311-5033 THPFOS 5.47 1029469 254 PFOS 5.68 2002764 3/14/2001 7:43 C:\CHEM\Rush.i\R010312.b RUSH0117.D 1311-5033MS THPFOS 5.47 880742 254 PFOS 5.69 5840312 3/14/2001 7:54 C:\CHEM\Rush.i\R010312.b RUSH0118.D 1311-5034 THPFOS 5.47 1023217 254 PFOS 5.68 3730551 3/14/2001 8:05 C:\CHEM\Rush.i\R010312.b RUSH0119.D 1311-5035 THPFOS 5.47 1012932 254 PFOS 5.68 5585758 3/14/2001 8:17 C:\CHEM\Rush.i\R010312.b RUSH0120.D 1311-5036 THPFOS 5.47 1026080 254 PFOS 5.68 4711539 3/14/2001 8:28 C:\CHEM\Rush.i\R01Q312.b RUSH0121.D 1311-5036MS THPFOS 5.47 860064 254 PFOS 5.68 7996407 3/14/2001 8:39 C:\CHEM\Rush.i\R010312.b RUSH0122.D 1311-5055 THPFOS 5.47 987998 254 PFOS 5.68 395287 3/14/2001 8:51 C:\CHEM\Rush.i\R010312.b RUSH0123.D 1311-5056 THPFOS 5.47 968034 254 PFOS 5.68 166967 3/14/2001 9:48 C:\CHEM\Rush.i\R010312.b RUSH0128.D 1311-5057 THPFOS 5.48 991221 254 PFOS 0 .0 0 a 3/14/2001 9:59 C:\CHEM\Rush.i\R010312.b RUSH0129.D 1311-5057MS THPFOS 5.48 856978 254 PFOS 5.69 4243033 3/14/2001 10:10 Q:\CHEM\Rush.i\R010312.b RUSH0130.D 1311-5058 THPFOS 5.48 997688 254 PFOS 5.69 300042 3/14/2001 10:22 C:\CHEM\Rush.i\R010312.b RUSH0131.D 1311-5059 THPFOS 5.47 958286 254 PFOS 5.69 391761 3/14/2001 10:33 C:\CH6M\Rush.t\R010312.b RUSH0132.D 1311-5060 THPFOS 5.47 975732 254 PFOS 5.68 847418 3/14/2001 10:44 C:\CHEM\Rush.i\RC10312.b RUSH0133.D 1311-5060MS THPFOS 5.46 840001 254 PFOS 5.68 4805368 3/14/2001 10:56 C :\CHEM\RushJ\R010312.b RUSH0134.D 1311-5061 THPFOS 5.47 967423 254 PFOS 5.68 1987989 " Lined out lamp point* *r* *bov* tha caltbraUon curva. 153.8 140.8 138.0 370.7 321.0 306.8 305.4 180.1 176.0 170.2 407.9 13.4 2.0 0.0 205.6 62.4 61.1 66.1 277.7 324.3 337.1 303.4 200.5 177.7 204.6 460.9 5.2 0.0 0.0 197.9 11.4 10.7 12.0 200.5 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 3.4 0.0 206.8 10.9 11.9 29.0 245.7 75.7 3M Environmental Laboratory 3M Environmental Laboratory E00-1311 PFOS Adsorb/Desorb Page 4 of 5 /Mid /*''((//'/ Page 523 of 703 3M Environmental Laboratory BACK TO MAIN Batch Sample List: MeOH Blanks Acquistion Instrument/Sequence: Rush / R010312_____________________ Date/Analyst of Reprocessing: 27-28 Mar 01 / MLA Batch Method: R010312.m_________________________________________ Quantitation Range: 5 to 501 ng/mL, Quadratic fit, Internal Standard Quant Inj Date 3/13/2001 12:13 3/13/2001 12:25 3/13/2001 14:52 3/13/2001 15:03 3/13/2001 17:31 3/13/2001 17:42 3/13/2001 20:10 3/13/2001 20:21 3/13/2001 22:49 3/13/2001 23:00 3/14/2001 1:28 3/14/2001 1:39 3/14/2001 4:07 3/14/2001 4:18 3/14/2001 6:46 3/14/2001 6:57 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 14:20 Batch C:\CHEM\Rush.i\R01Q312.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C :\C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\C H E M \R u s h .i\R 0 1 0 3 1 2 .b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C:\C HEMVRush. i\R010312.b C:\CHEM\Rush.i\R010312.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C:\CHEM\Rush.i\R010312.b C:\CHEM\Rush.i\R010312.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2.b C:\CHEM\Rush.i\R010312.b C:\CHEM\Rush.i\R010312.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C:\CHEM\Rush.i\R010312.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C:\CHEM\Rush.i\R0103l2.b C :\C H E M \R u sh .i\R 0 1 0 3 1 2 .b C :\C H E M \R u s h .i\R 0 1 0 3 1 2 .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 RUSH0Q14.D RUSH0015.D RUSH0028.D RUSH0029.D RUSH0042.D RUSH0043.D RUSH0056.D RUSH0057.D RUSHQ070.D RUSH0071.D RUSH0084.D RUSH0085.D RUSH0098.D RUSH0099.D RUSH0112.D RUSH01T3.D RUSH0126.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 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 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 5.68 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 67597 72910 27715 30881 26667 29144 26584 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 Page 524 of 703 3M Environmental Laboratory EOO-1311 PFOS A dsorb/D esorb Page 5 of 5 3M Environmental Laboratory PFOS Ads/Des EOO-1311 Internal Standard Quant, Reprocessing m ethod: H010222t.m, calibration standards S-250 ng/mL. 2.5 ngPFOS/mL standard did not meet accuracy requirments, 500,750 and 1000 ng/mL standards excluded to better fit the data. Q uadratic curve fib In] Date 2/22/01 20:51 2/22/01 21:02 2/22/01 21:13 2/22/01 21:24 2/22/0121:35 2/22/01 21:46 2/22/01 21:58 2/22/01 22:09 2/22/01 22:20 2/22/01 22:31 2/22/01 22:42 2/22/01 22:53 2/22/01 23:04 2/23/01 1:29 2/23/01 1:40 2/23/01 4:05 2/23/01 4:16 2/23/01 6:41 2/23/01 6:52 2/23/01 9:17 2/23/01 9:28 2/23/01 11:53 2/23/01 12:04 2/23/01 14:30 2-23/01 14:41 2/23/01 16:44 2/23/01 16:55 2/23/01 17:28 2/23/01 17:39 2/23/01 17:50 2/23/01 18:02 2/23/01 18:13 2/23/01 18:24 2/23/01 18:35 2/23/01 18:46 2/23/01 18:57 2/23/01 19:08 2/23/01 19:20 2/23/01 19:31 2/23/01 19:42 Batch D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chenAHillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\HilIary.i\H010222.b D:\chem\Hillary.i\H0l0222-b D:\chem\Hillary.t\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hiilaiy.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\HHlary.i\H010222-b D:\cbem\Hillary.i\H010222.b D:\cherri\Hiliary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H0l0222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H0l0222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222-b D:\chem\Hillary.iVH010222.b D:\cherrAHillary.i\HQ10222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H0l0222.b D:\chem\Hillary.i\H010222.b D:\chem\HiIiary.i\H01 Q222.b D:\chem\Killary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hi'llary.i\H010222.b D:\chem\Hillary.i\H010222.b D:\chem\Hillary.i\H0l0222.b D:\chem\Hillary.i\H0l0222.b D:\chem\Hillary.i\H010222.b D:Schem\Hiilary.j\H010222.b D:\chem\Hillary.i\H010222.b SampType File SAMPLE HILL0022.D CALIB 1 HILL0O23D CALIB 2 HILL0024.D CALIB 3 HILL0025.D CALIB 4 HILL0026.D CALIB_5 HILL0027.D CAUB 6 H1LL0028.0 CALIB.7 HILL0029.D CALIB 8 HILL0030.D CAUB 9 HILL0031.D C ALIBJ0 HILL0032.D SAMPLE HILL0033.D SAMPLE HILL0034.D CCALIBJ HILL0047.D CCALIBJ HILL0O48.D CCALIB 1 HILL0061.D CCALIBJ H1LL0062.D CCALIBJ HILL0075.D CCALIB 1 HILL0076.D CCALIB_1 HILL0089.D CCALIB 1 HILL0090.D CCALIB_1 HILL0103.D CCALIBJ HILL0104.D CCALIBJ HILL0117.D CCALIBJ HILL0118.D CCALIBJ HILL0129.0 CCALIB 1 HILL0130.D SAMPLE H1LL0133.D CALIBJ1 HILL0134.D CA LIB J2 HILL0135.D C ALIBJ3 HILL0136.D CALIBJ4 HILL0137.D C ALIBJ5 HILL0138.D CA LIB J6 HILL0139.D CALIB.17 HILL0140.D C A U B J 8 HILL0141.D C A LIB J 9 HILL0142.D C ALIBJ0 HILL0143.D SAMPLE HILL0144.D SAMPLE HILL0145.D Sample Name 00002-104^)1 00002-104-02 00002-104-03 00002-104-04 00002-104-05 00002-104-06 00002-104-07 00002-104-08 00002-104-09 00002-104-10 00002-104-11 00002-104-12 00002-104-13 00002-104-03 00002-104-10 00002-104-03 00002-104-10 00002-104-03 00002-104-10 00002-104-03 00002-104-10 00002-104-03 00002-104-10 00002-104-03 00002-104-10 00002-104-03 00002-104-10 00002-104-01 00002-104-02 00002-104-03 00002-104-04 00002-104-05 00002-104-06 00002-104-07 00002-104-08 00002-104-09 00002-104-10 00002-104-11 00002-104-12 00002-104-13 Mise Info Std amt (ng/mL) 2.5 5 10 25 40 50 75 100 250 500 750 1000 5 250 5 250 5 250 5 250 5 250 5 250 5 250 (0 Std) 2.5 5 10 25 40 50 75 100 250 500 750 1000 Compound Nan 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 Page 525 of 703 Page 1 o f4 BACK TO MAIN Samples E00-4001*S1 thru -4051-S1 RT 4.945 4.938 4.945 4 .9 4 5 4 .9 4 5 4.938 4 .9 4 4 4 .9 3 7 4.937 4.945 4 .9 3 2 4 .9 0 5 4 .9 4 6 4 .9 4 4 4.928 4 .9 3 7 4 .9 3 8 4 .9 0 3 4.934 4 .9 3 3 4 .9 0 4 4.921 4.914 4.93 4.818 4.91 4 .9 0 9 4 .9 0 9 4 .9 1 7 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 846048 950054 841012 986760 843661 965275 849853 960603 970213 975322 962803 955202 931719 913224 908508 891910 835096 767261 726914 710125 iei 877302 Dev: 75938 : 8.7% Amount Com pound 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 (*/- 30% average): 1140493 +30%: 614112 -30%: RT Area 5.169 87135 5.162 71607 5.169 130540 5.169 254321 5.169 527419 5.162 838037 5.168 1094896 5.161 1627972 5.162 2166581 5.169 5046746 5.156 9079135 5.171 12908429 5.163 16080347 5.168 128463 5.153 5084843 5.154 130987 5.162 5117167 5.155 124712 5.151 5115342 5.157 128458 5.163 5100493 5.145 126306 5.131 5001460 5.154 127270 5.147 5032612 5.135 123647 5.134 4974770 5.133 80947 5.134 70306 5.124 123635 5.121 246660 5.126 509141 5.127 809392 5.134 1075245 5.127 1576634 5.113 2094348 5.119 4914708 5.126 8822276 5.127 12478371 5.128 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 5.6 246.5 5.4 247.2 5.4 242.6 3.6 3.1 5.3 10.7 22.2 36.1 48.9 72.1 97.5 243.9 475.6 708.7 915.4 % Theoretical X 123.1% 120.7% 99.1% 99.3% 105.4% 104.3% 104.4% 102.1% X X 115.1% 99.9% 115.4% 100.5% 109.8% 99.2% 111.1% 9 9 .9 % 111.8% 9 8 .6 % 108.5% 98.9% 107.8% 97.0% X 106.7% 107.1% 88.8% 90.3% 9 7 .9 % 96.1% 97.5% 9 7 .6 % 9 5 .1 % X X 3M Environmental Laboratory PFOSAds/Des E00-1311 internal Standard Quant, Reprocessing method: H 010222tm , calibration standards 5-250 ng/mL. 2.5 ngPFOS/mL standard did not meet accuracy requirments, 500,760 and 1000 ng/mL standards excluded to better fit the data Quadratic curve fit In] Date Batch SampType File Sample Name Mise Info Compound Name 2/22/01 23:38 2/22/01 23:49 2/23/01 0:00 2/23/01 0:11 2/23/01 0:22 2/23/01 0:33 2/23/01 0:45 2/23/01 0:56 2/23/01 1:07 2/23/01 1:18 2/23/01 2:14 2/23/01 2:25 2/23/01 2:36 2/23/01 2:47 2/23/01 2:58 2/23/01 3:09 2/23/01 3:20 2/23/01 3:32 2/23/01 3:43 2/23/01 3:54 2/23/01 4:50 2/23/01 5:01 2/23/01 5:12 2/23/01 5:23 2/23/01 5:34 2/23/01 5.45 2/23/01 5:56 2/23/01 6:08 2/23/01 6:19 2/23/01 6:30 2/23/01 7:26 2/23/01 7:37 2/23/01 7:48 2/23/01 7:59 2/23/01 8:10 2/23/01 8:21 2/23/01 8:32 2/23/01 8:44 2/23/01 8:55 2/23/01 9:06 D :\ch e m \H illa ry .i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 Q 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\c h e m \H illa ry.i\H 0 1 0 222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\chem \H iliary.i\H 0l0222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\c h e m \H illa ry.i\H 0 1 0 222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\c h e m \H illa ry.i\H 0 1 0 222.b D :\c h e m \H iila ry .i\H 0 l0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D .'c h e m \H illa ry .i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D:Vchem\Hillary.i\H010222.b D :\ch e m \H itta ry.i\H 0 1 0 2 2 2 .b D:\chem\HNIary.i\H010222.b D :\c h e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\c h e m \H iH a ry.i\H 0 1 0 2 2 2 .b D:\chem\Hillary.i\HOl0222.b D:\chem\Hillary.i\H010222 b D :\cham \H illary.M 010222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\c h e m \J H illa ry .i \H 0 l0 2 2 2 .b D .'c h e m \H iiia ry .i\H 0 1 0 2 2 2 .b D :\chem \H illary.f\H 010222.b D :\chem \H illary.l\H 010222.b D :\ch e m \H ilia ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D:\Chem \HiUary.i\H010222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 b D :\chem \H illary.i\H 0l0222.b D :\ch e m \H illa ry.i\H 0 1 0222.b SAMPLE SAMPLE SAMPLE SAMPLE HILL0037.D 1311-4001-SI HILL0038.D 1311-4002-S1 HILL0039.D 1311-4003-S1 HILL0040.D 1311-4003MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0041.D 1311-4004-S1 HILL0042D 1311-4005-S1 HILL0043.D 1311-4006-SI HILL0O44.D 1311-4006MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0045.D 1311-4007-S1 HILL0O46.D 1311-4008-S1 HILL0051.D 1311-4009-S1 HILL0052.D 1311-4009MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL053.Q 1311-4010-S1 HILL0054.D 1311-4011-S1 HILL0055.D 1311-4012-S1 HILL0056.D 1311-4012MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0057.D 1311-4013-S1 HILL0058.0 1311-4014-S1 HILL0059D 1311-4015-S1 H1LL0060.0 1311-4015MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0O65D 1311-4016-S1 HILL0066.D 1311-4017-S1 H1LL0067.D 1311 -4018-SI HILL0O68.D 1311-4018MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0069.D 1311-4019-S1 HILL0O70.D 1311-4020-S1 HILL0071.D 1311-4021-S1 HILL0O72.D 1311-4021MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE H IL L 0 O 7 3 A 1 3 1 1 `4 0 2 2 - S I HILL0074.D 1311-4023-S1 HILL0079.D 1311-4024-S1 H1LL0O80.D 1311-4024MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE H IL L 0O 81.D 1 3 1 1 `4 0 2 5 - S I HILL0082.D 1311-4026-S1 HILL0083.D 1311-4027-S1 HILL0084.D 1311-4027MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0O85.D 1311-4028-S1 HILL0O66.D 1311-4029-S1 HILL0087.D 1311-4030-S1 HILL0088.D 1311-4030MS-S1 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 Page 526 of 703 Page 2 of 4 BACK TO MAIN Samples E00-4001-S1 thru -4051-S1 RT 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 .9 2 9 4.936 4 .9 3 7 4.938 4 .9 3 4 .9 3 4.936 4.931 4.93 4.939 4.932 4.925 4.933 4.931 4 .9 2 9 4 .9 3 7 4.947 4.938 4 .9 3 4 .9 3 2 4.937 4.929 4.931 4 .9 2 9 Area 944393 963890 942003 830932 945739 932519 933232 816057 944645 933140 965150 833273 971260 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 Amount Com pound Name RT Area Amount % Theoretical 249.3 249.3 249.3 249.3 249.3 249.3 249.3 2493 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 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 0 0 0 5.161 0 0 0 4102327 0 0 Q 5.153 0 0 0 4020982 5.161 5.162 5.17 5.154 1164609 1239235 1999524 5149900 5.161 5 .1 6 5.16 5.155 1233408 1214963 1183400 5007271 5 .1 5 4 5 .1 6 5.162 5.162 1195984 1232516 1212915 5041035 5.154 5.154 5 .1 6 5.155 1263565 1276111 1396036 5215525 5.154 5.163 5.156 5.149 1172949 1226450 1202381 5111162 S.15 5 .1 5 5 5.153 5.161 1537664 1206313 1250887 5936492 5.16S 5.162 5.162 5 .1 6 3 1453734 1398064 1265770 5704109 5.168 5.161 5 .1 6 2 5 .1 6 1418355 1267363 1377526 5191492 0.0 0.0 0.0 204.7 0.0 0.0 0.Q 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 PFOS Ads/Des E00-1311 BACK TO MAIN Samples E00-4001-S1 thru -4051-S1 3M Environmental Laboratory (0QT)J CD OMl O Ovl CO Internal Standard Quant, R eprocessing m ethod: H010222tm , calibration standards 5-250 n g/m L 2.5 ngPFOS/mL standard did no t meet a ccuracy requirm e n ts, 500, 750 and 1000 ng/m L standards excluded to b e tte r f it the data. Quadratic curve f i t Inj Date Batch SampType File Sample Name Mise Info C om pound Name RT Area 2/23/01 10:02 2/23/01 10:13 2/23/01 10:24 2/23/01 10:35 D:Vchem\Hiilary.i\H010222.b D ;\chem\H illary.i\H010222,b D :\chem \H illary.i\H 010222.b D :\chern\H illary.i\H 010222.b SAMPLE SAMPLE SAMPLE SAMPLE HILL0093.D 1311-4031-S1 HILL0094.D 1311-4032-S1 HILL0O95.D 1311-4033-S1 HILL0096.D 1311-4033MS-S1 THPFOS THPFOS THPFOS THPFOS 4.925 4.923 4.93 4.926 1015824 1079934 1055100 890829 2/23/01 10:46 2/23/01 10:57 2/23/01 11:09 2/23/01 11:20 D:\chem\Hillary.i\H0l0222.b D :\che m \H illa ry .i\H 0 1 0 2 2 2 .b D :\chem \H illary.i\H 010 2 2 2 .b D :\c hem \H illary.i\H 010222.b SAMPLE SAMPLE SAMPLE SAMPLE HILL0097.D 1311-4034-S1 HILL0098.D 1311-4035-S1 HILL0O99.D 1311-4036-S1 HILL0100.D 1311-4036MS-S1 THPFOS THPFOS THPFOS THPFOS 4.923 4.924 4.915 4.918 987405 1090655 1031470 841990 2/23/01 11:31 2/23/01 11:42 2/23/01 12:38 2/23/01 12:49 D :\c hem \H illary.i\H 010222.b D :\c hem \H illary.i\H 010222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\c h e m \H itl a ry .i \H 0 1 0 2 2 2 .b SAMPLE SAMPLE SAMPLE SAMPLE H1LL0101.D 1311-4037^1 HILL01O2.D 1311-4038-S1 H1LL0107.D 1311-4039-S1 HILL01O8.D 1311-4039MS-S1 THPFOS THPFOS . THPFOS THPFOS 4.922 4.922 4.918 4.915 995964 992751 985052 844071 2/23/01 13:00 2/23/01 13:12 2/23/01 13:23 2/23/01 13:34 2/23/01 13:45 2/23/01 13:56 2/23/01 14:07 2/23/01 14:18 2/23/01 15:14 2/23/01 15:25 2/23/01 15:37 2/23/01 15:48 D :\chem \H illary.i\H 010222.b D :\chem \H illary.i\H 010222.b D :\chem \H illary.i\H 010222.b D :\c h e m \H illa ry .t \H 0 1 0 2 2 2 .b D:\chem\HiUary.i\H010222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :Vchem\Hi 11ary.i\H010222.b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D:ichem\Hiflary. \H010222. b D :\c hem \H illary.i\H 010 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b SAMPLE SAMPLE SAMPLE SAMPLE H1LL01O9.D 1311-4040-S1 HILL0110.D 1311-4041-S1 HILL0111.D 1311-4042-S1 HILL0112.D 1311-4042MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0113.D 1311-4043-S1 HILL0114.D 1311-4044-S1 HILL0115.D 1311-4045-S1 HILL0116.D 1311-4045MS-S1 SAMPLE SAMPLE SAMPLE SAMPLE HILL0121.D 1311-4046-S1 HILL0122.D 1311-4047-S1 H1LL0123.D 1311-4048-S1 HLL0124.D 1311-4048MS-S1 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 4.91 4 .9 1 7 4.908 4.915 4.914 4.925 4 .9 2 2 4.923 4.923 4.92 4.923 4.91 990932 986341 982392 873132 984852 999207 997394 861434 1017804 993010 1007737 853140 2/23/01 15:59 2/23/01 16:10 2/23/01 16:21 2/23/01 16:32 D :\ch e m \H illa ry .i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\ch e m \H illa ry.i\H 0 1 0 2 2 2 .b D :\chem \H illary.i\H 010222.b SAMPLE SAMPLE SAMPLE SAMPLE HILL0125.D 1311-4049-S1 HILL0126.D 1311-4050-S1 HILL0127.D 1311-4051-S1 H1LL0128.D 1311-4051MS-S1 THPFOS THPFOS THPFOS THPFOS 4.916 4.91 4.915 4.911 986831 979691 959926 849190 Average; 972356 Std Dev: 85032 %RSD: 8.7% Amount 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 5 .1 5 0 0 0 4355290 0.0 0.0 0.0 200.9 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 36.6 33.0 28.9 224.8 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 5,149 5.147 5 .1 5 4 269994 236262 242527 4358791 11.5 9.9 10.2 209.8 PFOS PFOS PFOS PFOS 5.147 5 .1 4 4 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 10.4 209.5 % Theoretical Page 3 of 4 BACK TO MAIN Quantify Compound Sunmary Report EO0-1311 PFOS Adsorb/Desorb Sample List: C:\Masslynx^:oup020199 .pro\SampleDB\s001207 Last modified: Mon Dec 11 09:05:24 2000 Method: C: \Masslynx\uoup020199.pro\MethDB\s0Q1207 Last modified: Mon Dec 11 09:10:27 2000 Job Code: Printed: Mon Dec 11 09:23:38 2000 Compo u n d 1 : PFOS (499>99) , fune 1 * Name 1 s OO1207 _001 2 sO 01207._002 3 S001207._003 4 S001207.-004 5 S001207._005 6 S001207._006 7 sO 01207._007 8 S001207.-008 9 S001207._009 10 S001207._010 11 S001207.-011 12 S001207..012 13 S001207._013 14 S001207. 014 15 S001207..015 16 S001207. 016 17 sOO 1207. 017 18 S001207. 018 19 S001207._019 20 S001207..020 21 S001207. 021 22 SO01207..022 23 sOO 1207. 023 24 S001207 02 4 25 S001207._025 26 S001207..02 6 27 s O O 1207..027 28 3001207..028 29 sO 01207. 029 30 S0Q1207..030 31 S001207..031 32 sO 01207..032 33 S001207..033 34 S001207..034 35 S001207..035 36 S001207. 036 37 S001207 037 38 S001207..038 39 S001207 .039 40 S001207. 040 41 S001207. 041 42 S001207. 042 43 S001207. 043 44 S001207. 044 45 S001207. 045 46 S001207 046 47 S001207. 047 48 S001207. 048 49 S001207. 049 50 S001207..050 51 S001207 051 52 S001207..052 53 S001207..053 54 s0012 07_.054 55 S001207..055 56 S001207..056 57 s001207_.057 58 S O 0 1 2 O 7 . .058 59 S001207..059 60 S001207 .0 60 61 S001207..061 62 S001207..062 63 S001207..063 64 S001207..064 65 S001207 065 66 S001207..066 67 S001207..067 68 S001207..068 69 S001207..069 70 S001207..070 71 S001207..071 72 S001207..072 73 s OO1207..073 74 S001207..074 75 sOO 1207..075 76 S001207..076 77 s OO1207..077 78 S001207..078 79 s O O 12 07 .079 80 S001207..080 81 S001207. 081 82 S001207 082 83 s001207_ 083 84 s O O 1207 .084 85 S001207 085 86 s O O 12 07_ 086 87 s O O 12 07_.087 88 s001207_ 088 89 s001207_.089 study no Samplelist Text E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 L001.7 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 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 0 ppb.PFOS 00002-86-01, Aliq. 11-27-00 MLA EOO-1311 2.5 ppb PFOS 00002-86-02, Aliq. 11-27-00 MLA EOO-1311 5.00 ppb PFOS 00002-86-03, Aliq. 11-27-00 MLA E00-1311 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 EOO-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 EOO-1311 75.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA EOO-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 EOO-1311 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA EOO-1311 1001.7 ppb PFOS 00002-86-13, aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 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. 11-27-00 MLA E00-1311 2.5 ppb PFOS 00002-86-02, Aliq. 11-27-00 MLA E00-1311 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-O5, Aliq. 11-27-00 MLA E00-1311 40.0 ppb PFOS 00002-86-06, Aliq. 11-27-00 MLA E00-1311 50.1 ppb PFOS 00002-86-07 Aliq. 11-27-00 MLA EOO-1311 75.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA EOO-1311 100.2 ppb PFOS 00002-86-09, Aliq. 11-27-00 MLA EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-00 MLA EOO-1311 1001.7 ppb PFOS 00002-86-13, 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 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 10x E OO-131 1-3001-SI, 0.0mg/L, Ohr, No soil, 12/07/00 E00-1311 lOx EOO-1311-30O2-S1, 0.0mg/L, Ohr, No soil, 12/07/00 E00-1311 lOx E00-1311-3OO3-S1, O.Omg/L, Ohr, No soil, 12/07/00 E00-1311 lOx E 0 0 -1311-3003ms-Sl O.Omg/L, Ohr, No soil, 12/07/00 E00-1311 lOx EOQ-1311-3004-S1 0.5mg/L, Ohr, No soil, 12/07/00 E00-1311 250.4 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 EOO-1311 lOx EOO - 1311-3005-SI, 0.5mg/L, Ohr, No soil, 12/07/00 E00-1311 lOx E 00-131 1-3006-SI, 0.5mg/L, Ohr, No soil, 12/07/00 EOO-1311 l()x E 0 0 - 1 3 11-3006m s - S l ,0 . 5mg/L, Ohr, No soil, 12/07/00 E00-1311 l()x E 00-131 1 -3013-SI, O.Omg/L, Ohr, l:lclay, 12/07/00 EOO-1311 lOx E00-1311-3014-S1, O.Omg/L, Ohr, l:lclay, 12/07/00 E00-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 lOx E O O - 1311-3015-SI, O.Omg/L, Ohr, l:lclay, 12/07/00 EOO-1311 l()x E00-1311-3Q15ms-Sl, O.Omg/L, Ohr, lslclay, 12/07/00 EOO-1311 lOx E00-1311-3016-S1, O.Omg/L, Ohr, l:5clay, 12/07/00 E00-13-11 lOx E00-1311-3017-S1, O.Omg/L, Ohr, l:5clay, 12/07/00 EOO-1311 lOx E 0 0-1311-3018-SI, O.Omg/L, Ohr, ItSclay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 l()x E00-1311-3018ms-Sl, O.Omg/L, Ohr, l:5clay, 12/07/00 E00-1311 10x E OO-1311-3019-SI , 0.Omg/L, Ohr, l:25clay, 12/07/00 EOO-1311 l()x E00-1311-3020-S1, O.Omg/L, Ohr, l:25clay, 12/07/00 EOO-1311 lOx E00-1311-3021S1,O.Omg/L, Ohr, l:25clay, 12/07/00 EOO-1311 l()x E00-1311-3021ms-Sl, O.Omg/L, Ohr, l:25clay, 12/07/00 E00-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 lOx EOO-1311-3031-S1,0 . 5mg/L, Ohr, l:lclay, 12/07/00 E00-1311 lOx E 0 0 - 1 3 11-303 2 - S I ,0 ,5mg/L, Ohr, lrlclay, 12/07/00 EOO-1311 lOx EOO-1311-3033-SI,0. 5mg/L, Ohr, l:lclay, 12/07/00 E00-1311 lOx E 0 0 -13ll-3033ms-Sl,0.5rog/L, Ohr, lslclay, 12/07/00 E00-1311 lOx E00-1311-3034-S1.O.5mg/L,Ohr, l:5clay, 12/07/00 E00-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 lOx EQ0-1311-3035-S1,0.5mg/L,Ohr, l:5clay, 12/07/00 E00-1311 l()x E0Q-1311-303 6-Sl,0.5mg/L, Ohr, liSclay, 12/07/00 E00-1311 10x E00-1311~3036ms-Sl,0.5mg/L,Ohr, l:5cay, 12/07/00 EOO-1311 lClx E00-1311-3037-S1, 0 . 5mg/L,0hr, l:25clay, 12/07/00 EOO-1311 10x EOO-1311-3038-S1,0.5mg/L,0hr, l:25clay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 lOx E00-1311-3039-SI,0.5mg/L,Ohr, l:25clay, 12/07/00 E00-1311 lOx E00-1311-3039-S1,0.5mg/L,Ohr, l:25clay, 12/07/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-27-00 MLA Type Analyte Analyte Analyte Analyte Analyte Analyte 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 Blank Blank 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 Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Blank Blank Analyte Std Cone 2.50 5.00 10.00 25.00 40.00 50.10 75.10 100.20 250.40 500.90 1001.70 250.40 RT 7.080 7.082 7.079 7.092 7.091 7.092 7.080 7.094 7.093 7.082 7.082 7.092 7.089 7.092 7.082 7.079 7.079 7.101 7.091 7.089 7.079 7.080 7.093 7.093 7.092 7.094 7.080 7.080 7.082 7.081 7.091 7.091 7.104 7.091 7.092 7.089 7.105 7.105 7.093 7.103 7.093 7.093 7.094 7.094 250.40 7.086 7.105 7.098 7.109 7.094 250.40 250.40 250.40 250.40 7.106 7.115 7,106 7.105 7.104 7.106 7.103 7.104 7.092 7.091 7.106 7.106 7.092 7.104 7.105 7.093 7.091 7 .106 7.103 7.103 7.106 7.131 7.106 7.103 7.105 7.105 7.092 7.104 7.100 7.106 7.107 7.092 7.091 7.091 7.104 7.092 7.101 Page 1 Area 92 50144 46601 3 64 102 137 621 910 1561 3236 5034 5993 8189 9927 18824 29260 42301 262 123 78 117 534 805 1401 3018 4640 5547 7437 9567 18376 28180 40982 350 183 77 71 25 25 13130 227 14771 86 40 33 13912 67 13528 73 67 18197 97 53 23 13924 59 29 14015 18494 17814 82 13420 14735 64 27 2906 4003 6024 22183 17964 15658 55 24 18087 17898 23398 20000 20428 15260 72 77 20562 20568 137 86 52 108 p p b *Dev Flags M o d Co 0.00 bb bbl bbl 0.00 bb 0.00 bb 0.00 bb 0.00 -100 bb 0.00 -100 bb 0.00 -100 bb 14.34 -43 bb 33.17 -17 bb 48.19 -4 bb 86.02 15 bb 115.03 15 bb 269.69 8 bb 493.79 -1 bb 0.00 bbl bb 0.00 bb 0.00 bb 0.00 bb 0.00 -100 bbx 0.00 -100 bbx 0.00 -100 b b X 12.07 -52 bb 34.78 -13 bb 47.07 -6 bb 80.70 7 bb 115.72 15 bb 255.94 2 bb 469.41 -6 bb 848.70 -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 0.00 bb bb 289.20 0.00 0.00 15 bb bb bb 463.23 0.00 0.00 0.00 272.53 0.00 0.00 151.28 398.29 449.17 0.00 267.37 281.45 0.00 0.00 26.41 47.72 74.95 547.85 366.00 277.32 0.00 0.00 389.48 390.30 554.07 427.38 401.20 274.95 0.00 0.00 450.84 447.93 0.00 0.00 0.00 0.00 bb bb bb bb 9 bb bb bb bb bb bb bb bb 12 bb bb bb bb bb bb bb bb 11 bb bb bb bb bb bb bb bb 10 bb bb bb bb bb bb bb bb bb SOUP 020199: quantitated and printed by CMC on 12/11/00 3M Environmental Laboratory erne / u /cxj Page 529 of 703 BACK TO MAIN Quantify Compound Summary Report EOO-1311 PFOS Adsorb/Desorb Sample List: C:\Ma s s l y m A s o u p 0 2 0 1 9 9 . p r o \ S a m p l e D B \ s 0 0 1 2 0 7 Last modified: Mon Dec 11 09:05:24 2000 Method: C : \Ma33lynx\soup020199-pro\MethDB\*001207 Last modified: M o n Dec 11 09:10:27 2000 Job C ode: M o n Dec 11 09:23:38 2000 C o m pound 1: P F 0 8 (499>99), fune 1 # Name 90 sOO1207_090 91 sOO1207_091 92 s001207_Q 92 93 s0012Q 7_093 94 s0 0 1 2 0 7 _ 0 9 4 95 s001207_095 96 s0 0 1 2 0 7 _ 0 9 6 97 s0 0 1 2 0 7 _ 0 9 7 98 s0 0 1 2 0 7 _ 0 9 8 99 s 0 0 1 2 0 7 _ 0 9 9 100 s001207_100 101 s001207_101 102 s001207_102 103 s001207_103 104 sOQ12Q7_104 105 sOO1207_105 106 s001207_106 107 s001207_107 108 s001207_108 109 s001207_109 110 s0012Q7_110 111 s 0 0 1 2 0 7 _ lll 112 sOO1207_112 113 s 0 0 1 2 0 7 _ U 3 114 s001207_114 115 s001207_115 116 sOO1207_116 117 s001207_117 118 s001207_118 119 s001207_119 120 s001207_120 121 sOO1207_121 122 sOO1207_122 123 sOO1207_123 124 sOO1207_124 125 s001207_125 126 s001207_12 6 127 s001207_127 128 s001207_128 129 s001207_129 130 s001207_130 131 s001207_131 132 s001207_132 133 sOO1207_133 134 s001207_134 135 s001207_135 136 s001207_136 137 s001207_137 138 s001207_138 139 s001207_139 140 s001207_140 141 s001207,,141 142 s001207_142 143 s001207_143 144 s001207_144 145 s001207_145 146 sOO1207_146 147 sOO1207_147 148 s001207_148 149 s001207_149 150 s001207_150 151 sOO1207^151 152 s001207_152 153 sOO120 7 _153 154 s001207_154 155 s001207_155 156 s001207_156 157 s001207_157 158 s001207_158 159 s001207_159 160 s001207_160 161 sOO1207_161 162 s001207_162 163 s001207_163 164 s001207_164 165 s001207_165 166 s001207_166 167 s001207_167 168 s001207_168 169 s001207_169 170 s001207_170 171 s001207_171 172 s001207_172 173 s001207_173 174 s001207_174 175 sOO12Q7_175 176 s001207_176 177 sOO1207_177 178 s001207_178 study no Saraplelist Text EOO-1311 2.5 ppb PFOS 00002-86-02, Aliq. 11-27-00 MLA E O O - 1 3 11 5.00 ppb PFOS 00002-86-03, Aliq. 11-27-00 MLA EOO-1311 10.0ppb PFOS 00002-86-04, Aliq. 11-27-00 MLA EOO-1311 25.0ppb PFOS 00002-86-05, Aliq. 11-27-00 MLA EOO-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 EOO-1311 75.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA EOO-1311 100.2 ppb PFOS 00002-86-09, Aliq. 11-27-00 MLA EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 500.9 ppb PFOS 00002-86-11 Aliq. 11-27-QO MLA E00-1311 1001.7 ppb PFOS 00002-86-13, aliq. 11-27-00 MLA E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 lOx E00-l311-3040-Sl,0.5mg/L,2hr, l:lclay, 12/07/00 EOO-1311 lOx E00-1311-3041-S1.O.5mg/L,2hr, lslclay, 12/07/00 EOO-1311 lOx E00-I311-3042-Sl,0.5rag/L,2hr, l:lclay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 lOx EOO-1311-3042ms-SI,0.5mg/L,2hr, l:lclay, 12/07/00 EOO-1311 lOx EOO-1311-3043-SI,0.5mg/L,2hr, l:5clay, 12/07/00 EOO-1311 LOx EO0-1311-3044~Sl,0.Srag/L,2hr, l:5clay, 12/07/00 E00-1311 LOx E00~1311-3045-Sl,0.5mg/L,2hr, l:5clay, 12/07/00 EOO-1311 LOx E 0 0 - 1 3 U - 3 0 4 5 m s ~ S l , 0.5rog/L,2hr, l:5clay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 10x EOO-1311-3046-SI,0.5mg/L,2hr, l:25clay, 12/07/00 EOO-1311 lOx E00-1311-3047-SI,0.5mg/L,2hr, l:25clay, 12/07/00 EOO-1311 lOx E00-1311-3048-S1,0.5mg/L,2hr, l:25clay, 12/07/00 EOO-1311 lOx EO0-1311-3048ms-Sl,0.5mg/L,2hr, l:25clay, 12/07/00 E00-1311 10x B00-1311-3049-S1,0.5mg/L,4hr, l:lclay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq, 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 LOx B00-1311-3050-31,0.5mg/L,4h r , l:lclay, 12/07/00 EOO-1311 :.0x EO0-1311-3051-S1,0.5mg/L, 4hr, ltlclay, 12/07/00 EOO-1311 lOx EOO-13ll-3051ms-Sl,0.5mg/L,4hr, l:lclay, 12/07/00 EOO-1311 lOx E00-I311-3052-Sl,0.5mg/L,4hr, l:5clay, 12/07/00 EOO-1311 lOx EOO-1311-3053-S1,0.5ltig/L, 4hr, l:5clay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 lOx EO0-1311-3054-S1,0.5mg/L,4hr, l:5clay, 12/07/00 EOO-1311 lOx E00-1311-3054ms-SI, 0.5mg/L, 4hr, l : 5 d a y , 12/07/00 EOO-1311 lOx E00-1311-3055-SI,0.5mg/L,4hr, l:25clay, 12/07/00 EOO-1311 lOx E0-1311-3056-S1,0.5mg/L,4hr, l:25clay, 12/07/00 EOO-1311 lOx E00-13U-3057-Sl,0.5mg/L,4hr, l:25clay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. U / 1 6 / 0 0 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 ]Ox EOO-1311-3057ms-Sl,0.5mg/L,4hr, l:25ciay, 12/07/00 EOO-1311 l.Ox E00-1311-3067-S1,0.5mg/L, 1 6 h r , l:lclay, 12/07/00 EOO-1311 10x EOO-1311-3068-SI,0.5mg/L,16hr, l:lclay, 12/07/00 EOO-1311 lOx EO-1311-3069-S1,0.5mg/L,16hr, lslclay, 12/07/00 EOO-1311 1Ox EOO-1311-3 O69m s - S I ,O .5 m g / L ,16hr, l:lclay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO -1311 LOx EOO-1311-3070-S1,0.5mg/L,16hr, l:5clay, 12/07/00 E00-1311 lOx EOO-1311-3071-SI,0.5mg/L,16hr, l:5clay, 12/07/00 EOO-1311 1Ox E00-I311-3072-Sl,0.5mg/L,16hr, l:5clay, 12/07/00 EOO-1311 1Ox E00-1311-3072ms-SI,0 .5mg/L,16hr, l:5clay, 12/07/00 EOO-1311 1Ox E00-I311-3073-Sl,0.5rog/L,16hr, l:25clay, 12/07/00 EOO-1311 250.4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 E00-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 lOx E00-1311-3074-S1,0.5mg/L,16hr, l:25clay, 12/07/00 EOO-1311 lOx E00-1311-3075-51,0.5mg/L,16hr, l:25clay, 12/07/00 EOO-1311 lOx E O O -1311-3075ms-Sl,0 . 5mg/L,16hr,1:2Sclay, 12/07/00 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 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 0 ppb PFOS 00002-86-01, Aliq. 11-27-00 MLA E00-1311 2.5 ppb PFOS 00002-86-02, Aliq. 11-27-00 MLA EOO-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 EOO-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 E00-1311 50.1 ppb PFOS 00002-86-07 Aliq. 11-27-00 MLA EOO-1311 75.1 ppb PFOS 00002-86-08, Aliq. 11-27-00 MLA EOO-1311 100.2 ppb PFOS 00002-86-09, Aliq. 11-27-00 MLA EOO-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 EOO-1311 1001.7 ppb PFOS 00002-86-13, aliq. 11-27-00 MLA EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 EOO-1311 MeOH Blank, TN-A-4715, Aliq. 11/16/00 Type Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Blank Blank 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 Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte std Cone 2.50 5.00 10.00 25.00 40.00 50.10 75.10 100.20 250.40 500.90 1001.70 250.40 250.40 250.40 250.40 250.40 250.40 250.40 250.40 2.50 5.00 10.00 25.00 40.00 50.10 75.10 100.20 250.40 500.90 1001.70 RT 7.091 7.093 7.103 7.093 7.092 7.093 7.093 7.078 7.080 7.094 7.091 7.094 7.102 7.093 7.092 7.078 7.081 7.091 7.090 7.093 7.092 7.091 7.091 7.088 7.081 7.093 7.101 7.079 7.091 7,093 7.092 7.078 7.092 7.091 7.103 7.094 7.092 7.106 7.104 7.092 7.091 7.094 7.104 7.104 7.103 7.10 3 7.103 7.094 7.106 7.105 7.105 7.093 7.103 7.091 7.106 7.106 7.091 7.093 7.103 7.101 7.093 7.103 7.093 7.105 7.091 7.093 7.104 7.102 7.092 7.092 7.094 7.092 7.104 7,102 7.093 7.096 7.102 7.105 7.106 7.102 7.096 . 7.108 7.102 7.095 7.095 7.103 7.095 7.105 7.105 Page 2 Area 419 621 1098 2371 3561 4481 5972 7587 14437 21B88 33270 188 44 44 8077 6920 5280 14240 55 42 14422 1672 8831 8354 15956 14525 59 30 15297 15847 15684 20930 7184 14302 63 44 5740 6657 20690 7617 7312 15005 186 63 8406 16704 16616 16859 17098 15814 113 91 23164 7812 6696 10698 212 40 15733 77 36 8898 9049 9463 17151 17176 16217 71 39 16614 17931 23217 16363 87 61 141 98 410 646 1176 2556 3902 4700 6619 8118 15885 243 35 36145 225 130 ppb %Dev Flags Mod Co 0.00 -1O0 bbX 0.00 -100 bbX 0.00 -100 bbX 12.50 -SO bb 34.53 -14 bb 49.25 -2 bb 82.10 9 bb 112,16 12 bb 264.22 6 bb 484.43 -3 bb bbl 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 278.75 11 bb 0.00 bb 0.00 bb 317.10 bb 318.56 bb 326.30 bb 515.02 bb 113.88 bb 266-08 6 bb 0.00 bb 0.00 bb 88.39 bb 92.13 bb 431.57 bb 126-40 bb 113-16 bb 273.98 9 bb 0.00 bb 0.00 bb 136.92 bb 333.48 bb 326.15 bb 326.21 bb 319.46 bb 283.33 13 bb 0.00 bb 0.00 bb 525.54 bb 119.29 bb 99.92 166.04 433-97 276.31 bb bb bb 10 bb 0.00 bb 0-00 bb 140.62 bb 136.17 bb 152.02 bb 373.61 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 35-11 -12 bb 47.40 -5 bb 85.13 13 bb 114.14 14 bb 265.03 6 bb 492.46 -2 bb bbl 0.00 bb o.oo bb SOUP 020199: quantitated and printed by CMC on 12/11/00 3M Environmental Laboratory Page 530 of 703 BACK TO MAIN Q u a n tify Com pound S unroary R e p o rt E O O -1 3 1 1 PROS A d s o r b / D e s o r b S a m p le L i s t : b a s t m o d ifie d : M e th o d : L a s t m o d ifie d : Job Code: C : \M a s s ly n n \s o u p 0 2 0 1 9 9 .p ro \S a m p le D B \s 0 0 1 2 Q 7 Mon Dec 11 0 9 :0 5 :2 4 20 00 C :\M a s s ly n x \s o u p 0 2 0 1 9 9 .p ro \M e th D B \s 0 0 1 2 0 7 Mon Dec 11 0 9 :1 0 :2 7 2000 P rin te d : 1 Mon Dec 11 0 9 :2 3 :3 8 2000 C om pound 1 : PFOS ( 4 9 9 > 9 9 ), fu n e 1 # Name s tu d y no s a m p la lis t T e x t 179 sOQ12Q7_179 EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 Page 3 Type Analyte s td Cone RT 7.105 A rea 211 p p b % D ev F l a g s M o d Co 0.00 bb SOUP 0 2 0 1 9 9 : q u a n t i t a t e d a n d p r i n t e d b y CMC o n 1 2 / 1 1 / 0 0 3M Environm ental Laboratory CJnc i,3 /\ i /o O Page 531 of 703 3M Environmental Laboratory i SSIlIllSSlIISlIISSSIlSSISillSIIHISSlSSSlIIISllilSSSlSSIlSIllSIillISSSHiSl1 1\ I 51 I 1I Sl I I lit 11t t t 1 1 1 3 5 ! S S SI '1S ~iS S 3 S S S 1 5 3 ! S S S S S3 S 5 S S G 1 1 5 S & S S 1 G S S S GIS 3 S K S K G S 5 S 5 S E G G G S S g 3 g S S = l lllllllllllllllllllllillilllllilllillillllillll!llilllli||!illiliilliillllllil!|g|llllll|s ! gggggggggggggggggpgggggggggggggggggggggggggggggggggggggggggggggggggggggggggggggggggggggggs 1 l ? = - gg- s g g g g g - i sggggg' - s3gGgGgGGG' ^??gsssss??s sssss??s sssss J > > >- UJ O. 3 C TsM5H"ypohoyhyhS0h=h2IHoMoyM.H"WoHS^ jggg l!fIplii|iplfl|i||I= ! | l ? "l ! : ! : i l i i l l "? ! ! f l ggggggGSsGsEgggSvS5,,JJrM Sr.H H P rO O H ^^ ^ ^ " ^ S v U ^ ^ g gvg-"?g,?5ggi55^igS:=ZvvEi:EE:irn^i I - I W W s J | J -J -J J ! C ,J3 G G 3 ? 3 3 3 3 3 3 ? ? I? GG 33 g 3 E GG GG ;ss g g igg mr ip GGG 1 iGGt 333 gS ggg ?332 ggs S lffl "'GGGGGKj?-GG 333S3 S "i l i ? ? pRKl.ttK 33S33 S iH??r SPI.KGKGKG 5333 ;ggg ?g|igggg| p p iJ F S EE r-m m ini rmm mrm imm imm mir*i l * ' l ss5s ssss *ss s3 0 9 -8 *2 2 4 8 .6 0 2 4 8 .6 0 248.60 2 4 8 .6 0 2 4 8 .6 0 ggggggggggg a f 9 909 912 913 915 912 6 913 .9 14 .9 1 7 .9 07 .9 13 .9 14 6 .9 07 .9 14 .9 15 .9 24 .9 13 .9 14 6 .. 9 1 2 6 .9 14 .9 10 .9 15 924 .9 24 913 6 924 6 913 6 914 6 913 6 925 6 909 913 911 GgGGGK GSg|l gIlGIl li 3 2889 2593 3189 3064 3125 2657 2457 2712 2629 2467 2426 2401 2405 2355 2386 2381 2451 2505 2411 2439 2467 2342 2328 2440 2397 2508 2239 2102 2149 1819 2059 1777 1163 1560 1495 1851 1458 1636 1766 1570 1644 1719 1666 1762 2804 1774 1570 1798 1733 1819 1756 1776 2006 1714 1832 1955 1763 1742 1795 1825 1950 1918 1808 1816 s 212. 213. 207. 204. 210. 214. 228 . 225. S SGGSgS 329. 208. 184. 211. 203. 213. 207. 184. 193. 201. 195. 206 . 136. 183. 175. 217. 171. 192. 263. 246. 252. 213. 241. 208. 280 279 287 294 283 286 289 275 273. 286 281. 294. SSSSSSSSGSSS og S ss KSG32G 2 GGSSG ssgssg ssssss GGSSSS SS55S3 SgKSSSSSKSGG SSS53SGg5 ss 1 5 bb -1 b b 1 bb -15 bb -3 bb -16 bb -45 bb -2 7 bb -30 bb -13 bb -32 bb -23 bb -17 bb -2 6 b b -23 bb -19 bb -22 b b -17 bb 32 bb -17 bb -2 6 b b -16 bb -19 bb -14 bb -1 7 -1 7 -6 -1 9 -1 4 -8 -17 bb -18 bb -16 bb -14 bb -8 b b -9 bb -15 bb -15 bb 51 bb 45 bb 48 bb 26 bb 16 bb 28 bb 24 bb 17 bb 15 bb 13 bb 14 bb 11 b b SGGSGGGEGSGG gg ? bb bb bb bb bb bb ? SS?????????? Si 1 t s O ne la /u v Page 5 3 2 0f 703 BACK TO MAIN 3G BACK TO MAIN Quantify Compound Summary Report EOO-1311 Pros Adsorb/Desorb Sample List: C : \Masslynx\soup020199.pro\SarapleDB\3001207 Last modified: Mon Dec 11 09:05:24 2000 Method: C:\Masslynj<\3oup020199.pro\MethDB\s00l20? Last modified: Mon Dec 11 09:10:27 2000 Job Code: Printed: ---------4 ,------- Mon Dec 11 09:23:38 2000 Compound 2: THPFOS (427>80), fune 2 # Name 90 sOO1207_090 91 sOO12 07_091 92 S01207_092 93 s001207_093 94 s00 12 07 _09 4 95 s00 12 07 _09 5 96 sOO1207_096 97 sOO1207_097 98 sOO1207_098 99 s 00 1207_ 099 100 s001207_100 101 sOO12 07_101 102 S1207_102 103 s001207_103 104 s001207_104 105 s001207_105 106 s001207_106 107 sOO1207_107 108 s001207_108 109 sOO12 Q7_109 110 s001207_110 111 sOO1207_111 112 sOO1207_112 113 sOO1207_113 114 s001207_114 115 s001207_115 116 s001207_116 117 s001207_117 118 s001207_118 119 s001207_119 120 s001207_120 121 sOO12 07_121 122 s001207_122 123 sOO1207_123 124 sOO1207_124 125 s001207_125 126 s001207_126 127 s001207_127 128 s001207_128 129 s001207_129 130 sOO1207_130 131 s0012 07_131 132 s001207_132 133 sOO1207_133 134 sOO1207_134 135 s001207_135 136 s001207_136 137 sOO1207_137 138 s001207_138 139 sOO1207_139 140 s001207_140 141 sOO12 07_141 142 sOO1207_142 143 sOO1207_143 144 s001207_144 145 s0012 07_145' 146 sOO1207_146 147 sOO12O7_147 148 s001207_148 149 s001207,,149 150 s001207_150 151 s001207_151 152 s001207_152 153 s001207_153 154 s001207_154 155 s001207_155 156 s001207_156 157 s001207_157 158 s001207_15S 159 sOO1207_159 160 S01207_160 161 s0012 07_161 162 sOO1207_162 163 sOO1207_163 164 s001207_164 165 sOO1207_165 166 sOO1207_166 167 s001207_167 168 s00120?_168 169 s001207_169 170 s001207_170 171 s001207_171 172 sOO1207^172 173 s0 01 20 7,,1 73 .174 s001207_174 175 S001207_175 176 s001207_176 177 sOO1207_177 178 s001207_178 study no Sampleliat Text BOO-1311 2 . 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q . 1 1 - 2 7 - 0 0 MLA E0 0 -1 3 1 1 5 . 0 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 - 2 7 - 0 0 MLA E0 0 -1 3 1 1 1 0 . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 2 5 . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q . 1 1 - 2 7 - 0 0 MLA E 0 0- 13 11 4 0 . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 5 0 . 1 ppb PFOS 0 0 0 0 2 - 8 6 - 0 7 A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 7 5 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 1 0 0 . 2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 2 5 0 . 4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA E 0 0-1 311 5 0 0 . 9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 1 A l i q . 1 1 - 2 7 - 0 0 MLA E 0 0-1 311 1 0 p i . 7 ppb PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 - 2 7 - 0 0 MLA E 0 0-1 311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 E00-1311 lOx E00-1311-3040-SI, 0 . 5mg/L,2hr, l : l c l a y , 12/07/00 EOO-1311 lOx E0O-1311-3O41-S1,0 . 5 m q/L ,2hr, I r l c l a y , 12/0 7 /0 0 EOO-1311 lOx E 0 0 - 1 3 1 1 - 3 0 4 2 - S 1 , 0 . 5 m g /L ,2 h r, l s l c l a y , 1 2 /0 7 /0 0 EOO-1311 2 5 0 .4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 E0 0-1 311 lOx EOO- 1 3 1 1 - 3 0 4 2 m s - S I , 0 . 5mg/L, 2 h r , l s l c l a y , 1 2 / 0 7 / 0 0 EOO-1311 lOx E00 - 1 3 1 1 - 3 0 4 3 - S I , 0 . 5m g /L ,2 h r, l : 5 c l a y , 1 2 /0 7 /0 0 EOO-1311 lOx E 0 0 - I 3 1 1 ~ 3 0 4 4 -S l,0 .5 m g / L ,2 h r, l : 5 c l a y , 12/0 7 /0 0 EOO-1311 lOx E 0 0 - I 3 1 1 ~ 3 0 4 5 -S l,0 .5 m g / L ,2 h r, l : 5 c l a y , 1 2 /0 7 /0 0 E0 0-1 311 lOx EO0 - 1 3 1 1 - 3 0 4 5 r a s - S l , 0 . 5 m g / L , 2 h r , l : 5 c l a y , 1 2 / 0 7 / 0 0 E0 0 -1 3 1 1 2 5 0 , 4 ppb PFOS 0 0 0 0 2 - 8 6 - 1 0 , Aliq. 1 1 - 2 7 - 0 0 MLA EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 lOx E 0O-1311-3 O46-S 1,O. 5 m g /L ,2 h r, l : 2 5 c l a y , 1 2 /0 7 /0 0 EOO-1311 lOx E 0 0 - I 3 1 1 ~ 3 0 4 7 - S l , 0 . 5 m g / L , 2h r , l : 2 5 c l a y , 1 2 /0 7 /0 0 E0 0-1 311 LOx E O 0 - 1 3 1 1 - 3 O 4 8 - S 1 , 0 . 5mg/L, 2 h r , l : 2 5 c l a y , 1 2 / 0 7 / 0 0 E0 0-1 311 LOx EOO-1 3 1 1 - 3 0 4 8 m s - S l ( 0 . 5 m g / L , 2 h r , l : 2 5 c l a y , 1 2 / 0 7 / 0 0 E0 0-1 311 LOx E 0 0 - I 3 1 1 - 3 0 4 9 - S l , 0 . 5 m g / L , 4 h r , I r l c l a y , 1 2 / 0 7 / 0 0 EOO-1311 2 5 0 . 4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA E0 0-1 311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 E 0 0-1 311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 E00-1311 10x E00-I311-3Q50-Sl,0.5m g/L,4hr, I r lc l a y , 12/07/00 EOO-1311 10x E 0 0 - I 3 1 1 - 3 0 5 1 - S l , 0 . 5 m g / L , 4 h r , I r l c l a y , 1 2 /0 7 /0 0 EOO-1311 10x E 0 0 -1 3 1 1 -3 0 5 1 m s -S l,0 .5 m g /L . 4 h r, I r l c l a y , 12/0 7 /0 0 EOO-1311 LOx E 0 0 - 1 3 1 1 - 3 0 5 2 - S 1 , 0 . 5 ro g / L , 4 h r, I r S c l a y , 1 2 / 0 7 / 0 0 EOO-1311 :.0x E 0 0 - I 3 1 1 - 3 0 5 3 - S l , 0 . 5 m g / L , 4 h r, I r S c l a y , 1 2 /0 7 /0 0 E 0 0-1 311 2 5 0 . 4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 E 0 0-1 311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 EOO-1311 lOx E00-1 3 1 1 - 3 0 5 4 - S i , 0 . 5 m g/L ,4hr, l : 5 c l a y , 12 /0 7 /0 0 EOO-1311 lOx E 0 O ~1311-3O 54m s-S l,0.5 m g/L ,4hr, l : 5 c l a y , 12/0 7 /0 0 EOO-1311 10x E 0 0 - I 3 1 1 ~ 3 0 5 5 -S l,0 .5 m g / L ,4 h r, l : 2 5 c l a y , 12/0 7 /0 0 EOO-1311 l.Ox E0 0 - 1 3 1 1 - 3 0 5 6 - 3 1 , 0 . 5mg/L, 4h r , l : 2 5 c l a y , 1 2 / 0 7 / 0 0 E00-1311 lOx EOO-1311-3057-Sl,O.Smg/L,4hr, l:2 5 c la y , 12/07/00 EOO-1311 2 5 0 . 4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 E00-1 311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 EOO-1311 lOx E 0 0 -1 3 ll~ 3 0 5 7 m s ~ S l, 0 . 5 m g/L ,4hr, l : 2 5 c l a y , 12/0 7 /0 0 EOO-1311 lOx E 0 0 - 1 3 1 1 - 3 0 6 7 -S l,0 .5 m g / L ,1 6 h r, I r l c l a y , 12/0 7 /0 0 E00-1311 lOx E 00-I311-3068-Sl,0.5m g/L,16hr, I r lc l a y , 12/07/00 EOO-1311 lOx E 0 0 - I 3 1 1 - 3 0 6 9 - S l , 0 . 5 m g / L , 1 6 h r , I r l c l a y , 1 2 /0 7 /0 0 E00-1311 lOx E00-1311-3069ms-Sl,O.Smg/L,16hr, I r lc l a y , 12/07/00 EOO-1311 250-4 ppb PFOS 00002-86-10, Aliq. 11-27-00 MLA EOO-1311 MeOH B l a n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 E 0 0- 13 11 MeOH B l a n k , TN- A-4715, A l i q , 1 1 / 1 6 / 0 0 E00-1311 lOx E0O-1311-3O7O-S1,0.5mg/L,16hr, IrSclay, 12/07/00 E00-1311 lOx E00-I311-3071-Sl,0.5m g/L,16hr, IrS c la y , 12/07/00 EOO-1311 lOx E 0 0 - 1 3 1 1 - 3 0 7 2 ~ S l , 0 . 5 m g / L , 1 6 h r , l : 5 c l a y , 1 2 /0 7 /0 0 EOO-1311 lOx E0 - 1 3 1 1 - 3 0 7 2 m s - S l , 0 . 5 m g / L , 1 6 h r , l r 5 c l a y , 1 2 / 0 7 / 0 0 E00-1311 lOx E0O-1311-3O73-S1,0.5mg/L,16hr, l:2 5 c la y , 12/07/00 EOO-1311 2 5 0 . 4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 MeOH B l a n k , TN -A -47 15, A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 E00-1311 lOx E00 -1 3 1 1 - 3 0 7 4 - S I , 0 . 5m g/L,1 6hr, l : 2 5 c l a y , 12/07/00 EOO-1311 lOx E0O-131 1 -3 O 7 5 -S 1 ,0 . 5 m g /L ,1 6 h r, l : 2 S c l a y , 1 2 /0 7 /0 0 E00-1311 lOx BO0-1311-3 075RIS-S1,0 . 5mg/L, 16hr, l : 2 5 c l a y , 12/07/00 E0 0 -1 3 1 1 2 5 0 . 4 p p b PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA E0 0-1 311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 E 0 0-1 311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 EOO-1311 MeOH B l a n k , TN- A-4715, A l i q . 1 1 / 1 6 / 0 0 E 0 0- 13 11 0 p p b PFOS 0 0 0 2 - 8 6 - 0 1 , A l i q . 1 1 - 2 7 - 0 0 MLA E00-1 311 2 . 5 ppb PFOS 0 0 0 0 2 - 8 6 - 0 2 , A l i q . 1 1 - 2 7 - 0 0 MLA E0-1311 5 . 0 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 , A l i q . 1 1 - 2 7 - 0 0 MLA E 0 0-1 311 1 0 .0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 , A l i q . 1 1 - 2 7 - 0 0 MLA E00-1 311 2 5 . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 , A l i q . 1 1 - 2 7 - 0 0 MLA E 0 0-1 311 4 0 .0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 , A l i q . 1 1 -2 7 - 0 0 MLA EOO-1311 5 0 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 7 A l i q . 1 1 - 2 7 - 0 0 MLA E00-1 311 715.1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 LOO.2 ppb PFOS 0 0 0 0 2 - 8 6 - 0 9 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 2 5 0 .4 ppb PFOS 0 0 0 0 2 - 8 6 - 1 0 , A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 5 0 0 .9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 1 A l i q . 1 1 - 2 7 - 0 0 MLA EOO-1311 1 0 0 1 . 7 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 , a l i q . 1 1 - 2 7 - 0 0 MLA E00-1 311 MeOH B la n k , TN-A -47 15, A l i q . 1 1 / 1 6 / 0 0 E00-1 311 MeOH B l a n k , TN-A -47 15, A l i q . 1 1 / 1 6 / 0 0 Type Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Blank Blank Analyte Analyte Analyte oc 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 Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Std Cone 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 6.900 248.60 6.912 6.898 6.902 6.899 248.60 6.901 6.899 6.912 6.897 6.901 6.902 248.60 6.900 6.901 6.913 6.899 6.901 6.900 248.60 248.60 6.901 6.914 6.913 6.901 6.912 6.914 6.912 6.924 6.923 6.924 6.915 6.928 6.913 248.60 6.912 6.912 6.915 6.914 6.912 6.913 248.60 6.913 6.923 6.914 6.913 6.911 6.913 248.60 6.912 6.912 6.914 6.913 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 248.60 6.917 6.910 6.925 6.915 6.922 6.917 6.915 6.911 6.915 6.916 6.912 6.915 Page 5 Area 1909 1930 1903 1875 1879 1941 1858 1889 1871 1822 1904 ppb %Dev Flags Mod Co 224.21 -10 bb 226.74 -9 bb 223.57 -10 bb 220.27 -11 bb 220.74 -11 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 -20 bb -10 bb -12 bb -18 bb -15 bb -11 bb bb 213.05 214.36 216.79 219.93 226.57 228.17 -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 2 2 3 .44 231.38 -14 bb -12 bb -14 bb -6 bb -11 bb -7 bb 1882 1961 1886 1723 1887 2045 221.02 230.30 221.54 202.41 221.66 240.24 -12 bb -8 bb ~11 bb -19 bb -11 bb -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: quantitated andl printed by CMC on 12/11/00 3M Environm ental Laboratory C -M C 1*2/ i i / o G Page 533 of 703 BACK TO MAIN Quantify compound Suionary Report EOO-1311 PF08 Adsorb/Desorb Page 6 Sample List: C:\Masslyn>L\soup020199pro\SaropleDB\s001207 Last modified: Mon Dec 11 09:05:24 2000 Method: C:\Masslynx\soup020199.pro\MethDB\s001207 Last modified: Mon Dec 11 09:10:27 2000 Job Code: p_r_inAt_ed_: ____Mo_n_D_ec__11_0_9:_23_:_38_2_00_0____________________________________________ _________________ Compound 2 : THPFOS (427>80)# func 2 # Name study no Samplellst Text 179 s00 12 07 _ 17 9 EOO-1311 MeOH B la n k , TN- A-4 715 , A l i q . 1 1 / 1 6 / 0 0 Type Analyte Std Cone RT Area ppb SDev Flaas Mod Co SOUP 020199: Quantitated and printed by CMC on 12/11/00 3M Environm ental Laboratory t/u/o Page 534 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Decatur.PRO\SampleDB\t001215 Last modified: Mon Deo 18 10:45:28 2000 Method: C:\MASSLYNX\Decatur.PRO\MethDB\001215 Last modified: Mon Deo 18 10:50:01 2000 Job Code: Printed: Mon Dec 18 10:56:20 2000 ---- T------------------------------------------------ Compound 1: PFOS(499) 4 Name 1 t 0 0 1 2 1 5 001 2 t001215 002 3 t 0 0 1 2 15 003 4 t0 0 1 2 1 S _ 004 5 t0012l5~~005 6 t001215 006 7 t 0 01215 007 8 t001215 008 9 t001215 009 10 tQ01215_ 010 11 t 0 0 1 2 1 5 O il 12 t 0 0 1 2 1 5 _ 012 13 t 0 0 l 2 1 S _ 0 1 3 14 t 0 0 1 2 1 5 014 15 t 0 0 1 2 1 5 015 16 t001215 016 17 t 0 0 l 2 1 5 017 18 t 0 0 l 2 1 5 01B 19 1001215 019 20 t001215 020 21 t0 01 2 1 5 _ 0 2 1 22 t 0 0 l 2 1 5 022 23 t 0 0 l 2 1 5 023 24 t0 0 1 2 1 5 024 25 t 0 0 1 2 15 025 26 t001215~026 27 t 0 0 l 2 1 5 " 027 28 t 0 0 l 2 1 5 02B 29 t001215_029 30 t001215~030 31 t 0 0 1 2 15 031 32 t 0 01215_ 032 33 t 0 0 1 2 1 5 033 34 t 0 0 1 2 15 ~0 34 35 t00l21S~035 36 t 0 0 l 2 1 5 036 37 t 0 0 l 2 1 5 037 38 t0 0 1 2 1 5 038 39 t 0 01215 039 40 t0Q121 5~0 40 41 t 0 0 l 2 1 5 041 42 t 0 0 1 2 1 5 042 43 t 0 0 1 2 1 S 043 44 t 0 0 1 2 1 5 044 45 t 0 0 1 2 1 S _ 045 46 t001215~046 47 t 0 0 l 2 1 5 047 48 t0 0 1215_048 49 t 0 0 1 2 1 5 _ 049 50 t00l215~050 51 t001215~Q51 52 t 0 0 l 2 1 5 _ 0 5 2 53 tOO1215 053 54 t 0 0 1 2 1 5 054 55 t0 0 1 2 1 5 ~ 0 5 5 56 t0 0 l2 1 5 _ 0 5 6 57 t0 0 1 2 1 5 ~ 0 5 7 58 t001215~058 59 tOO1215 059 60 t001215 060 61 t001215 ~0 61 62 t 0 0 l 2 1 5 062 63 t 0 0 l 2 1 5 063 64 t 0 0 1 2 15 ~0 64 65 t001215_065 66 t001215~066 67 t0 0 1 2 1 5 067 68 t 0 0 1 2 1 5 068 69 t 0 0 l 2 1 5 _ 069 70 t00l215~070 71 t 0 0 1 2 1 5 ~ 071 72 t 0 0 1 2 15~072 73 1 001215 073 74 t 0 0 l 2 1 5 ~ 0 7 4 75 t 0 0 l 2 1 5 075 76 tOO1215 076 77 t 001215 077 78 t 0 0 l 2 1 5 ~ 0 7 B 79 t 0 0 l 2 1 5 079 80 t 0 0 l 2 1 5 080 81 t 0 0 1 2 1 5 081 82 t 0 0 l 2 1 5 082 Samplelxst Text MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN -A -47 40, A l i q . 1 0 0 1 . 7 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 1 0 0 1 . 7 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 2 . 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 10 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 25 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 40 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 5 0 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 7 7 5 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 1 0 0 . 2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 2 5 0 . 4 p p b PFOS 0 00 0 3 -1 4 1 5 0 0 . 9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 2 1 0 0 1 . 7 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 MeOH B l a n k , T N- A- 47 4 0, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . 0 p p b PFOS 0 0 0 0 2 - 0 6 - 0 1 2 . 5 p p b PFOS 0 0 0 0 2 - 0 6 - 0 2 5 p p b PFOS 0 0 0 0 2 - 0 6 - 0 3 10 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 25 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 40 p p b PFOS 0 0 0 0 2 - 0 6 - 0 6 5 0 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 7 7 5 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 1 0 0 . 2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 2 5 0 . 4 p p b PFOS 00 00 3- 14 1 5 0 0 . 9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 2 1 0 0 1 . 7 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN- A-4 740 , A l i q . lOx EOO-1311-3007 1 Ox E 0 0- 13 11 - 3O 0 8 lOx EOO-1311-3009 lOx EOO-131 1 - 3 0 0 9ms lOx E00-1311-3010 2 5 0 . 4 p p b PFOS 0 0 0 0 3 -1 4 1 MeOH B l a n k , T N- A- 47 4 0, A l i q . MeOH B l a n k , T N- A- 47 4 0, A l i q . lOx E0-1311-3011 lOx E 0 0-1311-3012 lOx EOO-13ll-3012m3 lOx EOO-1311-3130 lOx EOO-1311-3131 2 5 0 . 4 p p b PFOS 00 00 3- 14 1 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx EOO-1311--3132 1 Ox EOO-1311-3132ms lOx EOO-1311-3133 lOx EO O -1 31 1- 3134 10x E00-1311-3135 2 5 0 .4 p p b PFOS 00 00 3- 14 1 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx E 0 0 - 1 3 1 1 - 3 1 3 5ms lOx EOO-1311-3136 1 Ox EOO-131 1 -3 13 7 lOx EOO-1311-3138 lOx EOO-131 1 - 3 1 3 Bras 2 5 0 . 4 p p b PFOS 0 0 00 3 -1 4 1 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx EOO-1311-3139 lOx EOO-1311-3140 lOx 00-1311-3141 lOx EOO-1311-3141ms lOx EOO-1311-3142 2 5 0 . 4 p p b PFOS 00 00 3- 14 1 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx EOO-1311-3143 lOx EOO- 13 11-314 4 lOx E0 0 - 1 3 1 1 -3 1 4 4ras 10x EOO-L311-3145 lOx EOO--.1311--3146 2 5 0 . 4 p p b PFOS 00 00 3- 14 1 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC RT 6.481 6.371 6.488 6.489 6.433 6.400 6.417 6.425 6.445 6.377 6.496 6.484 6.417 6.481 6.445 6.200 6.180 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 6.284 6.469 6.400 6.481 6.411 6.488 6.443 6.237 6.401 6.292 6.260 6.406 6.485 6.476 6.445 6.245 6.420 6.437 6.361 6.485 6.429 6.4B4 6.453 6.360 6.375 6.240 6.207 6.256 6.272 6.473 6.423 6.268 6.489 6.470 6.480 6.478 6.488 6.484 Area 53206 30800 4641528 4 64 0503 36137 35552 35344 39095 61396 77059 119454 208147 296693 386893 542145 739832 1625157 2627391 4126B45 31200 20732 25271 32948 49820 64675 101190 203395 284054 345882 518826 638622 1490467 2357038 3944487 24270 23252 30587 27578 25569 1007052 26288 1371544 28127 25682 21374 25538 998865 587042 571685 1447645 27552 25476 492412 1536932 2205944 1406285 1523976 1529689 29026 26218 2204358 1996143 1996672 1935361 2548079 1536839 28963 28028 422345 583342 374356 1431728 1543781 1488024 28021 25200 1494674 1597102 2263636 2027915 1986134 1569815 Response ppm Flags 0.000 0.0 0 bb 0.000 0.00 bb 10770.559 729.75 bb 10872.952 740.43 bb .000 0.00 bb 0.000 0.00 bb 0.000 0.00 bb 99.457 0.00 bb 159.598 0.00 bb 200.633 0.00 bb 371.309 7 .6 8 bb 786.844 29.54 bb 1031.971 42.60 bb 1312.849 57.71 bb 1854.385 87.31 bb 2414.604 118.62 bb 5012.082 274.48 bb 8760.561 545.53 bb 15693.600 bbl 0.000 0.00 bb 0.000 0.00 bb 0.000 0.00 bb 107.336 0.00 bb 165.290 0.00 bbX 217.657 0 .0 0 bbX 349.543 6.54 bbX 720.329 26.02 bb 939.183 37.64 bb 1179.832 5 0 ,5 3 bb 1802.378 84.44 bb 2183.075 105.59 bb 5091.336 279.56 bb 8220.976 501.26 bb 13555.334 1123.76 bb 0.000 0.00 bb 0.000 0.00 bb 116.821 0.00 bb 104.562 0.00 bb 94.837 0.00 bb 3974.570 209.90 bb 101.042 . 0 .0 0 bb 5035.394 275.97 bb 0.000 0.00 bb 0.000 0.00 bb 78.074 0.00 bb 97.150 0.00 bb 3638.345 189.67 bb 2059.048 98.66 bb 1956.716 92.97 bb 5035.467 275.98 bb 0.000 0.00 bb 0.000 1849.585 0.00 bb 87.04 bb 4835.963 263.27 bb 6828.949 396.95 bb 4365.327 ' 233.83 bb 4958.838 271.08 bb 4997.809 273.57 bb 0.000 0.00 bb 0.000 0.00 bb 7547.557 449.46 bb 5741.427 322.07 bb 6032.791 341.64 bb 6022.490 340.94 bb 7906.309 476.71 bb 4764.796 258.78 bb 0.000 0.00 bb 0.000 0.00 bb 1448.580 65.07 bb 1737.042 80.84 bb 1095.122 45.98 bb 4389.666 235.33 bb 4605.736 248.78 bb 4509.151 242.75 bb 0.000 0.00 bb 0.000 0.00 bb 4578.029 247.05 bb 4 918.225 268.50 bb 7136.543 419.10 bb 6235.222 355.44 bb 5982.209 338.22 bb 4638.272 250.82 bb %Dev -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 Page 1 Quantitated and Printed by CMC on 18 Dec 00, Study E00-1311 . 3M Environm ental Laboratory f'sm c W /< r/o Page 535 of 703 BACK TO MAIN Quantify Compound Summary Ftport PFOS Adsorb/Desorb Study LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Decatur. PRO\SampleDB\t001215 Last modified: Mon Dec 18 10:45:28 2000 Method: C:\MASSLYNX\Decatur.PRO\MethDB\001215 Last modified: Mon Dec 18 10:50:01 2000 Job Code: Printed: Mon Dec 18 10:56:20 2000 ---- 1----------------------------- Compound 1: PFOS(499) # Name 83 t 0 0 1 2 1 5 _ 0 8 3 84 t0 0 1 2 1 5 084 85 t0 01215~085 86 t001215~086 B7 t 0 0 1 2 1 5 _ 0B7 88 t 0 0 1 2 1 5 088 89 t001215~089 90 t001215~090 91 t 0 0 1 215 ~0 91 92 t001215_ 092 93 t0 0 1 2 1 5 _ 093 94 t 0 0 1 2 1 5 094 95 t001215_ 095 96 t001215 096 97 t 0 0 1 2 1 5 ~ 097 98 t001215 098 99 t 0 0 1 2 1 5 099 100 t001215~100 101 t 0 01215 101 102 t001215 102 103 t001215~103 104 t0 01 215 ~1 04 105 t 0 0 1 2 15 105 106 t001215~106 107 t001215~107 108 t001215 108 109 t0 01215 109 110 t001215 110 111 t001215~111 112 t001215~112 113 t 0 0 1 2 1 5 _ 113 114 t 00 1215 ~1 14 115 t 0 0 l 2 1 5 ~ l 15 116 t 0 0 1 2 1 5 _ l 16 117 t 0 01215_ 117 118 t 0 0 1 2 15 118 119 t001215~119 120 t 001215^120 121 t 0 0 1 2 1 5 ~ 121 122 t 0 0 l 2 1 5 122 123 t 0 01215 123 124 tOQ121S_ 124 125 t001215~125 126 t001215 126 127 t 0 01215 127 128 t001215 128 129 t001215~129 130 t001215 130 131 t001215~131 132 t0 01215 132 133 t0 0 l 2 1 5 _ 133 134 t 0 0 12 15 _13 4 135 t o o i2 is ~ i3 s 136 t 0 0 1 2 15 136 137 t00X215_137 138 t001215_138 139 t001215~139 140 t 0 0 1 2 1 5 _ 140 141 t 0 0 1 2 1 5 _ 141 142 t 0 0 l 2 1 5 ~ 142 143 t0 0 1 2 1 5 143 144 t001215__144 145 t001215~14S 146 t 0 0 1 2 15 146 147 t001215~147 148 t O O l 215 14-8 149 t001215~14 9 150 t 0 0 l 2 1 5 " l50 151 t 0 0 1 2 1 5 _ 151 152 t00l2 1 5 ~ 1 5 2 153 t 0 0 1 2 1 5 _ 153 154 t 0 0 1 2 1 5 _ 154 155 tOO1215~155 156 t00l215~156 157 t001215~157 158 t001215~158 159 t 0 0 l 2 1 5 159 160 t 0 0 l 2 1 5 160 161 t 0 0 12 15~ 1 61 162 t00l215~*162 163 t 0 0 1 2 15 163 164 t 001215^164 Saoplelist Text MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -4 74 0, A l i q . lOx E 0 0 -1311-3147 lO x E 0 0 - 1 3 1 1 - 3 1 4 7m3 l O x E 0 0 - 1 3 1 1 - 3 14 0 lOx 00-1311-3149 lOx E0-1311-3150 2 5 0 . 4 p p b PFOS 0 0 0 03 -1 4 1 MeOH B l a n k , T N- A- 47 4 0, A l i q . MeOH B l a n k , T N- A- 47 4 0, A l i q . lO x E 0 0 - 1 3 1 1 - 3 150ms lOx EOO-1311-3151 10X E 0 0 - 1 3 1 1 -3 15 2 lOx E00-1311-3153 lOx EOO-131 1 - 3 153ras 2 5 0 . 4 ppb PFOS 0 0 0 03 -1 4 1 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN- A-4 740 , A l i q . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 2 . 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 10 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 25 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 40 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 5 0 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 7 7 5 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 1 0 0 . 2 p p b PFOS 0 0 0 0 2 - 8 6 - 0 9 2 5 0 . 4 p p b PFOS 0 0 0 03 -1 4 1 5 0 0 . 9 p p b PFOS 0 0 0 0 2 - 8 6 - 1 2 1 0 0 1 . 7 pp b PFOS 0 0 0 0 2 - 8 6 - 1 3 MeOH B l a n k , T N- A- 47 4 0, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx EOO-1311-3154 1 Ox EOO-.1311 -3 15 5 10X EOO-1311-3 156 l O x EOO-131 1 - 3 1 5 6ms XOx EOO-131 1 -3 15 7 2 5 0 . 4 p p b PFOS 0 0 0 0 3 -1 4 1 MeOH B l a n k , T N- A- 47 4 0, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . 10X EOO-131 1-3 15 8 lOx EOO-1311-3159 lOx EOO-131 1 - 3 159ni3 lOx EOO-1311-3160 lOx EOO--3.311--3161 2 5 0 . 4 p p b PFOS 0 0 0 0 3 -1 4 1 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , T N- A- 47 4 0, A l i q . lOx EOO-1311-3162 lOx EOO-1.311-3162ms lOx EOO-1311-3163 10X EOO-1311 -316 4 lOx E 0 0 - 1 3 1 1 - 3 1 65 2 5 0 . 4 p p b PFOS 00 00 3 -1 4 1 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx E00-1311-3165ms lOx EOO-1311-3166 lOx EOO-1311-3167 lOx E0-1311-3168 lOx EO0 - 1 3 1 1 - 3 1 68ras 2 5 0 .4 p p b PFOS 0 0 0 03 -1 4 1 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx E00-]311-3169 lOx EOO-]311-3170 lOx E00-1311-3171 lOx EOO-]311-317lm s lOx E 0 0 -]311-3172 2 5 0 .4 p p b PFOS 0 0 0 03 -1 4 1 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN- A-4740, A l i q . lOx EOO-1311 -317 3 lOx EOO-l311-3174 lOx EOO-l3 1 1 - 3174ms 2 5 0 .4 p p b PFOS 0 0 0 03 -1 4 1 MeOH B l a n k , TN- A-4 740 , A l i q . MeOH B l a n k , TN- A-4740, A l i q . lOx E00-1311-3184 lOx E0-1311-3185 lOx EOO-1311-3186 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 CMC 1 2 / 0 4 / 0 0 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 6.4 08 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 6.427 6.363 6.328 6.413 6.369 6.393 6.473 6.484 6.464 6.448 6.393 6.264 6.332 6.484 6.232 6.328 6.486 6.463 6.478 6.441 6.408 6.359 6.376 6.482 6.472 6.473 6.212 6.235 6.192 6.1B0 Area 27890 25986 2160923 2795560 467443 434046 307296 1592065 27504 26941 1372094 1471355 1462737 1400633 2166717 1624666 26765 29157 28941 27909 52247 65529 994BO 199217 299906 351140 531280 725423 1529458 2508341 4217609 26339 24228 1932000 1937864 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 2138339 1909649 1569463 25530 25032 1924000 1823228 2505717 1551613 32065 28836 27853 27101 25663 Response 0.000 0.000 6233.710 8625.720 1570.404 1307.942 917.941 4791.048 0.000 0.000 4490.274 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 7947.153 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 8 6 7 1 . B69 1514.172 1362.001 804.620 3928.931 5042.004 0.000 0.000 3790.616 4423.367 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 ' . ppm 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 .0 0 bbX 0 .0 0 bbX 3.05 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 212.07 bb 272.38 bb 0.00 bb 0.00 bb 253.48 bb 368.04 bb 319.84 bb 318-04 bt> 371.72 bb 287.97 bb 0.00 bb 0.00 bb 537.56 bb 68.64 bb 60.37 bb 30.48 bb 207.13 bb 276.40 bb 0.00 bb 0.00 bb 198.79 bb 237.42 bb 196.59 bb 361.74 bb 304,44 bb 247.42 bb 0.00 bb 0.00 bb 368,92 bb 346,68 bb 443.98 bb 239.44 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb %Dev od Comment 4 2 -100 -100 -61 -21 -9 -13 2 10 10 -8 -3 -6 9 15 10 -1 -4 Page 2 Quantitated and Printed by CMC on 18 Dec OO, Study EOO-1311 3M Environm ental Laboratory t em c (9- h t,/d c Page 536 of 703 BACK TO MAIN Quantify Compound Summary Report PFOS Adsorb/Desorb Study LC/MS Instrument: Tucker (LA052) Sample List: C:\MASSLYNX\Decatur-PRO\SampleDB\t001215 Last modified: Mon Dea 18 10:45:28 2000 Method: C: \MASSLYNX\Decatur.PRO\MethDE\G012l5 Last modified: Mon Dec 18 10:50:01 2000 Job Code: Printed: Mon Dec 18 10:56:20 2000 --- T----------------------------- Compound 1: PFOS(499) V Name 165 t 0 01215 165 166 t001215_ 166 167 t001215~167 168 t001215_168 169 t001215_169 170 t 0 0 1 2 1 5 --170 171 t 0 0 1 2 1 5 ~ 171 172 t0 01215 172 173 t001215~173 174 t0 0 1 2 1 5 174 175 t0 01215 175 176 t 0 0 1 2 15 176 177 t0 0 1 2 1 5 - 177 170 t00121S 178 179 t001215~179 180 t0 01215 100 181 t 0 0 1 2 1 5 _ 181 182 t001215~182 183 t0 01215 103 184 t 0 0 1 2 1 5 184 185 t0 01215 185 186 t001215~186 187 t001215~187 188 t0 01215 188 189 t001215 189 190 t0 0 1 2 l 5 _ 190 191 t 0 0 1 2 l 5 191 192 t0 0 1 2 l 5 192 193 t00121S~193 194 t 0 0 1 2 1 5 ~194 195 t0 01215 195 196 t0012l5_196 197 t 0 0 1 2 l 5 ~ 197 198 t001215 198 Samplelist Text lOx EOO- 1 3 1 1 - 3 1 8 6ms lOx EOO-1311-3187 2 5 0 .4 ppb PF0S 00003 -1 41 MeOH B l a n k , T N - A -4 74 0, A l i q . MeOH B l a n k , TN -A -4 74 0, A l i q . lOx EOO - 1 3 1 1 - 3 1 8 8 lOx BOO-1311-3189 lOx E00"1311-3189ms lOx BOO-1311-3190 lOx EOO-1311-3191 2 5 0 .4 p p b PFOS 0 00 0 3 -1 4 1 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . lOx BOO-1311-3192 lOx EOO--131 1 - 3 192ms 2 5 0 . 4 p p b PFOS 0 00 0 3 -1 4 1 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN -A -4 74 0, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . 0 p p b PFOS 0 0 0 0 2 - 8 6 - 0 1 2 . 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 2 5 p p b PFOS 0 0 0 0 2 - 8 6 - 0 3 10 p p b PFOS 0 0 0 0 2 - 8 6 - 0 4 25 p p b PFOS 0 0 0 0 2 - 8 6 - 0 5 40 p p b PFOS 0 0 0 0 2 - 8 6 - 0 6 5 0 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 7 7 5 . 1 p p b PFOS 0 0 0 0 2 - 8 6 - 0 8 1 0 0 . 2 ppb PFOS 0 0 0 0 2 - 8 6 - 0 9 2 5 0 . 4 p p b PFOS 0 00 0 3 -1 4 1 5 0 0 . 9 ppb PFOS 0 0 0 0 2 - 8 6 - 1 2 1 0 0 1 . 7 p p b PFOS 0 0 0 0 2 - 8 6 - 1 3 MeOH B l a n k , TN -A -47 40, A l i q . MeOH B l a n k , TN-A -47 40, A l i q . MeOH B l a n k , TN -A -47 40, A l i q . 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 CMC CMC CMC CMC CMC CMC CMC CMC CMC CMC RT 6.189 6.200 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 . 4 B0 6.481 6.421 6.482 6.48 6 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 33876 32005 24369 24595 1090006 26337 26588 1712977 32775 29504 26709 1122264 1590409 26766 26510 27913 31350 51199 72994 106025 197302 300365 36B099 547191 716285 1792194 2783510 4584416 23461 23905 25693 Response 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 0.00 bb 0.00 bb 0.00 bb 166.28 bb 0.00 bb 0.00 bb 257.05 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 .0 0 bbX 0 . 0 0 bbX 4 . 6 2 bbX 18.32 bb 33.49 bb 43.68 bb 72.10 bb 107.30 bb 2 6 7 . 8B bb 469.98 bb 959.07 bb Q.00 bb 0.00 bb 0.00 bb %Dev 1 3 11 -100 -100 -54 -27 -16 -13 -4 7 7 -6 -4 Page 3 Quantitated and Printed by GMC on 18 Dec 00, Study E00-1311 3M Environm ental Laboratory One (/(th e Page 537 of 703 BACK TO MAIN Q uantity Coapwgnd g u m *00-1i l l rroa Adaorb/Da Ampia L ia t: C:\H aaalynx\aoup020199.pro\Saqila01\a0013U U t x o d iila d : Wad Dae 13 04:47:59 2000 Hathod: C: \Kaaalynx\aoup020199. pre\K*EhOB\*001211 Laat a d i t lad: Job Coda: Nad Dac 11 0:$:* 2000 Ccaapound 1: PFOS (499>99), tunc 1 Nana tudy no Baxplaliat Txt 1 q$mi_ooi 00-1311 KaOH Blank, m-A-4715, A liq . 11/16/00 2 a001211.002 00-1311 1001.1 ppb PFOS 00002-06-13, a l i q . 11-27-00 MLA Typ Analyte Analyc, ) 0ffl2ll_003 00-1311 1001.7 ppb PPOS 00002-06-13. a l i q . H -2 7 -0 0 MLA Analyta 4 a001211.004 00-1311 MaOH Blank, TN-A-4715, A liq . 11/16/00 5 #001211.005 00-1311 KaOH Blank. TN-A-4715. A liq . 11/16/00 Analyta 6 #001211.006 00-1311 0 ppb pros 00002-06-01, A liq . 11-27-00 KLA A n aly to 2 a0012 11.007 00-1311 2 .5 ppb PFOS 00002-06-02, A liq . 11-27-00 KLA Analyta 0 #001211.000 00-1331 5.00 ppb Pros 00002-06-03. A liq . 11-27-00 HU Analyta 9 #001211.009 00-1311 10.0 ppb PFOiS 00002-86-04, A liq . 11-27-00 HU 10 001211.010 00-1311 2S.0 ppb pro:: 00002-86-05, A liq . 11-27-00 HU 11 *001211.011 00-1311 40.0 ppb PF: 00002-86-06, A liq . 11-27-00 HU Analyta 12 #001211.012 00-1311 50.1 ppb PFO:; 00002-06-07 A liq . 11-27-00 HU Analyta 13 001211.013 EOO-13U 75.1 ppb PPOS 00002-86-00, A liq . 11-27-00 HU Analyta 14 #001211.014 00-1311 100.2 ppb PFOS 00002-86-09, A liq . 11-27-00 MU Analyta 15 #001211.015 00-1311 250,4 ppb PFOS 00002-06-10, A liq . 11-27-00 MU 16 #001211.016 00-1311 400.7 ppb PFOS 00002-06-11, A liq . 11-27-00 MU A n aly ta 17 #001211.017 00-1311 S00.9 ppb PFOS 00002-86-12 A lia - 11-27-00 MU Analyta 00-1311 1001.7 ppb PFOS 00002-86-13, a l i q . 11-27-00 MU 19 #00121lZoi9 00-1311 KaOH Blank, TN-A-4715, A liq . 11/16/00 Analyta 20 * 001211.020 00-1311 KaOH Blank, 1W-A-471S. A liq . 11/16/00 21 #001211.021 E0&-1311 0 ppb pros 00002-06-01. A liq . 11-27-00 MU 22 * 001211.022 00-1311 2.5 ppb PFOS 00002-B6-02, A liq , 11-27-00 KU Blank Analyta^ 23 *001211.023 00-1311 5.00 ppb PFOS 00002-06-03, A liq . 11-27-00 HU 24 001211.024 00-1311 10.0 ppb PFOS 00002-06-04, A liq . 11-27-00 HU 25 001211.025 00-1311 2 5 .0 ppb PFOS 00002-06-05. A liq . 11-27-00 HU 26 *001211.026 00-1311 4 0 .0 ppb PPOS 00002-06-06, A liq . 11-27-00 MU 27 001211.027 00-1311 50.1 ppb PFOS 00002-06-07 A liq . 11-27-00 KU 20 001211.028 00-1311 75.1 ppb PFOS 00002-06-00, A liq . 11-27-00 KU 29 #001211.029 00-1311 100.2 ppb PFOS 00002-06-09, A liq . 11-27-00 KU 30 001211.030 00-1311 250.4 ppb PFOS 00002-06-10. A liq . 11-27-00 HU 31 001211.031 00-1311 400.7 ppb PFOS 00002-86-11. A liq . 11-27-00 KU 32 001211.032 00-1311 500.9 ppb PFOS 00002-06-11 A liq . 11-27-00 KU Standard 33 #001211.033 00-1311 1001.7 ppb PFOS 00002-86-13, a l i q . 11-27-00 KU Standard 34 001211.034 00-1311 KaOH Blank, TH-A-4715, A liq . 11/16/00 35 001211.035 00-1311 HaOH Blank, TH-A-4715, A liq . 11/16/00 Blank 36 001211.036 E00-1311 lOx EQ0-1311-3022-S1, O.Onq/L. 48hr, L .lC lay , 12/07/00 37 001211.037 00-1311 lOx 100-1311-3023-Sl, O.Oag/L, 48hr, lilC la y , 12/07/00 Analyta 38 001211.030 00-1311 lOx E00-1313-3024-S I. 0.0nq/L , 48hr, l.lC la y , 12/07/00 Analyta 39 *001211.039 00-1311 lOx 00-1311-3024m-Sl, O.Oxg/L, 48hr, lilC la y , 1 2 /0 7 ,. Analyta 40 001211.040 00-1311 lOx BO0-1311-3025-S1 O.0ng/L, 48hr, l i 5 C lay. 12/07/00 A nalyta 41 *001211.041 00-1311 250.4 ppb PFOS 00002-86-10, A liq . 11-27-00 KU QC 42 001211.042 00-1311 HoOH Blank, T9-A-4715, A liq . U /1 6 /0 0 43 001211.043 00-1311 KoOH Blank, TN-A-4715. A liq . 11/16/00 Analyta 44 001211.044 00-1311 lOx 00-1311-3026-Sl O.Ong/L. 48hr, liS C lay, 12/07/00 45 *001211.045 00-1311 lOx 00-1311- 3027- S i O.Otq/L, 4hr. liS C lay, 12/07/00 46 001211.046 00-1311 lOx B00-1311-027na-Sl O.Onq/L, 48hr. 1.5 C lay, 1 2 /0 7 .. Analyta 47 001211.047 00-1311 lOx 00-1311-1020-Sl O.Omq/L, 40hr, Ii2 5 C lay, 12/07/00 48 001211.048 00-1311 lOx 00-1311-3029-Sl O.Omg/L, 4Bhr, 1>25 C lay, 12/07/00 A nalyta 49 *001211.049 00-1311 250.4 ppb PFOS 00002-B6-10, A liq . 11-27-00 HU QC 50 *001211.050 00-1311 KoOH Blank. TH-A-4715, A liq . 11/16/00 Analyta 51 001211.051 00-1311 KaOH Blank, TH-A-4715, A liq . 11/16/00 Analyta 52 001211.0S2 00-1311 lOx EOO-1311-1030-Sl 0.0mg/L, 4hr, 1.25 Cl*y, 12/07/00 53 001211.053 E00-1311 lOx 800-1311-:i030na-Sl O.Oaig/t,, 48hr, 1.25 C lay, 1 2 /0 .. A nalyta 54 001213.054 00-1311 10k E00-1311-:iO5-Sl. 0.5m/L. 4Bhr, l.lC la y , 12/07/00 Analyta 5$ *001211.055 00-1311 10k EOO-1311-3059-SI, O.Smg/L, 48hr, l.lC la y , 12/07/00 Analyta 56 001211.056 00-1311 lOx 00-1311-:.0 60-SI, 0.5no/L , 48hr, lilC la y , 12/07/00 Analyte 57 001211.057 EOO-1311 250.4 ppb PFOS 00002-86-10, A liq . 11-27-00 HU QC 58 *001211.058 00-1311 KoOH Blank. TM-A-47X5, A liq . 11/16/00 A n aly ta 59 001211.059 00-1312 KoOH Blank, TO-A-4715, A liq . 11/16/00 Analyta 60 001211.060 00-3311 lOx EO0-1311-:-OOA-91, 0.5ia/L, 48hr, l.lC la y , 1 2 /0 7 .. Analyta 61 001211.061 00-1311 lOx 00-1311-3061-S I. 0.5no/L , 48hr, l.S C la y . 12/07/00 62 001211.062 EOO-1311 lOx EOO-1311-3062-S I, 0.5na/L , 48hr, 1 ;5Clay, 12/07/00 Analyte 63 001211.063 00-1311 lOx 00-1311-3063 -S i, O.Seg/C. ` h r, l.S C la y , 12/07/00 Analyte 64 001211.064 E00-1311 lOx EOO-1311-3063mm-Sl, O.Sag/L, 40hr, 1.5Clay, 1 2 /0 7 .. Analyta 65 001211.065 EOO-1311 250.4 ppb PFOS 00002-86-10, A liq . U -2 7 -0 0 MU QC 66 001211.066 00-1311 HaOH Blank, 'H.--A-4715, A liq . 11/16/00 00-1311 KaOH Blank. Th-A-4715. A liq . 11/16/00 68 00121lZ068 00-1311 lOx 00-1311-3064-51, O.Sag/L, 40hr. 1.2 5 cl* y , 12/07/00 69 001211.069 00-1311 lOx 00-1311-3065-SI, O.Saxi/L. *8hr, 1.25Clay, 12/07/00 Analyte 70 001211.070 00-1311 lOx EO0-1311-3066-S1, 0.Sg/L . 48hx, 1.25Clay, 12/07/00 71 #001211.071 00-1311 lOx OO-1311-3066ata-Sl, O.Sno/L, 48hr, 1.2SClay, 1 2 /0 . . Analyta 00-1311 lOx 00-1311-3085-SI, O.Saq/L, 36hr. l.lC la y , 12/07/00 A nalyta 00-1311 250.4 ppb PFOS 00002-86-10, A liq . 11-27-00 MU 74 aOOmiZo? EOO-1311 HaOH Blank. TH-A-4715, A liq . 11/16/00 QC Analyta 75 001211.075 00-1311 KaOH Blank. TM-A-4715. A liq . U /1 6 /0 0 Analyte 76 001211.016 00-1111 lOx E00-1311-30B6-S1, 0.5o/L , 36hr, l.lC la y , 12/07/00 77 #001211.077 EOO-1311 lOx 00-1311-3087-51, 0 .5 -q /L , 36hr, l.lC la y , 12/07/00 AnUyte 70 001211.070 EOO-1311 lOx OO-1311-3O0?*-S1, 0.5g/L. 36hc. l.lC la y , 1 2 /0 7 .. 79 001211.079 00-1311 lOx BOO-1311-3088 -S l, 0.5*m/L, 36hr. l.S C la y , 12/07/00 80 001211.000 00-1311 lOx EO0-13U-3O89-S1, O .S-g/L, 16hr, l.S C la y , 12/07/00 AMl^te 01 001211.001 00-1311 250.4 ppb FFOS 00002-06-10, A liq . 11-27-00 HU QC 82 001211.002 00-1311 MaOH Blank, TH-A-4715, A liq . U /1 6 /0 0 Analyte 83 001211.083 00-1311 HaOH Blank, TN-A-4715, A liq . U /1 6 /0 0 04 001211.084 00-1311 lOx 00-1311-3 390-SI, O.Swj/L, 36hs, l.S C la y , 12/07/00 Analyte 05 001211.085 00-1311 lOx EOO-1311-3390aw-Sl, 0 .5 ma/L. 36hr. 1.5Cly, 1 2 /0 7 .. A nalyte 86 001211.066 EOO-1311 lOx EOO-13U-3391-S1, 0.5 q /L , 1 6ht. 1.2 5 cl* y , 12/07/00 A nalyte 87 001211.087 00-1311 lOx EOO-1311-3 392-Si, O.im g/L. 36hr, li2 5 C U y . 12/07/00 Analyte 88 001211.088 00-1311 10x 00-1311-3393-S I, O.Siaj/L. 36hr. 1.2SCly, 12/07/00 Analyte 09 #001211.089 00-1311 250.4 ppb Pros 00002-86-10, A liq . U -2 7 -0 0 KU QC 90 001211.090 EOO-1311 KaOH Blank, TN-A-4715, A liq . U /1 6 /0 0 91 *001211.091 EOO-1311 MaOH Blank, TN-A-4715, A liq . 11/16/00 Analyta 92 *001211.092 EOO-1311 lOx EOO-UU-3093*-S1. O.Saq/L. 36hr, 1.25Cl*y, 1 2 /0 .. A nalyte 95 *0012uZo9S 96 001211.096 97 001211.097 98 *001211.090 99 *001211.099 100 001211.100 101 *001211.101 102 *001211.102 103 *001211.103 104 001211.104 105 #001211.105 106 *001211.106 107 001211.107 108 001211.108 109 #001211.109 110 #001211.110 111 001211.111 112 001211.112 113 001213.113 114 #001211.114 115 .001211,115 116 001211.116 117 001211.117 118 001211.118 119 001211.119 120 001211.120 121 001211.121 122 001211.122 123 001211.123 124 001211.124 125 001211.125 126 001211.126 127 001211.127 120 00121lZl28 00-1311 lOx EOO-1311-3096-s i i 0 ,5*a/l,! 48hr! l.lC la y ! 12/07/00 EOO-1311 lOx 00-13U-3096b -S 1 , Q.5ib/L , 48hr, l.lC la y , 1 2 /0 7 .. 00-1311 250.4 ppb PFOS 00002-06-10, A liq . U -2 7 -0 0 MU 00-1311 MaOH Blank. TN-A-4715, A U q. 11/16/00 00-1311 KaOH Blank. TN-A-4715. A liq , U /1 6 /0 0 00-1311 lOx EOO-1311-3097-s i , O.Sag/L, 48hr, l.S C la y , 12/07/00 00-1311 lOx EOO-13U-3O90-S1, 0 .5 a/L , 40hr, l.S C la y , 12/07/00 EOO-1311 lOx EOO-1311-3099-S I, O.Snq/L, 48b, l.S C la y , 12/07/00 EOO-1311 lOx 00-13U-3099m-Sl, 0.5io/L, 48hr, l.S C lay , 1 2 /0 7 .. EOO-1311 lOx EOO-1311-3:.00-Si, 0,5*xj/L, 40hr, 1 :25Clay, 12/07/00 00-1311 250.4 ppb PFOS 00002-06-10, A liq , U -2 7 -0 0 KU EOO-1311 KaOH Blank, TM-A-4715. A liq . U /1 6 /0 0 EOO-13U KaOH Blank, TN-A-4715, A liq . 11/16/00 00-1311 lOx 00-1311-3101-31, 0 .5na/L , l i h r , l:25C lay. 12/07/00 00-1311 lOx 00-1311-3!02-31, 0.5g/L . 4Bhr, 1.25Clay, 12/07/00 00-1311 lOx EOO-1311-3! 02na-S l, O.Sam/L, 40hr, 1.25Clay, 1 2 /0 .. EOO-1311 250.4 ppb PFOS 00002-06-10, A U q. U -2 7 -0 0 MU EOO-1311 KaOH Blank. TM-A-4715, A liq . U /1 6 /0 0 00-1311 HaOH Blank, TN-A-4715, A liq . U /1 6 /0 0 00-1311 0 ppb PFOS 000(2-86-01, A U q. 11-27-00 MU 00-1311 2 .5 ppb PFOS 3CO02-S6-O2, A liq . 11-27-00 KU 00-1311 5.00 ppb PFOS COOO2-06-O3, A U q. li-2 7 -0 0 MU 00-1311 10.0 ppb PFOS 80002-86-04. A liq . U -2 7 -0 0 MU 00-1311 2 5 .0 ppb PFOS a0002-$6-05, A U q. U -2 7 -0 0 MU 00-1311 40.0 ppb PFOS 00002-06-06. A liq . U -2 7 -0 0 KU 00-1311 50.1 ppb PFOS 00002-06-07 A liq , 11-27-00 MU 00-1311 75.1 ppb PFOS 00002-06-00, A liq . U -2 7 -0 0 MU 00-1311 100,2 ppb PFOS 00002-06-09, A liq . 11-27-00 KU 00-1311 250.4 ppb PFOS 00002-06-10. A liq . U -2 7 -0 0 KU EOO-1311 400.7 ppb PFOS 00002-06-11. A liq . 11-27-00 MU 00-1311 500.9 ppb PFO!! 00002-86-12 A liq . U -2 7 -0 0 MU E00-13U 1001.7 ppb PFOS 00002-96-13, a l i q . 11-27-00 KU 00-1311 KaOH Blank, TH-A-4715, A liq . 11/16/00 00-1311 MaOH Blank, TH-A-4715, A liq . U /1 6 /0 0 Analyte Analyte Analyte QC Analyta Analyta Analyta Analyte Analyta A n aly ta QC Analyte Analyta Analyta Analyta Analyte QC A n aly ta Analyte A n aly te Standard Analyte AT 7.145 7.129 7.117 7 .1 3 0 7 .1 3 0 7.110 7.116 7.107 7.092 7.092 7.103 7.103 7.103 7 .0 9 1 7 .0 9 6 7,116 7.104 7.094 7.103 250.40 7.092 7.091 7.104 7.105 7.094 7.093 7.091 250.40 7.103 7.091 7.104 7.105 7.093 7.107 7.102 7.107 7.091 7.103 7.098 7.103 7.096 7.091 7.094 7,093 7.099 7.107 7.104 250.40 7.091 7 .0 9 2 7.105 7.092 7.092 7.091 7 .0 9 0 7.082 7.105 250.40 500.90 1001.70 7.104 7.117 7.103 7.101 7.106 7.102 7.103 7.094 7.093 7.090 7.089 7 !q93 7.090 7.092 7.106 ppb VDev Piaga Hod C 684 1330 2780 4390 4994 6248 9379 10739 24773 25927 36014 121 2 01 655 835 1396 3057 4577 5902 7741 9856 18892 24539 27730 41307 351 203 B -6 bb 13632 1 14376 9369 0719 8862 16918 17657 17276 23519 16266 0619 16388 9154 9497 4027 18130 6 bb 17206 17570 17032 15528 5297 14567 14603 6135 6179 6700 13150 13931 13113 13542 13953 19163 12795 2063 3436 3693 5423 12652 2S -IOO bhx 40UP 020199: q u a n tica ta d and p r in ta d by CMC on 12/1S/O0 3M Environm ental Laboratory W I'cr/iilGO Page 538 of 703 BACK TO MAIN Quantify Coaqxeund unary Rapare EOO-1311 froa Adaorb/Daaorb l u c i a Id a t : C:\H aaalynx\aoup02 0i99.pro\Saapla0B \a00i211 Lase an d if ia d : Had Dae 13 08:47:39 300 Mathod: C:\M aaalynN\aoupU01. pro\MathDB\001211 Leak u o d ifla d : Had Dae 13 0*:5:*S 3003 P rin tad : Had Dae 13 04:56:49 200) Cuvound 3: TREPO (427*01, fune } > saaplallac 1 * 001211_001 5 E00-1311 eoo- m i 1001.1 TN-A-4715, A liq . 11/16/00 PFOS 00002-86-13, a l i q . 11-27-00 MU P!rOS 00002-06-13, 1i q . 11-27-00 MU 4 001211_004 00-1311 MaOH Blank, TN-A-4715, A liq . 11/16/00 5 aOOUll_O0S EOO-1311 KOH Blank, "N-A-4715, A liq . 11/16/00 6 *001211_00S 00-1311 0 ppb PPOS 011002-06-01, A liq . 11-27-00 MLA 7 001211_007 EOO-1311 2 .5 ppb Pros 00002-06-02, A liq . 11-27-00 MLA * a00121i_008 00-1311 5.00 ppb PFOH 00002-06-03, A liq . 11-27-00 MLA 9 001211_009 10 *001211^010 10.0 ppb pros: 00002-06-04, A liq . 11-27-00 MIA 25.0 ppb PPOS 00002-S6-05. A liq . 11-27-00 HLA 11 *001211_0U 12 *001211,,012 40.0 ppb pros: 00002-06-06, A liq . 11-27-00 MLA 50.1 ppb pros 00002-06-07 A liq . 11-27-00 SLA 13 a00l211_01) 75.1 ppb PPOS 00002-06-08, A liq . 11-27-00 HLA u omu.ow EOO-1311 100.2 ppb PFCS 00002-46-09, A U q. 11-27-00 MU. 15 *001211_015 EO-1311 250.4 ppb PfCS 00002-06-10, A liq . 11-27-00 HLA IS aOO1211_0lS EOO-1311 400.7 ppb PFiS 00002-06-11, A liq . 11-27-00 MLA 17 * 0 0 m i_ 0 1 7 00-1311 500.9 ppb PFCS 00002-86-12 A liq . 11-27-00 HLA 15 *001211_010 00-1311 1001.7 ppb Pros 00002-86-13, a l i q . 11-27- 1 *001211_019 EO-1311 MOK Blank. TH-A-4715. A liq . 11/16/00 20 *001211.0141 00-1311 KaOH Blank, TH-A-4715, A liq . 11/16/00 21 t00l2U _021 00-1311 0 ppb PFOS 00002-86-01. A liq . 11-27-00 MLA 22 *001211_022 EO-1311 2 .5 ppb PPOS 00002-86-02, A liq . 11-27-00 MLA 23 a0012ll_023 00-1311 5.00 ppb PPOS 00002-06-03. A liq . 11-27-00 MLA 24 a001211_024 00-1311 10.0 ppb PPOS 00002-06-04, A liq . 11-27-00 HLA 25 001211_025 EOO-1311 2 5 .0 ppb PFOS 00002-86-05. A liq . 11-27-00 KLA16 00121V_Q2& EOO-1311 40.(3 ppb PFOS 00002-06-06, A liq . U -27-00 HLA 27 a001211_027 EOO-1311 50.1 ppb PFOS 00002-86-07 A liq . 11-27-00 MLA 20 001211_028 00-1311 75.1 ppb PFOS 00002-06-08, A liq . 11-27-00 MLA 29 a001211~029 00-1311 100.2 ppb pro s 00002-06-09. A liq . 11-27-00 30 *001211_030 00-1311 250.4 ppb PFOS 00002-86-10, A1` 3-00' HLA 31 001211_031 B00-1311 400.7 ppb PFO.J 00002-06-11, A liq . 11-27-00 MLA : 32 001211.032 eoo-mi 500.9 ppb PFOS 00002-86-11 A U q. 11-27-00 HLA . 33 *001211.033 00-1311 1001.7 ppb PFOS 00002-06-13. a l i q . 11-27-00 MLA . 34 .001211_034 00-1311 MaOH Blank, TH-A-4715. A liq . 11/16/00 . 35 *001211_035 00-1311 M*OH Blank, TH-A-4715. A liq . 11/16/00 I 36 *001211.036 00-1311 lOx E00-13U- 1022-SI, 0 .0o/L , 48hr, lx lc la y . 12/07/00 3 37 *001211.031 lOx E00-1311-.1023-SI, O.Omg/L. 48hr, lx lc la y , 12/07/00 3 >S *001211.030 00-1311 lOx 00-1311-3024-61, O.Omq/L, 48hr, l : l c l a y , 12/07/00 . 39 *001211_039 00-1311 lOx EO0-1311-.lO24a-Sl, 0 .Outf/L, 48hr, lil C la y , 1 2 /0 7 .. , 40 *001211_040 E00-1311 lOx 0 0 -lJll-:i0 2 5 -S l O.Oaq/L, 48hr, 1:5 C lay. 12/07/00 , 41 *001211.041 EOO-1311 250.4 ppb PFOS 00002-86-10, A liq . 11-27-00 MLA < 42 *001211_042 00-1311 MeOH Blank. TH-A-4715, A liq . 11/16/00 3 43 *001211_043 00-1311 MaOH Blank. TH-A-4715, A liq . 11/16/00 i 44 *0012U_044 E0-1311 lOx 00-1311-:-026-81 O.Onq/L,48hr, 1x5 C lay, 12/07/00 , 45 *001211_045 E00-1311 lOx EOO-1111-3027-SI 0 .0aq/L ,40hr, 1x5 C lay. 12/07/00 3 *001211.046 00-1311 10* EO0-1311-3O27i*a-Sl O.Oaq/L, 40hr. 1x5 C lay, 1 2 /0 7 .. 1 47 a 1211_0 E0-1311 lOx EGO-1311-3028-61 0.0na/L ,48hr, 1x25 C lay. 12/07/00 1 *001211.040 00-1311 10* EOO-1311-3029-S1 0.0mu/L,4 0 h r, 1x25 C lay, 12/07/00 1 49 *001211.049 250.4 ppb PFOS 00002-86-10, A liq . U -2 7 -0 0 KLA 1 50 *001211.050 00-1311 M*OH -A-4715, A liq. 11/16/00 3 51 *001211.051 EOO-1311 MaOH Blank. TK-A-4715, A liq . 11/16/00 1 52 *001211.052 00-1311 lOx EOO-1311-303O-S1 0 .Oug/l, 48hr, lx2S C lay, 12/07/00 1 53 *001211.053 09-1311 10* E00-I311-303C*-Sl O.Omo/L . 48hr. 1x25 C lay, 1 2 /0 .. 1 54 *001211.054 E00-1311 lOx EOO-1311- 3058-SI, O.Smq/L.40hr, lilC la y . 12/07/00 I 55 *001211.055 00-1311 lOx EOO-1U1-1059-S I. 0 .5 a q /L ,4Bhr, lilC la y . 12/01/00 1 S *001211.05 EOO-1311 lOx EOO-1311-3060-51, O.Sna/L,48hr, lilC la y , 12/07/00 ) 57 *001211.057 00-1311 250.4 ppb PFOS 00002-86-10, A liq . 11-27-00 MLA < 50 *001211.050 EOO-1311 MaOH Blank. TN-A-4715. A liq . 11/16/00 3 59 001211.059 3-1311 MaOH Blank. TN-A-4715, A U q. 11/16/00 A 0 *001211.050 3-1311 lOx E00-1311-306C*a-Si, 0.5*a/L , 48hr, lilC la y , 1 2 /0 7 .. I 1 *001211.061 00-1 lOx EOO-1311-1061-91, 0.5mo/L,*8hr, liS C lay, 12/07/00 ) 62 001211.062 3-131: lOx 00-1311-3062-81, O.Sma/L,48hr. liS C lay , 12/07/00 I 3 *001211.063 lOx EOO-1311-3363-S I, O.Snq/L.4Bhr. liS C lay , 12/07/00 I <4 *001211.064 lOx EOO-1311-3 363M-S1, 0.5**j/L, 4Bhr, Ix iC lay , 1 2 /0 7 .. A 65 001211.065 250.4 ppb PPOS 00002-06-10. A U q. 11-27-00 MLA o 66 *001211.066 MaOH Blank, TN-A-4715, A liq . 11/16/00 A 67 0012U.067 MaOH Blank, TH-A-4715, A liq . 11/16/00 A 6* <001211.060 lOx EOO-1311-3064-S I. 0.5<j/L, 48hr, l:2S C l*y. 12/07/00 A 69 001211.069 lOx EOO-13U-3<165-31, 0.5nq/L , 40hr, lt25C ly. 12/07/00 A 70 *001211.070 lOx EO0-13U-3O66-S1, 0 .Sa/L , 40hr, lx25C lay, 12/07/00 3 71 001211^071 10* E00-1311-3066nx*-Sl. 0.5me/L. 48hr, lx25Cly, 1 2 /0 .. A 72 001211.072 10* E00-13U-300S-S1, O.ing/U , 36hr. lt l c l a y . 12/07/00 A 73 001211.073 250.4 ppb PFOS 00002-06-10, A liq . 11-27-00 MLA i 74 001211.074 MaOH Blank, W -A-4715. A liq . 11/16/00 / 75 001211~075 MeOH Blank, TN-A-4715, A U q. 11/16/00 A 76 001211.076 lOx EOO-1311-3U06-S1, 0 .5a/L , 36hr, lx lc la y , 12/07/00 77 001211.077 lOx EOO-1311-3007-SI, 0 . 5ng/Lr 36Kr, lilC la y , 12/07/00 70 *001211.070 lOx EOO-1311-3O07m*-Sl. 0.5no/L , 36hr, lilC la y , 12/Q 7.. 79 *001211.079 lOx EOO-13U-3O80-S1, O.Sio/L. 36hr, liS C lay , 12/07/00 *001211.0 lOx EOO-1311-3089-SI, O.Sa/L, 36hr, 1SClay, 12/07/00 01 a L211_0 EOO-1311 250.4 ppb PFOS 00002-86-10, A liq . 11-27-00 MLA 00-1311 MaOH Blank, TN-A-4715. A U q. 11/16/00 00-1311 MeOH Blank, TN-A-4715, A liq . 11/16/00 1211_C 00-1311 10* EOO-1311-1COO-SI. 0.5mq/L, 36hr. lxSCUy, 12/07/00 05 .00123 _ 00-1311 lOx E00-1311-lC90i*-Sl, O.Sxaq/L, 36hr, l:S C ly, 1 2 /0 7 .. 06 *001211.006 600-1311 lOx EOO-1311-1C91-S1, 0.5o/L . J6hr. li25C lay, 12/07/00 67 *001211.087 00-1311 lOx E00-13U-1092-S1, O.Smq/L, 36hr, ix25Clay, 12/07/00 80 ,001211.008 EOO-1311 lOx EOO-1311-1093-SI, 0 .5uo/L , 36hr. Ix25clay, 12/07/00 09 *001211.009 E OO-1311 250.4 ppb PFOS 00002-06-10, A liq . 11-27-00 MLA 90 001211.090 EOO-1311 KnOH Blank, TO-A-471S, A U q. 11/16/00 91 *001211.091 L MaOH Blank. TN-A-4715. A liq . 11/16/00 92 *001211~092 l ,10x E00-I311-J093i**-Sl. O.Snq/L, 36hr, li25C l*y, 1 2 /0 .. 93 *001211.093 . 1Ox EQ0-1311-3096-SX* O.S2/lZ 40hr[ lx lc la y ' 12/07/00 96 *00121llo96 . 10* E O O -im -3 0 9 6 -.-S l, 0 . 5mq/L, 4Bhr, lil C la y , 1 2 /0 7 .. 97 .001211.097 L 250.4 ppb PFOS OOOO2-06-UJ, A liq . 11-27-00 MLA 90 *001211.090 L MaOH Blank, TN-A-4715. A U q. 11/16/00 99 *001211.099 100 *001211.100 101 001211.101 102 *001211.102 1311 lOx EO0-1311-3099-S1, .5xq/t , lxSClay 12/01/00 Analyta 105*oomi"ios lxSClay 10* E O O -im -U O O -sl, O.Sng/L, 48hr. lx25Clay, 12/07/00 . 250.4 ppb PFOS 30002-06-10. A U q. 11-27-00 MLA . 106 *001211.106 MaOH Blank, 111-5-4715. A U q. 11/16/00 . 107 *001211.101 MaOH Blank. W-A-471S. A liq . 11/16/00 , 100 001211.101 lOx 00-1311-313 1 -S t. O.Smq/L. 4*he. lU S C la y . 12/01/00 . 109 *001211.109 110 *001211.110 111 *001211.111 lOx EOO-1311-1132-SI, O.Suq/L. 48hr, lx25Clay, 12/07/00 . lOx EOO-1311-3112nx*-Sl, O.Sraq/L. 48hr, li2 5 C lay , 1 2 /0 .. . 250.4 ppb PFOS 10002-06-10. A U q. 11-27-00 MLA : 112 *00121l"ll2 MeOH Blank, TN-A-4715,A liq . 11/16/00 . 113 *00X211.113 MaOH Blank, TN-A-471S,A U q. 11/16/00 , 114 *00121lZll4 0 ppb PFOS Q007.-86-01, A U q. 11-21-00 HLA . 115 *001211.115 2 .5 ppb PFOS 00002-86-02. A U q. 11-27-00 MLA . 116 *001211.116 5.00 ppb PFOS 00002-86-03,A U q,11-27-00 MLA : 117 *001211.117 10.0 ppb PFOS 011002-06-04,A U q.11-27-00 MLA : 118 *001211.110 25.0 ppb PFOS 011002-86-05,A liq .11-27-00 MLA : 119 *001211.119 40.0 ppb PPOS 0O002-86-06,A liq .U -2 7 -0 0 MLA 1 120 *001211.120 EOO 121 *001211.121 122 *001211.122 50.1 ppb PFOS 00002-86-07 A liq . 11-21-00 MIA 75.1 ppb PPOS 00002-06-08. A liq . 11-27-00 MLA 100.2 ppb PFOS ('0002-06-09, AUq. : : U -2 7 -0 0 MLA: 123 *<301211.123 250.4 ppb PFOS ('0002-06-10, A liq. U -2 7 -00 MLA: 124 *001211.124 400.7 ppb PFOS ( 0002-06-11. AUq. 11-27-00 MLA: 125 *001211.125 500.9 ppb PFOS (0002-06-12 A U q. U -27-00 MLA : 1081.1 ppb PFOS 00002-80-13. a l i q . 11-27-00 MLA ; MeOH Blank. TN-A-4715.A U q. 11/16/00 , MaOH Blank. TN-A-4715.A U q. 11/16/00 . 6.912 6.922 6.910 248.60 6.903 ppb M3*v Flag 0 2600 199.26 -20 bb 2666 203.67 -10 bb 3374 3715 3211 3700 3450 3769 3525 3062 3952 4131 3888 3450 3054 257.77 283.02 245.33 202.63 263,54 287.94 269.20 233.90 301.93 315.54 297.00 263.55 233.31 4 bb 14 bb -1 bb 14 bb 6 bb 16 bb 0 bb -6 bb 21 bb 27 bb 19 bb 6 bb -6 bb 3985 4050 4041 3077 3030 4111 4003 3927 3090 4117 3702 3016 3763 304.42 310.00 308.73 296.20 2 9 3 .1 8 314.05 311.07 300.01 2 9 7 .1 1 3 1 4 .4 0 2 0 8 .0 9 291.47 2 8 7 .4 5 22 bb 25 bb 24 bb 19 bb 10 bb 26 bb 25 bb 21 bb 20 bb 26 bb 16 bb 17 bb 16 bb 3221 1624 3700 3590 3641 246.04 276.87 282.63 274.84 278.14 -2 bb 11 bb 13 bb 10 bb 12 bb 3262 3363 3495 3533 35S4 3494 249.18 256.89 267.02 269.86 271.50 266.90 -0 bb 3 bb 7 bb 0 bb 9 bb 1414 3533 257.05 165.36 246.66 251.46 260.79 3171 3250 3173 3315 2S41 3202 242.21 248.26 242.40 253.21 194.10 250.71 -3 bb -1 bb -3 bb l bb -22 bb 1 bb 3169 3011 3185 3151 3200 3290 242.09 230.04 243.29 240.60 2 5 1 .1 6 251.32 3142 3222 2515 3164 2779 2032 240.00 246.15 196.10 256.98 212.26 216.36 -4 bb -1 bb -21 bb 1 bb -15 bb -13 bb 3016 2904 3209 3164 3252 3101 230.39 227.96 245.13 2 4 1 .7 4 2 4 0 .4 3 236.90 -3 bb -9 bb -2 bb -3 bb -1 bb -5 bb 276S 2419 3121 2666 2442 28S8 2537 2582 2600 203.70 186.54 218.3 0 193.84 197 .26 198.62 -19 bb -25 bb -13 bb -22 bb -21 bb -20 bb 2340 2263 2296 2515 170.74 -29 bb 172.06 -31 bb 175.36 -30 bb 192.14 -23 bb 2433 2784 2713 2413 2536 2773 2547 2494 2386 2619 2696 2390 2450 25Q5 105.90 212.69 207.23 184.36 193.75 211.05 194.54 190.49 182.25 200.04 205.98 182.54 187.18 191.40 -25 bb -14 bb -17 bb -26 bb -22 bb -15 bb -22 bb -23 bb -27 bb -20 bb -17 bb -27 bb -25 bb bb SOUP 020190: quantitated and printed by a* on 13/11/00 Cinc 13-1 R l v o 3M Environm ental Laboratory Page 539 of 703 E00-1311 PFOS Adsorb/Desorb Study# EOO-1311 Compound: PFOS Study: Adsorb/Desorb Analytical Instrument: Hillary on 12/14/00 Reprocessing Workstation: Dioana 12/18/00 batch H1214a1.b SwbpU JP SamWaDeac Run # Rap MW D atatila V ia l# PFBS PPb PFBS RT 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-05 25 ppb PFOS Calibration Std 5 26 H1214A1.M HII0026.D 5 247.0 6.57 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-06 40 ppb PFOS Calibration Std 6 27 H1214A1.M HIU0027.0 6 247.0 6.56 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-07 50.1 ppb PFOS Calibration Std #7 26 H1214A1.M HIII0028.D 7 247.0 6.57 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-08 75.1 ppb PFOS Calibration Std 8 29 H1214A1.M HIII0029.D 8 247.0 6.56 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-09 100.2 ppb PFOS Calibration Std 9 30 H1214A1.M HHI0030.D 9 247.0 6.56 248.6 ppb THPFOS/ 247 0 ppb PFBSO 00003-141 250.4 ppb PFOS Calibration Std #10 31 H1214A1.M HHI0031.D 10 247.0 6.56 248.6 ppb THPFOS/ 247 0 ppb PFBSO 00002-86-11 400.7 ppb PFOS Calibration Std #11 32 H1214A1.M HHI0032.D 11 247.0 6.56 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-12 500.9 ppb PFOS Calibration Std #12 33 H1214A1.M HIII0033.D 12 247.0 6.57 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-13 1001.7 ppb PFOS Calibration Std *13 34 H1214A1.M HHI0034.O 13 247.0 6.57 248.8 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 42 H1214A1.M HH0042.0 10 247.0 6.58 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 50 H1214A1.M HIII0050.0 10 247.0 6.56 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 58 H1214A1.M HHI005B.D 10 247.0 6.56 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 66 H1214A1.M HUI0066.0 10 247.0 6.S6 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 74 H1214A1.M HIII0074.D 10 247.0 6.55 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250 4 ppbPFOS CCV 82 H1214A1.M HII0082.D 10 247.0 6.53 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-05 25 ppb PFOS Calibration Std #25 99 H1214A1.M HII0069.P 5 247.0 6.53 248.6 ppb THPFOS/ 247 0 ppb PFBSC QQQ02.66-06 40 ppb PFOS Calibration Std #26 90 H1214A1.M HillO090.0 6 247.0 6.53 248 6 ppb THPFOS/ 247.0 ppb PFBSC 00002-86-07 50.1 ppb PFOS Calibration Std #27 91 H1214A1.M HMI0091.O 7 247.0 653 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-08 75.1 ppb PFOS Calibration Std #28 92 H1214A1.M HII0O92D 8 247.0 6.53 248.6 ppb THPFOS/ 247.0 ppb PFBSC 00002-86-09 100.2 ppb PFOS Calibration Sid #29 93 H1214A1.M HIID093.D 9 247.0 6.53 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 250.4 ppb PFOS Calibration Std #30 94 H1214A1.M HNI0094.D 10 247.0 6.53 248 6 ppb THPFOS/247.0 ppb PFBSO 00002-86-11 400.7 ppb PFOS Calibration Std #31 95 H1214A1.M HHI0095.D 11 247.0 6.52 248.6 ppb THPFOS/247.0 ppb PFBSO 00002-86-12 500.9 ppb PFOS Calibration Std #32 96 H1214A1.M HII0096 0 12 247.0 6.52 248.6 ppb THPFOS/247.0 ppb PFBSO 00002-86-13 1001.7 ppb PFOS Calibration Std #33 97 H1214A1.M HNI0097.0 13 247.0 6.52 BACK TO MAIN KLT on Dioana Page 540 of 703 PFB3 arai 1,030,547.8 1,040,277.3 1.026,578.8 1,014,268.6 1,023,443.3 1,041,050.4 1,037,341-3 1,042,652.9 1,011,920.4 1,031,956.0 1,028,888.3 1,025,626.2 1,014,181.1 996,439.1 976,924.5 958,626.4 959,545.8 964,280.1 943,308.6 955,510.1 966.756.3 955,342.4 961,285.8 938,365.9 THPFOS o?b THPFOS RT 248,6 7.64 248.6 7.54 246.6 7.55 248.6 7.54 248.6 7.54 246.6 7.54 24B.6 7 .5 4 248 6 7.54 248.6 7 .5 4 248.6 7.54 248 6 7.54 248 6 7 .5 3 248.6 7.53 248.6 7.54 248.6 7.52 248.5 7 .5 2 248.6 7.52 248.6 7.52 248.6 7 .5 2 248.6 7.53 240.6 7.52 248.6 7.52 246.6 7.52 248.6 7.52 THPfQ? a m 645,953.3 647,778.7 647,690.0 642,514.9 648,175.4 856,451.6 651,013.2 650,0933 644,701.0 655,563.3 653,181.1 655,857.3 6 3 8 ,7 4 5 .5 635,288 6 622,280.5 599,346.4 6 0 2 ,0 1 5 .6 613,825.4 598,254.6 609,668 4 614,913.3 605,318 9 611,212.4 586,889.6 PFOSRT 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 PFO Saw 363,570.1 581,518.3 707,780.0 1,040,160.4 1,364,384 8 3,252.367,8 4,659,772.5 5,851,683.5 10,197,639.0 3,223.236.8 3,217,212.5 3.228,307.5 3,122,512.0 3,115,688 0 3,056,680 8 338,940.8 530,461 8 666,795.0 968.530.0 1,265,481.5 3,006,623.0 4,449,853.5 5,420.927 5 9,330,660.0 PFOSppb 22.3 10.9% 39.4 1.5% 49.4 1.4% 77.3 3.0% 102.1 1.9% 257.6 2.9% 404.4 0.9% 499.9 0.2% 9994 0.2% 255.4 255.9 2.2% 255.7 2.1% 254.7 1.7% 254.7 1.7% 255.2 1 9% 22.4 10.4% 38.5 3.7% 49 1 2.0% 76.7 100.6 2.1% 0.4% 253.9 397.5 1.4% 0.8% 491.5 1.9% 1,006.4 0.5% 3M Environmental Laboratory EOO-1311 PFOS Adsorb/Oesorb e m ahtJB Study#EOO-1311 Compound: PFOS Study: Adsorb/Desorb Analytical Instrument: Hillary on 12/14/00 Reprocessing Workstation: Dioana 12/18/00 batch H1214b1.b 8am pla0efc R u n * RapMtd P a titila V ia l* PFBSppb PFBSRT 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-88-05 25 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-88-06 40 ppb PFOS 248.8 ppb THPFOS/247.0 ppb PFBSO 00003-86-07 50.1 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-86-08 75.1 ppb PFOS 248 6 ppb THPFOS/ 247 0 ppb PFBSO 00003-86-09 100.2 ppb PFOS 248.8 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 250.4 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-86-11 400.7 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-86-13 500.9 ppb PFOS 246.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-86-13 1001.7 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250 4 ppbPFOS CCV 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 248.8 ppb THPFOS/ 247 0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250 4 ppb PFOS CCV 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250.4 ppb PFOS CCV 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00003-141 CCV 250 4 ppbPFOS CCV 248 6 ppb THPFOS/ 247.0 ppb PFBSO 00003-86-05 25 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-06 40 ppb PFOS 248.6 ppb THPFOS/ 247 0 ppb PFBSO 00002-86-07 50.1 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-08 75.1 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002- 86-09 100.2 ppb PFOS 248 6 ppb THPFOS/ 247.0 ppb PFBSO 00003- 141 250.4 ppb PFOS 248.8 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-11 400 7 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-88-12 500.9 ppb PFOS 248.6 ppb THPFOS/ 247.0 ppb PFBSO 00002-86-13 1001.7 ppb PFOS Calibration Std 5 Calibration Std #6 Calibration Std #7 Calibration Std 8 Calibration Std *6 Calibration Std 810 Calibration Std *11 Calibration Std *12 Calibration Std *13 Calibration Std *25 Calibration Std *26 Calibration Std *27 Calibration Std *28 Calibration Std *29 Calibration Std *30 Calibration Std *31 Calibration Std *32 Calibration Std *33 7 H121481.M HII0089.D 5 8 H1214B1.M HII0090.D 6 9 H1214B1.M HII0091.D 7 10 H1214B1.M HHI0092D 8 11 H1214B1.M HIII0093.D 9 12 H1214B1.M HII0094 D 10 13 H1214B1.M HIII0095.D 11 14 H1214B1.M HIII0O96.D 12 15 H1214B1.M HHI0097.D 13 24 H1214BVM HIB0106.D 10 32 H1214B1.M HII0114.0 10 O a 5 z 40 H1214B1.M 10 48 H1214B1.M HW10130.0 10 56 H1214B1.M HIIKJ136.D 10 84 H1214B1M HH0146.D 10 71 H1214B1 M HII0153.0 5 72 H1214B1.M HII0154.D 6 73 H1214B1.M HII0155 0 7 74 H1214B1.M HII0156D 8 75 H1214B1.M Hrll0157.0 9 76 H1214B1.M HR0158.D 10 77 H1214B1.M HHI0159.D 11 78 H1214B1.M HII0160.D 12 79 H1214B1.M HII0161.D 13 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247 00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 247.00 6.53 6.53 6.53 6.53 6.53 6.53 6.52 6.52 6.52 8.51 6.53 6.54 6.55 6.55 6.54 6 54 6.55 6.54 6.54 6.55 6.54 6 54 6.54 6.54 BACK TO MAIN Page 5 41 o f 7 0 3 PFBS re 958628 38 959545.75 964280 13 943308.56 955510.06 966756.31 955342.44 961285.81 938365.88 958050.50 975048 89 979697.44 980846.19 980019.94 971858.69 958397.00 960911 56 963746.19 953208.50 960517.44 981974.94 959292.56 959614.31 962681.00 IH P FO g PEfr THPFOS RT IHPFQ S t m 248.60 248.60 248.80 248.60 248.60 248 80 2 4 8 .6 0 2 4 8 .6 0 2 4 8 .6 0 2 4 8 .8 0 2 4 8 .6 0 2 4 8 .8 0 2 4 8 .8 0 24860 24860 2 4 8 .6 0 2 4 8 .B0 2 4 8 .6 0 2 4 8 .6 0 2 4 8 .6 0 2 4 8 .6 0 248.60 248.60 2 4 8 .6 0 7,52 7.52 7.52 7.52 7.53 7.52 7,52 7.52 7.52 7.51 7.52 7.52 7.53 7.53 7.52 7.53 7.53 7.53 7.52 7 53 7.52 7.53 7 .5 2 7.52 599346 38 802015 56 613825 44 598254.83 609668 38 814913.25 805318.94 811212.44 586889.56 612734.63 625283.75 632811.69 631160.38 821435.50 631518.88 611969.38 622624.31 6 1 77 0 1 .1 9 616095.31 615547.44 627304.31 617991.38 812672.13 619999.75 PFPSRT 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 PFQ3 re 338940.84 530461.75 666795.00 968530 61 1265481.50 3006623 00 4449853.50 5420927 50 0330660.00 2997740.75 306687050 3078146.00 303383550 3045221.50 3060745.75 341318.56 533523.63 66917525 970864.25 1288105.75 3055103.75 4522913.50 5424030.50 9669561 00 PFOSPPto 22.65 36 94 49 59 77.47 101.64 256.44 401.52 496 38 1016.05 256.61 257.31 25500 251.73 257.06 254.00 22.25 37 69 49.44 75.78 102.54 255-34 399.54 495.35 989 84 9.4% 2.6% 1.0% 3.2% 1.4% 2.4% 0.2% 0.9% 1.4% 2.5% 2.8% 1.8% 0.5% 2,7% 1.4% 11 0% 5.8% 1.3% 0.9% 2.3% 2.0% 0.3% 1 1% 1.2% 3M Environmental Laboratory Environmental Laboratory Co S a m p le B atch H 0 1 0 4 0 5 .b , a n a ly z ed o n H illa ry 0 4 4 )5 -0 1 . P F O S A d s o rb /D e a o rb s a m p le s. M atrix: S o il/S Ig /S ed . Standard curve rang e used fo r calibration o f sam ples: 5-1002 ng/m L B atch m ethod; H010405.m Inj D ate B atch 4 /6/0 1 12 :53 D:VChem\H illary\H 010405.b 4/6/01 13:08 D:\Chem\Hiffajy\H010405.b 4 /6 /0 1 1 3 : 2 2 D:\Chem \HjHary\H010405.b 4 /6 /0 13:38 D:\ChemLHi!!ary\H 0'i0405.b 4/6/01 13:51 D:\Chem\Hillary\H010405.b 4/6/01 14:05 D:\Chem\Hillary\H010405.b 4/6/01 14:20 D:\Chem\Hillary\H010405.b 4/6/01 14:34 D:\Chem\Hillary\H010405.b 4/6/01 14:48 D:\Chem W Nary\H010405.b 4/6/01 15:03 D:\Chem\Hillary\H010405.b 4/6/01 15:17 D:\Chem\HiIlary\H010405.b 4/6/01 15:31 D:\Chem\Hillafy\H010405.b 4/6/01 15:46 D:\Chem\Hillary\H010405.b 4/7/01 4:57 D:\Chem\Hillary\H010405.b 4 /7/0 1 5:11 D:\Chem \H iH ary\H 010405.b 4/7/31 5:26 D:\Chem \Hillary\H0lO405.b 4/7/01 5:40 O:\Chem\HiHary\H010405.b 4/7/01 5:55 D:\Chem\Hillary\H010405.b 4/7/01 6:09 D:\Chem\Hillary\H010405.b 4/7/01 6:23 D:\Chem\Hillary\H010405.b 4/7/01 6:38 D:\Chem\Hiflary\H010405.b 4171016:52 0:iCbem \HitfaiyiW 010405.b 4/7/01 7:07 D:3hem\HiH3fy\H010405.b 4/7/01 7:21 D:\Chem \Hillaiy\H010405.b 4/7/01 7:35 D:\Chem\Hillary\H010405.b 4 /7/0 1 7 :5 0 D:\Chem \Htllary\H010405.b SampType SAMPLE CALIB_1 C A L IB ..2 C A LIB.3 CALIB_4 SAMPLE C A L (8 _5 CALIB_6 CAUB_7 CAUB_8 SAMPLE CAUB_9 C A U B .10 SAMPLE CAUB_11 C A LIB .12 CALIB_13 CALIB_14 SAMPLE CALIB_15 CAL!B_16 CALIB_17 CAUB_18 SAMPLE CAUB_19 CAUB_20 F ile HILL0016.D HILL0017.D HILL0018.D HILL0019.D HILL0020.D H IL L 00 21 .0 HLL0022.D H1LL0023.D HILL0024.D HILL0025.D H IL L 0 0 2 6 .D HILL0027.D H IL L 0 0 2 6 .D H IL L 0 0 8 3 .D H IL L 0 0 8 4 .D H IL L 0 0 8 5 .D H IL L 0 0 8 6 .D HILL0087.D H IL L 0 0 8 8 .D HILL0089.D H IL L 0 0 9 0 .D HILL0091.D H IL L 0 0 9 2 .D H IL L 0 0 9 3 .D H IL L 0 0 9 4 .0 H IL L 0 0 9 5 .D Sam ple Nam e O ng/m L PFOS in M eO H 2.5 ng/mL PFOS in M eOH 5 ng/mL PFOS in M eO H 1 0 ng/m L PFOS in M eO H 2 5 ng/mL PFOS in M eO H 4 0 ng/mL PFOS in M eOH 5 0 .1 ng/m L PFOS in M eOH 75 .1 ng/m L PFOS in M eO H 100.2 n g/m L PFOS in M eO H 2 5 0 .5 ng/m L PFOS in M eO H 400.6 ng/mL PFOS in M eO H 501 ng/mL PFOS in M eOH 1002 ng/m L PFOS in M eO H O ng/mL PFOS in M eO H 2 .5 ng/m L PFOS in M eO H 5 ng/m L PFOS in M eO H 1 0 ng/mL PFOS in M eOH 2 5 ng/m L PFOS in M eO H 4 0 ng/mL PFOS in M eOH 50 .1 ng/mL PFOS in M eO H 75.1 ng/m L PFOS in M eO H 100.2 ng/m L P FO S in M e O H 25 0.5 ng/mL P FO S in M eO H 40 0.8 ng/mL P F O S hi M eO H 501 ng/mL PFOS in M eO H 501 ng/mL PFOS in M eO H "O CC0OD) Ul ro Co- soj -- tP Inj D ate Batch 4 /6/0 1 12:25 D:\Chem1HiUa/yU-i010405.b 4 /6/0 1 12:39 P:\C hem\HiHary\H D10405.b 4/6/01 16:00 D:\Cbem\Hilla/y\H010405.b 4/6/01 16:14 D:\Chem\Hillary\H010405.b 4/6/01 19:21 D:\Chem\Hillary\H010405.b 4/6/01 19:36 D:\Chem W llary\H010405.b 4/6/01 22:43 D:\Chem\Hiilaiy\H010405.b 4/6/0 1 22 :57 D:VChem\H illary\H 010405.b 4/7/01 1:50 D:\Chem\Hillary\H010405.b 4/7/01 2:04 D:\Chem\Hillary\H010405.b 4/7/0 1 4:2 8 D:\Chem \Hillary\H01040S.b 4/7/01 4:43 D:\Chem\Hillary\H010405.b 5 4/7/0 1 8:04 D:VChem\HJa/y\H010405.b 4/7/01 8:18 D:\ChemlHiHary\H010405.b n SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE F ile H IL L 0 0 1 4 .D H IL L 0 0 1 5 .0 HILL0029 O H IL L 0 0 3 0 .0 H IL L 0 0 4 3 .D H IL L 00 44 .D H IL L 00 57 .D H IL L 0 0 5 8 .D H IL L 0 0 7 0 .D H IL L 0 0 7 1 .D H IL L 0 O 8 1 . D H IL L 0 0 8 2 .D H IL L 0 0 9 6 .D H IL L 0 0 9 7 .D Sam ple Name TN-A 4802 MeOH TN-A 48 02 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 eOH -- fv er ------o BACK TO MAIN H 0 1 0 4 0 5 .x ls M ise in fC o m p o u n d N aR T Area THPFOS 5.111 THPFOS 5.121 THPFOS 5.12 THPFOS 5.107 THPFOS 5.106 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 5.098 THPFOS 5.092 THPFOS 5.098 THPFOS 5.1 THPFOS 5.106 THPFOS 5.101 THPFOS 5.1 THPFOS 5.101 THPFOS 5.106 THPFOS 5.107 THPFOS 5.105 THPFOS 5.104 THPFOS 5.104 Am ount 853901 254 880305 254 900514 254 884801 254 891555 254 otraouo 254 905309 254 901986 254 902929 254 921590 254 890229 254 885051 254 906646 254 909918 254 901288 254 907830 254 893968 254 866284 254 854670 254 848217 254 818488 254 824040 254 839800 254 795504 254 790146 254 796759 254 A verage: 871828.1S38 Std Dev: 39409.57909 %RSD: 4,5% C om pound N arftT 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 Am ount 0 00 5.331 64194 3.942931 5.33 113000 6.364052 5.324 189968 10.48501 5.323 495541 26.37293 5.331 779774 41.22295 5.33 971274 ou.8533 5.331 1469171 77.71198 5.329 1921199 102.2878 5.322 4651125 255.0356 5.335 6791612 402.9106 5.322 8184382 501.689 5.33 14871358 994.5332 0 00 5.302 53650 3.326644 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 5.311 1278693 74 46758 5.309 1565685 97.01042 5.31 4111457 246.754 5.308 6004617 398.0979 5.314 7263676 498.2641 5.314 13221474 1009.264 1133377 +30%. 610280 -30% : 127% 105% 105% 103% 102% 103% 102% 64% 101% 100% 99% 109% 88% 93% 94% 95% 99% 97% 62% 99% 99% 101% M ise (n fC o m p o u n d NaRT 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 Am ount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 C om pound N a iflT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Am ount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 page 1 of 2 3M Environmental Laboratory In j Oat Batch SampTyp 4/6/01 16:29 D:\Chem\Hillary\H010405.b SAMPLE 4/6/01 16:43 D:\Chem\Hillaiy\H010405-b SAMPLE 4/6/0 1 16 :58 D:\Chem\H il1ary\H 010405.b SA M PL E 4/6/01 17:12 D:\Chem\Hillary\H010405.b SAMPLE 4/6/01 17:26 D:\Chem\Hillary\H010405.b SAMPLE 4/6/01 17:41 D:\Chem\HiHary\H010405.b SAMPLE 4/6/01 17:55 D \Chem\Hiltary\H010405.b SAMPLE 4 /6 /u i lu uy D:\Cnem \Hiiiary\H0i04u5.b SAMPLE 4 /6 /0 1 18:24 D:\Chem\HiHary\H010405.b SA M PL E 4/6/01 18:36 D:\Chem\Hillary\H010405.b SAM PLE 4 /6/0 1 18:52 D:'Chem\Hillary\H010405.b SA M PL E 4/6/01 19:07 D:\Chem\Hillary\H010405.b SAM PLE 4/6/01 19:50 D:\Chem\Hiliary\H010405.b SAMPLE 4/8/01 20:04 D:\Chem\Hillary\H010405.b SAMPLE 4/6/01 20:19 D:\Chem\Hillary\H010405.b SAMPLE 4 /6/0 1 20 :3 3 D:\Chem\H iJlary\H 010405.b SA M PLE 4/6/01 20:48 D:\Chem\Hillary\H010405.b SAMPLE 4 /6 /0 1 21 :02 D:\Chem tHiflary\H010405.b SA M PL E 4/6/01 21:16 O:\Chem\Hiilary\H010405.b SAMPLE 4 /6/0 1 21:31 D:\Chem\H i1iary\H 010405.b SA M PLE 4/6/01 21:45 O:\Chem\HiIlary\H010405.b SAMPLE 4/6/01 21:59 D:\Chem\Hiilary\H010405.b SAMPLE 4/6/01 22:14 D:\Chem\Hillary\H010405.b SAMPLE 4/6/01 22:28 D:\Chem\Hillary\H010405.b SAM PLE 4/6/01 23:11 D:\Chem\Hillary\H010405.b SAM PLE 4/6/01 23:26 D:\Chem\Hillary\H010405.b SAMPLE 4/6/0 1 23:40 D:\Chem\Hrtlary\H010405.b SAM PLE 4/6/0 1 23:55 D:\Chem\Hillary\H010405.b SAM PLE 4/7/01 0:09 D:\Chem\Hiilary\H010405.b SAMPLE 4/7/01 0:23 0:\Chem \Hiilary\H010405.b SAMPLE 4 /7/0 1 0 :3 8 D:\Chem \Hillary\H010405-b SA M PL E 4/7/01 0:52 D:\Chem\Hillary\H010405.b SAMPLE 4/7/0 1 1:07 D:\Chem\HiUary\H010405.b SA M PL E 4/7/01 1:21 D:\Chem\Hillary\H010405.b SAM PLE 4/7/0 1 1:36 D:\Chem\Hiilary\JH010405.b SA M PL E 4/7/01 2:19 D:\Chem\Hillary\H010405.b SAMPLE 4/7/01 2:33 D:\Chem\Hillary\H010405.b SAM PLE 4/7/01 2:47 D:\Chem\Hillary\H010405.b SAM PLE 4/7/01 3:02 D:\Chem\Hillary\H010405.b SAM PLE 4/7/01 3:16 D:\Chem\Hillary\H010405.b SAM PLE 4/7/01 3:31 D:\Chem\Hillary\H010405.b SAMPLE 4/7/01 3:45 D:\Chem\Hillary\H010405.b SAMPLE 4/7/01 3:59 D:\Chem\Hillary\H010405.b SAMPLE 4/7/01 4:14 D:\Chem\Hillary\H010405.b SAMPLE H I Sam ple Name HILL0031.D 2m g/L PFOS Study Number E 00-1311 HILL0032.D 2mg/L PFOS Study Number EOO-1311 HILL0033.D 2m g/L PFOS Study Number EOO-1311 HILL0034.D 2mg/L PFOS Study Number EOO-1311 H IL L 0035.D 10m g/L PFOS Study N um ber EOO-1311 HILL0036.D 10mg/L PFOS Study Number E00-1311 H IL L 0037.D 10m g/L PFOS Study N um ber EOO-1311 H il u j u j o .l* rru < u iu y n u m b er EOO-1311 K (L L 0 03 9.0 2m g/L PFOS Study N u m b er EOO-1311 H ILL0040.D 2m g/L PFOS Study N um ber EOO-1311 H ILL0041.D 5 ng/m L PFOS in M eO H H ILL0042.D 2 5 0 .5 ng/mL P F O S in M eO H H ILL0045.D 2m g/L PFOS Study N um ber EOO-1311 H IL L 0046.D 2m g/L PFOS Study N um ber EOO-1311 H IL L 0047.D 10m g/L PFOS S tudy N um ber EOO-1311 H IL L 0 0 4 8 .0 10m g/L PFOS S tudy N um ber EOO-1311 H ILL0049.D lOrng/L PFOS S tudy N um ber EOO-1311 H fLL0050.D tOmg/L PFOS Study N um ber EOO-1311 HILL0O51.D Omg/L PFOS Study N um ber EOO-1311 H IL L 0052.D Omg/L PFOS S tudy N um ber EOO-1311 H IL L 0053.D Omg/L PFOS Study N um ber EOO-1311 H ILL0054.D Omg/L PFOS S tudy N um ber EOO-1311 H ILL0055.D 5 ng/m L PFOS in M eO H H IL L 0056.D 2 5 0 .5 ng/mL P F O S in M eO H H ILL0059.D 10m g/L PFOS Study N um ber EOO-1311 H ILL0060.D 10m g/L PFOS Study N um ber EOO-1311 H IL L 0061.D 10m g/L PFOS S tudy N u m b er EOO-1311 H ILL0062.D 10m g/L PFOS Study N um ber EOO-1311 H ILL0063.D 10m g/L PFOS Study N um ber EOO-1311 H IL L 0 0 6 4 .0 10m g/L PFOS Study N um ber EOO-1311 H ILL0065.D 10m g/L PFOS Study N um ber EOO-1311 H ILL0066.D 10m g/L PFOS S tudy N um ber EOO-1311 H ILL0067.D Omg/L PFOS S tudy N um ber EOO-1311 H ILL0068.D 5 n g/m L PFOS in M eO H H ILL0069.D 2 5 0 .5 ng/mL P F O S in M eO H H IL L 0072.D Omg/L PFOS S tudy N um ber EOO-1311 H ILL0073.D Omg/L PFOS Study N u m b er EOO-1311 H ILL0074.D Omg/L PFOS Study N u m b er EOO-1311 HILL0075 D Omg/L PFOS Study N um ber EOO-1311 H ILL0076.D Omg/L PFOS Study N u m b er EOO-1311 H ILL0077.D Omg/L PFOS Study N u m b er EOO-1311 H ILL0078.D Omg/L PFOS Study N um ber EOO-1311 H IL L 0079.D 5 n g/m L PFOS in M eO H H1LL0080.D 2 5 0 .5 ng/mL P F O S in M eO H "0 Q> (Q CD Ol CO o 41 o CO BACK TO MAIN H010405.xls Mise InfCampaund NaRT Area THPFOS 5.112 THPFOS 5.12 THPFOS 5.113 THPFOS 5.112 THPFOS 5.106 THPFOS 5.115 THPFOS T-uocz-e 5.109 5.105 THPFOS 5.112 THPFOS 5.111 THPFOS 5.113 THPFOS 5.116 THPFOS 5.112 THPFOS 5.118 THPFOS 5.108 THPFOS 5.112 THPFOS THPFOS 5.106 5.112 THPFOS 5.114 THPFOS 5.109 THPFOS 5.104 THPFOS 5.098 THPFOS 5.112 THPFOS 5.098 THPFOS 5.105 THPFOS 5.107 THPFOS 5.105 THPFOS 5.105 THPFOS 5.111 THPFOS 5.105 THPFOS 5.1 THPFOS 5.105 THPFOS 5.098 THPFOS 5.1 THPFOS 5.102 THPFOS 5.097 THPFOS 5.091 THPFOS 5.091 THPFOS 5.094 THPFOS 5 092 THPFOS 0 THPFOS 0 THPFOS 5.085 THPFOS 5.091 Amount 831638 254 845717 254 845296 254 691267 254 895152 254 904138 254 908952 254 745233 840577 254 843047 254 941520 254 937854 254 852429 254 688430 254 911967 254 919538 254 916068 254 732339 254 684599 254 844692 254 809811 254 672064 254 660662 254 872477 254 809071 254 808820 254 809437 254 646037 254 853122 254 888681 254 854113 254 700905 254 1281548 254 999732 254 916425 254 1282301 254 1283570 254 1122340 254 1275724 254 1295458 254 00 00 1122048 254 1051408 254 Compound N aiH 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 ISTD>130% PFOS PFOS PFOS !STD>130% PFOS iSTD>130% PFOS PFOS ISTD>130% PFOS tSTD>130% PFOS ISTD<70% PFOS ISTD<70% PFOS PFOS PFOS Area 5.329 533 5.323 5322 5.323 5.333 5.326 5.322 5.329 5.321 5323 5.326 5.329 5.328 5.318 5322 5.323 5323 5.324 5.319 5.322 5.315 5322 5.315 5322 5.317 5322 5.323 5.322 5.315 5.31 5.315 5.308 531 5.312 5.307 5.302 5301 5304 5.303 5.297 5.295 5.295 5.308 Amount 1594908 91.89164 1011666 56.76517 1601969 102.4876 4370912 326.6226 789270 41.74738 986799 51.74131 730034 38.024 3483461 234.6907 1692254 96.60646 2112598 121.2132 112770 6.100833 4597708 247.1156 1619584 91.01251 4093613 305.1853 1001786 52.07933 996187 51.3553 998588 51.67698 3717782 256.6704 760291 40.69207 213559 12.2503 113509 7.04131 3059833 228.1126 109900 6.465906 4451710 258.0898 6644129 437.9532 7503267 503.5302 6451764 423.3709 8372595 746.0709 1011146 56.23727 1599452 86.08401 1567814 87.84356 4173504 305.6462 542210 20.16617 103957 5.373166 4298803 235.5874 144727 5.782359 92058 3.88763 2467820 105.8252 19186 1.282508 11715 1.007175 11778 0 2260129 0 95065 4.486151 4062781 191.3037 122.0 % 98.6% 129.3% 103.0% 107.5% 94.0% 89.7% 76.4% page 2 of 2 Environmental Laboratory co SSBataamtncpdhlaemrdBetcahutocrdhv:eRrR0a10n01g30e2302u.0sbje,tdai nfaolryczaeldibornatiRonutohf0s3a-m20p-l0e1s.: PFOS 5 -e - )a3te/20/01 14:17 BDa:\tCchhem\Rbsh\RC10320.b SSAamMpPTLyEpe 333333//////222222000000//////000000111111 111111455445::::::342514158942 DDDDDD::::::\\\\\\CCCCCChhhhhheeeeeemmmmmmlW\\\\RRRRRuuuuuusssSsshMhhhh\W\\\RRRRR000000111111CQ0000333333222222QC0000......bbbbbb 3333////22220000////00001111 11115666::::15421075 ODDO:::.V\\lCCCChhhteeieemmmm\\\RR\RRuuuusssshhhh\\\RRR000011110000333322220000....bbbb CCCAAALLU1IBBB_.J32 CCCAAALUUIBBB___765 CCSAAALMLIBIPBRLEAE 333///222100///000111 111676:::502490 DOD:::\\\CCChhheeemmmt\\fRRfcuuiSssfhfctt1WRR000111000333222000...bbb CSAAMUPBLJE0 SAMPLE 3333333///////22222221111111///////0000000111111111111117667776:::::::30143402186593 DDDDDDD:::::::\\\\\\\CCCCCCChhhbhhheeeeeeemmmmmmmVi\W\W\RRRR3uuuuuuusssss5shhhhhhh\\\\\\RRRRRR000000011111110000000333333322222220000000.......bbbbbbb 33333/////2222211111/////0000011111 1111166669:::::1245159482 DDDDD:::::V\\\\CCCCChhhhheeeeemmmmm\\\\R\RRRRuuuuussssshhhlhr\\\t1RRRR*000001111100000333332222200000.....bbbbb CCCAAALLLIBIIBBRJJ1231 CCCCCCSCSAAAAAAAAAMLMLLLLLUIPP1IJIBBBBBBLLS__JEJEJJ1J27864580 Adsnogrb/m/DLea(od) mples. Matrix: Soii/Sfg/Sed. JCJiYC S i i s i O I yysLr ~~S tO . \ FRRRRRRRRRRRRRRiUUUUUUUUUUUUUUleSSSSSSSSSSSSSSHHHHHHHHHHHHHH00000000000000OO0000000000101221222222232290645839281077.............DDDDDDDDDDD000 O25SIO.a5nnmgngn/pg/mgm/l/mLemLLNPLPFaPPFmOFOFeSOOSSSiinniiMnnMMeMeOOeeHOOHHH 25 ng/mL PFOS in MeOH 4500 nngg//mmLL PPFFOOSS inn MMeeOOHH 72145500050000nnnngnggg/gm////mmmmLLLLLPPPPFPFFFOFOOOSOSSSSiniiiinnnMnMMMMeOeeeeOOOHOHHHH O10n0g2/mngL/mPLFOPFSOinSMineMOHeOH RRRUUUSSSHHH000111322089...DD0 251.05ngnn/ggm//mmL LLPFPPOFFOOS SSiniiMnnMMeOeeHOOHH RRRRRRRRRUUUUUUUUUSSSSSSSSSHHHHHHHHH000000000111111111333333333273469615.........DDDDDDD00 24524571100550050000000nnnn2ngnngggng/ggn///gmm/mm//g/mmm/mLLLLmLLLLPPLPPPPPFFPFFPFFFOOFOOFOOOOSSOSSSSSSiiSiinniiinnnnniiMMnMMnMMMMeeMeeOOeeeOOeOOOeHOHHHOHHHHH j \ \ Q r- x CD T J C\ cm <CQD r U l 0- A A ~vl O CO Inj Da333333te//////3333222222////0000002222//////1111000000////111100110011112111120033477003::.:::::::24124035043496506278 BDOODDDDDDOa::::::::::\\\\\\\1\\tCCCCCCCCCcChfhhhhhhhhbieeeeeeeeeemmmmmmmmmm1\\\\\\\W\RRRRRRRRRuuuuuuuuuussssssss$shhhhhhhMhli\\\\\\\\\RRRRRRRRRR000000000011111111110000000000333333333322222222220000000000..........bbbbbbbbbb 3333333///////332222222//111111122///////110000000//111111100111111111336700596:::::::::010240250104777226 ODDODDDDD:::::::::\\\\\\\V\CCCCCCCCCthhhhhhhiheeeeeeeemmmmmemmmm\\\\\W\\RRRRRRR\RuuuuuuuususssssssmMhhhfhsNih\\\\RtRRRRRRRO00000000111111111000000000333333333222222222O00000000.........bbbbbbbbb SampType SSSSSSSSSSSSSSSAAAAAAAAAAAAAAAMMMMMMMMMMMMMMMPPPPPPPPPPPPPPPLLLLLLLLLLLLLLLEEEEEEEEEEEEEEE SSSSAAAAMMMMPPPPLLLLEEEE FRRRRRRRRRRRRRiUUUUUUUULUUUUle/SSSSSSSSSSSSSHHHHHHBHHHHHH000000000000000000000000014113563773840S762901346761............D.DDDDDDDDD000 RRRRRRUULUUU/SSSSSSHHHHHH000000111111220114562430......DDDD00 STTTTTTTTTTTTTNNaNNNNNNNNNNNm-------------AAAAAAAAAAAAAp4444444444444le66688666866880000000000000N2222222222222aMMMMMMMMMMMMMmeeeeeeeeeeeeeeOOOOOOOOOOOOOHHHHHHHHHHHHH TTTTTTNNNNNN------AAAAAA444444888866000000222222 MMMMMMeeeeeeOOOOOOHHHHHH BACK TO MAIN R010320 data export.xts X M ic In C om pound NaRT Ai h THPFOS 5.517 THPFOS THPFOS 5.498 5.494 THPFOS 5.495 THPFOS 5.496 THPFOS 5.494 THPFOS 5.495 THPFOS 5.496 THPFOS 5.503 THPFOS 5.49 THPFOS 5.409 THPFOS THPFOS 5.498 5.495 THPFOS 5.515 THPFOS THPFOS THPFOS THPFOS 5.512 5.505 5.497 5.488 THPFOS 5.496 THPFOS 5.502 THPFOS THPFOS 5.49 5.486 THPFOS THPFOS THPFOS 5.461 5.494 5.481 THPFOS 5.485 Amount 1068332 254 1083902 254 1104114 254 1091458 254 1096171 254 1098872 254 1099862 254 1090988 254 1108459 254 1106726 254 1104875 254 1112297 254 1114997 254 953251 254 962548 254 969366 254 960992 254 956214 254 951968 254 949455 254 944258 254 947155 254 938982 254 937508 254 931253 925949 254 254 Average: 1024228769 Std Dev: 77977.63877 SRSO ; 7.6% Com pound Nau*T Area Am ount PFOS 0 00 PFOS 5.706 128798 1.792859 PFOS 5.704 203183 4.185602 PFOS 5.705 358080 9.517807 PFOS 5.713 657796 26.7604 PFOS 5.704 1315734 43.05413 PFOS 5.719 1620397 54.18493 PFOS 5.72 2292365 80.39292 PFOS 5.72 2972281 105.9074 PFOS 5.707 6500194 263.4048 PFOS 5.706 9479668 421.7312 PFOS 5.709 11306172 524.921 PFOS 5.712 19396403 1093.974 PFOS 0 00 PFOS 5.729 118137 1.935806 PFOS 5.715 176963 4.131231 PFOS 5.715 295223 8.741336 PFOS 5.715 672093 23.66741 PFOS 5.713 1020740 36.41673 PFOS 5.719 1259208 48.22502 PFOS 5.707 1807434 72.45096 PFOS 5.712 2314201 95.1839 PFOS 5.705 4990995 233.5678 PFOS 5.711 7221977 367.9867 PFOS 5.698 8611158 464.2158 PFOS 5.702 14684901 859.5687 1331499 +30%: 716961 -30%: 64% 85% 107% 106% 106% tu7% 106% 105% 106% 105% 109% 83% 87% 5% 96% 96% 96% 95% 83% 92% 93% 96% Mise in C om pound NaRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS Aim 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 Com pound Nai#T Area Amount PFOS 5.738 50239 0 PFOS 5.733 33969 0 PFOS 5.719 53824 0 PFOS 5.718 36113 0 PFOS 5.704 36644 0 PFOS 5.701 30906 0 PFOS 5.714 37769 0 PFOS 5.706 33871 0 PFOS 5.694 42689 0 PFOS 5.697 35794 0 PFOS 5.715 41290 0 PFOS 5.712 36212 0 PFOS 5.733 44171 0 PFOS 5.727 38719 0 PFOS PFOS 5.733 5.72 50802 42724 0 0 PFOS 5.741 46381 0 PFOS 5.74 42661 0 PFOS 5.718 59486 0 Page 1 of 3 Page 545 of 703 I S' ! CD 5j Sf rQJ o- o 3 In] Da33te//2200//0011 1176::0562 BD0:a:V\tCcChhheemm\'RRuusshh\\Rfl001100332200..bb 333///222000///000111 111888:::243095 ODD.::V\\CCChhheeemmm\\\RRRuuussshhf\i\iRRR000111000333222000...bbb 333///222000///000111 111999:::30123 D:\Chem\Rush\R010320.b 0D::'\C'nhoewm\R\f<lui$shh\'SRi001i!0i3322Q0..bb 3333////22220000////00001111 22210009::::01241596 DDDD::::\\\\CCCChhhheeeemmmm\W\'fRflluuuusssshhhh\\\\RRRR000011110000333322220000....bbbb 3/20/01 21:12 O:\Chem\Rush\R010320.b 33//2200//0011 2211::4217 DO::\tCChfemm\\RRuusshh\R001100332200..bb 3333////22220000////00001111 22221222::::51235048 DDDD::::\\\\CCCChhhheeeemmmm\\\\RRRRuuuusssshhhh\\\RRR000011110000333322220000....bbbb 3/20/01 22:53 0:tChem\Rush\R010320.b 3333////22220000////00001111 22223333::::02357260 DDDD::::\\\\CCCChhhheeeemmmm\\\\RRRRuuuusssshhrhi\W\\RRR00O0l11Ol00033332222O000....bbbb 33333/////2222211111/////000001111110011:.:::0433112836 DDDDD:::::\\\\\CCCCCfhhhhieeeeemnmmmKW\i\RRRRuuuuusssssfhfhWHi\\WRRRt000001111100000333332222200000.....bbbbb 33333333////////2222222211111111////////0000000011111111 22223321::::::::1501542414047358 DDD00DDD::::::::ttV\\\\\CCCCCCCChfththhtiieheeeeeemmmefmmmnmli\\\l\RRRRRRRiRuuuuuuususssssshhfhhfhsii\ht\\\WWRRRRR000000001111111100000000333333332222222200000000........bbbbbbbb 3333////22221111////00001111 4444::::50232938 DDDD::::\\\\CCCChhhheeeemmmm\\\\RRRRuuuusssshhhm\\\RRRR000011110000333322220000....bbbb 3/21/01 5:06 D:VChem\RustlW010320.b 3333////22221111////00001111 5655::::40231945 DDDD::::\\\\CCCChhhheeeemmmm\\\tRRRRuuuusssshhhfi\\\tRRRR000011110000333322220000....bbbb 3/21/01 6:18 D:\Chem\Rush\R010320.b 333///222111///000111 677:.:331250 DDD:::\\\CCCbbheeemmrrt\\RRRuuussshmh\\RRRQ00111000333222000...bbb SSSSSSSSAAAAAAAamMMMMMMMpPPPPPPPTLLLLLLLyEEEEEEEpe FRRRRRRRMUUUUUUU*SSSSSSSHHHHHHH0000000000000033333334567933......DDDDDDD S11111113333333a1111111m1111111p3------555555-la51101110006003N60122666a---M-MSSSSm-S33S33S3--SS33 SSSSSSSSSSSSSSSSSSSSSSSSSSSAAAAAAAAAAAAAAAAAAAAAAAAAAAMMMMMMMMMMMMMMMMMMMMMMMMMMMPPPPPPPPPPPPPPPPPPPPPPPPPPPLLLLLLLLLLLLLLLLLLLLLLLLLLLEEEEEEEEEEEEEEEEEEEEEEEEEEE SSSSSSAAAAAAMMMMMM PPPPPPLLLLLLEEEEEE SSSSAAAAMMMMPPPPLLLLEEEE SSSSAAAAMMMMPPPPLLLLEEEE SAMPLE SAMPLE RRRRRRRRRUUUUUUUUUSSSSSSSSSHHHHHHHHHOO0000000000000000444444445089314207........,DDD000000 51121111133333335n11111110g1111111/nm-------5555555gL1111111/m3377737P7823484LF-----MMSSSSSOP33333SSFS--OSSin33SMineOMHeOH RRRRUUUUSSSSHHHH0000000055552341....DDD0 1111333311111111----5555222200118900---MSSS333S-S3 RRRRRRRRRRRRUUUUUUUUUUUUSSSSSSSSSSSSHHHHHHHHHHHH000000000000000000000000666566566655234856578167...........DDD.DDDDDDD00 5211111111333333353n111111110g11111111/-n-----m--5S5555S5g0L0000000/m33666363P31287939LFM----M--SSSSSSPOS333S333FS--OSSi33nSMineMOHeOH 11331111--55110034--SS33 RRUUSSHH00006790..DD RRUUSSHH00007721..DD RRRRRUUUUUSSSSSHHHHH00000000007777758967.....DDD00 RRRRRUUUUUSSSSSHHHHH00000000008888801234.....DDD00 521113353n1110g111/nm---555gL111/m300P955LF-M-SPSO3S3FS-OSin3SMineMOHeOH 111111111333333333111111111111111111---------555555555201102212113443141331045112MM-------SSSSSSS&S3333333--SS33 RRRRUUUUSSSSHHHH0000000088895690....DDOD 2511335n110g11/--mn55g0L0/3m3P&6LFM-SOPS3FS-OSi3nSMIneMOHeOH BACK TO MAIN R010320 data export.xb Mise (n C om pound NaRT Ara* THPFOS 5.49 THPFOS 5.489 THPFOS 5.483 THPFOS 5.484 THPFOS 5.482 THPFOS 5.488 THPFOS 5.481 THPFOS 5.489 THPFOS 5.488 THPFOS 5.476 THPFOS 5.474 THPFOS 5.467 THPFOS 5.473 THPFOS 5.47 THPFOS 5.474 THPFOS 5.464 THPFOS 5.47 THPFOS 5.474 THPFOS 5.484 THPFOS 5.481 THPFOS 5.494 THPFOS 5.494 THPFOS 5.484 THPFOS 5.4B1 THPFOS 5.48 THPFOS 5.474 THPFOS 5.474 THPFOS 5.474 THPFOS 5.472 THPFOS 5.472 THPFOS 5.474 THPFOS 5.469 THPFOS 5.48 THPFOS 5.469 THPFOS 5.487 THPFOS 5.46 THPFOS 5.466 THPFOS 5.46 THPFOS 5.468 THPFOS 5.467 THPFOS 5.462 THPFOS 5.474 THPFOS 5.476 THPFOS 5.48 THPFOS 5.507 THPFOS 5.5 THPFOS 5.498 THPFOS 5.484 THPFOS 5.487 THPFOS 5.482 Amount C om pound NarfIT Ama Amount 1141140 254 PFOS 5.7 8378440 346.5268 972009 254 PFOS 5.713 11297958 628.7308 1164447 254 PFOS 5.7 10830182 467.7061 1149419 254 PFOS 5.701 8920100 371.419 1150191 254 PFOS 5.692 11003403 485.0679 971562 254 PFOS 5.696 14359682 869.5144 1143796 254 PFOS 5.698 16261734 823.9911 1145084 254 PFOS 5,706 16806125 661.0869 1153317 254 PFOS 5.696 18715781 972.5325 963588 254 PFOS 5.586 21465315 1571.297 1116533 254 PFOS 5.691 240399 5.337048 1106644 254 PFOS 5.684 8190150 248.3279 1129661 254 PFOS 5.68 11805672 532.2945 1115042 254 PFOS 5.687 10778461 491.643 1104866 254 PFOS 5.684 10755750 496.1706 929426 254 PFOS 5.688 13780741 873.3741 1392582 254 ISTD>130% PFOS 5.68 9688288 332.321 1334256 254 !STO>130% PFOS S.691 7370016 244.5963 1299165 254 PFOS 5.701 7352450 2516495 1042408 254 PFOS 5.698 10536384 521.0775 1189027 254 PFOS 5,718 284331 6.217634 1136514 254 PFOS 5.711 263226 5.939702 1112285 254 PFOS 5.708 197941 3.962167 1098839 254 PFOS 5.705 6089384 245.5533 1119517 254 PFOS 5.697 317716 7.871924 925302 254 PFOS 5.696 4503593 210.2997 1099092 254 PFOS 5.692 7145864 298.1447 1103796 254 PFOS 5.691 8366381 360.5895 1103738 254 PFOS 5.689 7936805 337.682 916966 254 PFOS 5.689 11534998 687.0305 1094601 254 PFOS 5,691 16188690 870.1489 1093215 254 PFOS 5,686 15234507 801.5557 1108623 254 PFOS 5.69 14183081 713.1438 896026 254 PFOS 5.679 18427132 1394.184 1076701 254 PFOS 5.684 230960 5.308384 1068295 254 PFOS 5.877 58554S1 242.3321 1114973 254 PFOS 5.676 27484446 1826.764 1101102 254 PFOS 5.67 26318468 1743.664 1099381 254 PFOS 5.678 25601434 1676.69 904101 254 PFOS 5.677 28444487 2682.41 1297195 254 PFOS 5.679 12510960 490.2051 1309423 254 PFOS 5.691 12718685 494.7347 1316725 254 PFOS 5.686 14206011 567.6869 1041110 254 PFOS 5.691 16461602 95S.5121 1163007 254 PFOS 5.724 786091 22.65781 1101098 254 PFOS 5.717 579479 16.95932 1083524 254 PFOS 5.715 194687 4.02545 1071583 254 PFOS 5.701 5756548 236.5543 1075235 254 PFOS 5.704 1372684 46.22885 892740 254 PFOS 5.699 5063682 252.5315 106 8% 99.1% 79.2% 98 0% 106.2% 6.7% 80.5% 94.4% Paga 2 of 3 a 3 <D 3 O) o- 3/21/01 7:44 D:\CfcemtRush\R01D320.b 3/21/01 7:58 D:\Chem\Rush\R010320.b 3/21/01 8:13 D:\Chem\Rush\R010320.b 3/21/01 8:27 D:\ChemRushV70t0320.b j 2UQ-, R i 4, ft'lbrm\R!ififcipnina?n h 3/27/01 8:58 D:\Cbem\Rush\R010320.b 3/21/01 9:10 D:\Chem\Rush\R010320.b 3/21/01 9:24 D:\Chem\Rusii\R010320.b 3/21/01 9:39 D:\CtiefrfiRiati\ROKXao.b 3/21/01 9:53 D:VChem\Rush\R010320.b 3/21/01 10:36 D:\Chem\Rush\R010320.b 3/21/0110:51 D:\Chem\RusfHR010320.to 3/21/0111:05 D:\Chem\RusflW010320.b 3/21/01 11:19 D:1Chem\Rush\R010320.b 3/21/0111:33 D:\Chem\Rush\R01Q320.b 3/21/01 11:48 D:\Chem\Rush\R010320.b 3/21/0112:02 0:tCfiemWusft010320.b 3/21/0112:16 D:\Chem\Rush\R010320.b 3/21/0112:31 D:\Chem\Rush\R010320-b 3 /21 /0112:4S O:\Chem\Rush\R010320.b 3/21/01 13:28 0:VChemtRusfi010320.b 3/21/0113:43 D:\Chem\Rusft\R010320.b 3/21/0113:57 D:\Chem\Rush\R010320.b 3/21/01 14:11 D:\Chem\Rush\R010320.b 3/2110114:26 O:tChemWusfttf?00320.b 3/21/0114:40 D:\CbenrtRusblR010320.b 3/21/0114:54 D:\Chem\Rush\R010320.b 3/21/01 15:09 D:\Chem\Rush010320.b 3/21/01 15:23 0:tChemtf7usft1R010320.b 3/21/01 15:37 0:\Cfiem\RushW)10320.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 RUSH0091.D RUSH0092.D RUSH0093.D RUSH0094.D RUSH009S.D RU SH 00 9 6 . 0 RUSH0097.D RSH0D98.D RUSH0099.0 RUSH0100.D RUSH013.D RUSH104.D RUSH0105.D RUSH0106.0 RUSH0107.D RUSH0108.D RUSH0109.0 RUSH0110.D R U S H 0 1 1 . D RUSH0112.O RUSH0115.D RUSH0116.O RUSH0117.O RUSH0118.D RUSH0119.O RUSH0120.D RUSH0121.D RUSH0122.D RUSH0123.O RUSH0124.D 1311-5175-S3 1311-5176-S3 1311-5177-S3 1311-5177MS-S3 1311-5070-S3 131-57i-53 1311*5072-83 1311-5072MS-S3 5 ngimL PFOS in MeOH 2 5 0 ng/mL PFOS inMeOH 1311-5106-S3 1311-5107-S3 1311-5108-S3 1311-5108MS-S3 1311-5142-S3 1311-5143-S3 1311-5144-S3 1311-S144MS-S3 5 noML PFOS tel MeOH 2 5 0 ng/mL PFOS inMeOH 1311-5214-S3 1311*5215*83 13 1 I-5 2 1 6 -S 3 1311-5216MS-S3 1311-5178-S3 1311-5179-S3 1311-5180-S3 1311-5180MS-S3 5 ng/mL PFOS tel MeOH 2 5 0 ng/mL PFOS *t MeOH R010320 data xportjds 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 5.477 5.48 5.461 5.474 5.48 5.482 5.487 5.48 5.488 5.488 5.468 5.478 5.487 5.483 5.479 5.487 5.495 5.496 5.505 5.494 5.475 5.494 5.495 5.495 5.495 5.489 5.495 5.502 5.507 5.516 Page 546 of 703 Page 3 o f 3 BACK TO MAIN 594727 584723 $86756 493241 585323 583958 $65431 486275 1043914 1030333 56751 575234 575785 470125 562160 564713 562369 469121 1007161 990753 597930 601361 602126 493982 256310 243982 235402 2 0 7254 980889 965254 254 !STD<70% P F O S 254 ISTtX70% PFO S 254 ISTD<70% P F O S 254 ISTD<70% PFO S 254 ISTD<70% P F O S 254 r s n x 7 c % PFO S 254 !S-rr><7n% P F O S 254 1STD<70% P F O S 254 PFOS 254 PFO S 254 (STCX70% P F O S 254 ISTCX70H PFO S 254 1STD<70% P F O S 254 1STD<70% P F O S 254 STCX7C% P F O S 254 1STD<70% P F O S 254 ISTEX70% PFO S 254 ISTD<70% PFO S 254 PFOS 254 PFO S 254 ISTD<70% P F O S 254 ISTD<70% PFO S 254 ISTD<7D% P F O S 254 tSTD<70% P F O S 254 !STD<70% PFO S 254 ISTD<70% P F O S 254 ISTD<70% PFO S 254 JSTEK70% PFO S 254 PFO S 254 PFO S 5.687 5.89 5.671 5.677 5.60 5.692 5.697 5.683 5.705 5.705 5.678 5.695 5.607 5.693 5.697 5.705 5.705 5.70 5.729 5.704 5.678 5.607 5.705 5.705 5.705 5.699 5 .7 0 5 5.712 5.732 5.733 12480311 1436.243 13594600 1672.643 12514844 1471.128 14781329 2466.895 16506784 2244.559 14008293 1753.191 20965681 3271.008 2100484O 4437.245 224003 5,3 11072 567B114 238.7682 18483679 2811.823 21906531 3611.765 22382831 3734.170 25723614 6383.82 43895144 12220.39 45027123 12681.8 40886156 10776.59 41047544 14963.72 285240 7.850201 5343857 237.702 19058110 2717.521 21568804 3278.966 23695132 3809.243 24318664 5515.216 13564243 13542160 15594555 16464813 203009 5141212 6 2 2 9 .9 4 5 6755.161 9159.363 12590.65 5.030216 234.1441 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 106.2% 95.3% 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 157.0% 94.0% 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 5 UL INJECTION VOLUME 2 UL INJECTION VOLUME 2 UL INJECTION VOLUME 2 UL INJECTION VOLUME 2 UL INJECTION VOLUME 100.6% 93.5% Co S' <D nt Q) Cr O rt 0) 8" X Sample Batch H010405.b, analyzed on Hillary 04-054)1. PFOS Adeprfe/Desorb ample*. Matrix; Soil/SIg/Sed. Standard curve range used for calibration of samples: 10-1002 ng/mL Batch method: H010405.m (external Standard Quant) in] Date Batch 4/6/01 12:53 0:\ChemiHiUaryiHO1O4O5.b 4/6/01 13:08 O:\Chem\HiltarytH010405.b /A/n* t i n n ichem\HjJJary\H010405.b 4/6/01 13:36 D:tChem\HiUary\H010405.b 4/6/01 13:51 D:\Chem\HiUary\H010405.b 4/6/01 14:05 D:\Chem\HiUary\H010405.b 4/6/01 14:20 D:\Chem\HillaryW010405J 4/6/0114:34 D:\ChemUHillary\H0104O5.b 4/6/0114:48 D:\Chem\Hiilary1H010405.b 4/5/0115:03 D:\Chem\HiUarylH01040S.b 4/6/0115:17 D:1Chem\Hi!lary\H010405.b 4/6/0115:31 0:\Cftem\NiHa<y\H010405-b 4/6/01 15.46 D:\Chem\Hillary\H010405.b 4/7/014:57 D:\Chem\Hillary\H010405.b 4/7/01 5:11 D:VChem\Hiliary\HOl0405.b 4/7/01 5:26 D:\Chem\Hillary\H010405b 4/7/01 5:40 D:\Chem\Hillary\H010405.b 4/7/01 5:55 D:\ChemlHiHary\H010405.b 4/7/01 6:09 O:\Chem\HiKary\H010405.b 4/7/016:23 D:\Cbem\Hiilary1H010405.b 4/7/01 6:38 D:\Cbem\Hillary\H010405.b 4/7/01 6:52 D.-1Cbem1Hiliajy1H010405.b 4/7/01 7:07 D:\Chem\Hillary\H010405.b 4/7/01 7:21 D:\Chem\Hillary\H010405.b 4/7/01 7:35 D:\Chem\Nillary\H010405.b 4/7/01 7:50 0:VChem\HiHaiylH010405.b SampType SAMPLE CAUB 1 CAUB 2 CALIB 3 CAUB 4 SAMPLE CALIB_5 CAUB 6 CAUB 7 CAUB 8 SAMPLE CALIB 9 CALIB 10 SAMPLE CALIB 11 CALIB 12 CAUB 13 CAUB 14 SAMPLE CAUB 15 CALIB 16 CAUB 17 CAUB 18 SAMPLE CAUB 19 CALIB_20 File HILL0016.D HILL0017.D HILL0018D HiLLOGiS.D HILL0020.D H11L002I.D HILL0022.D HILL0023.D HILL0024.D H1LL0025.D HIIL0026.D HILL0027.D HLL0028.D HILL0083.0 HILL0084.0 HILL0085.D HILL0066.D HILL0067.D HILL0088.D HILL0089.D HILL0090.D HIIL0091.D HILL0092.D H1LL0093.D HLL0094.D HILL0095.D Sample Name O ng/mL PFOS in MeOH 2.5 ng/ml PFOS inMeOH 5 ng/ml PFOS in MeOH 1C ng/ml PFOS inMeOH 25 ng/mL PFOS in MeOH 4 0 ng/mL PFOS inMeOH 50.1 ng/ml PFOS in MeOH 75.1 ng/mLPFOS inMeOH 1002 ng/ml PFOS in MeOH 250.5 ng/mL PFOS in MeOH 400.8 ng/mL PFOS in MeOH 501 ng/ml PFOS inMeOH 1002 ng/ml PFOS inMeOH O ng/ml PFOS in MeOH 2.5 ng/ml PFOS inMeOH 5ng/mL PFOS in MeOH 10 ng/mLPFOS mMeOH 25 ng/mLPFOS inMeOH 40 ng/ml PFOS inMeOH 50.1 ng/ml PFOS in MeOH 75.1 ng/mL PFOSin MeOH 100.2 ng/mL PFOSin MeOH 250.5 rtg'mL PFOSin MeOH 400.8 ngfmL PFOS in MeOH 501 ng/ml PFOS inMeOH 501 ng/mL PFOS in MeOH In] Date Batch 4/6/01 12:25 D:\Chem\Hillaiy\H010405.b 4/6/01 12:39 D:\ChemiHiflary\H010405.b 4/6/01 16.00 D:\Chem\Hillary\H010405.b 4/6/01 16:14 D:\Chem\Hillaiy\H010405.b 4/6/01 19:21 D:\Chem\Hillary\H010405.b 4/6/01 19:36 D:\Chem\Hillary\H010405.b 4/6/01 22:43 D:\Chem\Hillary\H010405.b 4/6/01 22:57 D:\ChemWiilafy\H010405.b 4/7/01 1:50 D:\ChemMllary\H010405.b 4/7/01 2:04 D:\Chem\Hillary\H010405.b 4/7/01 428 D:\Chem\HiJlaiy\H010405.b 4/7/01 4:43 D:\Chem\HiUary\H010405.b 4/7/01 8:04 D:\Chem\Hiilary\H010405.b 4/7/01 8:18 D:\Chem\Hillary\H010405.b SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File HILL0014.D HILL0015.D HILL0029.D HILL0030.D HILL0043.O HILL0044.0 HILL0057.D HILL0058.D HILL0070.D HILL0071.D HILL0081.D HILL0082.D HILL0096.D HIIL0097.D Sample Name TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4602 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4602 MeOH TN-A4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Page 547 of 703 BACK TO MAIN HOI0405 external standard quanUdS M ise In fo Mise info C om pound NaRT A rts THPFOS 5.111 THPFOS 5.121 THPFOS 5.12 THPFOS 5.107 THPFOS 5.106 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 5.098 THPFOS 5.092 THPFOS 5.098 THPFOS 5.1 THPFOS 5.106 THPFOS 5.101 THPFOS 5.1 THPFOS 5.101 THPFOS 5.106 THPFOS 5.107 THPFOS 5.105 THPFOS 5.104 THPFOS 5.104 Am ount 853901 254 880305 254 900514 254 884801 254 891555 254 895606 254 905309 254 901986 254 902929 254 921590 254 890229 254 885051 254 906846 254 909918 254 901288 254 907830 254 893968 254 866284 254 854670 254 646217 254 818486 254 824040 839800 254 254 795504 254 790146 254 796759 254 A ve ra ge : 871828.1538 Std Dev. 39403,57909 % RSP: 4.5% C om pound N aiftT 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 Am ount 0 00 5.331 64194 0 5.33 113000 2.152886 5.324 189968 6,660505 5.323 495541 24.66062 5.331 779774 41.55324 5.33 971274 53.01579 5.331 1469171 83.12445 5.329 1921199 110.8424 5.322 4651125 285.988 5 335 6791612 432.6167 5.322 8184382 532.4149 5.33 14871358 1059.765 0 00 5.302 53650 0 5.301 95517 1.130466 5.31 158439 4.812732 5,316 425595 20.52568 5.311 675739 35.35348 5.31 647857 45.62096 5.311 1278693 71.55369 5.309 1665685 95.12972 5.31 4111457 250.3098 5.308 6004617 377.7554 5.314 7263676 466.0545 5.314 13221474 922.2377 1133377 +30%: 610280 -30%: 43% 67% 99% 104% 106% 111% 111% 114% 106% 106% 106% 23% 48% 82% 88% 91% 95% 95% 100% 94% 93% 92% C om p o u n d NaRT 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 Am ount 00 00 00 00 00 0a 00 00 00 00 00 00 00 00 C om pound N arftT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area 0 0 0 0 0 0 0 0 D 0 0 0 0 0 Am ount 00 00 00 00 00 00 00 00 00 00 00 00 00 Q0 e^ c page t of 2 3M Environmental Laboratory HQ1040S external standard quantxls inj Date Batch 4/6/01 16:29 D:\Cbem\Hillary\H010405.b 4/6/01 16:43 D:\Chem\Hillary\H010405.b 4/6/01 16:58 D:\Chem\Hillary\H010405.b 4/6/01 17:12 D:\Chem\Hillary\H010405.b 4/8/01 17:26 D:\Chem\Hillary\H010405.b 4/6/01 17:41 U:y-nem'tHiii5<yu4C104Q5.b 4/6/01 17:55 O:\ChemtHtUary\H010405.b I i D:tCtiem1HiUary'\H010405.b 4/6/01 18:24 OXhemlH(Hary\H0)0405.b 4/6/01 18:38 D:tChemtHillarytH01D405.b 4/6/01 18:52 0:1ChemiHiary\H010405.b 4/6/01 19:07 O:\Ct\em\Hillary\H010405.b 4/6/01 19:50 D:\Chem1KfHary\H010405.b 4/6/01 20:04 D:\Chem\Hitlary\H010405.b 4/6/01 20:19 O:\Chem1HillarytH010405.b 4/6/01 20:33 D:\ChemtHitfarytH010405.b 4/6/01 20.48 D:\Chem\HiWaiy\H010405.b 4/6/01 21:02 D:\Chem\Hillary\H01040S.b 4/6/01 21:16 O:\Chem\Hillary\H010405.b 4/6/01 21:31 D:\Chem\Hillary\H010405.b 4/6/01 21:45 D:\Chem\Hillary\H010405.b 4/6/01 21:59 D:\Chem\Hillary\H010405.b 4/6/01 22:14 D:\Chem\Hiltary\H010405.b 4/6/01 22:28 D:\Chem\HillaryU-l01Q405.b 4/6/01 23:11 D:\Chem\Hillary\H010405.b 4/6/01 23:26 D:\Chem\Hillary\H010405.b 4/6/01 23:40 D:\Chem\Hillarv\H010405.b 4/6/01 23:55 D:1Cbem\Hiliary\H010405.b 4/7/01 0:09 D:\Chem\Hillaty\H010405.b 4/7/01 0:23 D:\Chem\Hiliary\H010405.b 4/7/01 0:38 O:\Cbem\Hiilaiy\H010405.b 4/7/01 0:52 D:\Chem\Hillary\H010405.b 4/7/01 1:07 D:\Cbem\Hillary\H010405.b 4/7/01 1:21 D:\Cbem\Hillary\H010405.b 4/7/01 1:36 D:\Cbem\Hiltary\H0lO405.b 4/7/01 2:19 O:\Chem\Hiltary\H010405.b 4/7/01 2:33 D:\Chem\Hitlary\H010405.b 4/7/01 2:47 D:\Chem\Hillaty\H010405.b 4/7/01 3:02 D:\ChemVHillary\H010405.b 4/7/01 3:16 D:\Chem\Hillary\H010405.b 4/7/01 3:31 D:VChemtHiH*ytH0t0405.b 4/7/01 3:45 D:\Chem\HiffafylH010405.b 4/7/01 3:59 D:\Chem\HtllafylH010405.b 4/7/01 4:14 D:\Chem1Hiliary\HOlO405.b 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 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File Sample Name Mise Info HILL0031.0 2mg/L PFOS Study Number EOO-1311 1311-5043-S1 HILL0032.D 2mg/L PFOS Study Number EOO-1311 1311-5044-Si HILL0033.0 2mg/L PFOS Study Number EOO-1311 1311-5045-S1 HILL0034.D 2mg/L PFOS Study Number E00-1311 1311-5045MS-S1 HILL0035.D 10mg/L PFOS Study Number EOO-1311 1311-5049-S1 HILL0036.O 10mg/LPFOS StudyNumber EOO-1311 1311-5050-SI HILL0037.D 10mg/L PFOS StudyNumber EOO-1311 1311-5051-S1 HILL0038.0 10mg/L PFOS Study Number EOO-1311 1311-5051MS-S1 HILL0039.0 2mg/L PFOS Study Number EOO-1311 1311-5079-SI HILL0040.0 2mg/l PFOS Study Number EOO-1311 1311-5080-S1 HILL0041.D 5 ng/mL PFOS in MeOH HILL0042.D 250.5 ng/mL PFOS in MeOH HILL0O45.D 2mg/L PFOS StudyNumber EOO-1311 1311-508`1-SI HILL0046.D 2mg/L PFOS StudyNumber EOO-1311 1311-5061MS-S1 HILL0047.D 10mg/L PFOS Study Number E00-1311 1311-5085-S1 HILL0048.D 10mg/L PFOS Study Number 00-1311 1311-50B6-S1 HILL0049.D 10mg/L PFOS Study Number E00-1311 1311-5087-SI HILLD050.D 10mg/L PFOS Study Number 00-1311 1311-5067MS-S1 HILL0051.D Omg/L PFOS Study Number E00-1311 1311-5091-S1 HILL0052.D Omg/L PFOS Study Number EOO-1311 1311-5092-S1 HILL0053.D Omg/L PFOS Study Number 00-1311 1311-5093-S1 HILL0054.D Omg/L PFOS Study Number EOO-1311 1311-5093MS-S1 HILL0055.D 5 ng/mL PFOS inMeOH HILL0056.D 250.5 ng/mL PFOS in MeOH HILL0059.0 10mg/L PFOS Study Number EOO-1311 13-5121-S1 HJLL0060.D 10mg/L PFOS Study Number EOO-1311 311-5122-S1 HILL0061.D 10mg/L PFOS Study Number EOO-1311 1311-5123-S1 HILL0062.D 10mg/L PFOS Study Number EOO-1311 1311-5123MS-S1 HILL0063.D 10mg/L PFOS Study Number EOO-1311 1311-5157-S1 HILL0064.D 10mg/L PFOS StudyNumber EOO-1311 1311-5156-S1 HILL0065.D 10mgt PFOS Study Number EOO-1311 1311-5159-S1 HILL0066.0 lOmglL PFOS StudyNumber EOO-1311 1311-5159MS-S HILL0067.D Omg/L PFOS StudyNumber EOO-1311 1311-5181-SI HILL0068.D 5 ng/mL PFOS inMeOH HILL0069.D 250.5 ng/mL PFOS in MeOH HILL0072.D Omg/L PFOS Study Number EOO-1311 1311-5182-S1 HILL0073.0 Omg/L PFOS Study Number EOO-1311 1311-5163-S1 HILL0074.D Omg/L PFOS Study Number EOO-1311 1311-5183MS-S1 HILL0075.D Omg/L PFOS StudyNumber EOO-1311 1311-5199-S1 HILL0076.D Omg/L PFOS Study Number EOO-1311 1311-5200-S1 HILL0077.D Omg/L PFOS StudyNumber EOO-1311 1311-5201-S1 HILL0078.0 Omg/L PFOS StudyNumber 00-1311 1311-5201MS-S1 HILL0079.D 5 ng/mL PFOS (ftMeOH HILL0080.D 250.5 ng/mL PFOS in MeOH Compound NaRT Area THPFOS 5.112 THPFOS S.12 THPFOS 5.113 THPFOS 5.112 THPFOS 5.106 THPFOS 5.115 THPFOS 5.109 THPFOS 5.105 THPFOS 5.112 THPFOS 5.111 THPFOS 5.113 THPFOS 5.116 THPFOS 5.112 THPFOS 5.118 THPFOS 5.108 THPFOS 5.112 THPFOS 5.106 THPFOS 5.112 THPFOS 5.114 THPFOS 5.109 THPFOS 5.104 THPFOS 5.098 THPFOS 5.112 THPFOS 5.098 THPFOS 5.105 THPFOS 5.107 THPFOS 5.105 THPFOS 5.105 THPFOS 5.111 THPFOS 5.105 THPFOS 5.1 THPFOS 5.105 THPFOS 5.098 THPFOS 5.1 THPFOS 5.102 THPFOS 5.097 THPFOS 5.091 THPFOS 5.091 THPFOS 5.094 THPFOS 5.092 THPFOS 0 THPFOS O THPFOS 5.085 THPFOS 5.091 C("ZQ>D) or 00 0o0 page 2 o f2 BACK TO MAIN 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 IS TD>130% 254 Z54 254 IS TD>130% 254 tS TD>130% 254 254 ISTD> J30% 254 IS TD>130% 0 tSTD<70% 0 ISTD<70% 254 254 C om pound NarST 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 Area 5.329 5.33 5.323 5.322 5.323 5.333 5.326 5.322 5.329 5.321 5.323 5.326 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 5.317 5.322 5.323 5.322 5.315 5.31 5.315 5.308 5.31 5.312 5.307 0 5.301 0 0 0 5.295 5,295 5.308 Am ount 1594908 90.79793 1011666 55.44188 1801969 103.4959 4370912 267.3979 789270 42.1201 966799 53.94793 730034 38.58667 3483461 209.4461 1S92254 96.75814 2112598 122.6887 112770 2.139428 4597708 282.4334 1619584 92.30717 4093613 249.139 1001786 54.84818 996187 54.51181 998588 54.65605 3717782 224.6111 760291 40.39072 213559 8.044223 113509 2.182657 3059833 182.2781 109900 1.971553 4451710 272.7439 6644129 422.2516 7503267 483.1776 6451764 408.7904 6372595 546.1667 1011146 55.41063 1599452 91.07577 1567614 89.14206 4173504 254.3654 542210 27.42438 103957 1.623974 4298803 262.6366 144727 4.009669 00 2467820 144.8477 00 00 00 2260129 131.8644 95065 1.10404 4062781 247.1173 42 .8 % 112.7% 39.4% 108.9% 32 .5 % 104.8% 2 2 .1 % 9 8 .6 % Clay Clay Clay Clay Clay Clay Clay Clay Clay Loam C lay Loam Clay Loam Clay Loam Clay Loam Clay Loam C lay Loam Clay Loam Clay Loam C lay Loam C lay Loam Clay Loam Sandy Loam Sandy Loam Sandy Loam Sandy Loam Sedimant Sediment Sediment Sediment Sludge Sludge Sludge Sludge Sludge Sludge Sludge Sludge CMC 5 [ i l l ol sSSSiflSS ilHsti 1 1 1 IIP !!P 1 1 1 1 I1 .*ii!II!ii!!l!'iill|i|i!i|| `"asaaaaaaaaaa'aaaaaataaasa ! iflliilE iillliiliiiifliiiii Si H f "-- r "n r " " -- a- | Jim illlllililllliiiii 1 jiiiiiiiiiiiilliiiiiiiiili i <5iSSg*s*m*88S88525&8m lia loufuiuiidiAuiiAuiioioioiAiriiiiioiouiiriiAkntouiuiiriiri I O 3 oj '........................... r " 00=000000000000000000= s l ~Z II :"'Ew""ooS"eHP""llll||p1 lqQpQqqqqQqaDqpqQqDQpQQQQQ . .oSS b 5M5 M l!, H SSs5B5SB illllII!!!!!II!!l!I!!II qopqqpqqqppoqgppt ***** . ,8Sc iiiiS| iiiiiiiS ii|liili |sl||ll;|ill|ss3s;P sssssl m m m m r m ir ^ z 3M Environmental Laboratory O n C ^ H {a\ I Page 549 of 703 H01402.XS CO Inj Date Batch 4/2/01 16:26 D:\Chem\HiHary\H010402.b 4/2/0116:41 D:\ChemWHafy\H010402.b 4/2/01 16:55 D:\Chem\HiJlary\HOl0402.b 4/2/01 17:09 D:\Chem\Hillary\H010402.b 4/2/01 17:24 O:\Chem\Hiliary\H010402.b 4/2/01 17:36 D:\Chem\HiUafy\H010402.b 4/2/01 17:53 D:\Chem\Hillary\H010402.b 4/2/01 18:07 D:\Chem\Hillary\H010402.b 4/2/01 18:21 D:\Chem\Hiliary\H010402.b 4/2/0118:36 D:\Chem\Hillary\H010402.b 4/2/01 18:50 D:hem\HiHary\HO10402.b 4/2/01 19:04 D:\Chem\Hillary\H010402.b 4/2/01 19:48 D:\Chem\Hiltary\H010402.b 4/2/01 20:02 D:\Chem\Hillary\H010402.b 4/2/01 20:16 D:\Chem\Hillary\H010402.b 4/2/01 20:31 D:\Chem\Hillary\H0104Q2.b 4/2/01 20:45 D:\Chem\Hillary\H010402.b 4/2/01 20:59 D:\Chem\Hillary\H010402.b 4/2/01 21:43 D:\Chem\Hillafy\H010402.b 4/2/01 22:11 D:VChem\Hillary\H010402.b 4/2/01 22.40 D:\Chem\Hillary\H010402.b 4/2/01 23:09 D:\Chem\Hiflary\H010402.b 4/2/01 23:38 D:\CfiemtHiHary\H010402.b 4/3/01 0:06 D:\Chem\Hillary\H010402.b 4/3/01 0:35 D:VChem\Hillary\H010402.b 4/3/01 1:04 O:\Chem\Hillary\H010402.b 4/3/01 1:33 D:\Chem\Hillaiy\H010402.b 4/3/01 2:02 D:\Chem\Hillary\H010402.b 4/3/01 2:16 D:\Chem\Hillary\H010402.b 4/3/01 2:31 D:\ChemWflary\H010402.b 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 File HJLL0O32.D HILL0033.D HILL0034.D HILL0035D HILL0036.D HILL0037.D HILL0038.D HILL0039.D HILL0040.D HILL0041.D HILL0042.D HILL0043.D HILL0046.D HILL0047.D HILL0048D HILL0049.D HILL050.D HILL0051.D HILL0054.D HILL0056.D HLL0058.D HILL0060.D H IL L 0 0 6 2 D HILL0064.D HILL0066.D HILL0068.D HILL0070.D HILL0072.D HILL0073.D HILL0074. D Sample Name 2mg/L PFOS Study Number EOO-1311 2mg/L PFOS Study Number 00*1311 5m g/l PFOS Study Number 00-1311 Sttiq/L PFOS Study Number EOO-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Number 00-1311 10mg/L PFOS Study Number 00-1311 10mg/L PFOS Study Number 00-1311 10m&/t PFOS Study Number EOO-1311 10mg/L PFOS Study Number 00-1311 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH 50rog/L PFOS Study Number 00-1311 50mg/L PFOS Study Number EOO-1311 50mg/L PFOS Study Number 00-1311 50mg/L PFOS Study Number 00-1311 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH Omg/L PFOS Study Number EOO-1311 Omg/L PFOS Study Number 00-1311 Omg/L PFOS Study Number 00-1311 Omg/L PFOS Study Number EOO-1311 Omg/L PFOS Study Number EOO-1311 Omg/L PFOS Study Number EOO-1311 Omg/L PFOS Study Number EOO-1311 Omg/L PFOS Study Number 00-1311 5mg/L PFOS Study Number EOO-1311 5mg/L PFOS Study Number 00-1311 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in MeOH Mise 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 Page 550 of 703 page 2 of 2 BACK TO MAIN Area Amount 5.115 1099043 254 5.112 840525 254 5.119 1140615 254 5.134 1121827 254 5.121 1105544 254 5.119 914972 254 5.126 1092485 254 5.127 1128533 254 5.12 1141776 254 5.125 912742 254 5.127 929004 254 5.127 B75517 254 5.133 1161781 254 5.133 1078087 254 5.127 1116896 254 5.128 951406 254 5.128 924450 254 5.119 875539 254 5.112 1559964 254 5.111 1546480 254 5.107 1539293 254 5.099 1521208 254 5.106 1584873 254 5.098 1594416 254 5.097 1612740 254 5.098 15B2196 254 5.099 1615581 254 5.105 1590591 254 5.105 5.098 1403089 1313803 254 254 ISTD>130% ISTD130% 1STD>130% 1STD>130% 1STD>130% ISTD>130% IS T D *1 3 0 % ISTD>130% ISTD>130% 1STD>130% STD* 130% JSTD*130% C om pound ttariRT Aid s Amount PFOS 5.339 91766 2.852832 PFOS 5.336 3307625 190.4263 PFOS 5.336 250070 9.070036 PFOS 5.358 255601 9.465038 PFOS 5.345 202135 7.399684 PFOS 5.343 3416478 180.0553 PFOS 5.35 415060 16.4674 PFOS 5.351 524864 20.40436 PFOS 5.351 516752 19.82583 PFOS 5.349 3833223 204.1541 PFOS 5.351 115605 4.724463 PFOS 5.344 4809365 272.8592 PFOS 5.35 2608914 105.3019 PFOS PFOS 5.35 2143323 92.71704 5.351 1964759 82.4808 PFOS 5.353 4992173 259.5911 PFOS 5.345 121763 5.05741 PFOS 5.343 4808081 272.7724 PFOS PFOS 0 00 0 00 PFOS 0 00 PFOS 5.324 3196100 98.2237 PFOS 0O PFOS PFOS 000 000 PFOS 5.329 3075509 90.56476 PFOS 0 00 PFOS 000 PFOS PFOS 5.329 100877 2.321977 5.322 4689812 171.6327 94.5% 108.9% 101.1% 108.9% 46.4% 68.5% BACK TO MAIN s ^ 3 <X> rcr O 2 sX S am ple Batch R010329b.b, analyzed on R ush 03-29-01. PFOS A dsorb/D esorb sam ples. M atrix: S oil/S lg/S ed. S ta n d a n i c u rv e range use d fo r c a lib ra tio n o f sa m p le s : 5-501 n g /m L (2.5 ng/mL std n o t in c lu d e d d ue to th e h ig h e r sa m p le c o n c e n tra tio n range). B atch m ethod: R010329.m Inj Date B atch 3/30/01 14:44 D :\C hetn\R ush\R 01032 9.b 3/30/01 14:58 D :\Ch em \Ru shVR0132S. 3/30/01 15:13 D :\Chem VRush\R010329.b 3/30/01 15:27 D:\C hem \R ush\R 010329.b 3/30/01 15:41 D :\C hem \R ush\R 010329 .b 3/30/01 15:56 D:\ChemVRush\R010329.b 3/30/01 16:10 D:\ChemVRush\R010329.b 3/30/01 16:25 D :\C hem \R ush\R 010329 .b 3/30/01 16:39 D:\C hem \R ush\R 010329.b 3/30/01 16:53 D:\ChemVRush\R010329.b 3/30/01 17:08 D :VChem \RusM R010329.b 3/30/01 17:22 D :\C hem \R usb\R 010329.b 3/30/01 17:36 D:\ChemVRush\R010329.b 3/31/01 10:24 D :VChe m\R ushVR010 3 29.b 3/31/01 10:38 D :\C hem \R usb\R 010329.b 3/31/01 10:53 D :\C hem \R ush\R 010329 .b 3 /3 f/0 f 11:07 D :\C heni\R ush\R 010329.b 3/31/01 11:21 D :\C hem \R ush\R 010329.b 3/31/01 11:36 D:\C hem \R ush\R 010329.b 3/31/01 11:50 D:\C hem \R ush\R 010329.b 3/31/01 12:04 D:\Chem\RushVR010329.b 3/31/01 12:19 D :\C hem \R ush\R 010329 .b 3/31/01 12:33 D:\C hem \R ush\R 010329.b 3/31/01 12:48 D AChemVRu sh\R 010329 .b 3/31/01 13:02 DAChem\RushVR010329.b 3/31/01 13:16 D AChemVRu shVROI 0329 .b Sam pType SAMPLE CAL!S_1 CALIB 2 CALIB 3 CALIB 4 CALIB 5 CALIB 6 C A L IB _ 7 CALIB 8 CALIB_9 SAMPLE CALIB 10 SAMPLE SAMPLE C A LIB 11 CALIB 12 C A LIB 13 C A LIB 14 C A LIB 15 C A LIB 16 C A LIB 17 C A LIB 18 CALIB 19 SAMPLE CALIB 20 SAMPLE File Sample Nam e RU SH 0104.D 0 ng/m L PFOS in MeOH R U S H 010S .D 2.5 n g/m L PFO S in M eOH RU SH 0106.D 5 ng/m L PFO S in M eOH RU SH 0107.D 10 ng/m L PFO S in MeOH R U S H 0 1 0 8 .0 25 ng /m L PFO S in M eO H RUSH01O9.D 4 0 ng/m L PFOS in MeOH RUSH0110.D 50.1 ng/m L PFOS in MeOH R U S H 0111.D 75.1 ng /m L PFO S in M eO H R U S H 0 1 12.D 100.2 n g/m L PFO S in M eOH RUSH0113.D 250.5 ng/m L PFOS in MeOH R U S H 114.D 400.8 ng /m L PFO S in M eO H R U S H 0115.D 501 n g /m L PFO S in M eO H RUSH0116.D 1002 ng/m L PFOS in MeOH RUSH0186.D 0 ng/m L PFOS in M eOH RUSH0187.D 2.5 ng/m L PFOS in MeOH RUSH0188.D 5 ng/m L PFO S in M eOH RUSH0189.D 10 ng/mL PFO S in MeOH RUSH0190.D 25 ng/m L PFOS in MeOH R U SH 0191.0 4 0 ng/m L PFOS in MeOH RUSH 0192.0 50.1 ng/m L PFO S in M eOH R U S H 0193.D 75.1 n g/m L P F O S in M eO H RUSH0194.D 100.2 ng/m L PFOS in M eOH RUSH0195.D 2 5 0 .5 ng/m L PFOS in M eOH RUSH0196.D 400.8 ng/m L PFOS in M eOH RUSH0197.D 501 ng/m L PFOS in MeOH RUSH0198.D 1002 ng/m L PFOS in MeOH M ise In fo C o m p o u n d NariRT A re a Am ount THPFOS 5.574 845852 254 THPFOS 5.561 850507 254 THPFOS 5.57 805498 254 THPFOS 5.574 844287 254 THPFOS 5.574 874781 254 THPFOS 5.575 874280 254 THPFOS 5.575 856450 254 THPFOS 5.562 857550 254 THPFOS 5.568 863358 254 THPFOS 5.578 806157 254 THPFOS 5.574 858200 254 THPFOS 5.57 909424 254 THPFOS 5.568 813760 254 THPFOS 5.52 760278 254 THPFOS 5.534 761291 254 THPFOS 5.517 731965 254 THPFOS 5.515 771260 254 THPFOS 5.511 764462 254 THPFOS 5.517 789541 254 THPFOS 5.524 769770 254 THPFOS 5.517 764856 254 THPFOS 5.526 787147 254 THPFOS 5.519 733566 254 THPFOS 5.522 775073 254 THPFOS 5.525 827129 254 THPFOS 5.525 744097 254 C om pound ART Area Am ount PFOS 000 PFOS 5.771 234324 2.8 0 3 6 1 9 PFOS PFOS PFOS 5.78 5.773 5.777 259067 4.511131 372504 n QR9F?? 750617 25.05443 PFOS 5.778 1074369 39.99818 PFOS 5.778 1261642 50.16737 PFOS 5.765 1770429 75.B725 PFOS 5.771 2201517 98.11491 PFOS PFOS 5.789 4379739 251.4603 5.777 6738768 408.2194 PFOS 5.773 8394525 508.9853 PFOS 5.778 12942478 1114.479 PFOS 000 PFOS PFOS PFOS 5.744 5.727 5.725 222040 254163 358164 3.400639 5.463481 9.856614 PFOS 5.721 666714 25.61491 PFOS 5.727 980488 40.53221 PFOS 5.734 1138146 50.39724 . PFOS 5.727 1583158 76.11235 PFOS 5.729 2037660 99.93338 PFOS 5.729 3963988 249.7285 PFOS 5.733 6072032 406.9537 PFOS 5.728 7615022 507.1578 PFOS 5.728 11828829 1113.673 90.2% 89.8% 100.2% 99.7% 100.1% 101.0% 97.9% 100.4% 101.6% 109.3% 98.6% 102.5% 101.1% 100.6% 101.3% 99.7% 99.7% 101.2% A ve ra o e : 809251.5 S td Dev: 50097.37 % R S P : 6.2% 1052027 +30%: 566476 -30%: P r O' <->0 o - 7T 4- - Page 551 of 703 page 1 of 4 BACK TO MAIN Co ? ^S3' 2 ^CD3 O0)' S am ple B atch RQ10329b.b, analyzed on R ush 03-29-01. PFOS Adsorb/Desorfc sam ples. M a trix: Soil/SJg/Sed. S ta n d a r d c u rv e ra n g e u s e d fo r c a lib ra tio n o f s a m p le s : 5-501 n g /m L (2.5 ng/mL s td n o t In c lu d e d d u e to th e h ig h e r s a m p le c o n c e n tra tio n range). B a tch m e th o d : R010329.m ' fn i Date B atch Jnj D ate B a tc h 3/30/01 14:15 D \C hem \R ush\R 010329.b 3/30/01 14:29 D :\C hem \R ush\R 010329.b 3/30/01 17:51 D :\C hem \R ush\R 010329 .b o CD cn D:\Chem \Rush\R010329.b 3/30/01 18:20 D;VChem\Rush\R010329.b 3/30/01 21:27 D:\Chem \Rush\R010329.b 3/30/01 21:41 D:\Chem \Rush\R010329.b 3/31/01 0:48 D:\Chem \Rush\R010329.b 3/31/01 1:03 D :\C hem \R ush\R 010329 .b 3/31/01 4:10 D:\Chem \Rush\R010329.b 3/31/01 4:24 D :\C hem \Rush\R010329.b 3/31/01 7:31 D :\C hem \R ush\R 010329 .b 3/31/01 7:46 D:\Chem \Rush\R010329.b 3/31/01 9:41 D :\C hem \R ush\R 010329 .b 3/31/01 9:55 D:\C hem \R ush\R 010329.b 3/31/01 10:09 D:\C hem \R ush\R 010329.b 3/31/01 13:31 D :\C hem 1R ush\R 010329.b Sam pType Sam pType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File S am ple Name File Sample Nam e RUSHQ102.D TN-A 4802 M eO H KSH 003.D 7N-A 4902 MeOH RUSH0117.D TN-A 4802 M eO H RSH0118.D TN-A 4802 M eO H RUSH0119.D TN-A 4802 MeOH RUSH0132.D TN-A 4802 MeOH RUSH0133.D TN-A 4802 MeOH RUSH148.D TN-A 4802 MeOH RUSH0147.D TN-A 4802 MeOH RUSH0160.D TN-A 4802 MeOH RUSH0161.D TN-A 4802 MeOH RUSH0174.D TN-A 4802 MeOH RUSH0175.D TN-A 4802 MeOH RUSH0183.D TN-A 4802 MeOH RUSH0184.D TN-A 4802 MeOH RUSH0185.D TN-A 4802 MeOH RUSH0199.D TN-A 4802 MeOH M ise In fo C o m p o u n d NariRT M ise In fo C om p o u n d N a i# T THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS A re a A re a 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Am ount Am ount 00 00 0n 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Compound hR T Compound fftT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A re a Am ount Area Am ount 5.792 144070 0 5.789 136863 0 5.798 170024 0 5.793 144025 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 TJJ CQ CD Nccnn) 0o3 page 2 of 4 Environmental Laboratory BACK TO MAIN CO Sam ple Batch R010329b.b, analyzed on Rush 03-29-01. PFOS Adsorb/Desorb sam ples. Matrix: Soil/SIg/Sed. S ta n d a rd c u rve range used fo r calibration o f sam p les: 5-501 ng/m L (2.5 ng/mL std n ot in clu d ed d ue to th e h ig h e r sa m p le co n cen tratio n range). Batch m ethod: R01Q329.m in} D ate Batch tnj Date Batch 3/30/01 18:34 D:\C hem \R ush\R 010329.b 3/30/01 18:48 D :\C nem \R usniR G 032S.& 3/30/01 19:03 D :\C hem \R ushW 010329.b 3/30/01 19:17 D:\C hem \R ush\R 010329.b 3/30/01 19:32 D:\C hem \R ush\R 010329.b 3/30/01 19:46 D:\C hem \R ush\R 010329.b 3/30/01 20:00 D :\C hem \Rush\R010329.b 3/30/01 20:15 D :\C hem \R ush\R 010329 .b 3/30/01 20:29 D:tChem \Rush\R010329.b 3/30/01 20:43 D:\C hem \R ush\R 010329.b 3/30/01 20:58 D:\C hem \R ush\R 010329.b 3/30/01 21:12 D:\C hem \R ush\R 010329.b 3/30/01 21:55 D:\C hem \R ush\R 010329.b 3/30/01 22:10 D:\C hem \R ush\R 010329.b 3/30/01 22:24 D:\Chem \Rush\R010329.b 3/30/01 22:39 D:\Chem \RushtR010329.b 3/30/01 22:53 D\Chem\Rush)R010329.b 3/30/01 23:07 D:\Chem \Rush\R010329.b 3/30/01 23:22 D :\C bem \R ush\R 010329 .b 3/30/01 23:36 D :\C hem \Rush\R010329.b 3/30/01 23:51 D :\C hem \R ush\R 010329 .b 3/31/01 0:05 D :\Chem \Rush\R010329.b 3/31/01 0:20 D:\Chem \Rush\R010329.b 3/31/01 0:34 D:\Chem \Rush\R010329.b SampType SampType SAMPLE sam ple 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 File Sample Name R U S H 012 0 .D Study N um ber EOO-1311 R U S H 0121 .D Study N um ber E 0 0 -1 311 R U S H 0122.D Study N um ber E 0 0 -1 311 RU SH 0123.D Study N um ber E00-1311 R U S K 0124.D Study Number E00-1311 R U S H 0125.D Study N u m b e r EOO-1311 R U S H 0 1 2 6 .D Study N um ber EOO-1311 R U S H 0127.D Study N um ber E 0 0 -1 311 R U S H 0 1 2 8 .D Study N um ber EOO-1311 RUSH0129.D Study N um ber EOO-1311 RUSHQ130.D 5 ng/m L PFOS in MeOH R U S H 0131.D 2 5 0 .5 ng/m L P F O S in M eO H RUSH0134.D Study N um ber EOO-1311 RUSH0135.D Study N um ber EOO-1311 RU SH 0136.D Study N um ber E 00-1311 RU SH 0137.D Study N um ber E 00-1311 RSH0138.D Study N um ber EOO-1311 RUSH0139.D Study Num ber EOO-1311 RUSH0140.D Study N um ber EOO-1311 RUSH0141.D Study N um ber 00-1311 RUSH0142.D Study N um ber EOO-1311 R U SH0143.D S tudy N um ber EOO-1311 RUSH0144.D 5 ng/m L PFOS in MeOH RUSH145.D 2 5 0 .5 ng/m L PFOS in M eOH Mise info Com pound N a tfiT Area Amount Mise info Com pound N a i* T Area Amount THPFOS 5.574 700662 254 THPFOS THPFOS 5.565 C WQ 880404 820419 254 254 THPFOS 5.57 821252 254 THPFOS 5.579 673700 254 THPFOS 5.573 843531 254 THPFOS 5.568 821307 254 THPFOS 5.56 824221 254 THPFOS 5.554 655636 254 THPFOS 5.551 814171 254 THPFOS 5.547 794288 254 THPFOS 5.553 791691 254 THPFOS 5.562 835122 254 THPFOS 5.571 804691 254 THPFOS 5.57 644452 254 THPFOS 5.567 873023 254 THPFOS 5.567 887648 254 THPFOS 5.56 926167 254 THPFOS 5.561 7 58299 254 THPFOS 5.568 824449 254 THPFOS 5.574 804628 254 THPFOS 5.567 789160 254 THPFOS 5.57 774516 254 THPFOS 5.568 768622 254 Com pound NRT Area Amount Com pound NRT Area Amount PFOS 5.777 3839014 254.22 PFOS 5.769 2916166 135.13 PFOS 5.779 2814668 1 4 1 .1 1 PFOS PFOS 5.781 2547623 5.789 5475251 142 7 427.65 PFOS 5.776 1878094 83.18 PFOS 5.779 1731214 77.82 PFOS 5.763 1739800 77.95 PFOS 5.75 4384199 329.52 PFOS 5.755 3390903 179.53 PFOS 5.757 258302 4.64 PFOS 5.756 4310524 252.17 PFOS 5.765 3594706 187.10 PFOS PFOS 5.774 3233585 5.773 5569928 171.68 465.00 PFOS 5.77 2283901 101.23 PFOS 5.77 2361032 103.30 PFOS 5.763 2579566 109.27 PFOS 5.764 5414508 359.43 PFOS 0 0 0 .0 0 PFOS 5.784 203794 1.98 PFOS 0 0 0 .0 0 PFOS 5.78 250673 4.59 PFOS 5.771 4 2 05216 2 5 3.74 92.9% 100.7% 91.7% 101.3% (Q0T)! CD CJl 07 CO o-si CO page 3 of 4 BACK TO MAIN 5 3 3CD U) oO0r)-' 2 5 Sam ple Batch R010329b.b, analyzed on Rush 03-29-01. PFOS Adsorb/Desorb sam ples. Matrix: Soil/SIg/Sed. S tandard curve range used fo r calibration o f sam ples: 5-501 ng/m L (2.5 ng/mL std n o t included due to the high e r sample conce ntratio n range). Batch m ethod: R010329.m In) Date Batch 3/31/01 1:17 D:\Chem\Rush\ROl0329.b 3/31/01 1:32 D:\Chem\Rush\K1329.b 3/31/01 1:46 D:\Chem\Rush\R010329.b 3/31/01 2:00 D:\Chem\Rush\R010329.b 3/31/01 2:15 D:\Chem\RushtR010329.b 3/31/01 2:29 D:\Chem\Rush\R010329.b 3/31/01 2:43 D:\Chem\Rush\R010329.b 3/31/01 2:58 D:\Chem\RushVR010329.b 3/31/01 3:12 D:\Chem\RusMRQ10329.b 3/31/01 3:27 D:\Chem\Rush\R010329.b 3/31/01 3:41 D:\Chem\RushtR010329.b 3/31/01 3:55 D:\Chem\Rush\R010329.b 3/31/01 4:39 D:\Chem\Rush\R010329.b 3/31/01 4:53 D:\Chem\Rush\R010329.b 3/31/01 5:07 D:\Chem\Rush\R010329.b 3/31/01 5:22 D:\Chem\Rush\R010329.b 3/31/01 5:36 D:\Chem\Rush\R010329.b 3/31/01 5;50 D:\Chem\Rush\R010329.b 3/31/01 6:05 D:\Chem\Rush\R010329.b 3/31/01 6:19 D:\Chem\Rush\R010329 .b 3/31/01 6:34 D:\Cbem\Rush\R010329 .b 3/31/01 6:48 D:\Chem\Rush\R01D329.b 3/31/01 7:02 D:\Chem\Rush\R010329.b 3/31/01 7:17 D:\Chem\Rush\R010329.b 3/31/01 8:00 D:\Chem\Rush\R010329.b 3/31/01 8:14 D:\Chem\Rush\R010329.b 3/31/01 8:29 D:\Cbem\Rush\R010329.b 3/31/01 8:43 D:\Chem\Rush\R010329.b 3/31/01 0:57 D:\Chem\RushtR010329.b 3/31/01 9:12 D:\Chem\RushtR010329.b 3/31/01 9:26 D:\Chem\Rush\R010329.b 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 File Sample Name RUSH0148.D Study Number E00-1311 RUSH0149.D Study Number E00-1311 RUSH0150.D Study Number E00-1311 RUSH0151.0 Study Number E00-1311 RUSH0152.D Study Number E00-1311 RUSH0153.D Study Number EOO-1311 RUSH0154.D Study Number EOO-1311 RUSH0155.D Study Number E00-1311 RUSH0156.D Study Number E00-1311 RUSH0157.D Study Number EOO-1311 RUSH0158.D 5 ng/mL PFOS in MeOH RUSH0159.D 250.5 ng/mL PFOS in MeOH RUSH162.D Study Number E00-1311 RUSH0163.D Study Number E00-1311 RUSH0164.0 Study Number E00-1311 RUSH0165.D Study Number EOO-1311 RUSH0166.D Study Number EOO-1311 RUSH0167.D Study Number EOO-1311 RUSH0168.D Study Number EOO-1311 RUSH0169.D Study Number E00-1311 RUSH0170.D Study Number E00-1311 RUSH0171.D Study Number E00-1311 RUSH0172.D 5 ng/mL PFOS in MeOH RUSH0173.D 250.5 ng/mL PFOS in MeOH RUSH0176.D Study Number EOO-1311 RUSH0177.D Study Number EOO-1311 RUSH0178.D Study Number E00-1311 RUSHO179.0 Study Number EOO-1311 RUSHO180.D Study Number EOO-1311 RUSH0181.0 5 ng/mL PFOS in MeOH RUSH0182.D 250.5 ng/mL PFOS in MeOH Mise Into Compound NarAT 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 5.568 648571 254 5.571 777614 254 5.56 773093 254 5.57 765384 254 5.56 699682 254 5.554 752148 254 5.553 740653 254 5.552 760503 254 5.547 630350 254 5.54 726006 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 5.528 615539 254 254 5.524 771909 254 5.528 694870 254 5.525 717026 254 5.525 618466 254 5.524 70677 254 5.526 709256 254 Com pound MCT Area Amount PFOS 5.778 3031707 207.59 PFOS 5.774 1604497 75.82 PFOS 5.763 1592359 75.66 PFOS 5.773 1911308 95.65 PFOS 5.763 4619176 324.00 PFOS 5.757 6721579 486.79 PFOS 5.756 7944853 627.78 > 501 ug/L PFOS 5.749 7336093 541.01 > 501 ug/L PFOS 5.75 8586480 885.44 > 501 ug/L PFOS 5.743 3782037 238.27 PFOS 5.753 251147 5.22 104.4% PFOS 5.744 4087493 261.45 104.4% PFOS 5.743 3926573 236.36 PFOS 5.751 3793091 226.44 PFOS 5.75 5938887 541.09 > 501 ug/L PFOS 5.74 6989609 530.96 > 501 ug/L PFOS 5.736 7352037 532.24 > 501 ug/L PFOS 5.739 7301746 543.57 > 501 ug/L PFOS 5.728 9140058 1045.56 > 501 ug/L PFOS 5.736 5403042 303.36 PFOS 5.739 5358582 279.64 PFOS 5.743 4454099 283.95 PFOS 5.742 253008 5.23 104.5% PFOS 5.735 3903435 247.03 98.6% PFOS 5.738 6430648 604.83 > 501 ug/L PFOS 5.727 740559 29.08 PFOS 5.738 236023 5.29 PFOS 5.735 210945 3.49 PFOS 5.728 3041758 221.42 PFOS 5.741 249768 5.69 113.9% PFOS 5.736 3915802 256.72 102.5% Page 554 of 703 page 4 of 4 BACK TO MAIN CO ? S3' C5D oT teCOu'r 2 cf >5 (0Q)D CD Occnnl o --* 'vl o CO Sample Batch R010329a.b, analyzed on Rush 03-29-01. PFOS Adsorb/Desorb samples. Matrix: Soil/SIg/Sed. Standard curve range used for calibration of samples: 5-501 ng/mL (2.5 ng/mL std not included due to the higher sample concentration range). Batch method: R010329.m Inj Date Batch SampTypeFile Sample Name Mise InfCompouncRT Area Amount 3/29/01 19:04 D:\Chem\RSAMPLE RUSH00220 ng/mL PFOS in MeOH THPFOS 5.581 937536 254 3/29/01 19:19 D:\Chem\RCALIB_1 RUSH00232.5 ng/mL PFOS in MeOH THPFOS 5.587 932041 254 3/29/01 19:33 D:\Chem\RCALIB_2 RUSH00245 ng/mL PFOS in MeOH THPFOS 5.582 892607 254 3/29/01 19:47 D:\Chem\RCALIB_3 RUSH002510 ng/mL PFOS in MeOH THPFOS 5.59 941200 254 3/29/01 20:02 D:\Chem\RCALIB_4 RUSH002625 ng/mL PFOS in MeOH THPFOS 5.586 952213 254 3/29/01 20:16 D:\Chem\RCALIB_5 RUSH002740 ng/mL PFOS in MeOH THPFOS 5.581 964296 254 3/29/01 20:30 D:\Chem\RCALIB_ 6 RUSH002850.1 ng/mL PFOS in MeOH THPFOS 5.588 940694 254 3/29/01 20:45 D:\Chem\RCALIB_7 RUSH002975.1 ng/mL PFOS in MeOH THPFOS 5.582 913845 254 3/29/01 20:59 D:\Chem\RCALIB_ 8 RUSH0030100.2 ng/mL PFOS in MeOH THPFOS 5.584 931382 254 3/29/01 21:13 D:\Chem\RCALIB_9 RUSH0031250.5 ng/mL PFOS in MeOH THPFOS 5.581 882940 254 3/29/01 21:28 D:\Chem\RSAMPLE RUSH0032400.8 ng/mL PFOS in MeOH THPFOS 5.577 925627 254 3/29/01 21:42 D:\ChemlRCALIB_10 RUSH0033501 ng/mL PFOS in MeOH THPFOS 5.582 989407 254 3/29/01 21:57 D:\Chem\RSAMPLE RUSH00341002 ng/mL PFOS in MeOH THPFOS 5.585 884676 254 3/30/01 14:44 D:\Chem\RSAMPLE RUSH0104O ng/mL PFOS in MeOH THPFOS 5.574 845419 254 3/30/01 14:58 D:\Chem\RCALIB_11 RUSH01052.5 ng/mL PFOS in MeOH THPFOS 5.561 850637 254 3/30/01 15:13 D:\Chem\RCALIB_12 RUSH01065 ng/mL PFOS in MeOH THPFOS 5.57 805498 254 3/30/01 15:27 D:\Chem\RCALIB_13 RUSH01071O ng/mL PFOS in MeOH THPFOS 5.574 844287 254 3/30/01 15:41 D:\Chem\RCALIB_14 RUSH010825 ng/mL PFOS in MeOH THPFOS 5.574 874781 254 3/30/01 15:56 D:\Chem\RCALIB_15 RUSH010940 ng/mL PFOS in MeOH THPFOS 5.575 874280 254 3/30/01 16:10 D:\Chem\RCALIB_16 RUSH011050.1 ng/mL PFOS in MeOH THPFOS 5.575 856450 254 3/30/01 16:25 D:\Chem1RCALIB_17 RUSH011175.1 ng/mL PFOS in MeOH THPFOS 5.562 857550 254 3/30/01 16:39 D:\Chem\RCALIB_18 RUSH0112100.2 ng/mL PFOS in MeOH THPFOS 5.568 863358 254 3/30/01 16:53 D:\Chem\RCALIB_19 RUSH011325O.5 ng/mL PFOS in MeOH THPFOS 5.578 806157 254 3/30/01 17:08 D:\Chem\RSAMPLE RUSH0114400.8 ng/mL PFOS in MeOH THPFOS 5.574 858200 254 3/30/01 17:22 D:\Chem\RCALIB_20 RUSH0115501 ng/mL PFOS in MeOH THPFOS 5.57 909424 254 3/30/01 17:36 D:\Chem\RSAMPLE RUSH01161002 ng/mL PFOS in MeOH THPFOS 5.568 813760 254 CompouncRT Area Amount PFOS 00 0 PFOS 5.797 233998 2.84 PFOS 5.793 265016 4.50 PFOS 5.793 397179 9.07 PFOS 5.789 812531 25.37 PFOS 5.784 1183051 40.13 PFOS 5.798 1389031 50.34 PFOS 5.792 1906080 76.36 PFOS 5.787 2452896 101.14 PFOS 5.791 4875108 253.12 PFOS 5.787 7451045 415.73 PFOS 5.785 9377197 519.76 PFOS 5.788 14614178 1161.45 PFOS 0 0 0.0 0 PFOS 5.771 234682 3.73 PFOS 5.78 259067 5.40 PFOS 5.778 372504 9.78 PFOS 5.777 750517 25.55 PFOS 5.778 1074369 40.21 PFOS 5.778 1261642 50.20 PFOS 5.765 1770429 75.43 PFOS 5.771 2201517 97.27 PFOS 5.789 4379739 247.92 PFOS 5.777 6738768 402.04 PFOS 5.773 8394525 501.13 PFOS 5.778 12942478 1096.91 89.9% 90.7% 101.5% 1 0 0 .1 % 100.5% 101.7% 100.9% 1 0 1 .0 % 103.7% 107.9% 97.8% 1 0 2 .2 % 100.3% 1 0 0 .2 % 100.4% 97.1% 99.0% 1 0 0 .0 % Average: 890317.9 Std Dev: 49995.31 %RSD: 5.6% 1157413 +30%: 623223 -30%: Page 1 of 4 on e pg BACK TO MAIN Co Environmental Laboratory Sample Batch R010329a.b, analyzed on Rush 03-29-01. PFOS Adsorb/Desorb samples. Matrix: Soil/SIg/Sed. Standard curve range used for calibration of samples: 5-501 ng/mL (2.5 ng/mL std not included due to the higher sample concentration range). Batch method: R010329.m Inj Date Batch SampTypeFile 3/29/01 18:35 D:\Chem\RSAMPLE RUSI 3/29/01 18:50 D:\Chem\RSAMPLE RUSi 3/29/01 22:11 D:\Chem\RSAMPlE RUSi 3/29/01 22:25 D:\Chem\RSAMPlE RUSi 3/30/01 0:49 D:\Chem\RSAMPLE RUSI 3/30/01 1:03 D:\Chem\RSAMPLE RUSi 3/30/01 4:11 D:\Chem\RSAMPLE RUSI 3/30/01 4:25 D:\Chem\RSAMPLE RUSi 3/30/01 7:32 D:\Chem\RSAMPLE RUSI 3/30/01 7:46 D:\Chem\RSAMPLE RUSI 3/30/01 10:54 D:\Chem\RSAMPLE RUSI 3/30/01 11:08 D:\Chem\RSAMPLE RUSI 3/30/01 14:15 D:\Chem\RSAMPLE RUSI 3/30/01 14:29 D:\Chem\RSAMPLE RUSI 3/30/01 17:51 D:\Chem\RSAMPLE RUSI 3/30/01 18:05 D:\Chem\RSAMPLE RUSI 3/30/01 18:20 D:\Chem\RSAMPLE RUSI amo ! MeOH : MeOH ! MeOH ! MeOH : MeOH : MeOH : MeOH ! MeOH : MeOH : MeOH : MeOH : MeOH MeOH : MeOH MeOH MeOH MeOH Mise InCompountRT 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 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 CompoumRT 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 (0QT)I (D cn CO71) O --h o CO Page 2 of 4 BACK TO MAIN Co Sample Batch R6i0323a.b, analyzed on Rash 03-29-01. PFOS Adsorb/Desorb samples. Matrix: Soif/SIg/Sed. r~ Standard curve range used for calibration of samples: 5-501 ng/mL (2.5 ng/mL std not inciuued due to the higher sample concentration range). QClr Batch method: R010329.m o Inj Date Batch SampTypeFilo Sample Name Mise IniCompouncRT Area Amount CompountRT Area Amount 2 3/29/01 22:40 D:\Chem\RSAMPLE RUSH0037Study Number EOO-1311 THPFOS 5.588 874070 254 PFOS 5.791 3351053 159.93 3/29/01 22:54 D:\Chem\RSAMPLE RUSH0038Study Number EOO-1311 THPFOS 5.582 901936 254 PFOS 5.785 3334462 152.92 3/29/01 23:08 D:\Chem\RSAMPLE RUSH0039Study Number EOO-1311 THPFOS 5.588 905901 254 PFOS 5.791 3176252 143.26 3/29/01 23:23 D:\Chem\RSAMPLE RUSH0040Study Number EOO-1311 THPFOS 5.586 727872 254 PFOS 5.79 5858869 415.70 3/29/01 23:37 D:\Chem\RSAMPLE RUSH0041Study Number EOO-1311 THPFOS 5.581 881852 254 PFOS 5.791 6787348 391.37 3/29/01 23:52 D:\OiemlRSAMPLE RUSH0042Study Number EOO-1311 THPFOS 5.582 884596 254 PFOS 5.785 4533069 230.09 3/30/01 0:06 D:\Chem\RSAMPLE RUSH0043Study Number E00-1311 THPFOS 5.583 880085 254 PFOS 5.787 6721663 387.34 3/30/01 0:20 D:\Chem\RSAMPLE RUSH00445 ng/mL PFOS inMeOH THPFOS 5.582 890865 254 PFOS 5.799 279066 5.09 1 0 1 .8 % 3/30/01 0:35 D:\Chem\RSAMPLE RUSH0045250.5 ng/mL PFOS in MeOH THPFOS 5.58 877456 254 PFOS 5.791 4855798 253.86 101.3% 3/30/01 1:18 D:\Chem\RSAMPLE RUSH0048Study Number EOO-1311 THPFOS 5.588 694334 254 PFOS 5.792 8882466 795.21 3/30/01 1:32 DAChemIRSAMPLE RUSH0049Study Number E00-1311 THPFOS 5.583 970838 254 PFOS 5.793 2166125 82.81 3/30/01 1:47 D:\Chem\RSAMPLE RUSH0050Study Number EOO-1311 THPFOS 5.582 911997 254 PFOS 5.792 2081596 85.11 3/30/01 2:01 D:\Chem\RSAMPLE R(JSH0051Study NumberEOO-1311 THPFOS 5.575 884872 254 PFOS 5.778 1925950 80.38 3/30/01 2:15 D:\Chem\RSAMPLE RUSH0052Study NumberEOO-1311 THPFOS 5.575 711307 254 PFOS 5.785 4807882 329.29 3/30/01 2:30 D:\Chem1RSAMPLE RUSH0053Study NumberEOO-1311 THPFOS 5.571 895811 254 PFOS 5.781 7066726 404.55 3/30/01 2:44 D:\ChemlRSAMPLE RUSH0054Study NumberEOO-1311 THPFOS 5.569 893422 254 PFOS 5.779 7171691 414.16 3/30/01 2:59 D:\Chem\RSAMPLE RUSH0055Study NumberEOO-1311 3/30/01 3`13 OACharriNPS^MPInF CU<LUn<CfiiWy_Mr.mhf r^np.1TI1 . THPFOS XH^cnc 5.568 900655 5.567 716S83 254 254 PFOS PEOS 5.771 7483683 r 777 433.98 501 ug/L 3/30/01 3:27 D:\Chem\RSAMPLE RUSH0057Study NumberEOO-1311 THPFOS 5.575 868476 254 PFOS 5.785 471637 13.57 3/30/01 3:42 D:\Chem\RSAMPLE RUSH00585 ng/mL PFOS in MeOH THPFOS 5.581 868387 254 PFOS 5.798 272404 5.11 1 0 2 .1 % 3/30/01 3:56 D:\Chem\RSAMPLE RUSH0059250.5 ng/mL PFOS in MeOH THPFOS 5.581 845346 254 PFOS 5.792 4664476 252.91 1 0 1 .0 % 3/30/01 4:39 D:\Chem\RSAMPLE RUSH0062Study NumberEOO-1311 THPFOS 5.581 879621 254 PFOS 5.791 207413 2.29 3/30/01 4:54 DAChemVRSAMPLE RUSH0063Study Number E00-1311 THPFOS 5.578 865113 254 PFOS 5.788 175186 1.09 3/30/01 5:08 D:\Chem\RSAMPLE RUSH0064Study Number E00-1311 THPFOS 5.573 713593 254 PFOS 5.783 3349187 205.86 3/30/01 5:22 D:\Chem\RSAMPLE RUSH0065Study NumberEOO-1311 THPFOS 5.581 856465 254 PFOS 5.785 2228859 99.69 3/30/01 5:37 D:\Chem\RSAMPLE RUSH0066Study Number EOO-1311 THPFOS 5.581 844166 254 PFOS 5.784 2133042 96.20 3/30/01 5:51 D:\Chem\RSAMPLE RUSH0067Sludy NumberEOO-1311 THPFOS 5.582 848621 254 PFOS 5.785 1411558 58.15 3/30/01 6:06 D:\Chem\RSAMPLE RUSH0068Study NumberEOO-1311 THPFOS 5.579 669997 254 PFOS 5.782 4285086 306.23 3/30/01 6:20 D:\Chem\RSAMPLE RUSH0069Study Number E00-1311 THPFOS 5.577 818557 254 PFOS 5.78 7109748 460.98 3/30/01 6:34 D:\Chem\RSAMPLE RUSH0070Study NumberEOO-1311 THPFOS 5.582 815811 254 PFOS 5.785 5211826 305.78 3/30/01 6:49 D:\Chem\RSAMPLE RUSH0071Study Number EOO-1311 THPFOS 5.574 823985 254 PFOS 5.777 8017544 539.08 > 501 ug/L 3/30/01 7:03 D:\Chem\RSAMPLE RUSH00725 ng/mL PFOS in MeOH THPFOS 5.571 823981 254 PFOS 5.788 275231 5.85 117.0% 3/30/01 7:17 D:\Chem\RSAMPLE RUSH0073250.5 ng/mL PFOS in MeOH THPFOS 5.578 821611 254 PFOS 5.781 4574902 255.88 1 0 2 .1% Page 557 of 703 Page 3 of 4 BACK TO MAIN I sS1 33 ' 3 a ST ooar>- Sample Batch R010329a.b, analyzed on Rush 03-29-01. PFOS Adsorb/Desorb samples. Matrix: Soil/SIg/Sed. Standard curve range used for calibration of samples: 5-501 ng/mL (2.5 ng/mL std not included due to the higher sample concentration range). Batch method: R010329.m 3/30/01 8:01 D:\Chem\RSAMPLE RUSH0076Study Number EOO-1311 THPFOS 5.568 690116 254 PFOS 3/30/01 8:15 D:\Chem\RSAMPLE RUSH0077Study Number EOO-1311 THPFOS 5.579 956969 254 PFOS 3/30/01 8:29 D:\Chem\RSAMPLE RUSH0078Study Number EOO-1311 THPFOS 5.574 870548 254 PFOS 3/30/01 8:44 D:\Chem\RSAMPLE RUSN0079Study Number E00-1311 THPFOS 5.581 845769 254 PFOS 3/30/01 8:58 D:\Chem\RSAMPLE RUSH0080Study Number EOO-1311 THPFOS 5.574 710436 254 PFOS 3/30/01 9:13 D:\Chem\RSAMPLE RUSH0081Study Number EOO-1311 THPFOS 5.576 852256 254 PFOS 3/30/01 9:27 O:\Chem\RSAMPLE RUSH0082Study Number EOO-1311 THPFOS 5.576 913113 254 PFOS 3/30/01 9:42 D:\ChemVRSAMPLE RUSH0083Study Number E00-1311 THPFOS 5.585 834426 254 PFOS 3/30/01 9:56 D:\Chem\RSAMPLE RUSN0084Study Number E00-1311 THPFOS 5.578 702989 254 PFOS 3/30/01 10:10 D:\Chem\RSAMPLE RUSH0085Study Number EOO-1311 THPFOS 5.581 919415 254 PFOS 3/30/01 10:25 D:\Chem\RSAMPLE RUSH00865 ng/mL PFOS in MeOH THPFOS 5.579 828884 254 PFOS 3/30/01 10:39 D:\Chem\RSAMPLE RUSH0087250.5 ng/mL PFOS in MeOH THPFOS 5.573 820925 254 PFOS 3/30/01 11:37 D:\Chem\RSAMPLE RUSH0091Study 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 RUSH0093Study Number E00-1311 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 RUSH0095Study Number E00-1311 THPFOS 5.579 833417 254 PFOS 3/30/01 12:49 D:\Chem\RSAMPLE RUSH0096Study Number E00-1311 THPFOS 5.573 660626 254 PFOS 3/30/01 13:03 D:\Chem\RSAMPLE RUSH0097Study Number EOO-1311 THPFOS 5.575 831428 254 PFOS 3/30/01 13:17 D:\Chem\RSAMPLE RUSH0098Study Number E00-1311 THPFOS 5.572 822165 254 PFOS 3/30/01 13:32 D:\Chem\RSAMPLE RUSH0099Study Number E00-1311 THPFOS 5.576 815744 254 PFOS 3/30/01 13:46 D:\Chem\RSAMPLE RUSH01005 ng/mL PFOS in MeOH THPFOS 5.569 788928 254 PFOS 3/30/01 14:01 D:\CtiemiRSAMPLE RUSH0101250.5 ng/mL PFOS in MeOH THPFOS 5.574 788989 254 PFOS 5.778 10151474 5.782 4102214 5.778 3443662 5.784 3186935 5.777 5795265 5.779 6155804 5.779 8769331 5.788 5927478 5.781 8168548 5.785 4411967 5.789 270806 5.783 4516252 5.785 4018521 5.78 6442026 5.784 1056562 5.785 376593 5.789 275264 5.783 3353185 5.785 846945 5.775 885719 5.779 850807 5.779 261893 5.777 4409485 976.13 > 501ug/L 183.73 166.25 156.55 423.27 359.52 529.37 > 501ug/L 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% Page 558 of 703 Page 4 of 4 BACK TO MAIN a mmmi JssassSSiil3saas3sasa3s3S9Slii3 a 8 ^ s s S S s 8 s a !j goooooooooooooooooooooooooooooooa aittititSrttitSritJttittitSiittttStittttttItitta: il sl?sH ysassssssssssasssssjjaaaaaaaaaass dOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOO llllllllllillllllllllilllllllllSl J iiliilillllillil I|E|I|!|I? ffiH iiH ih" lliiiiiillliilllilillilliiii S,-3 oa 5 l1i1j!iHsifiiSiiSfiSiitifiSiSisisiiiUiiSiSiiiiiHiiBiixiaiziisiKigiii 3M Environm ental Laboratory Page 559 of 703 BACK TO MAIN t I sssgsisiaEsiassg^aKissRgaiISSISiltBisSaBiasKlIiililBsSiUgiisSBBiissssii i --!--ill-1-- SSS^gfcilsSBSSUSiSSsS a iiia!!iaas!aiiissa35Hasss5saa5Ss9s555sa5S5aggsssg55sssssss=sss=ssBsasassgss ii:oao;oSiioSo ioao id^o&o iQotfocoltSiSo oaiotooSooio oSotooaS:oo&oiotSo iototao!ocoLQSo o(otpiipvooipi.oQo !ppQp.o6o.tpi.ooioi.ooi&o oo:oioaotQo a;ootoia a 3H399S9933993l93*lH3S9955399339H!99H335!315!!99Smmms$9m!9S9 88 h i i i i f S i i l i l ! 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J iil!H!llltl!fltfifE|!i!!fi||ij|[!jj|i(j IlllllllllllllllllflliunilllllllW imm.mm.m.m.mm, page 563 of 703 ] qoooooooo a?oSo "is fc ViRK88S8a85i8RaR8R8S888iQ * in<iiobn<nooc><ioooiooirin ] {KtEKMKEKiilKKI ! i i li!SlSSlll!1311iiiil!Il im m m m n n m m 3M Environmental Laboratory 33383388888883398888888 I !i!I!11111!!111111ii111 ooodfiiioaDDSftOQdoafiaad R=S$35gi5RR$::5S8!S*5?!J? I S|i55|lSI|?l`l*l`?i*|<|*i'|SiSSSiSI5i5iSs5SpSi Page 564 of 703 3' 3 3CD ST oC0)r 3 c? _>> r "D X Ca _Q O' O c?- Sam ple B atch H0104G4.b, analyzed on H illary 04-04-01. PFOS AdsortwDesorb samples. M atrix: Soil/SIg/Sed. S tandard curve range used fo r calibration o f sam ples: 10-400.8 ng/m L Batch m e thod: H010404.m (External Standard Quant) Inj Date Batch 4/4/01 18:17 D:\Chem\Hltary\H010404.b 4/4/01 13:01 D:\ChemVHillary\H010404.b 4/4/01 18:46 D:\Chem\Hillary\H0lO404.b 4/4/01 19:00 D:\Chem\Hillary\H010404.b 4/4/01 19:14 DXhem\H/ilary\H010404.b 4/4/01 19:29 D:\Chem\HiWary\H010404.b 4/4/01 19:43 D:\Chem\HiHafy\H010404.b 4/4/01 19:57 O:\Chem\HiHary\H010404.b 4/4/01 20:12 D:\Chem\HiHary\H010404.b 4/4/01 20:26 D:\Chem\Hiltaiy\H010404.b 4/4/01 20:41 D:\Chem\Hiilary\H010404.b 4/4/01 20:55 D:\Chem\Hillary\H010404.b 4/4/01 21:09 D:\Cbem\Hillaiy\H010404.b 4/5/01 11:19 D:1ChenrtHillaiy\H010404.b 4/5/01 11:33 D:\Chem\HiHaiy\H010404.b 4/5/01 11:47 D:\Chem\Htllary\H010404.b 4/5/01 12:02 D:\Chem\Hillary\H010404.b 4/5/01 12:16 D:\ChemtHillary\H010404.b 4/5/01 12:31 D:\Chem\HiHary\H010404.b 4/5/01 12:45 D:\Chem\HiRafy\H010404.b 4/5/01 12:59 D:\Chem\HiHarylH010404.b 4/5/01 13:14 D:\Chem\HiBary\H010404.b 4/5/01 13:28 D:\Cfiem\HiliaryiH010404.b 4/5/01 13:42 D:\Chem\Hillary\H010404.b 4/5/01 13:57 D:\Chem\Hillary\H010404.b 4/5/01 14.11 D:\Chem\Hillary\H010404.b SampType SAMPLE CALIB_1 CAUB_2 CAUB_3 CAUB_4 CAUB_5 CALIB_6 CALIB_7 CALIB_8 CALIB.9 CAUB_10 SAMPLE SAMPLE SAMPLE CAU8_11 CAUB_12 CAUB_13 CAUB.14 CALIB_15 CALIB_16 C A U B .1 7 CALJB_18 CAUB_19 CAUB_20 SAMPLE SAMPLE File HILL0016.D HILL0017.D MiU-OOIS.D HILL0019.D HILL002Q.0 HILL0021.D HILL0022.D HILL0023.D HILL0024.D HILL0025.D H1LL0026.D HILL0027.D HILL0028.D H IL L 0 0 8 7 .0 HILL0088.D HILL0089.D HILL0090.D HILL0091.0 HILL0092.D HILL0093.D HILL0094.D HILL0095.D HILL0096.D HILL0097.D HILL0098.D HILL0099.D Sam ple Name O ng/mL PFOS in MeQH 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 ng/mL PFOS in MeOH 50.1 ng/m l PFOS in MeOH 75.1 n g /m l PFOS in MeOH 100.2 ng/ml PFOS in MeOH 250. S ng/toL PFOS in MeOH 400.8 ng/mL PFOS in MeOH 501 ng/mL PFOS in MeOH 1002 ng/ml PFOS in MeOH O ng/mL PFOS in MeOH 2.5 n g /m l PFOS in MeOH 5 ng/mL PFOS in MeOH 1 0 n g /m l PFOS in MeOH 25 n g /m l PFOS in MeOH 4 0 ng/m l 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/ml PFOS in MeOH Inj Date Batch 4/4/01 14:41 D:\Chem\Hillary\H010404.b 4/4/01 14:56 D;1Chem\Hillary\H010404.b 4/4,131 15:39 D:\Chern\Hillary\H0104Q4.b 4/4/01 15:53 D:\Chem\Hillary\H010404.b 4/4/01 17:48 D:\Chem\Hillaiy\H010404.b 4/4/01 18:03 D:\ChenrtHiHary1H010404.b 4/4/01 21:24 D:\Chem\Hillary\H010404.b 4/4/01 21:38 D:lChe/nlH/Na/y\H010404.b 4/5/01 0:45 O:\Cfiem\Hillary\H010404.b 4/5/011.00 D:\Chem\Hillary1H010404.b 4/5/01 4:07 D:\Chem\HiKafy1H010404.b 4/5/01 4:21 D:\Chem\Hillary\H010404.b 4/5/01 7:28 D:\Chem\Hillaty\H010404.b 4/5/01 7:43 D:\Chem\Hillary\H010404.b 4/5/01 10:50 D:\Chem\Hillary\H010404.b 4/5/01 11:04 D:\Chem\Hillary\H010404.b 4/5/01 14.-26 D:\Chem\Hillary\H010404.b 4/5/01 14:40 D:\Chem\Hillafy\H010404.b SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File HILL00Q1.D H1LL0002.D HILL0005.D HILL0006.D HILL0014.D HILL0015.D HILL0029.D HILL0030.D HILL0043.D HILL0044.D HILL0057.D HILL0058.D HILL0071.D HIL10072.D HILLOOS5.D HILL0086.D HILL0100.D HILL0101.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 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 TN-A 4802 MeOH TN-A 4802 MeOH Page 565 of 703 BACK TO MAIN H010404 external standard quanfxis Mise InfCompound NaRT Are* THPFOS 5.113 THPFOS 5.112 THPFOS 5.112 THPFOS 5.112 THPFOS 5,113 THPFOS 5.111 THPFOS 5.112 THPFOS 5.113 THPFOS 5.114 THPFOS 5.113 THPFOS 5.112 THPFOS 5.113 THPFOS 5.114 THPFOS 5.092 THPFOS 5.091 THPFOS 5.093 THPFOS 5.09 THPFOS 5.092 THPFOS 5.091 THPFOS 5.096 THPFOS 5.096 THPFOS 5.093 THPFOS 5.092 THPFOS 5.092 THPFOS 5,093 THPFOS 5.099 Amount 906085 254 689526 254 877571 254 902673 254 890573 254 931996 254 903996 254 884697 254 899166 254 857703 254 891222 254 907981 254 840757 254 1261932 254 1203313 254 1167470 254 1191649 254 1181183 254 1183842 254 1129902 254 1099744 254 1100820 254 1030699 254 1039403 254 1052373 254 962330 254 Average: 1123435.385 Sid Dev: 85107.0234 %RSD: 7.6% Compound NarflT Area Amount PFOS 0 00 PFOS 5.329 72734 1.190813 PFOS 5.329 110448 3.153981 PFOS 5.329 204980 8.082456 PFOS 5.33 540471 25 66227 PFOS 5.329 883838 43.79626 PFOS 5329 1058705 53.09021 PFOS 5.33 1555089 79.67175 PFOS 5.331 2075718 107.8776 PFOS 5.323 4653038 252.4225 PFOS 5.329 7377624 414.1189 PFOS 5.33 9097217 520.8761 PFOS 5.331 15189218 92B.379 PFOS 0 00 PFOS 5.301 62293 0 647625 PFOS 5.31 98724 2.543506 PFOS 5.307 188223 7.208022 PFOS 5.309 494122 23.22532 PFOS 5.301 813449 40.06864 PFOS 5.315 975991 48.69034 PFOS 5.315 1451814 74.11635 PFOS 5.31 1962240 101.7013 PFOS 5.309 4432636 239.7418 PFOS 5.309 6951500 388.2267 PFOS 5.31 8649088 492.7043 PFOS 5.309 14944991 911.1632 1460466 +30%; 786405 -30%: 63% 81% 103% 105% 106% 106% 106% 101% 103% 104% 93% 51% 72% 93% 100% 97% 99% 101% 96% 97% 90% 91% Mise InfCompound NaRT 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 Amount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Compound NartiT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 00 00 00 00 0o 00 0o 00 0o 00 00 00 00 00 00 00 00 00 page 1 of 2 Page 566 of 703 3M Environmental Laboratory In j Date Batch 4/4/01 21:52 D:\Chem\Hillary\H010404.b 4/4/01 22:07 D:\Chem\Hillary\H010404.b 4/4/01 22:21 D:\Chem\Hillary\H010404.b 4/4/01 22:36 D:\Chem\HHIary\H010404.b 4/4/01 22:50 D:\Chem\Hillary\H010404.b 4/4/01 23:04 D:\Chem\Hillary\H010404.b 4/4/01 23:19 D:\Chem\Hillafy\H010404.b 4/4/01 23:33 D:\Chem\Hillary\H010404.b 4/4/01 23:48 D:\Chem\Hillary\H010404.b 4/5/01 0:02 D:\Chem\Hillary\H010404.b 4/5/01 0:16 D:\Chem\Hillary\H010404.b 4/5/01 0:31 D:\Chem\Hillary\H010404.b 4/5/01 1:14 D:\Chem\Hillary\H010404.b 4/5/01 1:28 D:\Chem\Hillary\H010404.b 4/5/01 1:43 D:\Chem\Hillary\H010404.b 4/5/01 1:57 D:\Chem\Hillary\H010404.b 4/5/01 2:11 D:\Chem\Hillary\H010404.b 4/5/01 2:26 D:\Chem\Hillary\H010404.b 4/5/01 2:40 D:\Chem\Hillary\H010404.b 4/5/01 2:55 D:\Chem\Hillary\H010404.b 4/5/01 3:09 D:\Chem\Hillary\H010404.b 4/5/01 3:23 D:\Chem\Hillary\H010404.b 4/5/01 3:38 D:\Chem\Hillary\H010404.b 4/5/01 3:52 D:\Chem\Hillary\H010404.b 4/5/01 4:35 D:VChem\Hillary\H010404.b 4/5/01 4:50 D:\Chem\Hillary\H010404.b 4/5/01 5:04 D:\Chem\Hillary\H010404.b 4/5/01 5:19 D:\Chem\Hiilary\H010404.b 4/5/01 5:33 D:\Chem\Hiliary\H010404.b 4/5/01 5:47 D:\Chem\HillaryUH010404.b 4/5/01 6:02 D:VChem\Hillary\H010404.b 4/5/01 6:16 D:\Chem\Hillary\H010404.b 4/5/01 6:31 D:\Chern\HUIary\H010404.b 4/5/01 6:45 D:\Chem\Hillary\H010404.b 4/5/01 6:59 D:\Chem\Hillary\H010404.b 4/5/01 7:14 D:\Chem\HUIary\H010404.b 4/5/01 7:57 D:\Chem\Hillary\HD10404.b 4/5/01 8:11 O:\Chem\Hillary\JH010404.b 4/5/01 8:26 D:\ChemVHillary\H010404.b 4/5/01 8:40 D:\Chem\Hiilary\H010404.b 4/5/01 6:55 D:\Chem\Hillary\H010404.b 4/5/01 9:09 D:\Chem\Hillary\H010404.b 4/5/01 9:23 D:\Chem\HilIary\H010404.b 4/5/01 9:38 D:\Chem\Hillary\H010404.b 4/5/01 9:52 D:\Chem\J-iiliary\JH010404.b 4/5/01 10:07 D:\Chem\Hillary\H010404.b 4/5/01 10:21 D:\Chem\Hillary\H010404.b 4/5/01 10:36 DXhem\Hittary\H010404.b 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 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File Sample Name HILL0031.D Omg/L PFOS Study Number E00-1311 HILL0032.D Omg/L PFOS Study Number EOO-1311 HILL0033.D Omg/L PFOS Study Number EOO-1311 HILL0034.D Omg/L PFOS Study Number EOO-1311 HILL0035.D Omg/L PFOS Study Number EOO-1311 HILL0O36.D Omg/L PFOS Study Number E00-1311 HILL0037.D Omg/L PFOS Study Number EOO-1311 HILL0038.D Omg/L PFOS Study Number EOO-1311 HILL0039.D Smg/LPFOS Study Number EOO-1311 HILL0040.D 5mg/L PFOS Study Number EOO-1311 HILL0041.D 5 ng/mL PFOS in MeOH HILL0O42D 250.5 ng/mL PFOS in MeOH HILL0045.D 5mg/L PFOS Study Number EOO-1311 HILL0046.D 5mg/L PFOS Study Number EOO-1311 HILL0047.D 5mg^. PFOS Study Number EOO-1311 HILL0O48.D 5mg/L PFOS Study Number E00-1311 HILL0049.D 5mg/L PFOS Study Number EOO-1311 HILL0050.D 5mg/L PFOS Study Number EOO-1311 HILL0051.D 5mg/L PFOS Study Number EOO-1311 HILL0052.D 5mg/LPFOS Study Number EOO-1311 HILL0053.D 5mg/L PFOS Study Number E00-1311 HILL0054.D 5mg/L PFOS Study Number EOO-1311 HLL0O55.D 5 ng/mL PFOS in MeOH HILL0056.D 250.5 ng/mL PFOS in MeOH HILL0059.D 5mg/L PFOS Study Number EOO-1311 HILL0060.D 5mg/L PFOS Study Number EOO-1311 HILL0061 D 5mg/L PFOS Study Number E00-1311 HILL0062.D 5mg/L PFOS Study Number E00-1311 HILL0063D 5mg/L PFOS Study Number E00-1311 HILL0064.D 5mg/L PFOS Study Number EOO-1311 HILL0065.D Smg/LPFOS Study Number EOO-1311 HILL0066.D Smg/LPFOS Study Number EOO-1311 HILL0067.D 5mg/L PFOS Study Number E00-1311 HILL0068.0 5mg/L PFOS Study Number E00-1311 HILL0069.D 5 ng/mL PFOS in MeOH HILL0070.D 250.5 ng/mL PFOS in MeOH HILL0073.D 5mg/L PFOS Study Number E00-1311 HILL0074.D 5mg/LPFOS Study Number EOO-1311 HILL0075.D Smg/LPFOS Study Number EOO-1311 HILL0076.D 5mg/L PFOS Study Number E00-1311 HILL0077.D 5mg/L PFOS Study Number E00-1311 HILL0O78.D Smg/L PFOS Study Number E00-1311 HILL0079.D 5mg/L PFOS Study Number EOO-1311 HILL0060.D 5mg/LPFOS Study Number EOO-1311 HILL0081-D 5mg/LPFOS Study Number EOO-1311 HILL0082.D Smg/LPFOS Study Number EOO-1311 HILL0083.D 5 ng/mL PFOS in MeOH HILL0084.D 25 0 .5 ng/mL PFOS in MeOH BACK TO MAIN H010404 external standard quanLxls Mise InfCompound NaRT Area THPFOS 5.108 THPFOS 5.111 THPFOS 5.107 THPFOS 5.106 THPFOS 5.098 THPFOS 5.1 THPFOS 5.094 THPFOS 5.099 THPFOS 5.099 THPFOS 5.098 THPFOS 5.105 THPFOS 5.106 THPFOS 5.098 THPFOS 5.098 THPFOS 5.105 THPFOS 5.099 THPFOS 5.094 THPFOS 5.098 THPFOS 5.097 THPFOS 5.091 THPFOS 5.091 THPFOS 5.099 THPFOS 5.104 THPFOS 5098 THPFOS 5.099 THPFOS 5.1 THPFOS 5.099 THPFOS 5.099 THPFOS 5.098 THPFOS 5.099 THPFOS 5.098 THPFOS 5.092 THPFOS 5.091 THPFOS 5.09 THPFOS 5.092 THPFOS 5.098 THPFOS 5.091 THPFOS 5.098 THPFOS 5.097 THPFOS 5.099 THPFOS 5.092 THPFOS 0 THPFOS 0 THPFOS 5 085 THPFOS 5.085 THPFOS 5.084 THPFOS 5.087 THPFOS 5.088 Amount Compound NanfitT Area Amount 1562301 254 ISTD>130% PFOS 0 00 1575594 254 ISTD>130% PFOS 0 00 1560062 254 ISTI 130% PFOS 0 00 1537278 254 ISTD>130% PFOS 5.316 3170996 168.3053 1599896 254 iSTD>130% PFOS 0 00 1613917 254 !STD>130% PFOS 0 00 1644662 254 ISTD>130% PFOS 0 00 1579150 254 ISTD>130% PFOS 5.309 2970771 157.1483 1587389 254 ISTD>130% PFOS 0 00 1567309 254 ISTD>130% PFOS 0 00 1307817 254 PFOS 5.315 101216 2.673254 1186004 254 PFOS 5.316 4607627 249.8049 1569488 254 1STD>13Q% PFOS 5.315 202756 7.966382 1521100 254 ISTD130% PFOS 5.315 3255972 173.0552 1563690 254 ISTD>130% PFOS 5.315 80242 1.581493 1535494 254 ISTD>130% PFOS 0 00 1528194 254 ISTD>130% PFOS 0 00 1514404 254 !STD>130% PFOS 5.315 3115242 165.1936 1537963 254 ISTD>130% PFOS 5.314 76776 1.401129 1529992 254 ISTD>130% PFOS 5.308 96528 2.429182 1541462 254 ISTD>130% PFOS 5.308 166651 6.082828 1500713 254 !STD>130% PFOS 5.309 3133475 166.2108 1341697 254 PFOS 5.314 103787 2.80712 1248317 254 PFOS 5.308 4550667 246.5252 1687410 254 ISTD>130% PFOS 5.309 183857 6 980244 1546322 254 ISTD>130% PFOS 5.31 148784 5.151322 1570952 254 ISTD>130% PFOS 5.316 80452 1.592421 1511291 254 ISTD>130% PFOS 5.316 3105298 164.639 1520307 254 ISTD>130% PFOS 5.315 81053 1.623698 1536695 254 ISTD>130% PFOS 5.316 74150 1.264487 1504984 254 ISTD>130% PFOS 5.308 119473 3.624028 1472241 254 ISTD>130% PFOS 5.302 3098377 164.2531 1543912 254 ISTD>130% PFOS 5.308 134114 4.386787 1511129 254 ISTD>130% PFOS 5.301 179554 6.755777 1329935 254 PFOS 5.309 99459 2.581776 1263173 254 PFOS 5.308 4490291 243.0532 1537210 254 ISTD>130% PFOS 5.308 181284 6.84002 1489558 254 ISTD>130% PFOS 5.308 3114794 165.1686 1509221 254 iSTD>130% PFOS 5.307 76643 1.394208 1509704 254 ISTD>130% PFOS 5.309 138272 4.603457 1492328 254 !STD>130% PFOS 5.309 231419 9.462838 0 0 ISTD<70% PFOS 5.302 3063518 162.3102 0 0 ISTD<70% PFOS 5.295 191090 7.357605 1474993 254 ISTD>130% PFOS 5.302 170926 6.305766 1466047 254 ISTD>130% PFOS 5.302 88860 2.030021 1443304 254 PFOS 5.301 2902477 153.3541 1338206 254 PFOS 5.304 100507 2.63634 1274099 254 PFOS 5.296 4412461 238.5841 53.5% 99.7% 56.1% 98.4% 51.6% 97.0% 52.7% 95.2% page 2 of 2 BACK TO MAIN 3M Environmental Laboratory <(0TQD)3 OO )l cOo H0104l2.xls Sam ple B atch H010412.b, analyzed on H illa ry 04-12-01. PFOS A d s o rb /D a so rb samples. M atrix: Soil/Slg/Sed. S ta n d a rd cu rve range used fo r calib ra tio n o f sam ples: 10-400.8 ng/m L B a tc h m ethod: H010412.m Inj Date Batch 4/12/01 17:51 D:\Chem\Hillary\H010412A.b 4/12/01 18:05 DAChem\Hillary\H010412A.b 4/12/01 18:19 D:\Chem\Hillafy\HQ10412A.b 4/12/01 18:34 D:\Chem\Hillary\HQ104 !2A.b 4/12/01 18:48 D:\Chem\Hi(/ary\H0104 l2A.b 4/12/01 19:03 D:\Chem\Hiilary\H010412A.b 4/12/01 19:17 D:\ChemlHillarylH010412A.b 4/12/01 19:31 D:\Chem\Hiilary\H010412A.b 4/12/01 19:46 D:\Chem\Hillary\H0l 0412A.b 4/12/01 20:00 D:\Chem\Hiliary\H010412A.b 4/12/01 20:15 D:\Chem\Hillary\H0104l2A.b 4/12/01 20:29 D:\Chem\Hillary\H010412A.b 4/12/01 20:43 D:\Chem\Hillary\H010412A.b 4/13/01 7:02 D:\Chem\Hiilary\H010412A.b 4/13/01 7:17 D:\Chem\Hiitary\H010412A.b 4/13/01 7:31 D:\Chem\Hillary\H010412A.b 4/13/01 7:45 D:\Chem\Hillary\H010412A.b 4/13/01 8:00 O:\Chem\HHlaty\HO10412A.b 4/13/01 8:14 D:\Chem\Hillary\H010412A.b 4/13/01 8:29 D:\Chem\Hillary\H010412A.b 4/13/01 8:43 D:\Oiem\Hillary\H0104l2A.b 4/13/01 8:58 D:\Chem\Hillary\HQ10412A.b 4/13/01 9:12 D:\Oiem\Hiliary\H010412A.b 4/13/01 9:26 D:\Chem\Hillary\H010412A.b 4/13/01 9:41 D:\Chem\Hillary\H010412A.b 4/13/01 9:55 D:\Chem\Hillary\H010412A.b SampType SAMPLE GAUBJ CALIB_2 CALIBJ3 CALB_4 CAUB_5 CALIB_6 CAUB_7 CALIB_8 CALIB_9 CALiB_10 SAMPLE SAMPLE SAMPLE CALIBJ1 CAL(B_12 CALIBJ3 C A U B J4 CAUB_15 CALIBJ6 CAL1BJ7 CALIBJ8 CALIB_ 19 CALIB_20 SAMPLE SAMPLE Rie HILL0016.D HILL0017.D HILL0018.D HlLLOOiS.D HILL0020. D H1LL0021.D HILL0022.D HILL0023.D HILL0024.D HILL0025.D HILL0026.D HILL0027.D HILL0028.D HILL0071.D HILL0072.D HILL0073.D H1LL0074.D HILL0075.D HILL0076.D HILL0077.D HILL0078.D HILL0079.D HILL0080.D HILL0081.O H1LL0082.D HILL0083.D Sample Name Mise In f C om pound Na RT Area 0 ng/mL PFOS in MeOH THPFOS 5.106 2.5 ng/mL PFOS in MeOH THPFOS 5.105 5 ng/mL PFOS in MeOH THPFOS 5.097 10 ng/mL PFOS in MeOH THPFOS 5105 25 ng/mL PFOS in MeOH THPFOS 5.098 40 ng/mL PFOS in MeOH THPFOS 5.093 50.1 ng/mL PFOS in MeO THPFOS 5.090 75.1 ng/mL PFOS in MeO THPFOS 5.105 100,2 ng/mL PFOS in Me THPFOS 5.105 250.5 ng/mL PFOS in Me THPFOS 5.104 400.8 ng/mL PFOS in Me THPFOS 5.106 501 ng/mL PFOS in MeOH THPFOS 5.106 1002 ng/mL PFOS in MeO THPFOS 5.104 0 ng/mL PFOS in MeOH THPFOS 5.099 2.5 ng/mL PFOS in MeOH THPFOS 5.099 5 ng/mL PFOS in MeOH THPFOS 5.096 10 ng/mL PFOS in MeOH THPFOS 5.098 25 ng/mL PFOS in MeOH THPFOS 5,099 40 ng/mL PFOS in MeOH THPFOS 5.092 50.1 ng/mL PFOS in MeO THPFOS 5.092 75.1 ng/mL PFOS in MeO THPFOS 5.098 100.2 ng/mL PFOS in Me THPFOS 5.085 250.5 ng/mL PFOS in Me THPFOS 5.09 400.8 ng/mL PFOS in Me THPFOS 5.099 501 ng/mL PFOS in MeOH THPFOS 5.097 1002 ng/mL PFOS in MeO THPFOS 5.084 Amount 1010690 254 1014600 254 1026197 254 1049688 254 1021363 254 1028355 254 1027805 254 1029130 254 1037720 254 1024200 254 1016328 254 1009794 254 1000810 254 882895 254 892938 254 895922 254 899640 254 884732 254 900766 254 891237 254 894208 254 891115 254 885221 254 886337 254 884329 254 859448 254 Com pound NanftT 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 00 5.323 55595 1.292822 5.314 99110 3.44801 5.315 177299 7180736 5.308 486699 23.08044 5.303 777632 37.59613 5.308 980853 47.89974 5.315 1465942 72.43472 5.315 1929805 95.25510 5.314 4613300 236.1376 5.309 7015531 367.2555 5.316 8452648 449.0379 5.314 15272484 848.646 0 00 5.309 53548 1.559602 5.307 98474 4.135939 5.308 180985 8.847021 5.316 474366 26.17914 5.302 771667 42.81933 5.302 963004 54.47431 5308 1455847 83 09964 5.296 1905711 109.9345 5.308 4583269 272.6371 5.309 6974946 420.9773 5.3 8446498 515.6745 5.294 14860206 971.933 Average: 888368.3077 Std Dev: 10482.05486 % RSP: 1.2% 1154879 +30%; 621858 -30%: 69% 72% 82% 94% 96% 96% 95% 94% 92% 90% 85% 83% 68% 105% 107% 109% 111% 110% 109% 105% 103% 97% Inj Date Batch SampType File Sample Name Mise Inf C om pound Na RT Area 4/12/01 17:22 D:\Chem1Hillary\H010412A.b SAMPLE HILL0014.D TN-A 4802 MeOH THPFOS 0 4/12/01 17:36 D:\Cnem\Hitlary\H010412A.b SAMPLE HILLD015.D TN-A 4802 MeOH THPFOS 0 4/12/01 20:58 D:\Chem\Hillary\H010412A.b SAMPLE H1LL0029.D TN-A 4802 MeOH THPFOS 0 4/12/01 21:12 D:VChem\Hillary\H0l 0412A.b SAMPLE HILLO030.D TN-A 4802 MeOH THPFOS 0 4/13/01 0:19 DACham\Hi!lary\H010412A.b SAMPLE HILL0043.D TN-A 4802 MeOH THPFOS 0 4/13/01 0:33 D:\Chem\Hillary\H010412A.b SAMPLE H1LL0044.D TN-A 4802 MeOH THPFOS 0 4/13/01 3:41 D:\Chem\Hillary\H010412A.b SAMPLE HILL0057.D TN-A 4802 MeOH THPFOS 0 4/13/01 3:55 D:\Chem\Hiliary\H010412A.b SAMPLE HILL0058.D TH-A4802 MeOH THPFOS 0 4/13/01 6.33 D:\Chem\Hiliary\H010412A.b SAMPLE HILL0069.D TN-A 4802 MeOH THPFOS 0 4/13/01 6:48 D:\Chem\Hillary\H010412A.b SAMPLE HILL0070.D TN-A 4802 MeOH THPFOS 0 4/13/01 10:10 D:\Chem\Hillary\H010412A.b SAMPLE HILL0084.D TN-A 4802 MeOH - L 4/13/01 10:24 D:\Chem\Hillary\H010412A.b SAMPLE H1LL0085.D TN-A 4802 MeOH THPFOS THPFOS 0 0 Amount 00 00 00 00 00 00 00 00 00 00 00 00 Compound NanRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS Area 0 0 0 0 0 0 0 0 0 0 0 0 Amount 00 00 00 00 00 00 00 00 00 00 00 00 IAJ 0 Page 1 of 2 3M Environmental Laboratory inj Date Batch 4/12/01 21:26 D:\Chem\Hillary\H010412A.b 4/12/01 21:41 D:\Chem\Hillary\H010412A.b 4/12/01 22:10 D:\Chem\Hi!lary\H010412A.b 4/12/01 22:24 D:\Chem\Hillary\H010412A-b 4/12/01 22:38 D:\Chem\Hillary\H010412A-b 4/12/01 22:53 D:\Chem\Hillary\H01Q412A.b 4/12/01 23:07 D:\Chem\HiJlary\H010412A-b 4/12/01 23:21 D:\Chem\Hillary\H010412Ab 4/12/01 23:36 D:\Chem\Hilla/y\H010412A.b 4/12/01 23:50 D:\Chem\Hillary\H010412A.b 4/13/01 0:05 D:\Chem\HiHary\H010412A-b 4/13/01 0:46 D:\Chem\Hillary\H010412A-b 4/13/01 1:02 0:\Chem\Hillary\H010412A.b 4/13/011:17 D:\Chem\Hillary\H010412A.b 4/13/01 1:31 D:\Chem\Hiliary\H010412A.b 4/13/01 1:45 D:\Chem\Hillary\H010412A.b 4/13/01 2:00 D:\Chem\Hillary\H010412A-b 4/13/01 2:14 D:\Chem\Hillary\H010412A b 4/13/01 2:29 D:\Chem\Hiliary\H010412A.b 4/13/01 2:43 D:\Chem\Hillafy\H010412A.b 4/13/01 2:57 D:\Chem\Hiilary\H010412A.b 4/13/01 3:12 D:\Chem\Hillary\H010412Ab 4/13/01 3:26 D:VChem\Hillary\H010412A.b 4/13/01 4:09 D:\Chem\Hiliary\H010412A.b 4/13/01 4:24 D:\Chem\Hillary\H010412A-b 4/13/01 4:38 D:\Chem\Hillary\H010412A.b 4/13/01 4:53 D:\Chem\Hillary\H010412A.b 4/13/01 5:07 D:\Chem\Hillary\H010412A.b 4/13/01 5:21 D:\Chem\Hillary\H010412A.b 4/13/01 5:36 D:\Chem\Hillary\H010412A.b 4/13/01 5:50 O:\Chem\Hillary\H010412A.b 4/13/01 6:05 D:\Chem\Hillary\H010412A.b 4/13/01 6:19 D:\Chem\Hillary\H010412A.b 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 File H IL L 0 0 3 1 .D H IL L 0 0 3 2 .D 1IILLW iW .U H IL L 0 0 3 4 .D H IL L 0 0 3 5 .D H IL L 0 0 3 6 .D H IL L 0 0 3 7 .D H IL L 0 0 3 8 .D H IL L 0 0 3 9 .D HILL0040.0 H IL L 0 0 4 1 .D H IL L 0 0 4 2 .D H IL L 0 0 4 5 .D H IL L 0 0 4 6 .D H IL L 0 0 4 7 .D H IL L 0 0 4 8 .D H IL L 0 0 4 9 .D H IL L 0 0 5 0 .D H IL L 0 0 5 1 .D HILL0052.D HILL0053.D HILL0054.D H IL L 0 0 5 5 .D H IL L 0 0 5 6 .D H1LL0059.D HILL0060.D H IL L 0 0 6 1 .D H IL L 0 0 6 2 .D H IL L 0 0 6 3 .D H IL L 0 0 6 4 .D H IL L 0 0 6 5 .D H IL L 0 0 6 6 .D H IL L 0 0 6 7 .D H IL L 0 0 6 8 .D Sample Name l 1311-5184-S1 1311-5185-S1 1311-5186*31 1311-5186MS-S1 1311-5107-S1 1311-5188-S1 1311 -6 1 89-S1 1311-5189MS-S1 1311-5190-S1 1311-5191-S1 5ng/mL PFOS in MeOH 250.5 ng/m L PFOS in Me 1311 -5 1 02-S1 1311-5192MS-S1 1311-5202-S1 1311-5203-S1 1311-5204-S1 1311-5204MS-S1 1311-5205-S1 1311-5206-S1 1311-5207-S1 1311-5207MS-S1 5 ng/mL PFOS in MeOH 250.5 ng/mL PFOS in Me 1311-52Q8-S1 1311-5209-S1 1311-5210-S1 1311-5210MS-S1 1311-5211-S1 1311-5212-S1 1311-5213-S1 1311-5213MS-S1 5 ng/mL PFOS in MeOH 250.5 ng/m L PFOS in Me v 3 f ov c Page 568 of 703 BACK TO MAIN H 01 0 4 1 2 .X S : InfCompound Na RT Area THPFOS 5.098 THPFOS 5.098 THPFOS 5T352 THPFOS 5.086 THPFOS 0 THPFOS 5 .0 8 5 THPFOS 5.084 THPFOS 5.1 THPFOS 5.091 THPFOS 5.105 THPFOS 5.09 THPFOS 5.093 THPFOS 5.098 THPFOS 5.111 THPFOS 5.092 THPFOS 5.084 THPFOS 5.084 THPFOS 5.084 THPFOS 5.084 THPFOS 5.092 THPFOS 5.083 THPFOS 5.084 THPFOS 5.085 THPFOS 5.092 THPFOS 5.084 THPFOS 5.083 THPFOS 5.096 THPFOS 5.084 THPFOS 5.091 THPFOS 5.091 THPFOS 5.09 THPFOS 5.097 THPFOS 5.099 THPFOS 5.098 Amount Compound NanftT Area Amount 1421318 254 STD> 130%PFOS 5.308 121664 2.881555 1386660 254 STD> 130%PFOS 5308 244130 7.549882 35*040 254 SiD>i3U7oPF0S 6.309 154787 4.341296 1167677 254 STD>130%PFOS 5.303 2811652 124.1501 0 0 ISTD<70% PFOS 5.293 290916 0 1378613 254 STD> 130%PFOS 5 302 303230 9.81694 1378731 254 STD>130%PFOS 5.301 261759 8.262414 1203962 254 STD>130%PFOS 5.318 2936973 125.8164 1027099 254 PFOS 5.301 255948 11.32774 843460 254 PFOS 5.315 265286 14.70451 933401 254 PFOS 5.3 95650 3.752122 909322 254 PFOS 5.303 4533055 262.1838 1068135 254 PFOS 5.316 142453 5.346159 819845 254 PFOS 5.322 3212267 204.5971 1481313 254 STD>130%PFOS 5.302 111849 2.360961 1430325 254 STD>130%PFOS 5.302 91312 1.759256 1442269 254 STD> 130%PFOS 5.301 81813 1.392345 1273255 254 STD> 130%PFOS 5.294 2746281 110.9006 1406869 254 STD>130%PFOS 5.301 242229 7.349539 1404007 254 STD>13Q%PFOS 5.309 188695 5.399388 1398417 254 STD>130%PFOS 5.301 183603 5.239191 1228700 254 STD>130%PFOS 5.301 2820818 118.2271 1163680 254 STD>130%PFOS 5.302 95002 2.67728 1059764 254 PFOS 5.302 4415425 217.9421 1078804 254 PFOS 5.301 327252 14.12675 1062929 254 PFOS 5.293 266793 11.4209 1137098 254 PFOS 5.306 193712 7.255599 868940 254 PFOS 5.301 3239017 194.376 1076643 254 PFOS 5.308 342271 14.87953 1079410 254 PFOS 5.301 531168 23.89509 1083530 254 PFOS 5.307 545049 24.46187 872902 254 PFOS 5.307 3604117 215.9226 882171 254 PFOS 5.309 101365 4.393428 851213 254 PFOS 5.315 4585830 284.0595 75.0% 104.7% 53.5% 87.0% 87.9% 113.4% Page 2 of 2 BACK TO MAIN R 0 1 0 4 1 2.xls ! 2 CD UJ rQ> oo 2 g- 3 r\ 3 r u Q) CQ CD O) a> CD O -- OJ 0 Oo c3 x P c S am p le B atch R 0104012.b, an a ly zed on R u sh 04-12*01. PFOS A dsorb/D esorto s a m p le s. Matrix: S oll/S lg/S ed. S ta n d ard curve range u sed for calibration o f sam p les: 10-1002 ng/mL (2.5,5 ng/mL std not included d u e to th e higher sam p le co n cen tratio n range). B atch m ethod: R010412.m -- InJ D a te B atch 4/12/01 17:41 U:\Cherm Ru3htRG10412.b 4/12/01 17:56 D:\Chem\Rush\R010412.b 4/12/01 18:10 D:\Chem\Rush\R010412.b 4/12/01 18:24 D:\Chem\Rush\R010412.b 4/12/01 18:39 D:\ChemVRush\R010412.b 4/12/01 18:53 D:\Chem\Rush\R010412.b 4/12/01 19:08 D :\Chem \Rush\R010412.b 4/12/01 19:22 D :\C hem \R ush010412.b 4/12/01 19:36 D:\Chem\Rush\R010412.b 4/12/01 19:51 D:\Chem \R ush\R 0104l2.b 4/12/01 20:05 D:\Cbem\Rushy701D412.b 4/12/01 20:19 D:\Chem\Rush\R010412.b 4/12/01 20:34 D :\C hem \R ush\R 0104l2.b 4/13/01 12:53 D:\Chem \Rush\R010412.b 4/13/01 13:07 D:\Chem \Rush\R010412.b 4/13/01 13:22 D:\Chem\RuslAR010412.b 4/13/01 13:36 D :\Chem \Rush\R010412.b 4/13/01 13:50 D:\Chem\Rush\R010412.b 4/13/01 14:05 D:\Chem \R ush\R 0104l2M 4/13/01 14:19 D:1Chem\Rush\R010412.to 4/13/01 14:33 D:\Chem\Rush\R01D412.b 4/13/01 14:48 D :\Chem \Rush\R010412.b 4/13/01 15:02 D:\Chem\Rush\R010412.b 4/13/01 15:17 D:\Cbem \Ru shVRO10412.b 4/13/01 15:31 D:\Chem\Rush\R010412.b 4/13/01 15:45 D:\Chem\Rush\R010412.b Sam pType SAMPLE CALIB 1 CALIE 2 CALIB 3 CAUB 4 SAMPLE CALIB 5 CALIB 6 CALIB 7 CAUB 8 SAMPLE CAUB 9 CALIBRO SAMPLE CAUB 11 CAUB 12 CAUB 13 CAUB 14 SAMPLE CAUB 15 CAUB 16 CAUB 17 CALIB 18 SAMPLE CALIBRI 9 CAUB_20 File RUSH0017.D RUSH16.D RUSH0019.0 RUSH0020.D RUSH021.D R U S H 0 0 2 2 .D RUSHOQ23.D RUSHO24.D R U S H 0 0 2 5 .D RUSH0026.D R U S H 0 0 2 7 .D RUSH0028.D RUSH0029.D RUSH0097.D RUSH0098.D RUSH0099.D R U S H 0 1 0 0 .D R U S H 0 1 0 1 .D RUSH12.D RUSH0103.D RUSH0104.D RUSH105.D RUSH0106.D RUSH0107.D RUSH0108.D R U S H 0 1 0 9 .D Sam ple Name 0 ng/mL P FO S in MeOH 2 .5 ng/m L P F O S in MeOH 5 ng/mL P FO S in MeOH 1 0 ng/mL P FO S in MeOH 25 ng/mL P FO S in MeOH 4 0 ng/mL P FO S in MeOH 5 0.1 ng/mL P FO S in MeOH 75.1 ng/mL P FO S in MeOH 100.2 ng/mL P FO S in MeOH 2 5 0 .5 ng/mL P FO S in MeOH 400.8 ng/mL P FO S in MeOH 501 ng/mL P FO S in MeOH 1002 ng/mL P F O S in MeOH O ng/mL P FO S in MeOH 2 .5 ng/mL P F O S in MeOH 5 ng/mL PFO S in MeOH IO ng/mL P FO S in MeOH 25 ng/mL PFO S in MeOH 4 0 ng/mL P F O S in MeOH 50 .1 ng/mL P FO S in MeOH 75.1 ng/mL P FO S in MeOH 100.2 ng/mL P FO S in MeOH 2 5 0 .5 ng/mL P FO S in MeOH 400.8 ng/mL P FO S in MeOH 501 ng/mL P FO S in MeOH 1002 ng/mL PFO S in MeOH Mise InfCom pouncRT A rea Amount THPFOS 5.583 598645 254 THPFOS 5.585 600613 254 THPFOS 5.585 601845 254 THPFOS 5.593 600915 254 THPFOS 5.574 597942 254 THPFOS 5.58 601700 254 THPFOS 5.588 602030 254 THPFOS 5.577 604353 254 THPFOS 5.579 599001 254 THPFOS 5.587 592421 254 THPFOS 5.58 598537 254 THPFOS 5.581 586806 254 THPFOS 5.585 586018 254 THPFOS 5.543 576686 254 THPFOS 5.554 579447 254 THPFOS 5.559 584774 254 THPFOS 5.551 565534 254 THPFOS 5.549 579881 254 THPFOS 5.551 577089 254 THPFOS 5.545 576872 254 THPFOS 5.555 579170 254 THPFOS 5.551 582102 254 THPFOS 5.558 578231 254 THPFOS 5.551 570124 254 THPFOS 5.553 566337 254 THPFOS 5.545 571690 254 C om pounrflT 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 rea A m ount 00 0 5.795 124534 0 5.788 162745 2.292686 5.789 236433 7.373546 5.777 479447 24.55608 5.783 712400 41.080268 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 00 0 5.764 108854 0 5.762 146886 1.502829 5.754 222698 6.829581 5.752 463425 24.442741 5.754 683988 41.135446 5.748 831833 52.479175 5.758 1172649 78.947857 5 7 5 5 1482631 103.52283 5.761 3120176 251.71766 5.754 4477040 398.70415 5.756 5297025 497.2204 57 4 8 9058485 999.91911 45.9% 737% 98.2% 102.4% 103.7% 104.2% 102.7% 100.2% 98.7% 30.1% 68.3% 97.8% 102.6% 104.7% 105.1% 103.3% 100.5% 99.2% A verage: 587644.7 S td Dev: 11704.42 % RSD: 2.0% 763938 +30%: 411351 -30%: Inj D ate B atch 4/12/01 17:13 D:\Chem\Rush\R010412.b 4/12/01 17:27 D:\Chem\Rusti\R010412A 4/12/01 20:48 D:\Chem\Rush\R010412.b 4/12/01 21:03 D:\Chem\Rush\R010412.b 4/13/01 0:09 D:\Chem\Rush\R010412.b 4/13/01 0:24 D:\Chem \Rush\R010412.b 4/13/01 3:31 D:\Chem\Rush\R010412.b 4/13/01 3:45 D:\Chem\Rush\R010412.b 4/13/01 6:52 D:\Chem\Rush\R010412.b 4/13/01 7:06 D:\Chem1RushlR010412.b 4/13/01 9:16 D:\Chem\Rush\R010412.b 4/13/01 9:31 D :tChem \Rush\R010412.b 4/13/01 12:09 D:\Chem\Rush\R010412.b 4/13/01 12:24 D:\Chem \Rush\R010412.b 4/13/01 12:38 D:\Chem\Rush1R010412.b 4/13/01 16:00 D:\Chem\Rush\R010412.b 4/13/01 16:14 D:\Chem\Rush1R010412.b S am pType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File RUSH015.D RUSHOOW.D RUSH0030.D RUSH0031.D RUSH0044.D RUSH0045.D RUSH0058.D RUSH0059.D RUSH0072.D RUSH0073.D RUSH0082.D RUSH0083.D RUSH0094.D RUSH0095.D RUSH0096.D RUSH0110-D RUSH0111.D Sam ple 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 Mise InfContpounrRT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS A rea 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 A m ount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 CompountRT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A rea A m ount 5.8 92075 5799 71408 5797 88361 5795 74724 5785 70265 5.782 66840 5793 69743 5776 66261 5792 67260 5769 63670 5763 66988 5762 62760 5764 67549 5777 60061 5.775 59600 5.79 76873 5768 61967 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page 1 of 2 Page 570 of 703 s 3' s 3 CD S or cSr r--T O Q) 3* y* In j D ate B a tc h 4 /1 2 /0 1 21:17 D :\C h e m \R u s h \R 0 1 0 4 12.b 4 /1 2 /0 1 21:31 D :\C h em \R u sh \R 010412b 4 /1 2 /0 1 2 1 :4 6 D :\C bem \R ush\R 010412.b 4 /12/01 22:00 D A C hem \R ush\R 010412.b 4 / 2 / 0 1 2 2 :1 4 D : \C h e m \R i s h \R 0 1 0 4 1 2 . b 4 /1 2 /0 1 22:29 D :\C h em \R u sh \R 010 4 1 2.b 4/12/01 22:43 D :\C hem \R ush\R 010412.b 4 /12/01 22:57 D:\C hem \R ush\R Q 10 4 1 2.b 4 /1 2 /0 1 23:12 D :\C hem \R ush\R 010412.b 4 /12/01 23:26 D :\C bem \R ush\R 010412.b 4 /1 2 /0 1 23:40 O :\C hem \R ush\R 010 4 1 2.b 4/1 2 /0 1 23:55 D :\C h em \R u sh \R 010412.b 4 /1 3 /0 1 0:38 D :\C h em \R u sh \R 010 4 1 2.b 4/13/01 0:52 D :\C bem \R ush\R 010 4 1 2 .b 4 /1 3 /0 1 1:07 D :\C h e m \R u s b W 0 1 0 4 1 2 .b 4 /1 3 /0 1 1:21 D :\C h e m \R u s h \R 0 1 0 4 1 2.b 4 /1 3 /0 1 1 :3 6 D :\C b e m \R u s h \R 0 1 0 4 1 2 .b 4/13 /0 1 1:50 D :\C ftem \R ush\R 010 4 1 2-b 4/13/01 2:04 D :\C h em \R u sh \R 010412.b 4/13/01 2:19 D :\C hem \R ush\R 010412-b 4 /13/01 2:33 D :\C hem \R ush\R 010412.b 4/13/01 2:47 D :\C b em \R u sh \R 010412.b 4/13/01 3:02 D :\C bem \R u sb W 010412.b 4 /13/01 3:16 D :\C hem \R ush\R 010412.b 4/13/01 3:59 D :\C h em \R u sh \R 010412.b 4/13/01 4:14 D :\C h em \R u sh \R 010412.b 4/13/01 4:28 D :\C h em \R u sh \R 010412.b 4/13/01 4:43 D :\C h em \R u sh \R 010412.b 4 /13/01 4:57 D :\C hem \R ush\R 010412.b 4 /1 3 /0 1 5:11 D :\C b e m \R u s h \R 0 1 0 4 1 2.b 4/13/01 5:26 D :\C hem \R usb\R 010412.b 4/13/01 5:40 D :\C h em \R u sh \R 010412.b 4 /13/01 5:55 D :\C hem \R ush\R 010412.b 4/13/01 6:09 D :\C h em \R u sh \R 010412.b 4/13/01 6:23 D :\C h em \R u sh \R Q 10412.b 4/13/01 6:38 D :\C hem \R ush\R 010412.b 4 /1 3 /0 1 7:21 D :\C h e m \R u s h \R 0 1 0 4 1 2.b 4/13/01 7:35 D :\C h em \R u sh \R 010412.b 4/13/01 7:50 D :\C b e m lR t/5 b 0 1 0 4 2 .b 4/13/01 8:04 D :\C hem \R ush\R 010 4 1 2.b 4 /1 3 /0 1 8 :18 D :\C h em \R u sh \R 010 4 1 2.b 4/13/01 8:33 D :\C h em \R u sh \R 010412.b 4/13/01 8:47 D :\C h em \R u sh \R 010412.b 4 /1 3 /0 1 9:02 D :\C h em \R u sh \R 010 4 1 2.b 4/1 3 /0 1 9:45 D :\C b em \R u sh \R 010 4 1 2.b 4/13/01 10:00 D :\C h em \R u sb \R 010 4 1 2 .b 4/13/01 10:14 D :\C hem \R usfttR 01O 412.b 4/13/01 10:28 D :\C h em \R u sh \R 010412.b 4/13/01 10:43 D :\C b em \R u sh \R 0104 1 2 .b 4/13/01 10:57 D :\C h em \R u sh \R 010 4 1 2.b 4/13/01 11:12 D :\C h em \R u sh \R 010412.b 4/13/01 11:26 D :\C b em \R u sh \R 010412.b 4/1 3 /0 1 11:41 D :\C h em \R u sh \R 010 4 1 2.b 4/13/01 11:55 D :\C h em \R u sh \R 010412.b Sam pType 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 R te R U SH O 032.D R U S H 0033.D R U SH O 034.D R U SH O 035.D R U S H 0036.D RU 5H O C 37.D R U S H 0038.D R U S H 0039.D R U S H 0040.D R U S H 0041.D R U S H 0042.D R U SH 0043.D R U S H 0046.D R U S H 0047.D R U S H 0048.D R U SH 0049.D R U SH 0050.D R U SH 0051.D RUSHO 52.D R U SH 0053.D R U SH 0054.D R U SH 0055.D R U SH O 056.D R U SH 0057.D R U SH 0060.D R U SH 0061.D R U SH 0062.D R U SH 0063.D R U SH 0064.D R U SH 0065.D R U SH 0066.D R U SH 0067.D R U SH 0068.D R U SH 0069.D R U SH 0070.D R U S H 0 G 7 1 .D R U S H 0074.D R U S H 0075.D R U SH 0O 76.D R U S H 0077.D R U S H 0078.D R U S H 0079.D R U S H 0080.D R U S H 0081.D R U S H 0084.D R S H 0085.D R U S H 0086.0 R U S H 0087.D R U S H 0088.D R U S H 0089.D R U S H 0090.D R U S H 0091.D R U S H 0092.D R U S H 0093.D S am pfe Nam e 1311-5124-S 1 1311-5125-S 1 1 3 1 1-S126-S1 1311-5126M S -S 1 1311-5127-S 1 1311-5128-S 1 1311-5129-S 1 1311-5129M S -S 1 1311-5130-S 1 1311-5131-S 1 5 n g /m l P F O S in M e O H 2 5 0 .5 ng/m L P F O S in M e O H 1311-5132-S t 1311-5132M S-S1 1311-5133-S 1 1 3 1 1 -5 1 3 4 -S 1 1311-5135-S 1 1311-5135M S-S1 1 3 1 1 -5 1 3 6 -S 1 1 3 1 1 -5 1 3 7 -S 1 1 3 1 1 -5 1 3 8 -S 1 1311-5138M S -S 1 5 n g /m L P F O S in M e O H 2 5 0 .5 ng/m L P F O S in M e O H 1311-5139-S 1 1 3 1 1 -5 1 4 0 -S 1 1311-5141-S 1 1 3 1 1 -5 1 4 1 M S-S1 1311-5142-S 1 1311-5143-S 1 1 3 1 1 -5 1 4 4 -S 1 131t-5144M S -S l 1311-5145-S t 1311-5146-S 1 5 n g /m l P F O S in M e O H 2 5 0 .5 n g /m L P F O S in M e O H 1311-5147-S 1 1311-5147M S -S 1 131-5J48-S 1 1 3 1 1 -5 1 4 9 -S 1 1311-5150-S 1 1311-5150M S -S 1 5 ng/m L P F O S in M e O H 2 5 0 .5 n g /m L P F O S In M e O H 1311-5151 -S I 1 3 1 1 -5 1 5 2 -S 1 T 3-5 1 5 3 -S 1 1311-5153M S -S 1 1 3 1 1 -5 1 54 -S 1 1 3 1 1 -5 1 5 5 -S 1 1 3 1 1 -5 1 5 6 -S 1 1311-5156M S -S 1 5 ng/m L P F O S in M e O H 2 5 0 .5 ng/m L P F O S in M eO H BACK TO MAIN R 0 1 0 4 1 2 jd s Mise infC om poancR T A rea A m ount THPFOS 5.56 677530 254 THPFOS 5.571 656863 254 THPFOS 5.557 633889 254 THPFOS 5.551 650748 254 THPFOS 5.566 615903 254 THPFOS 5.572 613221 254 THPFOS 5.565 606355 254 THPFOS 5.565 485715 254 THPFOS 5.567 594618 254 THPFOS 5.565 575974 254 THPFOS 5.572 592560 254 THPFOS 5.553 586770 254 THPFOS 5.565 614286 254 THPFOS 5.557 483260 254 THPFOS 5.565 587357 254 THPFOS 5.565 585569 254 THPFOS 5.572 585514 254 THPFOS 5.565 477977 254 THPFOS 5.566 565186 254 THPFOS 5.567 580244 254 THPFOS 5.564 577866 254 THPFOS 5.562 480568 254 THPFOS 5.559 577392 254 THPFOS 5,572 578945 254 THPFOS 5.551 595025 254 THPFOS 5.55 639476 254 THPFOS 5.557 616815 254 THPFOS 5.559 496627 254 THPFOS 5.558 608824 254 THPFOS 5.551 600876 254 THPFOS 5.565 607245 254 THPFOS 5.559 554564 254 THPFOS 5.572 600380 254 THPFOS 5.545 588635 254 THPFOS 5.562 584267 254 THPFOS 5.561 584334 254 THPFOS 5.565 602683 254 THPFOS 5.558 481237 254 THPFOS 5.572 584694 254 THPFOS 5.571 579440 254 THPFOS 5.554 560769 254 THPFOS 5.565 464515 254 THPFOS 5.559 571261 254 THPFOS 5.551 577867 254 THPFOS 5.572 579739 254 THPFOS 5.561 567823 254 THPFOS 5.565 566066 254 THPFOS 5.549 451967 254 THPFOS 5.553 560862 254 THPFOS 5.566 547161 254 THPFOS 5.557 562481 254 THPFOS 5.554 446367 254 THPFOS 5.547 570884 254 THPFOS 5.558 564635 254 r* '- C om poiinrfiT A rea A m ount PFOS 5.77 3454739 235.14955 PFOS 5.774 3355208 235.64253 PFOS 5.753 3182334 230.80435 PFOS 5.747 6054164 493.84798 PFOS 5.769 444477 21.144501 PFOS 5.762 168978 2.504388 PFOS 00 0 PFOS 5.775 221.25701 PFOS 5.777 480775 24.842763 PFOS 5.769 373656 18.057138 PFOS 5.775 158302 2.158669 PFOS 5.756 3218501 256.73464 PFOS 5.768 502482 25.246348 PFOS 5.76 2628517 254.1411 PFOS 5.775 1602422 112.23406 PFOS 5.768 1852365 133.55448 PFOS 5.775 1878850 135.81745 PFOS 5.768 3662482 386.68394 PFOS 5.769 1220182 85.185002 PFOS 5.77 1144435 76.52B101 PFOS 5.767 1130123 75.760492 PFOS 5.772 3167549 321.0065 PFOS 5.769 157432 2.385234 PFOS 5.775 3179184 257.08626 PFOS 5.754 2160001 157.04195 PFOS 5.754 2298555 155.2245 PFOS 5.761 2208338 154.50156 PFOS 5.769 4097578 424.19511 PFOS 5.768 1622807 109.20753 PFOS 5.754 1479479 99.477125 PFOS 5.775 1456259 96.43578 PFOS 5.762 3859865 343.24391 PFOS 5.775 214358 5.865127 PFOS 00 0 PFOS 5.772 152719 1.92182 PFOS 5.764 3226476 258.79876 PFOS 00 0 PFOS 5.761 2325043 220.44504 PFOS 5.782 1727840 123.28243 PFOS 5.775 1311565 90.083398 PFOS 5.757 1985675 152.50789 PFOS 5.775 3830754 423.93446 PFOS 5.769 155989 2.401694 PFOS 5.754 3239422 263.57325 PFOS 5.775 5190205 470.27597 PFOS 5.757 5181003 481.76818 PFOS 5.76B 4993539 461.55284 PFOS 5.752 6454778 867.49401 PFOS 5.75 3101765 259.29449 PFOS 5.769 3159998 273.24465 PFOS 5.768 3121769 260.40515 PFOS 5.757 4577579 559.64233 PFOS 5.757 157988 2.553111 PFOS 5.761 3184410 265.50383 43.2% 102.5% 47.7% 102.6% 38.4% 103.3% 48.0% 105.2% 51.1% 106.0% Page 2 of 2 CO 5> 33' 2CD f COrQ-->r 3 3" 5 c0To)l CD c-nj o o-N l CO BACK TO MAIN Sam ple Batch H010309.b, analyzed on Hillary 03*09-01. PFOS AdsorblDesorb aamples. S tandard curve range uaed fo r calibration o f sam ples: 5-400.8 ng/m L (501 ng/m L std no t Included due to th e lo w sam ple concentration range). Batch method: H010309.m Inj D ate Batch SampType 3/9/01 19:38 D:\Chem\Hiliary\H010309.b SAMPLE 3/9/01 19:49 D:\Chem\Hillary\H010309.b CALIB 1 3/9/01 20:01 D:\Chem\Hillary\H010309.b CALIS 2 3/9/01 20:12 D:\Chem\Hillary\H010309.b CALIB 3 3/9/01 20.24 D.\Chero\Hia/y1H010309. b CALIB 4 3/9/01 20:35 D:\Chem\Hillary\H010309.b CAUB 5 3/9/01 20:46 D:\Chem\Hillary\H010309.b CALIB 6 3/9/01 20:58 D:\Chem\Hillary\H010309.b CALIB 7 3/9/01 21:09 D:\Chem\Hillary\H010309.b CALIB 8 3/9/01 21:20 D:\Chem\Hillary\H010309.b CALIB 9 3/9/01 21:32 D:\Chem\Hillary\H010309.b CALIB 10 3/9/01 21:43 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 19:09 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 19:20 D:\Chem\Hill3iy1H010309.b CAUB 11 3/10/01 19:31 D:\Chem\Hillary\H010309.b CAUB 12 3/10/01 19:43 D:\Chem\Hillary\H010309.b CAUB 13 3/10/01 19:54 D:\Chem\Hillary\H010309.b CAUB 14 3/10/01 20:05 D:\Chem\Hillary\H010309.b CALIB 15 3/10/01 20:17 D:\Chem\Hillary\H010309.b CAUB 16 3/10/01 20:28 D:\Chem\Hillary\H010309.b CALIB 17 3/10/01 20:40 D:\Chem\Hillarv\H010309.b CAUB 18 3/10/01 20:51 D:\Chem\Hillary\H010309.b CCAUB 1 3/10/01 21:02 D:\Chero\Hjllary\H010309.b CAUB 20 3/10/01 21:14 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 0:22 D :\Chem\Hillary\H010309.b CCALIB 1 3/10/01 0:33 D:\Chem\Hillary\H010309.b CCALIB 1 3/10/01 3:01 D:\Chem\Hiliary\H010309.b CCAUB 1 3/10/01 3:13 D:\Chem\Hillary\HO10309.b CCAUB 1 3/10/01 5:41 D:\Chem\Hillafy\H010309.b CCAUB 1 3/10/01 5:52 D:\Chem\HiIlary\H010309.b CCALIB 1 3/10/01 8:20 D:\Chem\Hillary\H010309.b CCALIB 1 3/10/01 8:31 D:\Chem\Hillary\H010309.b CCAUB 1 3/10/01 10:59 D:\Chem\Hillary\H010309.b CCALIB 1 3/10/01 11:11 D:\Chem\Hillary\H010309.b CCAUB 1 3/10/01 13:39 D:\Chem\Hillary\H010309.b CCALIB 1 3/10/01 13:50 D:\Chem\Hillary\H010309.b CCAUB 1 3/10/01 16:07 O:\Chem\HiKary\H010309.b CCALIB 1 3/10/01 16:18 D:\Chem\Hillary\H010309.b CCAUB 1 3/10/01 18:23 D:\Chem\Hillary\H010309.b CCALIB 1 3/10/01 18:35 D:\Chem\Hillary\H010309.b CCAUB_1 File HILL0021-D HILL0022.D HILL0023.D HILL0024.D HILL0025.D HILL0026.D HILL0027.D HILL002B.D HILL0029.D HILL0030.D HILL0031.0 HILL0032.D HILL0145.D HILL0146.D HILL0147.D HILL0148.D HILL0149.D HILL015 0 .D HILL0151.D HILL0152.D HILL0153.D HILL0154.D HILL0155.D HILL0156.D Sample Name O ng/mL P F O S n MeOH 2.5 ng/mL PFO S in MeOH 5 ng/mL PFO S in MeOH 1 0 ng/mL P F O S in MeOH 25 ng/mL PFO S in MeOH 4 0 ng/mL P F O S in MeOH 5 0 .1 ng/mL PFO S in MeOH 75.1 ng/mL PFO S in MeOH 100.2 ng/mL PFO S in MeOH 2 5 0 .5 ng/mL PFO S in MeOH 4 00.8 ng/mL PFO S in MeOH 501 ng/mL PFO S in MeOH 0 ng/mL P F O S in MeOH 2.5 ng/mL PFO S in MeOH 5 ng/mL P F O S in MeOH 1 0 ng/mL P FO S in MeOH 25 ng/mL P F O S in MeOH 4 0 ng/mL P FO S in MeOH 5 0 .1 ng/mL PFOS in MeOH 75.1 ng/mL PFO S in MeOH 100.2 ng/mL PFO S in MeOH 250.5 ng/mL PFO S in MeOH 4 00.8 ng/mL PFO S n MeOH 501 ng/mL PFO S in MeOH Mise 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 Amount Compound Name 5.049 1073281 254 PFOS 5.041 1072804 254 PFOS 5.05 1108750 254 PFOS 5.042 1078365 254 PFOS 5.035 1076706 254 PFOS 5.039 1100085 254 PFOS 5.043 1076389 254 PFOS 5.036 1055026 254 PFOS 5.045 1081297 254 PFOS 5.044 1069673 254 PFOS 5.036 1034737 254 PFOS 5.036 1060526 254 PFOS 5.023 868621 254 PFOS 5.015 B70619 254 PFOS 5.008 912239 254 PFOS 5.013 886038 254 PFOS 5.016 880755 254 PFOS 5.008 920893 254 PFOS 5.017 5.015 899166 876782 254 PFOS 254 PFOS 5.014 901662 254 PFOS 5.008 899022 254 PFOS 5.009 898706 254 PFOS 5.014 899348 254 PFOS RT Area 0 5265 5.274 5.273 5.259 5.271 5.274 5.267 5.269 5.268 5.267 5.26 0 5.240 5.232 5.237 5.247 5.232 5.241 5.246 5.238 5.232 5.233 5.238 Amount 00 86451 2.270782 143416 4.248778 231909 7.730027 622426 22.54388 1029067 37.23449 1260789 46.98954 1838015 70.79131 2464526 93.43521 5867511 233.6441 8794548 373.3181 10677107 449.019 00 79391 2.700768 150012 5.673501 233970 9.723374 607127 27.10542 998520 43 38523 1226451 54.99273 1767680 82.31103 2372952 108.4295 5738392 274.4434 8461603 417.364 10729909 541.808 HILL0046.D HILL0047.D HILL0060.D H IL L 0 0 9 1 .D HILL0074.D HILL0075.D HILL0088.D HILL0089.D HILL01O2.D HILLQ103-D HILL0116.D HILL0117.D HILL0129. D HILL013O.D HILL0141.D H1LL0142.D 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFO S in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/m L PFO S in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFO S in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFO S in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFOS in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFOS in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFOS in MeOH 5 ng/mL P F O S in MeOH 2 5 0 .5 ng/mL PFOS in MeOH A veraae: 963395.417 Std Dev: 94153.7839 %RSD; 9-6% THPFOS 5.029 THPFOS 5.031 THPFOS 5.028 THPFOS 5.029 THPFOS THPFOS THPFOS 5.027 5.023 5.028 THPFOS 5.021 THPFOS 5.033 THPFOS 5.035 THPFOS 5.017 THPFOS THPFOS 5,021 5.02 THPFOS 5.017 THPFOS 5.014 THPFOS 5.019 +30%: 1278414 -30%: 688377 1094159 1070122 1064793 1063455 986230 978168 922698 906571 909132 908551 869545 872093 863500 870533 886391 877876 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 5.253 5.262 5.252 5.253 5.259 5.247 5.253 5.245 5.257 5.266 5.241 5.245 5.244 5.241 5.238 5.243 133354 3.9456 5756785 228.8809 143353 4.362347 5711016 228.462 137467 4.656142 5653787 246.9623 136789 5.015913 5622338 266.1543 140176 5.256986 5636922 266.3707 135055 5.302878 5547134 273.4256 137478 5.423749 5593609 276.4058 141405 5.473911 5639356 276.3196 85% 77% 90% 93% 94% 94% 92% 93% 93% 113% 97% 108% 108% 110% 109% 106% 110% 104% 79% 91% 87% 91% 93% 99% 100% 106% 105% 106% 106% 109% 108% 110% 109% 110% 3 |p 8) ol BACK TO MAIN 3M Environmental Laboratory Inj Date Batch SampType 3/9/01 19:15 D:\Chem\HiIlary\H010309.b SAMPLE 3/9/01 19:27 D:\Chem\Hiiiary\H010309.b SAMPLE 3/9/01 21:55 D:\Chem\Hiilary\H0103O9.b SAMPLE 3/9/01 22:06 D:\Chem\Hillary\H010309.b SAMPLE 3/9/01 22:17 D:\Chem\Hiliary\H010309.b SAMPLE 3/10/01 0:45 D:\Qhem\HUIary\H010309.b SAMPLE 3/10/01 0:56 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 3:24 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 3:38 D:\Chem\HilIary\H010309.b SAMPLE 3/10/01 6:03 D:\Chem\Hiliary\H010309.b SAMPLE 3/10/01 6:15 D:\Chem\HiIiary\H010309.b SAMPLE 3/10/01 8:43 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 8:54 D:\Chem\Hillary\H0103O9.b SAMPLE 3/10/01 11:22 D:\Chem\Hdlary\H010309. b SAMPLE 3/10/01 11:34 D:\Cftem\Hillary\H010309.b SAMPLE 3/10/01 14:02 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 14:13 D:\Chem\HiIlary\H010309.b SAMPLE 3/10/01 16:30 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 16:41 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 18:46 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 18:57 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 21:25 D:\Chem\Hillary\H010309.b SAMPLE File__________ Sample Name HILL0019.D HILL0020.D HILL0033.D HILL0034.D HILL0035.D HILL0048.D HILL0049.D HILL0062.D HILL0063.D HILL0076.D HILL0077.D HILL0090.D HILL0091.D HILL0104.D HILL01O5.D HILL0118.D HILL0119.D HILL0131.D HILL0132.D HILL0143.D HILL014-4.D HILL0157.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 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Mise 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 Area 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount Compound Name RT Area 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 0 0 PFOS 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 20788 0 19572 0 0 9584 0 9496 0 9444 0 0 0 8875 0 0 0 0 0 0 0 17138 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 C/v\C 3 I o Page 572 of 703 3M Environmental Laboratory (T)I (t> cn o o --h o's i CO Inj Date______ Batch SampType File Sample Name 3/9/01 22:29 D:\Chem\Htllary\H010309.b SAMPLE 3/9/01 22:40 D:\Chem\HiIlaiy\H010309.b SAMPLE 3/9/01 22:51 D:\Chem\Hillary\H010309.b SAMPLE 3/9/01 23:03 D:\Chem\Hillary\H010309.b SAMPLE 3/9/01 23:14 D:\Chem\Hillary\H010309.b SAMPLE 3/9/01 23:25 D:\Chem\Hillary\H010309.b SAMPLE 3/9/01 23:37 D:\Chem\Hiliary\H010309.b SAMPLE 3/9/01 23:48 D:\Chem\Hillary\H010309.b SAMPLE 3/9/01 23:59 D:\Chem\J-iitiary\H010309.b SAMPLE 3/10/01 0:11 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 1:08 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 1:19 D:\Chem\Hlllary\H010309.b SAMPLE 3/10/01 1:30 D:\Chem\Hiliary\H010309.b SAMPLE 3/10/01 1:42 D:\Chem\Hil1ary\H010309.b SAMPLE 3/10/01 1:53 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 2:04 D:\Chem\HiHary\H010309.b SAMPLE 3/10/01 2:16 D:\Chem\HiIlary\H010309.b SAMPLE 3/10/01 2:27 D:\Chem\Htllary\H010309.b SAMPLE 3/10/01 2:39 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 2:50 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 3:47 D:\Chejn\HiUaiy\H010309.b SAMPLE 3/10/01 3:58 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 4:10 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 4:21 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 4:32 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 4:44 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 4:55 D:\ChemlHiWaiytH010309.b SAMPLE 3/10/01 5:06 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 5:18 D:\Chm\Hillary\H010309.b SAMPLE 3/10/01 5:29 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 6:26 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 6:38 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 6:49 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 7:00 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 7:12 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 7:23 D:\Chem\HHIary\H010309.b SAMPLE 3/10/01 7:34 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 7:46 D:\Chem\Hillary\H010309.b SAMPLE HILL0036.D HILL0037.D HILL0038.D HILL39.D HILL0040.D HILL0041.D HILL0042.D HILL0043.D HILL0044.D HILL0045.D HILL0050.D HILL0051.D HILL0052.D HILL0053D HILL0054.D HILL0055.D HILL0056.D HILL0057.D HILL0058.D HILL0059.D HILL0064.D HILL0065.D HILL0066.D HILL0067.D HILL0068.D HILL0069.D HILL0070.D HILL0071.D HILL0072.D HILL0073.D HILL0078.D HILL0079.D HfLLOOSO.O HILL0081.D HILL0082.D HILL0083.D HILL0084.D H1LL0085.D E00-1311-4103-S1 EOO-1311-4104-S1 E0O-1311-4105-S1 E00-1311-4105-SI-MS EOO-1311-4106-S1 E0O-1311-4107-S1 E00-1311-4108-S1 EOO-1311-4108-S1-MS EOO-1311-4109-S1 E00-1311-4110-S1 EOO-1311-4111-S1 EOO-1311-4111-S1-MS EOO-1311-4112-S1 E00-1311-4113-S1 E00-1311-4114-S1 E00-1311-4114-S1-MS EOO-1311-4115-S1 EOO-1311-4116-S1 EOO-1311-4117-S1 EOO-1311-4117-S1-MS EOO-1311-4118-S1 E00-1311-4119-S1 E00-1311-4120-S1 EOO-1311-4120-S1-MS EOO-1311-4004-S2 EOO-1311-4005-S2 EOO-1311-4006-S2 EOO-1311-4028-S2 EOO-1311-4030-S2 EOO-1311-4034-S2 EOO-1311-4035-S2 E00-1311-4036-S2 E00-1311-4058-S2 EOO-1311-4059-S2 EOO-1311-4060-S2 EOO-1311-4064-S2 E00-1311-4065-S2 EOO-1311-4066-S2 BACK TO MAIN MiseInfo Compound Name RT______ Area_______ Amount Compound Name 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 5.034 5.038 5.042 5.029 5.038 5.035 5.026 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 5.029 5.022 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 1028599 874849 1468017 1055707 1050237 865040 1073533 1045079 1036444 869342 1043258 1053741 1654927 836338 1046939 1038327 1024946 665270 996797 1004358 1012908 843094 941893 914587 910770 951757 912591 919151 924250 924751 879571 889204 808447 870882 914404 869706 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 5.266 5.269 5.266 5.26 5.20 5.266 5.25 5.26 5.258 5.282 5.259 5.26 5.266 5.26 5.263 5.252 5.252 5.259 5.253 5.247 5.254 5248 5.253 5.254 0 0 0 5.253 5.255 5253 0 0 5.259 5248 5.258 0 0 0 234470 8.012285 215844 6.1690 237536 8.375534 3963142 190.9672 452939 11.53411 325164 11.51244 304848 10.78999 4001498 195.2086 173898 5.573715 179135 5.956354 165195 5.468121 3920789 190.0809 170915 5.648499 176264 5.788465 330413 7.103971 3890653 196.3716 177753 5.890369 181171 6.081276 164575 5.516164 3867704 188.3056 180616 6.353969 176677 6.139234 176413 6.068331 3760328 187.8729 00 00 00 270433 10.5406 264195 10.7588 58201 1.571008 00 00 230289 9.632074 260133 10.88282 290040 13.58092 00 00 00 C M C 3 p s I O) 3d co o 3 CD C3 S' oOr0--)' o >5 (Qu0) CD c"nsi o o" s i CO Inj Date______ Batch_________________ SampType 3/10/01 7:57 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 8:09 D:\Chem\Hiilary\H010309.b SAMPLE 3/10/01 9:06 D:\Chem\HiIlary\H010309.b SAMPLE 3/10/01 9:17 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 9:28 D:\Chem\HHlary\H010309.b SAMPLE 3/10/01 9:40 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 9:51 D:\Chem\Hiliary\H010309.b SAMPLE 3/10/01 10:03 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 10:14 D:\Chem\Hitlary\H010309.b SAMPLE 3/10/01 10:25 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 10:37 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 10:46 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 11:45 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 11:56 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 12:08 D:\Chem\Hillary\H01Q309.b SAMPLE 3/10/01 12:19 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 12:30 D:\Chem\HiHary\H010309.b SAMPLE 3/10/01 12:42 D:\Cham\Hillary\H010309.b SAMPLE 3/10/01 12:53 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 13:05 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 13:16 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 13:27 D:\Chem\HjJlaiy\H010309.b SAMPLE 3/10/01 14:24 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 14:36 D:\Chem\Hillary\H01Q309.b SAMPLE 3/10/01 14:47 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 14:59 D:\Chem\Hiilary\H010309.b SAMPLE 3/10/01 15:10 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 15:21 D:\Chem\Hitlary\H010309.b SAMPLE 3/10/01 15:33 D:\Chem\Hillary\H01Q309.b SAMPLE 3/10/01 15:44 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 15:56 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 16:52 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 17:04 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 17:15 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 17:26 D:\Cbem\Hillary\H010309.b SAMPLE 3/10/0117:38 D:\Chem\Hiila(y\H010309.b SAMPLE 3/10/01 17:49 D:\Chem\Hillary\H010309.b SAMPLE 3/10/01 18:01 D:\Chem\HUIary\H010309.b SAMPLE 3/10/01 18:12 D:\Chem\Hillary\HQ10309.b SAMPLE Pie___ HILL0066.D HILL0087.D HILL0092.D HILL0093.0 HILL0094.D HILL0095.D HILL0096.D HILL0097.D HILL0098.D HILL0099.0 HILL0100.D HILL0101.D HILL0106.D HILL0107.D HILL0108.D HILL0109D HILL011O.D HILL0111.D HILL0112.D HILL0113.D HILL0114.D HILL0115.D HILL0120.D HILL0121.D HILL0122.D H1LL0123.D H1LL0124.D HILL0125.D HILL126.0 HILL0127.D HILL0128.D HILL0133.D HILL0134.D HILL0135.D HILL0136.D HILL0137.D HILL0138.D HJLL0139.D HILL0140.D Sample Name EOO*1311-4088-S2 E0O-1311-4O89-S2 E00-1311-4090-S2 E00-1311-4094-S2 E00-1311-495-S2 E00-1311-4096-S2 E00-1311-4118-S2 EOO-1311-4119-S2 EOO-1311-420-S2 EOO-1311-4004-S3 E0O-1311-4005-S3 EOO-1311-4006-S3 EOO-1311-4028-S3 E00-1311-4030-S3 EOO-1311-4035-S3 E0O-1311-4036-S3 EOO-1311-4058-S3 EOO-1311-4059-S3 E00-1311-4060-S3 EOO-1311-4064-S3 EOO-1311-4065-S3 EOO-1311-4066-S3 EOO-1311-4088-S3 EOO-1311-4089-S3 EOO-1311-4090-S3 EOO-1311-4094-S3 EOO-1311-4095-S3 EOO-1311-4096-S3 E00-1311-4118-S3 E00-1311-4119-S3 EOO-1311-4120-S3 EOO-1311-4004-S4 EOO-1311-4005-S4 EOO-1311-4006-S4 EOO-1311-4028-S4 EOO-1311-4030-S4 EOO-1311-4034-S4 EOO-1311-4035-S4 EOO-1311-4036-S4 BACK TO MAIN Mise 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 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.028 5.028 5.03 5.043 5.046 5.035 5.042 5.036 5.036 5.041 5.034 5.028 5.029 5.029 5.028 5.029 5.029 5.028 5.029 5.028 5.023 5.023 5.018 5.014 5.022 5.02 5.021 5.013 5.023 5.013 5.021 5.014 5.008 5.014 5.015 5.014 5.013 5.010 5.016 Amount Compound Name RT 863099 871362 917602 858296 897083 886919 874070 899816 902577 877509 849226 898143 871502 887421 878559 762849 669217 833081 851363 865697 837908 814470 838311 861294 830608 810226 819327 726839 874200 878280 825209 B40917 883425 893529 824667 976257 823949 864200 823859 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 254 PFOS 5.252 5.259 5.254 0 0 0 5.266 5.267 5.267 5.265 0 0 5.253 5.26 0 0 5.253 5.252 5.253 0 0 0 5.242 5.238 5.246 0 0 0 5.247 5.245 5.245 0 0 0 5.246 5.238 0 0 0 541521 24.56545 495693 22.1666 547710 23.31443 00 00 00 357854 15.64721 357623 15.15864 411360 17.54001 646257 29.04163 00 00 244415 10.39046 242159 10.08219 00 00 1Q1283 3.728289 130273 5.345841 260640 11.43662 00 00 00 373867 17.14026 497521 22.52586 491684 23.11219 00 00 00 199280 8.254569 118886 4.49281 928893 45.09718 00 00 00 270001 12.30281 223658 8.300946 00 00 00 emc s|a&/oi Wo-'4 3M Environmental Laboratory Sample Batch R010405.b, analyzed on Hillary 04-06*01. PFOS Adsorb/Desorb samples. Matrix: Soil/SIg/Sed. Standard curve range used for calibration of samples: 25-1002 ng/mL Batch method: R010405.m' Inj Date Batch 4/6/01 13:07 D:\Chem\Rush\R010405.b 4/6/01 13:22 D:\Chem\Rush\R010405.b 4/6/01 13:36 DAChem\Rush\R01040S.b 4/6/01 13:50 D:\Chem\Rush\R010405.b 4/6/01 14:05 O:\Chem\Rush\R010405.b 4/6/01 14:19 D:\Chem\Rush\R010405.b 4/6/01 14:34 D:\Chem\Rush\R010405.b 4/6/01 14:48 D:\Chem\Rush\R010405.b 4/6/01 15:02 D:\Chem\Rush\R010405.b 4/6/01 15:17 D:\Chem\Rush\R010405.b 4/6/01 15:31 D:\Chem\Rush\R010405.b 4/6/01 15:45 D:\Chem\Rush\R010405.b 4/6/01 16:00 D:\Chem\Rush\R010405.b 4/7/01 6:23 D:\Chem\Rush\R010405.b 4/7/01 6:37 D:\Chem\Rush\R010405.b 4/7/01 6:52 D:\Chem\Rush\R010405.b 4/7/01 7:06 D:\Chem\Rush\R010405.b 4/7/01 7:20 D:\Chem\Rush\R010405.b 4/7/01 7:35 D:\Chem\Rush\R010405.b 4/7/01 7:49 D:\Chem\Rush\R010405.b 4/7/01 8:04 D:\Chem\Rush\R010405.b 4/7/01 8:18 O:\Chem\Rush\R010405.b 4/7/01 8:32 D:\Chem\Rush\R010405.b 4/7/01 8:47 D:\Chem\Rush\R010405.b 4/7/01 9:01 D:\Chem\Rush\R010405.b 4/7/01 9:15 D:\Chem\Rush\R010405.b SampType R ie Sample Name SAMPLE RUSH0017.D O ng/mL PFOS in MeOH C A U 8 J RUSH0018.D 2.5 ng/mL PFOS in MeOH CALIB.2 RUSH0019.D 5 ng/mL PFOS in MeOH CALIB_3 RUSH0020.D 1 0 no/mL PFOS in MeOH CALiB.4 RUSH0021 .D 25 ng/mL PFOS in MeOH SAMPLE RUSH0022.0 4 0 ng/mL PFOS in MeOH CAUB_5 RUSH0023.D 50.1 ng/mL PFOS in MeOH CALIB_6 RUSH0024.D 75.1 ng/mL PFOS in MeOH CALIB.7 RUSH0025.D 100.2 ng/mL PFOS in MeOH CAUB.8 RUSH0026.D 25 0 .5 ng/mL PFOS in MeOH SAMPLE RUSH0027.D 400.8 ng/mL PFOS in MeOH CAUB_9 RUSH0028.D 501 ng/mL PFOS in MeOH CAUBJO RUSH0029.D 1002 ng/mL PFOS in MeOH SAMPLE RUSH0089.0 0 ng/mL PFOS in MeOH CALIB_11 RUSH0090.D 2.5 ng/mL PFOS in MeOH CALI8_12 RUSH0091.D 5 ng/mL PFOS in MeOH CALIB.13 RUSH0092.D 1 0 ng/mL PFOS in MeOH C A L I8 J 4 RUSH0093.D 25 ng/mL PFOS in MeOH SAMPLE RUSH0094.D 4 0 ng/mL PFOS in MeOH CAUB.15 RUSH0095.D 50.1 ng/mL PFOS in MeOH C A U B J6 RUSHQ096.D 75.1 ng/mL PFOS in MeOH CALIB_17 RUSH0097.D 100.2 ng/mL PFOS in MeOH CALIB.18 RUSH0098.0 250.5 ng/mL PFOS in MeOH SAMPLE RUSH0099.D 400.6 ng/mL PFOS in MeOH CALIB.19 RUSH0100.D 501 ng/mL PFOS in MeOH CALIBJ20 RUSH0101.D 1002 ng/mL PFOS in MeOH n r -"0 a Inj Date Batch 4/6/01 12:39 D:\Chem\Rush\R010405.b 4/6/01 12:53 D:\Chem\Rush\R010405.b 4/6/01 16:14 D:\Chem\Rush\R010405.b 4/6/01 16:29 D:\Chem\Rush\R010405.b 4/8/01 19:35 D:\Chem\Rush\R010405.b 4/6/01 19:50 D:\Chem\Rush\R010405.b 4/6/01 22:57 D:\Chem\Rush\R010405.b 4/6/01 23:11 D:\Chem\Rush\R010405.b 4/7/01 2:18 D:\Chem\Rush\R010405.b 4/7/01 2:33 D:\Chem\Rush\R010405.b 4/7/01 5:40 D:\Chem\Rush\R010405.b 4/7/01 5:54 D:\Chem\Rush\R010405.b 4/7/01 6:09 D:\Chem\Rush\R010405.b 4/7/01 9:30 D:\Chem\Rush\R010405.b 4/7/01 9:44 D:\Chem\Rush\R010405.b SampType File Sample Name SAMPLE RUSH0015.D TN-A 4802 MeOH SAMPLE RUSH0016.D TN-A 4802 MeOH SAMPLE RUSH0030.D TN-A 4802 MeOH SAMPLE RUSH0031.D TN-A 4802 MeOH SAMPLE RUSH0044.D TN-A 4802 MeOH SAMPLE RUSH0045.D TN-A 4802 MeOH SAMPLE RUSH0058.D TN-A 4802 MeOH SAMPLE RUSH0059.D TN-A 4802 MeOH SAMPLE RUSH0072.D TN-A 4802 MeOH SAMPLE RUSH0073.0 TN-A 4802 MeOH SAMPLE RUSH0066.D TN-A 4602 MeOH SAMPLE RUSH0087.D TN-A 4802 MeOH SAMPLE RUSH0086.D TN-A 4802 MeOH SAMPLE RUSH0102.D TN-A 4802 MeOH SAMPLE RUSH0103.D TN-A 4802 MeOH c Page 575 of 703 BACK TO MAIN R010405 internai standard.xls Mise InfCom pound N iR T Arsa THPFOS 5.573 THPFOS 5.572 THPFOS 5.563 THPFOS 5.577 THPFOS 5.571 THPFOS 5.573 THPFOS 5.566 THPFOS 5.563 THPFOS 5.557 THPFOS 5.573 THPFOS 5.564 THPFOS 5.561 THPFOS 5.568 THPFOS 5.573 THPFOS 5.568 THPFOS 5.553 THPFOS 5.57 THPFOS 5.561 THPFOS 5.559 THPFOS 5.557 THPFOS 5.554 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 560525 254 564583 254 554331 254 565266 254 588047 254 551336 254 559057 254 550680 254 533362 254 556117 254 553124 254 576802 254 550084 254 548419 254 553360 254 530697 254 544285 254 560621 254 525351 254 Compound NarftT Area Amount PFOS 0 00 PFOS 5.775 145698 0 PFOS 5.767 177596 0 PFOS 5 787 255188 4252316 PFOS 5.774 520711 26.14863 PFOS 5.770 778358 46.19528 PFOS 5.769 895968 58.81603 PFOS 5.766 1254456 89.78046 PFOS 5.76 1593523 119.474 PFOS 5.776 3289063 289.5214 PFOS 5.767 4814176 446.0827 PFOS 5.764 5878253 542.0292 PFOS 5.771 9460515 1071.163 PFOS 0 00 PFOS 5.785 119802 0 PFOS 5.763 142789 0 PFOS 5.773 210206 0.031512 PFOS 5.771 430360 18.72559 PFOS 5.762 643226 34.73718 PFOS 5.767 755748 47.18652 PFOS 5.764 1044359 73.14746 PFOS 5.764 1341441 99.1613 PFOS 5.768 2714138 242.7883 PFOS 5764 4031839 377.1597 PFOS 5.755 4912946 461.7658 PFOS 5.754 7877904 900.0327 A v a r a : 552630.6923 S td D e v: 14747.09531 %RSD: 2.7% 718420 +30%: 386841 -30%: 0% 43% 105% 115% 117% 120% 119% 116% 111% 108% 107% 0% 0% 75% 87% 94% 97% 99% 97% 94% 92% 90% Mise InfC om pound NaRT 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 Amount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Compound NarRT Area PFOS 5.785 PFOS 5.781 PFOS 5.79 PFOS 5.774 PFOS 5.781 PFOS 5.796 PFOS 5.776 PFOS 5.775 PFOS 5.763 PFOS 5.766 PFOS 5.778 PFOS 5.784 PFOS 5.775 PFOS 5.782 PFOS 5.765 Amount 106775 0 91016 0 103874 0 84825 0 82678 0 76114 0 82141 0 76802 0 76352 0 71081 0 74088 0 69593 0 67762 0 83254 0 64445 0 page 1 of 2 Page 576 of 703 3M Environmental Laboratory Inj Date Batch 4/6/01 16:43 D:\Chem\Rush\R010405.b 4/6/01 16:57 D:\Chem\Rush\R010405.5 4/6/01 17:12 D:\Chem\Rush\R010405.b 4/6/01 17:26 D:\Chem\Rush\R010405.b 4/6/01 17:40 D:\Chem\Rush\R010405.b 4/6/01 17:55 D:\Chem\Rush\R010405.b 4/6/01 18:09 D:\Chem\Rush\R010405.b 4/6/01 18:23 D:\Chem\Rush\R010405.b 4/6/01 18:38 D:\Chem\Rusti\R010405.b 4/6/01 18:52 D:\Chem\Rush\R010405.b 4/6/01 19:07 D:\Chem\Rush\R010405.b 4/6/01 19:21 D:\Chem\Rush\R010405.b 4/6/01 20:04 D:\Chem\Rush\R010405.b 4/6/01 20:18 D:\Chem\Rush\R010405.b 4/6/01 20:33 D:\Chem\Rush\R010405.b 4/6/01 20:47 D:\Chem\Rush\R010405.b 4/6/01 21:02 D:\Chem\Rush\R010405.b 4/6/01 21:16 D:\Chem\Rush\R010405.b 4/6/01 21:30 D:\Chem\Rush\R010405.b 4/6/01 21:45 D:\Chem\Rush\R010405.b 4/6/01 21:59 D:\Chem\Rush\R010405.b 4/6/01 22:13 D:\Chem\Rush\R010405.b 4/6/01 22:28 D:\Chem\Rush\R01Q4Q5.b 4/6/01 22:42 D:\Chem\Rush\R010405.b 4/6/01 23:25 D:\Chem\Rush\R010405.b 4/6/01 23:40 D:\Chem\Rush\R010405.b 4/6/01 23:54 D:\Chem\Rush\R010405.b 4/7/01 0:09 D:\Chem\Rush\R010405.b 4/7/01 0:23 D:\Chem\Rush\R010405.b 4/7/01 0:37 D:\ChemVRush\R010405.b 4/7/01 0:52 D:\Chem\Rush\R010405.b 4/7/01 1:06 D:\Chem\Rush\R010405.b 4/7/01 1:21 D:\Chem\Rush\R010405.b 4/7/01 1:35 D:\Chem\Rush\R010405.b 4/7/01 1:49 D:\Chem\Rush\R010405.b 4/7/01 2:04 D:\Chem\Rush\R010405.b 4/7/01 2:47 D:\Chem\Rush\R010405.b 4/7/01 3:01 D:\Chem\Rush\R010405.b 4/7/01 3:16 D:\Chem\Rush\R010405.b 4/7/01 3:30 D:\Chem\Rush\R010405.b 4/7/01 3:45 D:\Chem\Rush\R010405.b 4/7/01 3:59 D:\Chem\Rush\R010405.b 4/7/01 4:13 D:\Chem\Rush\R010405-b 4/7/01 4:28 D:\Chem\Rush\R010405.b 4/7/01 4:42 D:\Chem\Rush\R010405.b 4/7/01 4:57 D:\Chem\Rush\R010405.b 4/7/01 5:11 D:\Chem\Rush\R010405.b 4/7/01 5:25 D:\Chem\RushNR010405.b 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 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE File Sample Name RUSH0032.D Study Number EOO-1311 RUSH0033.D Study Number EOO-1311 RUSH0034.D Study Number EOO*1311 RUSH0035.D Study Number EOO-1311 RUSH0036.D Study Number EOO-1311 RUSH0037.D Study Number EOO-1311 RUSH0038.D Study Number E00-1311 RUSH0039.D Study Number EOO-1311 RUSH0040.D Study Number EOO-1311 RUSH0041.D Study Number EOO-1311 RUSH0042.D 5 ng/mL PFOS in MeOH RUSH0043.D 250.5 ng/mL PFOS in MeOH RUSH0046.D Study Number EOO-1311 RUSH0047.D Study Number EOO-1311 RUSH0048.D Study Number EOO-1311 RUSH0049.D Study Number EOO-1311 RUSH0050.D Study Number EOO-1311 RUSH0051.D Study Number EOO-1311 RUSH0052.D Study Number EOO-1311 RUSH0053.D Study Number EOO-1311 RUSH0054.D Study Number EOO-1311 RUSH0055.D Study Number EOO-1311 RUSH0056.D 5 ng/mL PFOS in MeOH RUSH0057.D 250.5 ng/mL PFOS in MeOH RUSH0060.D Study Number EOO-1311 RUSH0061.D Study Number EOO-1311 RUSH0062.D Study Number EOO-1311 RUSH0063.D Study Number EOO-1311 RUSH0064.D Study Number EOO-1311 RUSH0065.D Study Number EOO-1311 RUSH0066.D Study Number EOO-1311 RUSH0067.D Study Number EOO-1311 RUSH0068.D Study Number EOO-1311 RUSH0069.D Study Number EOO-1311 RUSH0070.D 5 ng/mL PFOS in MeOH RUSH0071.D 250.5 ng/mL PFOS in MeOH RUSH0074.D Study NumberEOO-1311 RUSH0075.D Study Number EOO-1311 RUSH0076.D Study Number EOO-1311 RUSH0077.D Study Number EOO-1311 RUSH0078.D Study Number EOO-1311 RUSH0079.0 Study Number EOO-1311 RUSHX80.D Study NumberEOO-1311 RUSH0081.D Study Number EOO-1311 RUSH0082.D Study Number EOO-1311 RUSHX83.D Study Number EOO-1311 RUSHX84.D 5 ng/mL PFOS in MeOH RUSH0085.D 250.5 ng/mL PFOS in MeOH BACK TO MAIN R010405 internal standards# Mise InfCompound NaRT Area THPFOS 5.567 THPFOS 5.569 THPFOS 5.565 THPFOS 5,567 THPFOS 5.559 THPFOS 5.564 THPFOS 5.563 THPFOS 5.571 THPFOS 5.572 THPFOS 5.571 THPFOS 5.559 THPFOS 5.562 THPFOS 5.566 THPFOS 5.558 THPFOS 5.565 THPFOS 5.554 THPFOS 5.546 THPFOS 5.559 THPFOS 5.551 THPFOS 5.561 THPFOS 5.566 THPFOS 5.509 THPFOS 5.564 THPFOS 5.572 THPFOS 5.561 THPFOS 5.57 THPFOS 5.565 THPFOS 5.561 THPFOS 5.568 THPFOS 5.561 THPFOS 5.551 THPFOS 5.565 THPFOS 5.567 THPFOS 5.561 THPFOS 5.547 THPFOS 5.556 THPFOS 5.56 THPFOS 5.561 THPFOS 5.549 THPFOS 5.557 THPFOS 5.552 THPFOS 5.544 THPFOS 5.562 THPFOS 5.546 THPFOS 5.549 THPFOS 5.547 THPFOS 5.552 THPFOS 5.556 Amount 549655 254 546340 254 551952 254 543996 254 556241 254 556130 254 557637 254 467615 254 560192 254 553257 254 577885 254 567895 254 558163 254 546057 254 558505 254 554244 254 550480 254 539432 254 547053 254 559047 254 549045 254 543578 254 563324 254 566595 254 551418 254 563119 254 551121 254 533687 254 559718 254 538081 254 549935 254 536497 254 548462 254 553442 254 544796 254 549611 254 539554 254 530879 254 538799 254 550406 254 540857 254 518943 254 536710 254 544277 254 552811 254 537984 254 544157 254 535679 254 Compound NaiflT Area Amount PFOS 5.77 692574 41.69038 PFOS 5.765 614092 35.16084 PFOS 5.768 997270 68.33123 PFOS 5.777 3033445 268.9711 PFOS 5.762 266009 4.684134 PFOS PFOS 5.774 0 512785 25.53605 00 PFOS 5.782 2253516 226.2934 PFOS 5.775 358332 12.22107 PFOS PFOS 5.781 0 341742 11.19223 00 PFOS 5.765 3181790 270.4896 PFOS 5 .7 7 6 308908 8.188777 PFOS 5.761 2580190 221.0756 PFOS 5.775 800286 50.04657 PFOS 5.757 921208 61.22001 PFOS 5.749 965063 65.68839 PFOS 5.769 2988304 266.8858 PFOS 5.762 2199435 182.5679 PFOS 5.784 2334379 190.9566 PFOS 5.769 2803089 242.2879 PFOS PFOS 5.792 0 4428533 422.8252 00 PFOS PFOS PFOS PFOS 5.775 0 0 0 3078172 260.7912 00 00 00 PFOS 5.771 2297114 197.9487 PFOS 5.778 305322 7.818031 PFOS 5.771 269990 5.7797 PFOS 5.761 280197 6.14042 PFOS PFOS PFOS PFOS 5.768 0 0 0 2329314 199.9928 00 00 00 PFOS PFOS 5.759 0 2913640 253.3329 00 PFOS PFOS PFOS 5.764 0 0 2181139 0 0 187.322 0 0 PFOS 5.762 218149 1.206327 PFOS 5.747 2172754 191.5666 PFOS 5.773 738133 47.25497 PFOS 5.756 865021 57.65922 PFOS 5.752 981309 66.77067 PFOS PFOS 5.757 0 2761164 243.8076 00 PFOS 5.759 2787890 247.8607 0 .0 % 108.0% 0 .0 % 104.1% 0 .0 % 101.1% 0 .0 % 98.9% page 2 of 2 BACK TO MAIN Co S' s3' 3 C3D 5T C3OD2 T3 CD CO CD c-0n -oh -nI o CO Sam ple Batch R010402b.b, analyzed on Rush 04-02-01. PFOS Adsorb/D esorb sam ples. M atrix: Soil/SIg/Sed. S ta n d a rd c u rv e ran g e u sed fo r c a lib ra tio n o f s a m p le s : 10-1002 n g /m L (2.5 a n d 5 n g /m L s td n o t In c lu d e d due to th e h ig h e r sa m p le c o n c e n tra tio n ran g e ). Batch m ethod: R010402b.m te Batch 4/3/01 8:10 D:\Chem \Rush\R010402.b 4/3/01 8:24 D :\Chem \Rush\R010402 b 4/3/01 8:38 D:\Chem \Rush\R010402.b 4/3/01 8:53 D:\Chem \Rush\R010402.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:\Chem \Rush\R010402.b 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 \Rush\R010402.b 4/3/01 10:33 D :\Chem \Rush\R010402.b 4/3/01 10:48 D:\Chem \Rush\R010402.b 4/3/01 11:02 D :\Chem \Rush\R010402.b 4/3/01 22:19 D :\Chem \Rush\R010402.b 4/3/01 22:33 D:\Chem \Rush\R010402.b 4/3/01 22:47 D:\Chem\Rush\R010402. b 4/4/01 23:02 D:\Chem \Rush\R010402.b 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 D:\Chem \Rush\R010402.b 4/4/01 10:37 D :\Chem \Rush\R010402.b 4/4/01 10:51 D:\Chem \Rush\R010402.b 4/4/01 11:05 D:\Chem \Rush\R010402.b 4/4/01 11:20 D:\ChemVRush\R010402.b SampType SAMPLE CALIB 1 CALIB 2 CALIB 3 CALIB 4 SAMPLE CALIB 5 CALIB 6 CALIB 7 CALIB 8 SAMPLE CALIB 9 CALIB 10 SAMPLE CALIB 11 CALIB 12 CALIB 13 CALIB 14 SAMPLE CALIB 15 CALIB 16 CALIB 17 CALIB 18 SAMPLE CALIB 19 C A L IB R O R ie RUSH0104.D RUSH0105. D RUSH0106.D RUSH0107.D RUSH0108.D RUSH01O9.D RUSH0110.D RUSH0111.D RUSH0112.D RUSH0113.D RUSH0114.D RUSH0115.D RUSH0116.D RUSHQ163.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 Sam ple Name 0 ng/m L PFOS in MeOH 2.5 ng/m L PFOS in MeOH 5 ng/m L PFOS in MeOH 1 0 ng/m L PFOS in MeOH 25 ng/m L PFOS in MeOH 4 0 ng/mL PFOS in MeOH 50.1 ng/mL PFOS in MeOH 75.1 ng/m L PFOS in MeOH 100.2 ng/m L PFOS in MeOH 2 5 0 .5 ng/m L PFOS in MeOH 400.8 ng/m L PFOS in MeOH 501 ng/m L PFOS in MeOH 1002 ng/m L PFOS in MeOH O ng/m L PFO S in MeOH 2.5 ng/m L PFOS in MeOH 5 ng/m L PFOS in MeOH 1 0 ng/m L PFOS in MeOH 25 ng/m L PFOS in MeOH 4 0 ng/m L PFOS in MeOH 50.1 ng/m L PFOS in MeOH 75.1 ng/m L PFOS in MeOH 100.2 ng/m L PFOS in MeOH 2 5 0 .5 ng/m L PFOS in MeOH 400.8 ng/m L PFOS in MeOH 501 ng/m L PFOS in MeOH 1002 ng/m L PFOS in MeOH M ise In C om poun RT Area THPFOS 5.545 THPFOS 5 .5 4 6 THPFOS 5 .5 5 8 THPFOS 5 .5 5 3 THPFOS 5 .5 5 3 THPFOS 5 .5 4 3 THPFOS 5.553 THPFOS 5 .5 5 THPFOS 5.541 THPFOS 5 .5 4 4 THPFOS 5 .5 4 6 THPFOS 5 .5 4 THPFOS 5 .5 4 2 THPFOS 5 .5 3 7 THPFOS 5 .5 4 4 THPFOS 5 .5 4 8 THPFOS 5.551 THPFOS 5 .5 3 THPFOS 5.551 THPFOS 5.559 THPFOS 5.625 THPFOS 5.609 THPFOS 5 .5 9 9 THPFOS 5.595 THPFOS 5 .5 9 4 THPFOS 5 .5 9 3 Amount 691265 254 707691 254 726641 254 702679 254 711476 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 650311 254 717155 254 686050 254 714496 254 669513 254 683159 254 707430 254 Com poun RT Area A m ount PFOS 00 0 PFOS 5.756 192592 0 PFOS 5.768 249725 1.588495 PFOS 5.757 339511 7.167098 PFOS 5.756 641983 24.24615 PFOS 5.739 905841 41.026119 PFOS 5.749 1085138 51.837004 PFOS 5.753 1535613 78.469104 PFOS 5.744 1912604 102.76639 PFOS 5.747 4147316 2 4 6.4199 PFOS 5.749 5754500 391.55477 PFOS 5.743 6939227 488.84633 PFOS 5.745 12088828 974.5569 PFOS 00 0 PFOS 5.747 181340 0 PFOS 5.758 238783 2.406374 PFOS 5.754 311745 7.661761 PFOS 5.733 614103 26.666053 PFOS 5.747 872886 42.732009 PFOS 5.762 1054849 54.680469 PFOS 5.828 1572840 79.825492 PFOS 5.819 1906689 106.54576 PFOS 5.81 4102314 255.81083 PFOS 5.805 5711729 418.05636 PFOS 5.797 6776340 506.61571 PFOS 5.796 11937411 1028.811 31.8% 71.7% 97.0% 102.3% 103.5% 104.5% 102.6% 98.4% 97.6% 48.1% 76.6% 106.7% 106.6% 109.1% 106.3% 106.3% 102. 1% 101. 1% A veraae: 689821.2308 S td Dev: 34866.78097 896768 +30%: 482875 -30%: A O 0^ Page 1 of 3 BACK TO MAIN 3M Environmental Laboratory Sam ple B atch R010402b.b, analyzed on Rush 04-02-01. PFOS Adsorb/Desorb sam ples. M atrix: Soil/SIg/Sed. S ta n d a rd c u rv e ra n g e u se d fo r c a lib ra tio n o f sa m p le s : 10-1002 n g /m L (2.5 a n d 5 n g /m L s td n o t in c lu d e d d ue to th e h ig h e r s a m p le c o n c e n tra tio n range). Batch m ethod: R010402b.m Inj Date B a tch 4/3701 7:41 D:\Chem \Rush\R010402.b 4/3/01 7:55 D:\Chem \Rush\R010402.b 4/3/01 11:16 D :\C hem \R ush\R 010402b 4/3/01 11:31 D:\Chem \Rush\R010402.b 4/3/01 11:45 D:\Chem \Rush\R010402.b 4/3/01 14:52 D:\Chem \Rush\R010402.b 4/3/01 15:07 D:\Chem \Rush\R010402.b 4/3/01 18:14 D:\Chem \Rush\R010402.b 4/3/01 18:28 D:\Chem \Rush\R010402.b 4/3/01 21:35 D:\Chem \Rush\R010402.b 4/3/01 21:50 D:\Chem \Rush\R010402.b 4/3/01 22:04 D:\Chem \Rush\R010402.b 4/4/01 11:34 D:\Chem \Rush\R010402.b 4/4/01 11:49 D:\Chem \Rush\R010402.b SampType SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE F ile RUSH0102.D RUSH013.D RUSH0117.D RUSH0118.D RUSH0119.D RUSH0132.D RUSH0133.D RUSHQ146.D RUSH0147.D RUSH0160.D RUSH0161-D RUSH0162.D RUSH0176.D RUSH0177.D Sam ple 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 M ise In C om poun RT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS A re a 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Amount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Compoun RT A re a Amount PFOS 5.772 131207 PFOS 5.764 128138 PFOS 5.768 153626 PFOS 5.771 130584 PFOS 5.764 126241 PFOS 5.764 130330 PFOS 5.765 119643 PFOS 5.763 122906 PFOS 5.77 120557 PFOS 5.761 145239 PFOS 5.764 143817 PFOS 5.768 144439 PFOS 5.818 154900 PFOS 5.824 133822 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page 2 of 3 Page 578 of 703 BACK TO MAIN 3M Environmental Laboratory Sam ple Batch R010402b.b, analyzed on Rush 04-02-01. PFOS Adsorb/D esorb sam ples. M atrix: Soil/SIg/Sed. S ta n d a rd c u rv e ran g e u se d fo r c a lib ra tio n o f s a m p le s : 10-1002 n g /m L (2.5 a nd 5 n g /m L s td n o t in c lu d e d due to th e h ig h e r s a m p le c o n c e n tra tio n range). B atch m ethod: R010402b.m Inj Date Batch 4/3/01 11:59 D:\Chem \Rush\R010402.b 4/3/01 12:14 D:\Chem \Rush\R010402. b 4/3/01 12:28 D:\Chem \Rush\R010402.b 4/3/01 12:43 D:\Chem \Rush\R010402.b 4/3/01 12:57 D:\Chem \Rush\R010402.b 4/3/01 13:11 D:\Chem\Rush\RQ10402.b 4/3/01 13:26 D:\Chem\Rush\R010402. b 4/3/01 13:40 D:\Chem \Rush\R010402.b 4/3/01 13:55 D:\Chem \Rush\R010402.b 4/3/01 14:09 D :\Chem \Rush\R010402.b 4/3/01 14:23 D:\Chem \Rush\R010402.b 4/3/01 14:38 D :\Chem \Rush\R010402.b 4/3/01 15:21 D:\Chem \Rush\R010402.b 4/3/01 15:35 D:\Chem \Rush\R010402.b 4/3/01 15:50 D:\Chem \Rush\R010402.b 4/3/01 16:04 D:\Chem\RushVR010402.b 4/3/01 16:19 D:\Chem \Rush\R010402.b 4/3/01 16:33 D :\Chem \Rush\R010402.b 4/3/01 16:47 D:\Chem \Rush\R010402.b 4/3/01 17:02 D :\Chem \Rush\R010402.b 4/3/01 17:16 D:\Chem \Rush\R010402.b 4/3/01 17:31 D:\Chem \Rush\R010402.b 4/3/01 17:45 D:\Chem \Rush\R010402.b 4/3/01 17:59 D:\Chem \Rush\R010402.b 4/3/01 18:43 D:\Chem \Rush\R010402.b 4/3/01 18:57 D :\Chem \Rush\R010402.b 4/3/01 19:11 D:\Chem \Rush\R010402.b 4/3/01 1 9 2 6 D:\Chem \Rush\R010402.b 4/3/01 19:40 D:\Chem \Rush\R010402.b 4/3/01 19:55 D:\Chem \Rush\R010402.b 4/3/01 20:09 D:\Chem \Rush\R010402.b 4/3/01 20:23 D:\Chem \Rush\R010402.b 4/3/01 20:38 D:\Chem \Rush\R010402.b 4/3/01 20:52 D:\Chem\Rush\R010402. b 4/3/01 21:07 D:\Chem\RushVR010402.b 4/3/01 21:21 D:\Chem \Rush\R010402.b 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 RUSH0120.D RUSH0121.D RUSH0122.D RUSH0123.D RUSHQ124.D RUSH0125.D RUSH0126.D RUSH0127.D RUSH0128.D RUSH0129.D RUSH0130.D RUSHQ131.D RUSH0134.D RUSH0135.D RUSH0136.D RUSH0137.D RUSH0138.D RUSH0139.D RUSH0140.D RUSH0141.D RUSH0142.D RUSH0143.D RUSH0144.D RUSH0145.D RUSH0148.D RUSH0149.D RUSH0150.D RUSH0151.D RUSH0152.D RUSH0153.D RUSH0154.D RUSH0155.D RUSH0156.D RUSH0157.D RUSH0158.D RUSH0159.D Sam ple Name Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber E00-1311 5 ng/mL PFOS in MeOH 2 5 0 .5 ng/m L PFOS in MeOH Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study N um ber E00-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 5 ng/m L PFOS in MeOH 2 5 0 .5 ng/m L PFOS in MeOH Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber EOO-1311 Study Num ber E00-1311 Study Num ber EOO-1311 Study Num ber E00-1311 Study Num ber EOO-1311 Study Num ber E00-1311 Study Num ber EOO-1311 5 ng/m L PFOS in MeOH 2 5 0 .5 ng/mL PFOS in MeOH M ise In C o m p o u n RT Area THPFOS 5.554 THPFOS 5 .5 4 7 THPFOS 5.558 THPFOS 5 .5 5 THPFOS 5.558 THPFOS 5.554 THPFOS 5.552 THPFOS 5.546 THPFOS 5.553 THPFOS 5.552 THPFOS 5.549 THPFOS 5.54 THPFOS 5 .5 4 4 THPFOS 5 .5 4 7 THPFOS 5 .5 5 2 THPFOS 5 .5 6 THPFOS 5.54 THPFOS 5.548 THPFOS 5.554 THPFOS 5 .5 4 7 THPFOS 5.54 THPFOS 5.549 THPFOS 5.551 THPFOS 5 .5 5 3 THPFOS 5 .5 5 5 THPFOS 5 .5 4 THPFOS 5 .5 4 6 THPFOS 5 .5 4 THPFOS 5.544 THPFOS 5.534 THPFOS 5.539 THPFOS 5 .5 3 9 THPFOS 5 .5 5 THPFOS 5.543 THPFOS 5.55 THPFOS 5.554 Amount Com poun RT Area Amount 725886 254 PFOS 5.757 978597 42.932438 690051 254 PFOS 5.75 933343 43.120798 701604 254 PFOS 5.761 940734 42.621787 577118 254 PFOS 5.76 3533131 276.70087 667527 254 PFOS 5.754 2610383 160.75044 674789 254 PFOS 5.757 2478325 149.07008 668248 254 PFOS 5.755 2680467 165.7409 550211 254 PFOS 5.749 4917918 443.49026 652849 254 PFOS 5.749 5170053 380.66422 655706 254 PFOS 5.755 5129723 374.88948 680355 254 PFOS 5.759 253055 2.715008 693668 254 PFOS 5.751 4099082 264.97215 680330 254 PFOS 5.747 5372136 379.28766 570439 254 PFOS 5.75 7416165 721.85686 656434 254 PFOS 5.755 2754639 174.99347 674502 254 PFOS 5.763 2672733 163.32509 679000 254 PFOS 5.743 2840570 174.34555 660801 254 PFOS 5.751 5013884 360.82333 684382 254 PFOS 5.757 1412950 74.086291 688891 254 PFOS 5.75 1505023 7 9 446466 667236 254 PFOS 5.744 1329804 70.91215 669472 254 PFOS 5.752 3830875 254.76073 711232 254 PFOS 5.754 247651 1.768823 711428 254 PFOS 5.756 4044257 252.72329 918872 254 STD>130%PFOS 00 0 885106 254 PFOS 00 0 945311 254 STD>130%PFOS 00 0 703724 254 PFOS 5.743 2896965 170.99756 856144 254 PFOS 00 0 834838 254 PFOS 00 0 816843 254 PFOS 00 0 623341 254 PFOS 5.742 2925075 200 24318 851433 254 PFOS 00 0 837861 254 PFOS 00 0 641250 254 PFOS 5.753 234427 2.461139 631991 254 PFOS 5.757 3979419 286.41899 54.3% 105.8% 1588.9% 28.3% 35.4% 100.9% 49 2% 114.3% Page 3 of 3 P a g e 579 o f 7 0 3 BACK TO MAIN 3M Environmental Laboratory 03 r -o ' 0 S am ple B atch RQ10402a.bt analyzed o n R ush 04-02-01. PFOS A dsorb/D esorb s a m p le s. M atrix: S oil/S Ig/S ed. S ta n d a rd c u rv e ra n g e u se d fo r c a lib ra tio n o f s a m p le s : 5 -4002 n g /m L (2.5 n g /m L s td n o t in c lu d e d d u e to th e h ig h e r s a m p le c o n c e n tra tio n ra n g e ). B atch m eth o d : R010402a.m S tK 5 ( (S ~ (c \ In j Date 4/2/01 12:30 4/2/01 12:44 4/2/01 12:59 4/2/01 13:13 4/2/01 13:27 4/2/01 13:42 4/2/01 13:56 4/2/01 14:11 4/2/01 14:25 4/2/01 14:39 4/2/01 14:54 4/2/01 15:08 4/2/01 15:22 4/3/01 8:10 4/3/01 8:24 4/3/01 8:38 4/3/01 8:53 4/3/01 9:07 4/3/01 9:21 4/3/01 9:36 4/3/01 9:50 4/3/01 10:04 4/3/01 10:19 4/3/01 10:33 4/3/01 10:48 4/3/01 11:02 B a tc h D:\Chem \Rush\R010402.b D :\C h e rrA R u s h \R 0 1 0 4 0 2 .b D:\Chem \Rush\R010402.b D :\C hem \R ush\R 010402 .b D :\C hem \R ush\R 010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D :\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D :\C hem \R ush\R 010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D :\C hem \R ush\R 010402 .b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b D AChemVRu s h \R 0 10402 .b S am pType SAMPLE CALIB 1 CALIB 2 CALIB 3 CALIB 4 SAMPLE CALIB 5 CALIB 6 CALIB 7 CALIB 8 SAMPLE CALIB 9 C A LIB 10 SAMPLE C A LIB 11 C A LIB 12 C A LIB 13 C A LIB 14 SAMPLE C A LIB 15 C A LIB 16 C A LIB 17 CALIB 18 SAMPLE C A L IB J 9 CALIB_20 F ile RUSH0022.D RUSH0023.D R U S H 0 O 2 4 .D RUSH0025.D RUSH0026.D RUSH0027.D RUSH0028.D RUSH029.D RUSH0030.D RUSH0031.D RUSH0032.D RUSH0033.D RUSH0034.D RUSH01O4.D R U S H 1 0 5 .D RUSH0106.D RUSH0107.D RUSH0108.D RUSH0109.D RUSH0110.D RUSH0111.D RUSH0112.D RUSH0113.D RUSH0114.D RUSH0115.D RUSH0116.D S am ple Name 0 ng/m L PFO S in MeOH 2.5 ng/m L PFO S in MeOH 5 ng/m L PFO S in MeOH 1 0 ng/m L PFO S in MeOH 25 ng/m L PFO S in MeOH 4 0 ng/m L PFO S in MeOH 5 0 .1 ng/m L P F O S in M eOH 75.1 ng/m L P F O S in M eOH 100.2 ng/m L PFOS in MeOH 2 5 0 .5 ng/m L PFOS in MeOH 400.8 ng/m L PFOS in MeOH 501 ng/m L P F O S in MeOH 1002 ng/m L PFOS in MeOH O ng/m L PFO S in MeOH 2.5 ng/m L PFO S in MeOH 5 ng/m L PFO S in MeOH 1 0 ng/m L PFO S in MeOH 25 ng/m L PFO S in MeOH 4 0 ng/m L PFO S in MeOH 50 .1 ng/m L PFO S in M eOH 75.1 ng/m L PFO S in MeOH 100.2 ng/m L PFO S in MeOH 2 5 0 .5 ng/m L PFOS In MeOH 400.8 ng/m L PFOS in MeOH 501 ng/m L PFO S in MeOH 1002 ng/m L PFO S in M eOH M ise In fC o m p o u n c ftT 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 re a Am ount 5.549 673492 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 7 11160 254 5.564 714631 254 5.567 739760 254 5.545 691238 254 5.546 707818 254 5.558 726641 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 C om pouncR 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 re a Am ount 00 0 5.76 201953 1.38861 5.769 259654 3.944702 5.763 339488 8.769619 5.769 641564 25.343497 5.763 908997 40.988941 5.767 1106262 52.140717 5.768 1545079 77.738587 5.769 1912602 102.07183 5.77 4155372 250.46887 5.764 5885914 406.28894 5.774 6981587 505.86859 5.77 12248403 1 053.3589 00 0 5.756 193236 0.616118 5.768 249725 3.252923 5.757 339511 8.507324 5.756 641983 24.690572 5.739 905841 40.723752 5.749 1085138 51.118799 5.753 1535613 76.928129 5.744 1912604 100.70449 5.747 4147316 244.83253 5.749 5754500 394.96094 5.743 6939227 497.41946 5.745 12088828 1022.9766 78.9% 87.7% 101.4% 102.2% 104.1% 103.5% 101.9% 100.0 % 1 0 1 .0 % 65.1% 85.1% 98.8% 101.6 % 102.0 % 102.4% 100.5% 97.7% 99.3% Averaae: 709288.4 S td Dev: 17649.55 % R S D : 2.5% 922075 +30%: 496502 -30%: 03 a CT l\ 1 of 4 Page 580 of 703 BACK TO MAIN Co 31 S' =CD3 rQ)COr 2 & S am ple B a tch R010402a.b, analyzed on R ush 04-02-01. PFOS A dsorb/D esorb s a m p le s. M atrix: S oil/S Ig/S ed. S ta n d a rd c u rv e ra n g e u s e d fo r c a lib ra tio n o f s a m p le s : 5 -4 9 8 2 -n g /m L (2.5 n g /m L s td n o t In c lu d e d d u e to th e h ig h e r s a m p le c o n c e n tra tio n ra n g e ). B a tch m ethod: R010402a.m S O \ C tv y <. $ In j Date 4/2/01 12:01 B a tch D;1Ctoem\Rusb\R010402.b S am pType SAMPLE F ile RUSH0020.D S am ple Name TN-A 4B02 MeOH M ise InfC om pouncR T THPFOS Area 0 4/2/01 12:16 D :\C hem \R ush\R 010402 .b SAMPLE RUSH0O21.D T N -A 4 8 0 2 MeOH THPFOS 0 4/2/01 15:37 D :\C hem \R u sh \R 0 1 0 4 Q 2 .b SAMPLE RUSH0035.D TN -A 4802 MeOH THPFOS 0 4/2/01 15:51 D:\Chem \Rush\R010402.b SAMPLE RUSH0O36.D T N -A 4 8 0 2 M eOH THPFOS 0 4/2/01 18:15 D :\Chem \Rush\R010402.b SAMPLE RUSH0046.D TN -A 4802 MeOH THPFOS 0 4/2/01 18:29 D:\Chem \Rush\R010402.b SAMPLE RUSH0047.D TN -A 4802 MeOH THPFOS 0 4/2/01 21:36 D:\Chem \Rush\R010402.b SAMPLE RUSHD060.D T N -A 48 0 2 M eOH THPFOS 0 4/2/01 21:51 D:\C hem \R ush\R 010402.b SAMPLE RUSH0061.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 1:12 D:\C hem \R ush\R 010402.b SAMPLE RUSH075.D T N -A 4 8 0 2 M eOH THPFOS 0 4/3/01 4:19 D:\Chem \Rush\R010402.b SAMPLE RUSH0088.D TN -A 4802 MeOH THPFOS 0 4/3/01 4:34 D:\Chem \Rush\R010402.b SAMPLE RUSH0089.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 7:55 D:\Ch em\Rush'iR010402.b SAMPLE RUSH0103.D TN -A 4802 MeOH THPFOS 0 4/3/01 11:16 D :\C h e m \R u sh \R 0 10402.b SAMPLE RUSH0117.D TN -A 4802 MeOH THPFOS 0 4/3/01 11:31 D :\C h e m \R u sh \R 0 10402.b SAMPLE RUSHD118.D T N -A 48 0 2 M eOH THPFOS 0 4/3/01 11:45 D:\Chem \Rush\R010402.b SAMPLE RUSH0119.D TN -A 4802 MeOH THPFOS 0 Am ount 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 00 Com po un (FT PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS A re a Am ount 5.764 155059 5.771 133949 5.792 160821 5.78 138099 5.77 138330 5.761 134138 5.792 136128 5.771 130679 5.754 139503 5.754 127186 5.778 129477 5.774 128456 5.772 131523 5.764 125537 5.768 153626 5.771 130584 5.764 126241 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0T}J CQ CD cono o-osoi Page 2 of 4 BACK TO MAIN 3M Environmental Laboratory S am ple Batch R 010402a.b, analyzed on R ush 04-02-01. PFOS Adsorb/D esorb sam ples. M atrix: S oil/SIg/Sed. S ta n d a rd c u rv e ra n g e u s e d fo r c a lib ra tio n o f s a m p le s : S -W W ' n g /m L {2.5 n g /m L s td n o t in c lu d e d d u e to th e h ig h e r s a m p le c o n c e n tra tio n ra n g e ). B a tch m ethod: R010402a.m C i*C _ \ In j Date B a tc h S am pType F ile Sam ple Name M ise In fC o m p o u m ftT Area Am ount 4/2/01 16:06 D:\Chem \Rush\R010402.b SAMPLE RUSH0037.D Study N um ber E00-1311 THPFOS 556 720158 254 4/2/01 16:20 D:\Chem \Rush\R010402.b SAMPLE RUSH0038.D Study N um ber E00-1311 THPFOS 5.546 709660 254 4/2/01 16:34 D:\Chem \Rush\R010402.b SAMPLE RUSH0039.D Study N um ber EOO-1311 THPFOS 5.556 722650 254 4/2/01 16:49 D:\Chem \Rush\R010402.b SAMPLE RUSH0040.D Study N um ber EOO-1311 THPFOS 5.548 707567 254 4/2/01 17:03 D :\C hem \R ush\R 010402.b SAMPLE R U S H 0041D S tudy N u m b e r EOO-1311 THPFOS 5.548 713572 254 4/2/01 17:17 D:\Chem \Rush\R010402.b SAMPLE RUSH0042.D S tudy N u m b e r EOO-1311 THPFOS 5.546 724968 254 4/2/01 17:32 D:\Chem \Rush\R010402.b SAMPLE RUSH043.D Study N um ber EOO-1311 THPFOS 5.554 721402 254 4/2/01 17:46 D:\Chem \Rush\R010402.b SAMPLE RUSHD044.D 5 ng/m L PFO S in M eOH THPFOS 5.546 753692 254 4/2/01 18:01 D:\Chem \Rush\R010402.b SAMPLE RUSHD045.D 2 5 0 .5 ng /m L PFO S in M eOH THPFOS 5.551 746193 254 4/2/01 18:44 D:\Chem \Rush\R010402.b SAMPLE RUSH0048.D Study N um ber E00-1311 THPFOS 5.554 710136 254 4/2/01 18:58 D:\Chem \Rush\R010402.b SAMPLE RUSH0049.D Study N um ber EOO-1311 THPFOS 5.551 709407 254 4/2/01 19:13 D :\C h e m \R u sh \R Q 1 0 4 02.b SAMPLE RUSH0050.D S tudy N um ber EOO-1311 THPFOS 5.56 687539 254 4/2/01 19:27 4/2/01 19:41 D:\Chem \Rush\R010402.b D :\C hem \R ush\R 010402.b SAMPLE SAMPLE RUSH051.D RUSH0052.D S tudy N u m b e r EOO-1311 S tudy N u m b e r EOO-1311 THPFOS THPFOS 5.563 5.557 693912 573314 254 254 4/2/01 19:56 D:\Chem \Rush\R010402.b SAMPLE RUSH0053.D Study N um ber EOO-1311 THPFOS 5.558 689156 254 4/2/01 20:10 D:\Chem \Rush\R010402.b SAMPLE RUSH0054.D Study N u m b e r EOO-1311 THPFOS 5.555 698632 254 4/2/01 20:24 D:\Chem \Rush\R010402.b SAMPLE RUSH0055.D Study N um ber E00-1311 THPFOS 5.558 701032 254 4/2/01 20:39 D:\Chem \Rush\R010402.b SAMPLE RUSH0056.D S tudy N u m b e r EOO-1311 THPFOS 5.564 697975 254 4/2/01 20:53 D :\C hem \R ush\R 010402.b SAMPLE RUSH0057.D S tudy N um ber EOO-1311 THPFOS 5.566 722953 254 4/2/01 21:08 D :VChem\Rush\R010402.b SAMPLE RUSH0058.D 5 ng/m L PFO S in M eOH THPFOS 5.575 742816 254 4/2/01 21:22 D:\Chem \Rush\R010402.b SAMPLE RUSH0059.D 2 5 0 .5 ng/m L PFOS in MeOH THPFOS 5.56 738144 254 4/2/01 22:05 D:\Chem \Rush\R010402.b SAMPLE RUSH0062.D S tudy N u m b e r EOO-1311 THPFOS 5.561 724679 254 4/2/01 22:20 D:\Chem \Rush\R010402.b SAMPLE RUSH0063.D S tudy N um ber EOO-1311 THPFOS 5.56 732716 254 4/2/01 22:34 D:\Chem \Rush\R010402.b SAMPLE RUSH0064.D Study N u m b e r EOO-1311 THPFOS 5.551 709950 254 4/2/01 22:48 D :\C h e m \R u sh V R 0 1 0 4 0 2 .b SAMPLE RUSH0065.D Study N um ber E00-1311 THPFOS 5.541 717003 254 4/3/01 23:03 D:\Chem \Rush\R010402.b SAMPLE RUSH0066.D S tudy N um ber E 00-1311 THPFOS 5.546 703450 254 4/3/01 23:17 D:\Chem \Rush\R010402.b SAMPLE RUSH0067.D S tudy N u m b e r E 00-1311 THPFOS 5.541 699666 254 4/3/01 23:31 D:\Chem \Rush\R010402.b SAMPLE RUSH0068.D S tudy N u m b e r EOO-1311 THPFOS 5.533 585285 254 4/3/01 23:46 D:\Chem \Rush\R010402-b SAMPLE RUSH0069.D Study N u m b e r E 00-1311 THPFOS 5.539 675221 254 4/3/01 0:00 4/3/01 0:15 D:\Chem \Rush\R010402.b D :\C hem \R u s h ^ 0 1 D402.b SAMPLE SAMPLE RUSH0070.D RUSH0071.D S tudy N u m b e r E 00-1311 S tudy N u m b e r E 0 0 -1 311 THPFOS THPFOS 5.532 5.533 679762 576140 254 254 4/3/01 0:29 4/3/01 0:43 D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b SAMPLE SAMPLE RUSH072.D RUSH0073.D 5 ng/m L PFOS in MeOH 2 5 0 .5 ng/m L PFOS in M eOH THPFOS THPFOS 5.535 5.543 704091 709848 254 254 C om pouncR T Area Am ount PFOS 5.764 1429691 69.243301 PFOS 5.749 1319817 63.879261 PFOS 5.759 1351379 64.31529 PFOS 5.751 3 8 35296 2 3 6 .7 3 6 1 7 PFOS 5.758 6391949 450.7897 PFOS 5.756 4812925 305.70323 PFOS 5.757 5198125 339.49098 PFOS 5.756 266077 3.60348 PFOS 5.754 4140558 243.77425 PFOS 5.757 7163224 528.02219 PFOS 5.761 2 1 97087 1 1 9 .0 9 9 3 8 PFOS 5.77 928960 42.675468 PFOS 5.766 697046 28.725867 PFOS 5.76 3034950 229.85155 PFOS 5.768 2174774 121.84417 PFOS 5.765 2284600 127.2331 PFOS 5.761 2386809 133.63027 PFOS 5.767 4749637 315.49117 PFOS 5.769 1411113 67.811262 PFOS 5.792 262089 3.595994 PFOS 5.77 4133826 246.60414 PFOS 5.764 1328107 62.727361 PFOS 5.763 1708104 84.309464 PFOS 5.747 4317226 273.50922 PFOS 00 0 PFOS 00 0 PFOS 00 0 PFOS 5.736 2892741 211.04908 PFOS 5.742 643295 26.676048 PFOS 5.735 647862 26.69003 PFOS 5.736 3230023 246.93617 PFOS 5.745 259698 4.196199 PFOS 5.739 4132026 258.85952 72.1% 97.3% 71.9% 98.4% 83.9% 103.3% Page 3 of 4 Page 582 of 703 BACK TO MAIN 3M Environmental Laboratory S am ple B atch R010402a.b, analyzed on R ush 04-02-01. PFOS A dsorb/D esorb sa m p le s. M a trix: Soil/S lg/S ed. S ta n d a rd c u rv e ra n g e u s e d fo r c a lib ra tio n o f s a m p le s : 5-1002-n g /q iL (2.5 n g /m L s td n o t in c lu d e d d u e to th e h ig h e r s a m p le c o n c e n tra tio n ra n g e ). B a tch m ethod: R010402a.m 5&\ /jfY 7 4/3/01 1:27 D :\C h e m \R u sh \R 0 10402 .b SAMPLE RUSH0076.D S tudy N u m b e r EOO-1311 THPFOS 5.565 700501 4/3/01 1 :41 D:\Chem \Rush\R010402.b SAMPLE RUSH0077.D Study N u m b e r EOO-1311 THPFOS 5.552 679568 4/3/01 1:55 D :\Chem \Rush\R010402.b SAMPLE RUSH0078.D Study N um ber E00-1311 THPFOS 5.56 670067 4/3/01 2:10 D :\C hem \R ush\R 0i0402.b SAMPLE RUSH0079.D S tudy N u m b e r E 00-1311 THPFOS 5.544 568572 4/3/01 2:24 D:\Chem \Rush\R010402.b SAMPLE RUSH0080.D S tudy N u m b e r EOO-1311 THPFOS 5.54 650461 4/3/01 2:38 D:\Chem \Rush\R010402.b SAMPLE RUSH0081.D S tudy N u m b e r EOO-1311 THPFOS 5.533 638505 4/3/01 2 :5 3 D:\Chem \Rush\R010402.b SAMPLE RUSH0082.D Study N u m b e r EOO-1311 THPFOS 5.539 648526 4/3/01 3:07 D :\Chem \Rush\R010402.b SAMPLE RUSH0083.D S tudy N u m b e r EOO-1311 THPFOS 5.534 560495 4/3/01 3:22 D :\C hem \R ush\R 010402 .b SAMPLE RUSH0084.D S tudy N u m b e r EOO-1311 THPFOS 5.54 660562 4/3/01 3:36 D :\C h e m \R u sh \R 0 10402 .b SAMPLE RUSH0085.D Study N u m b e r EOO-1311 THPFOS 5.531 672433 4/3/01 3:50 D :\C h e m \R u sh \R 0 10402.b SAMPLE RUSH0086.D 5 ng/m L P F O S in M eOH THPFOS 5.543 700545 4/3/01 4:05 D :\Chem \Rush\R010402.b SAMPLE RUSH0087.D 2 5 0 .5 ng/m L PFOS in MeOH THPFOS 5.554 709410 4/3/01 5:02 4/3/01 5:17 D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b SAMPLE SAMPLE RUSH0091.D RUSH0092.D S tudy N u m b e r EOO-1311 S tudy N u m b e r EOO-1311 THPFOS THPFOS 5.551 5.546 669389 683096 4/3/01 5:31 D:\Chem \Rush\R010402.b SAMPLE RUSH0093.D S tudy N u m b e r EOO-1311 THPFOS 5.543 683769 4/3/01 5:45 4/3/01 6:00 D:\Chem \Rush\R010402.b D:\Chem \Rush\R010402.b SAMPLE SAMPLE RUSH0094.D RUSH0095.D Study N u m b e r EOO-1311 S tudy N u m b e r EOO-1311 THPFOS THPFOS 5.54 5.553 702574 672540 4/3/01 6:14 D:\Chem \Rush\R010402.b SAMPLE RUSH0096.D S tudy N u m b e r EOO-1311 THPFOS 5.544 690375 4/3/01 6:29 D :\C h e m \R u sh \R 0 1 0 4 0 2 .b SAMPLE RUSH0097.D Study N um ber E00-1311 THPFOS 5.544 677814 4/3/01 6:43 D:\Chem \Rush\R010402.b SAMPLE RUSH0098.D S tudy N u m b e r E 00-1311 THPFOS 5.544 674569 4/3/01 6:57 D:\Chem \Rush\R010402.b SAMPLE RUSH0099.D S tudy N u m b e r E 00-1311 THPFOS 5.539 565914 4/3/01 7:12 D:\Chem \Rush\R010402.b SAMPLE RUSH0100.D 5 ng/m L PFO S in MeOH THPFOS 5.545 710818 4/3/01 7:26 D :\Chem \Rush\R010402.b SAMPLE RUSH0101.D 2 5 0 .5 ng/m L PFOS in MeOH THPFOS 5.547 699529 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 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 1BBB695 4300957 4141363 3611282 3972287 6061330 1849680 2010670 254899 4162725 4302522 6535234 6711588 6936083 8479425 0 0 0 2730205 259422 4064532 107.11332 111.28782 106.22388 361.44666 289.87301 249.67287 276.01481 580.02025 105.37736 114.12314 4.00928 261.48317 293.38551 491.9271 509.06131 513.00765 715.92273 0 0 0 204 82416 4.0507 258.26619 80.2% 104.4% 81.0% 103.1% Page 4 of 4 Page 583 of 703 3M Environmental Laboratory E00-1311 PFOS Ads/Des BACK TO MAIN Sam ple Batch R010314.b, analyzed on H illary 03-14-01. PFOS Adsorto/Desorb sam ples. M atrix: S e d im e n t - t, vl '.'X J . >~> f l1 D S ta n d a rd c u rv e ran g e u se d fo r c a lib ra tio n o f sa m p le s: 2.5-250.5 n g /m L (400.8 a n d 501 n g /m L s td n o t in c lu d e d d u e to th e lo w e r s a m p le c o n c e n tra tio n ra n g e ). Batch m ethod: R010314t.m Inj Date 3/14/01 21:05 3/14/01 21:19 3/14/01 21:33 3/14/01 21:48 3/14/01 22:02 3/14/01 22:16 3/14/01 22:31 3/14/01 22:45 3/14/01 23:00 3/14/01 23:14 3/14/01 23:28 3/14/01 23:43 3/15/01 2:49 3/15/01 3:03 3/15/01 6:10 3/15/01 6:24 3/15/01 9:31 3/15/01 9:45 3/15/01 12:52 3/15/01 13:06 3/15/01 13:50 3/15/01 14:04 3/15/01 14:18 3/15/01 14:33 3/15/01 14:47 3/15/01 15:01 3/15/01 15:16 3/15/01 15:30 3/15/01 15:44 3/15/01 15:59 3/15/01 16:13 3/15/01 16:28 B a tch D:\chem\Rush. i\R010314.b D:\chem\Rush. i\R010314.b D:\chem \Rush.ftR010314.b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D:\chem\Rush. i\R010314.b D :\chem \R ush.i\R 010314 .b D :V ch e m \R u s h .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D:\chem \Rush.i\R010314.b D:\chem \Rush.i\R010314.b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \Rush.i\R010314.b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b SampType SAMPLE C A L IB _ 1 CALIB_2 CALIB_3 CALIB_4 CALIB_5 CALIB_6 CALIB_7 CALIB_8 CAL!B_9 C ALIB_t0 SAMPLE C C A L IB _ 1 CCAL1B_1 C C A L IB _ 1 C C A L IB _ 1 C C A L IB _ 1 CCALIB_1 CCALIB_1 CCALIB_1 SAMPLE CALIB_11 CALIB_12 CALIB_13 CALIB_14 CALIB_15 C A LIB J6 C A LIB J7 CALIB_18 CALIB_19 CALIB_20 SAMPLE F ile RUSH0017.D RUSH0018.D RUSH0019.D RUSH0020.D RUSH0021.D RUSH0022.D RUSH0023.D RUSH0024.D RUSHOQ25.D RUSHOQ26.D RUSH0027.D RUSH0028.D RUSH0041.D RUSH0042.D RUSH0055.D RUSH0056.D RUSHOQ69.D RUSH0070.D RUSH0083.D RUSH0084.D RUSH00&7.D RUSH0088.D RUSH0089.D RUSH0090.D RUSH0091.D RUSH0092.D RUSH0093.D RUSH0094.D RUSH0095.D RUSH0096.D RUSH0097.D RUSH0098.D Sam ple Name 01003-07-01 01003-07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-03 01003-07-10 01003-07-01 01003-07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 M ise Info Com pound Name 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 5.48 5 .4 7 5.46 5 .4 5 5.46 5.46 5 .4 6 5.47 5 .4 7 5.46 5.46 5.46 5 .4 7 5 .4 7 5 .4 7 5.48 5.47 5.46 5 .4 7 5.46 5 .4 7 5 .4 7 5.46 5.47 5 .4 7 5 .4 7 5.46 5.46 5.46 5.46 5 .4 6 5 .4 7 Area 1009005 1002399 1006538 1013743 1002095 1014289 998269 1016405 1001184 1022553 1019780 1018171 1050373 1036120 1050495 1042671 1051910 1047495 1051525 1042848 1053861 1050989 1056424 1041839 1040134 1051034 1043368 1052178 1038121 1028679 1035833 1034919 Average: 1032038.969 Std Dev: 18725 % RSD: 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 Com pound 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 RT 0 .0 0 5 .6 8 5 .6 8 5 .6 7 5.67 5 .6 8 5 .6 8 5 .6 8 5 .6 9 5 .6 8 5.67 5.68 5.69 5.69 5 .6 9 5 .6 9 5 .6 9 5 .6 8 5.69 5 .6 8 0.00 5.69 568 5 .6 9 5 .6 9 5.68 5 .6 8 5.68 5 .6 8 5 .6 8 5 .6 8 5 .6 8 A re a 0 129429 209405 338471 783497 1209876 1458055 2128988 2648411 5889029 8711721 10307257 194784 5934195 196061 5889851 188546 5823836 187794 5774991 0 121720 183452 317434 756712 1162752 1426057 2Q81314 2616038 5630191 8331328 9922517 Amount 0.0 2.7 5.5 9.9 26.3 41.9 52.5 78.5 102.3 257.9 427.4 536.5 4.7 256.1 4.7 251.8 4.5 246.9 4.4 245.7 0.0 2.2 4.3 8.9 24.3 38.6 48.7 73.6 96.7 242.1 394 9 498.5 QC IS range (*/- 30% average): +30%. 1341651 -30%: 722427 %Dev 108.0% 109.3% 99.3% 105.1% 104.8% 104.7% 104.3% 102. 1% 103.0% XX XX 93.4% 102.3% 94.3% 100.5% 09.1% 98.6% 8 8 .6 % 98.1% 89.4% 85.2% 88.9% 97.0% 96.5% 97.3% 97.8% 96.6% 96.7% XX XX Page 584 of 703 Page 1 of 3 BACK TO MAIN EOO-1311 PFOS Ads/Des 3M Environmental Laboratory Sam ple Batch R010314.b, analyzed on H illary 03-14-01. PFOS Adsorb/D esorb sam ples. M atrix: S ed im e n t S ta n d a rd c u rv e ra n g e u se d fo r c a lib ra tio n o f sa m p le s: 2.5-250.5 n g /m L (400.8 a n d 501 n g /m L Std n o t in c lu d e d due to th e lo w e r s a m p le c o n c e n tra tio n range). B atch m ethod: RO10314Lm Inj Date B a tch SampType File Sam ple Name M ise Info Com pound Name RT Area 3/15/01 0:26 3/15/01 0:40 3/15/01 0:54 3/15/01 1:09 3/15/01 1:23 3/15/01 1:37 3/15/01 1:52 3/15/01 2:06 3/15/01 2:20 3/15/01 2:35 3/15/01 3:47 3/15/01 4:01 3/15/01 4:15 3/15/01 4:30 3/15/01 4:44 3/15/01 4:58 3/15/01 5:13 3/15/01 5:27 3/15/01 5:41 3/15/01 5:56 3/15/01 7;07 3/15/01 7:22 3/15/01 7:36 3/15/01 7:50 3/15/01 8:05 3/15/01 8:19 3/15/01 8:34 3/15/01 8:48 3/15/01 9:02 3/15/01 9:17 3/15/01 10:29 3/15/01 10:43 3/15/01 10:57 3/15/01 11:12 3/15/01 11:26 3/15/01 11:40 3/15/01 11:55 3/15/01 12:09 3/15/01 12:23 3/15/01 12:38 D:\chem\Rush i\R010314 b D :\chem \R ush.i\R 010314 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D:\chem\Rush. i\R010314.b D :\chem \R ush.i\R 010314 .b D :1 ch e m \R u sh .A R 0 1 0 3 1 4 .b D :\ch e m V R u s h .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.t\R 010314 b D:1chem\Rush.i\R010314. b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b PiVchemWueh. i\ft010314.fe D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b D :\chem \R ush.i\R 010314 .b D :\chem \Rush.i\R010314b D :\chem \R ush.i\R 010314 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D:\chem\Rush. i\R010314.b D :\chem \R ush.i\R 010314 .b D: \chem\Rush. i\R010314. b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D:\chem\Rush. i\R010314.b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\chem \R ush.i\R 010314 .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 RUSH0031.D RUSH0032.D RUSH033.D RUSH0034.D RUSH0035.D RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039 D RUSH0040.D RUSH0045.D RUSH0046.D RUSH0047.D RUSH0048.D RUSH0049.D RUSH0050.D RUSH0051.D R U S H 0052. D RUSH0053 D RUSHQ054.D RUSH0069iP RUSH0060.D RUSH0061.D RUSH0062.D RUSH0063.D RUSH0064.D RUSH0065.D RUSH0066.D RUSH0067.D RUSH006B D RUSH0073.D RUSH0074.D RUSH0075.D RUSH0076.D RUSH0077.D RUSH0078 D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0082.D 1311-4121-S1 1311-4122-S1 1311-4123-S1 1311-4123MS-S1 1311-4124-S1 1311-4125-S1 1311-4126-S1 1311-4126MS-S1 1 3 1 1 --4 1 27 -S 1 1311-4128-SI 1311-4129-S1 1 3 1 1-4129MS-S1 1311-4130-S1 1311-4131-S1 1 3 1 1-4132-S1 1 3 1 1-4132MS-S1 1311-4133-S1 1311-4134-S1 1311-4135-S1 1311-4135MS-S1 4311-4136-S1 1311-4137-S1 1311-4138-SI 1311-4138MS-S1 1311-4139-S1 1311-4140-S1 1311-4141-S1 1 3 1 1-4141MS-S1 1311-4142-S1 1311-4143-S1 1311-4144-S1 1311-4144MS-S1 1 3 1 1-4145-S1 1311-4146-SI 1311-4147-SI 1311-4147MS-S1 1311-4148-S1 1 3 1 1-4149-S1 1311-4150-S1 1311-4150MS-S1 - 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 .4 7 5 .4 7 5 .4 7 5 .4 7 5 .4 8 5 .4 8 5 .4 6 5 .4 8 5 .4 8 5 .4 8 5 .4 8 5.48 5 .4 8 5 .4 9 5 .4 8 5.49 5.48 5.51 5 .4 8 5 .4 8 040 5 .4 8 5 .4 7 5.47 5 .4 7 5 .4 7 5 .4 8 5,47 5 .4 8 5.47 5 .4 8 5.46 5 .4 7 5 .4 6 5 .4 7 5.46 5.47 5 .4 7 5 ,4 7 5 .4 7 1425324 1078944 1090803 931360 1093465 1057249 1038845 903745 1084923 1074853 1660202 947684 1095965 1091572 1101888 919194 1073078 1081264 1077793 921307 O 1099389 1083504 947454 1086262 1087521 1075484 915669 1079679 1108514 1091080 895662 1070260 1090781 1088406 898964 1055605 1052012 1055409 887792 Average: 1062023 Std Dev: 137692 % RSD: 13.0% Am ount Com pound Name RT Area A m ount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 0 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 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 0.00 0.00 0.00 5 .6 8 0 .0 0 0 .0 0 0.00 5.69 5.69 5.69 5.70 5.69 5 .6 9 5 .7 0 5 .6 9 5.71 5 .6 9 5 .7 3 5 .6 9 5.70 5.69 5 .6 9 5.69 5.69 5.69 5 .6 9 5 .6 8 5 .7 0 5 .6 9 5.70 5 .6 9 5 .6 9 5.68 5 .6 9 5 .6 8 5 .6 8 5 .6 8 5 .6 9 5 .6 9 0 0 0 4322756 0 0 0 4220111 1155260 4106846 1343718 5004132 799984 725496 822873 4874564 729534 759438 769202 4762247 23881 757619 757822 4939810 684895 677314 687097 4776931 673507 716747 688862 4609795 640428 644391 636594 4605162 649889 645335 651186 4565770 0.0 0.0 0.0 197.9 0.0 0.0 0.0 199.4 37.0 156.8 27.3 231.6 24.3 21.9 25.0 232.9 22.5 23.3 23.7 225.7 &0 22.8 23.2 228.1 20.7 20.4 21.0 228.2 20.4 21.3 20.7 224.5 19.5 19.2 19.0 223.2 20.1 20.0 20.2 224.3 Page 585 of 703 Page 2 of 3 E 0-3H PFOS AtJs/Des BACK TO MAIN 3M Environmental Laboratory Sam ple Batch R010314-b, analyzed on H illary 03-14-01. PFOS Adsorb/Desorb sam ples. M atrix: S edim ent S ta n d a rd c u rv e ra n g e u se d f o r c a lib ra tio n o f sa m p le s : 2.5-250.5 n g /m L (400.8 a n d 501 n g /m L s td n o t in c lu d e d d ue to th e lo w e r sa m p le c o n c e n tra tio n range). B atch m ethod: R010314t.m In] Date B a tch SampType File Sam ple Name M ise Info Com pound Name RT Area 3/14/01 20:36 3/14/01 20:50 3/14/01 23:57 3/15/01 0:11 3/15/01 3:18 3/15/01 3:32 3/15/01 6:39 3/15/01 6:53 3/15/01 10:00 3/15/01 10:14 3/15/01 13:21 3/15/01 13:35 3/15/01 16:43 3/15/01 16:57 D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D :V ch e m \R u sh .i\R 0 1 0 3 1 4 .b D:\chem \Rush.i\R010314.b D:\chem \Rush.i\R010314.b D :\ch e m \R u sh .i\R 0 1 0 3 1 4 .b D:\chem\Rush. i\R010314.b D :\chem \R ush.i\R 010314 .b D:\chem \Rush.i\R010314.b D:\chem \Rush.i\R0l0314.b D :\chem \R ush.i\R 010314.b . D:\chem\Rush.i\R010314.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0015.D RUSH0016.D RUSH0029.D RUSH0030.D RUSH0O43.D RUSH0044.D RUSH0057.D RUSH0058.D RUSH0071.D RUSH0072.D RUSH008S.D RUSH0086.D RUSH0099.D RUSH010Q.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 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS. 0.00 0 .0 0 0.00 0.00 0.00 0 .0 0 0 .0 0 0 .0 0 0.00 0.00 0 .0 0 0.00 0.00 0.00 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Am ount Com pound Name RT A re a 0 PFOS 5.70 40923 0 PFOS 5.63 29136 0 PFOS 5.69 40534 0 PFOS 5.63 30463 0 PFOS 5.64 33501 0 PFOS 5.64 26360 0 PFOS 5.69 57454 0 PFOS 5.70 51654 0 PFOS 5.69 57753 0 PFOS 5.68 53172 0 PFOS 5.68 57830 0 PFOS 5.70 45965 0 PFOS 5.68 56083 0 PFOS 5.68 47554 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 Q.O 0.0 Page 586 of 703 Page 3 of 3 BACK TO MAIN 3M Environmental Laboratory S a m p le B a tc h R010309.b, a nalyzed on R ush 03-09-01. PFOSA d s o rb /D e s o rb sa m p le s . M atrix: C n trl and S o ils 1,2, & 3. S ta n d a rd c u rv e ran g e u se d fo r ca lib ra tio n o f sa m p le s : 10-501 n g /m L (2.5, a nd 5 n g /m L s td n o t in c lu d e d d ue to th e h ig h e r s a m p le c o n c e n tra tio n range). Batch m ethod: R010314Lm Inj Date B a tch 3/9/01 20:26 D:\chem \Rush.i\R010309.b 3/9/01 20:37 D:\chem \Rush.i\R010309.b 3/9/01 2 0 4 8 p:\chem \R ush.i\R 010309.b 3/9/01 21: OU U:\chem\Rush.i\R0103Q9.b 3/9/01 21:11 D :\chem \Rush.i\R010309.b 3/9/01 21:22 D:\chem \Rush.i\R010309.b 3/9/01 21:33 D:\chem \Rush.i\R010309.b 3/9/01 21:44 D:\chemVRush.iVR010309.b 3/9/01 21:56 D:\chem \Rush.i\R010309.b 3/9/01 22:07 D:\chem \R ush.i\R 0103O9.b 3/9/01 22:18 D:\chem \Rush.i\R010309.b 3/9/01 22:29 D :\chem \Rush i\R010309 b 3/10/01 0:54 D:\chem\Rush.i\RQ10309.b 3/10/01 1:06 D:\chem \R ush.i\R 010309.b 3/10/01 3:31 D :\chem \Rush.i\R010309.b 3/10/01 3:42 D:\chem \Rush.i\R010309.b 3/10/01 6:07 D:\chem \Rush.i\R010309.b 3/10/01 6:19 D.\chem \Rush.i\R010309.b 3/10/01 8:44 D :\chem \Rush.i\R010309.b 3/10/01 8:55 D:\chem\Rush.i\RQ10309. b 3/10/01 11:21 D:\chem \Rush.i\R010309.b 3/10/01 11:32 D:\chem \R ush.i\R 010309.b 3/10/01 13:58 D :\chem \Rush.i\R010309.b 3/10/01 14:09 D:\chem \Rush.i\R010309.b 3/10/01 16:34 D:\chem \Rush.i\R010309.b 3/10/Q1 16:46 D:\chem \Rush.i\R010309.b 3/10/01 18:38 D:\chem\Rush.i\R01Q309.b 3/10/01 18.49 D:\chem \R ush.i\R 010309.b 3/10/01 19:22 D :\chem \Rush.i\R010309.b 3/10/01 19:33 D:\chem \Rush.i\R010309 b 3/10/01 19:45 D:\chem \Rush.i\R010309.b 3/10/01 19:56 D:\chem \Rush. i\R 010309. b 3/10/01 20:07 D:\chem\Rush.i\R010309.b 3/10/01 20:18 D:\chem\Rush. i\R010309. b 3/10/01 20:29 D:\chem\Rush.i\R010309.b 3/10/01 20:40 D:\chem\Rush.i\R010309.b 3/10/01 20:52 D:\chem\Rush. i\R010309 b 3/10/01 21:03 D:\chem\Rush.i\R010309.b 3/10/01 21:14 D:\cfiem \Rush.i\R010309 b 3/10/01 21:25 D:\chem\Rush.i\R010309.b SampType SAMPLE SAMPLE CAL! EM C A L IB _ 2 C A L IB _ 3 CALIB_4 CALIB_5 CALIB_6 C A L IB _ 7 CAL!B_8 CALIB_9 C A LIB J0 CCALIB_1 CCALIB_1 CCALIB_1 C C ALIBJ C C ALIBJ C C ALIBJ C C ALIBJ CCALIB_1 C C ALIBJ C C ALIBJ C C ALIBJ C C ALIBJ C C ALIBJ C C ALIBJ C C ALIBJ C C ALIBJ SAMPLE SAMPLE CAL1BJ1 C A LIB J2 C A LIB J3 C ALIBJ4 C ALIBJ5 C ALIBJ6 C A LIB J7 CAL IBJ 8 C ALIBJ9 CALIB_20 File Sam ple Name RUSH0022.D 01003-07-01 RUSH0023.D 01003-07-02 RUSH0024.D 01003-07-03 RUSH0025.D 01003-07-04 RUSH0026.D 01003-07-05 RUSH0027.D 01003-07-06 RUSHOO20.D 01003-07-07 RUSH0029.D 01003-07-08 RUSH0030.D 01003-07-09 RUSH0Q31.D 0 1 003-07-1Q RUSH0032.D 01003-07-11 RUSH0033.D 01003-07-12 RUSH0046.D 5 ng/m L PFOS RUSH0047.D 250.5 ng/m L PFOS RUSH0060.D 01003-07-03 RUSH0061.D RUSH0074.D 01003-07-10 01003-07-03 RUSH0075.D 01003-07-10 RUSH0088.D 01003-07-03 RUSH0089.D RUSH0102.D 01003-07-10 01003-07-03 RUSH0103.D 01003-07-10 RUSH0116.D 01003-07-03 RUSH0117.D 01003-07-10 RUSH013O.D 01003-07-03 RUSH0131.D 01003-07-10 RUSH0141.D 01003-07-03 RUSH0142.D 01003-07-10 RUSH0145.D 01003-07-01 RUSH0146.D 01003-07-02 RUSH0147.D 01003-07-03 RUSH0148.D 01003-07-04 RUSH0149.D 01003-07-05 RUSH0150.D 01003-07-06 RUSH0151.D 01003-07-07 RUSH0152.D 1003-07-08 RUSH0153.D 01003-07-09 RUSH0154.D 01003-07-10 RUSH0155.D 01003-07-11 RUSH0156.D 01003-07-12 M ise Info 2.5 ng/mL PFOS 5.0 ng/mL PFOS 10 ng/mL PFOS 25 ng/ML PFOS 40 ng/mL PFOS 50 ng/mL PFOS 75.1 ng/mL PFOS 100.2 ng/mL PFOS 250.5 ng/mL PFOS 400.8 ng/mL PFOS 501 ng/mL PFOS 2.5 ng/mL PFOS 5.0 ng/mL PFOS 10 ng/m L PFOS 25 ng/ML PFOS 40 ng/mL PFOS 50 ng/mL PFOS 75.1 ng/m L PFOS 100.2 ng/mL PFOS 250.5 ng/mL PFOS 400.8 ng/mL PFOS 501 ng/m L PFOS om pound Name RT THPFOS 5.571 THPFOS THPFOS 5 .5 6 9 5 .5 6 6 THPFOS 5 .5 7 9 THPFOS 5 .5 7 9 THPFOS 5.577 THPFOS 5.566 THPFOS 5.572 THPFOS 5.563 THPFOS 5.557 THPFOS 5.553 THPFOS 5.566 THPFOS 5.55 THPFOS 5.55 THPFOS THPFOS 5.538 5.547 THPFOS 5.536 THPFOS 5 .5 4 8 THPFOS 5 .5 3 9 THPFOS THPFOS 5.543 5 .5 6 5 THPFOS 5 .5 5 2 THPFOS 5 .5 4 6 THPFOS 5 .5 4 4 THPFOS 5.54 THPFOS 5.53 THPFOS 5 .5 3 7 THPFOS 5.543 THPFOS 5.547 THPFOS 5.551 THPFOS 5.53 THPFOS 5.54 THPFOS 5 .5 3 THPFOS 5.543 THPFOS 5.537 THPFOS 5.543 THPFOS 5 .5 4 7 THPFOS 5 .5 5 THPFOS 5.54 THPFOS 5.543 Area 1468051 1464363 1466531 1454968 1451878 1446455 1446507 1431459 1426618 1421352 1446399 1409274 1275681 1266963 1199867 1189673 1186907 1174775 1189770 1195540 1228262 1192842 1191068 1162130 1174278 1176312 1186818 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 om pound Name RT PFOS 5.711 PFOS 5 .7 7 9 PFOS 5.783 PFOS 5.789 PFOS 5.796 PFOS 5.794 PFOS 5.783 PFOS 5.782 PFOS 5.773 PFOS 5.767 PFOS 5.764 PFOS 5.776 PFOS 5 .7 6 PFOS 5.76 PFOS 5.748 PFOS 5.764 PFOS 5 .7 5 3 PFOS 5.758 PFOS 5.756 PFOS 5 .7 6 PFOS PFOS 5 .7 7 5 5.769 PFOS 5.763 PFOS 5.761 PFOS 5.757 PFOS PFOS 5 .7 4 5 .7 4 7 PFOS 5.753 PFOS 5 .6 8 7 PFOS 5.761 PFOS 5 .7 4 7 PFOS PFOS PFOS 5.757 5 .7 4 7 5.76 PFOS 5.755 PFOS 5.753 PFOS 5.757 PFOS 5.767 PFOS 5.75 PFOS 5.753 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 A m ount 9.0 6.6 2.9 7.6 23.6 38.3 48.6 73.0 96.3 236.5 375.1 471.6 3.4 254.4 3.6 269.2 3.7 269.1 3.7 273.7 3.7 271.1 3.9 270.7 3.6 269.0 3.8 270.1 10.2 8.1 3.7 9.0 264 43.6 54.1 82.0 107.5 265.3 419.8 527.1 X 76% 94% 96% 97% 97% 96% 94% 94% 94% below LOQ 102% below LOQ 107% below LOQ 107% below LOQ 109% below LOQ 108% below LOQ 107% X 90% 105% 109% 108% 109% 107% 106% 105% 105% Page 1 of 4 (yrf- P j J 4 Page 587 of 703 3M Environmental Laboratory 3/9/01 23:03 D:\chem \R ush.i\R 010309 b 3/9/01 23:14 D:\chem \R ush.i\R 010309.b 3/9/01 23:25 D:\chem \R ush.i\R 010309.b 3/9/01 23:36 D:\chem\Rush. i\R 010309.b 3/9/01 23:47 D :\chem \Rush-i\R010309.b 3/9/01 23:58 D:\chem\Rush.i\R010309.b 3/10/01 0:10 D:\chem\Rush.i\R010309.b 37T070 0!Z5 u:\cnem vK usn.i\K U iujua.D 3/10/01 0:32 D :\chem \R ush.i\R 010309.b 3/10/01 0:43 D:\chem \Rush. i\R 010309.b 3/10/01 1:39 D.Achem\Rush.i\R010309.b 3/10/01 1:50 D :\chem \Rush.i\R010309.b 3/10/01 2:01 D :\chem \Rush.i\R010309.b 3/10/01 2:13 D:\chem\Rush. i\R010309.b 3/10/01 2:24 D:\ctiem\Rush.i\R010309.b 3/10/01 2:35 D:\chem\Rush.i\R010309.b 3/10/01 2.46 D:\chem\Rush.i\R010309.b 3/10/01 2:57 D :\chem tRush.i\R010309.b 3/10/01 3:06 D :\chem \Rush.i\R010309.b 3/10/01 3:20 D:\chem\Rush.i\R010309.b 3/10/01 4:16 D:\chem\Rush.i\R010309.b 3/10/01 4:27 D:\chem\Rush.i\R010309.b 3/10/01 4:38 D:\chem\Rush.i\R010309.b 3/10/01 4:49 D:\chem\Rush.i\R010309.b 3/10/01 5:00 D:\chem\Rush-i\R010309.b 3/10/01 5:11 D :\chem \Rush.i\R010309.b 3/10/01 5:23 D:\chem\Rush. i\R010309.b 3/10/01 5:34 D:\chem\Rush.i\R010309.b 3/10/01 5:45 D:\chem\Rush.i\R010309.b 3/10/01 5:56 D:\chem\Rush.i\R010309.b 3/10/01 6:52 D:\chem\Rush.i\R010309.b 3/10/01 7:03 D:\chem\Rush.i\R010309.b 3/10/01 7:15 D:\chem\Rush.i\R010309.b 3/10/01 7:26 D:\chem\Rush.i\R010309.b 3/10/01 7:37 D:\chem \Rush.i\R010309.b 3/10/01 7:48 D:\chem\Rush.i\R010309.b 3/10/01 7:59 D:\chem\Rush.i\R010309.b 3/10/01 8:11 D:\chem \Rush. i\R010309. b 3/10/01 8:22 D:\chem\Rush.i\R010309.b 3/10/01 8:33 D:\chem\Rush.i\R010309.b 3/10/01 9:29 D :\chem \Rush.i\R010309.b 3/10/01 9:40 D :\diem \Rush.i\R010309.b 3/10/01 9:51 D:\chem \Rush.i\R010309.b 3/10/01 10:03 D :\chem \Rush.i\R010309.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SMFlE 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 RUSH0036.D RUSH0037.D RUSH0038.D RUSH0039.D RUSH0040.D RUSH0041.D RUSH0042.D KUSH0043.U RUSH0044D R U S H 0 0 4 5 .0 RUSH0050D RUSH0051.D RUSH0052.D RUSH0053.D RUSH0054.D RUSH0055.D RUSH0056.D RUSH0057.D RUSH0058.D RUSH0059.D RUSH0064.D RUSH0065.D RUSH0066.0 RUSH0067.D RUSH0068.D RUSH0069.D RUSH0070.D RUSH0071.D RUSH0072.D RUSH0073.D RUSH0078.D RUSH0079.D RUSH0080.D RUSH0081.D RUSH0082.D RUSH0063.D RUSH84.D RUSH0085.D RUSH0086.D RUSH0087.D RUSH0092.D R U S H 0093.0 RUSH0094.D RUSH0095.D 1311-4058-S4 1311-4059-S4 1311-4064-S4 1311-4065-S4 1311-4066-S4 1311-4088-S4 1311-4089-S4 1311-4090-S4 1311-4094-S4 1311-4095-S4 1311-4096-S4 1311-4118-S4 1311-4119-S4 1311-4120-S4 1311-4004-S5 1311-4005-S5 1311-4006-S5 1311-4028-S5 1311-4030-S5 1311-4034-S5 1311-4035-S5 1311-4036-S5 1311-4058-S5 1311-4059-S5 1311-4060-S5 1311-4064-S5 1311-4065-S5 1311-4066-S5 1311-4088-S5 1311-4089-S5 1311-4090-S5 1311-4094-S5 1311-4095-S5 1311-4096-S5 1311-4118-S5 1311-4119-S5 1311-4120-S5 1311-4004-S6 1311-4005-S6 1311-4006-S6 1311-4006MS-S6 1311-4028-S6 1311-4030-S6 1311-4030MS-S6 Soil! Soil1 Soil2 Soil2 Soil2 Soit2 Soil2 Soil2 Soil3 Soil3 Soil3 Soil3 Soil3 Soil3 Cntrl Cntri Cntrl Cntrl Cntrl Som SoiH SoiH SoiH SoiH SoiH Soil2 Soil2 Soil2 Soil2 Soil2 Soil2 Soil3 Soil3 Soil3 Soil3 Soil3 Soii3 Cntrl Cntrl Cntrl Cntrl Cntri Cntrl Cntri Page 588 of 703 Page BACK TO MAIN 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 5.546 5.545 5.547 5.55 5.556 5.55 0 5.544 5.549 5.537 5.557 5.554 5.551 5.547 5.551 5.543 5.541 5.548 5.55 5.547 5.539 5.537 5.544 5.536 5.535 5.54 5.544 5.544 5.552 5.542 5.547 5,55 5.551 5.542 5.536 5.537 5.539 5.539 5.539 5.533 5.57 5.565 5.569 5.57 1463951 1400698 1086434 1289185 1063982 1351089 0 1366635 1099645 1234304 62815 1038219 1172073 1188995 1269801 1239213 1295229 1187969 1957411 1453881 1153414 1099339 1282394 1246108 1223354 1264548 1228663 1263001 1235655 1193060 1318378 1180237 1226490 1308839 1290456 1336550 1245142 1304860 1261162 1247359 1071760 1300949 1303672 1032466 254 254 254 254 254 254 0 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 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 PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.756 5.762 0 0 0 5.768 5.706 5.761 0 5.684 5.704 5.764 5.768 5.757 0 0 0 5.758 5.767 0 0 0 5.754 5.753 5.753 0 0 0 5.769 5.759 5.764 0 0 0 5.753 5.754 5.757 0 0 0 5.78 5.775 5.786 5.78 488283 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 0 0 1393130 1451794 1656632 0 0 0 747647 955425 958092 0 0 0 5486963 444872 428399 5773407 9.6 9.6 0.0 0.0 0.0 76.8 0,0 21.0 0.0 94.0 4.2 123 178 15.9 0.0 0.0 0.0 10.3 6.2 0.0 0.0 0.0 27.1 27.1 32.9 0.0 0.0 0.0 40.3 43.8 45.4 0.0 0.0 0.0 189 24.1 26.3 0.0 0.0 0.0 217.8 9.9 9.4 241.4 2 of 4 3M Environmental Laboratory 3/10/01 10:14 D:\cham1Rush. AR010309. b 3/10/01 10:25 D:\chem\Rush.i\R010309.b 3/10/01 10:36 D:\chem\Rush.iVRQ10309.b 3/10/01 10:47 D:\chem \R ush.i\R 010309.b 3/10/01 10:59 D:\chem\Rush.iVR010309.b 3/10/01 11:10 D:\chem\Rush. i\R010309. b 3/10/0112.06 D.\ehem\Rush.i\R010309 b 3/10/01 12:17 D:\chern\Rush.i\ROl0309.b 3/m /m n Vhom \Pnh \o n im n Q k 3/10/01 12:39 D:\chemVRush.i\R010309.b 3/10/01 12:51 D :\chem \Rush. i\R 0 10309. b 3/10/01 13:02 D:\chem\Rush.i\R010309.b 3/10/01 13:13 D:\chem\Rush.i\R010309.b 3/10/01 13.24 D.VchemVRush AR 010 3 0 9 .b 3/10/01 13:35 D:\chem\Rush.i\R0l03O9.b 3/10/01 13:46 O:\chem\Rush. AR010309.b 3/10/01 14:43 D:\chem\Rush.i\R010309.b 3/10/01 14:54 D:\chem \Rush.AR010309.b 3/10/01 15:05 D:\chem\Rush. i\R010309.b 3/10/01 15:16 D:\chem \Rush.i\R010309.b 3/10/01 15:27 D:\chem \Rush.i\R010309.b 3/10/01 15:39 D:\chemVRush.i\R010309.b 3/10/01 15:50 D:\chem\Rush.i\R010309.b 3/10/01 16:01 D:\chem \R ush.i\R O l0309.b 3/10/01 16:12 O:\chemVRush.iVR010309.b 3/10/01 16:23 D:\chem\Rush.i\R010309.b 3/10/01 17:19 D:\chem\Rush. i\R010309,b 3/10/01 17:30 D:\chem\Rush. i\R010309. b 3/10/01 17.42 D:'^hem 'vRush.i\R010309.b 3/10/01 17:53 D:\chem\Rush. i\R010309. b 3/10/01 18:04 D:\chem\Rush.i\R010309.b 3/10/01 18:15 D:\chem\Rush.i\R010309.b 3/10/01 18:26 D:\chem \Rush.i\R0l0309.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE CAMPI P 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 RUSH0098. RUSH0099.D RUSH0100.D RUSH0101.D R U S H 0106.0 RUSH0107.D oi icu n m a n 1311-4034-S6 1311-4035-S6 1311-4036-S6 1311-4036MS-S6 1311-4058-S6 1311-4059-S6 1311-4060-S6 1311-4060MS-S6 1311.4054 eg RUSH0109.D RUSH0110.D RUSH0111.D R L/S H 0112.0 RUSH0113.O RUSH0114.D RUSH011S.D R U S H 0 1 2 0 .0 RUSH0121.D RUSH0122.D RUSH0123.D RUSH0124.D RUSH0125.D RUSH0126.D RUSH0127.D RUSHQ128.0 RUSH0129.D RUSH0134.D RUSH0135.D RUSH0136.D RUSH0137.D RUSH0138.D RUSH0139.D RUSH0140.D 1311-4065-S6 1311-4066-S6 1311-4066MS-S6 1311-4068-S6 1311-4089-S6 1311-4090-S6 1311-4090MS-S6 1311-4094-S6 1311-4095-S6 1311-4096-S6 1311-4096MS-S6 1311-4118-S6 1311-4119-s e 1311-4120-S6 1311-4120MS-S6 1311-4004-S7 1311-4005-S7 1311-4006-S7 1311-4028-S7 1311-4030-S7 1311-4034-S7 1311-4035-S7 1311-4036-S7 1311-4058-S7 So.l1 SoiH SoiH Soi)1 Soin s o in Soin Soin Sci2 Soil2 Soil2 Soil2 Soit2 So.l2 Soil2 Soii2 Soil3 Soil3 Soil3 Soil3 Soil3 Soil3 Soil3 Soi!3 Cntri Cntrl Cntri Cntrl Cntri Soin S o ill Soin Soin Page 589 of 703 Page BACK TO MAIN 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 5.565 5 .5 7 2 5 .5 7 2 5.565 5.565 5 .5 5 9 5 .5 5 6 5.565 5.56 5 .5 5 7 5 .5 5 9 5.551 5.565 5 .5 5 3 5 .5 5 7 5 .5 4 3 5.561 5.551 5.543 5 .5 3 8 5.543 5 .5 4 4 5 .5 4 5 5.537 5.53 5 .5 4 4 5 .5 4 3 5 .5 3 8 5 .5 3 7 5 .5 3 5 5.53 5 .5 3 9 5 .5 3 2 1333744 1338340 1245746 1068189 1280942 1242425 1262511 1213422 1253433 1250558 1239303 1034913 1258690 1250794 1285551 1080374 1242888 1231504 1217872 1050039 1289869 1232248 1307515 1053782 1230396 1250384 .1221946 1266595 1192244 1218042 1194839 1252105 1194656 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 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 5 .7 7 5 5 .7 7 5 5 .7 7 6 5.766 5 .7 7 5 0 0 5 .7 6 8 5 .7 7 5 5 .7 7 5 .7 7 5 5 .7 6 0 0 0 5.755 5 .7 6 5.754 5 .7 5 5 5 .7 4 7 0 0 0 5 .7 4 8 5 .7 4 8 0 5.74 0 5 .7 4 2 0 0 0 5657330 1095297 1011012 1003621 5974975 0 0 0 5360487 1362179 1415860 1334234 6447671 0 0 0 5229681 1101877 1018381 993087 6331963 0 0 0 432393 423701 0 375306 0 962584 0.0 0.0 0.0 226.5 29.6 28.0 27.2 208.2 0.0 0.0 0.0 220.8 38.5 40.5 36.7 260.5 0.0 0.0 0.0 211.0 29.6 28.5 25.9 262.6 0.0 0.0 0.0 9.9 10.4 0.0 8.9 0.0 27.7 3 of 4 3M Environmental Laboratory 3/9/01 20:04 D:\chem\Rusfi.i\R010309.b 3/9/01 20:15 D :\chem \Rush.i\R010309.b 3/9/01 22:40 D :\chem \Rush.i\R010309.b 3/9/01 22:51 D :\chem \R ush.i\R 010309.b 3/10/01 1:17 D :\chem \R ush.i\R 010309.b 3/10/01 1:28 D :\chem \Rush.i\R010309.b 3/10/01 3:53 D:\chem\Rush.i\R010309.b 3/10/014:04 D:\chem\Rush i\R 010309b 3/10/01 6:30 D:\chem\Rush.i\R010309.b 3/10/01 6:41 D'Achem\RustviVR0103Q9.b 3/10/01 9:07 D:\chem\Rush.i\R010309.b 3/10/01 9:18 D:\chem\Rush.i\R010309.b 3/10/01 11:43 D:\chem\Rush.i\R010309.b 3/10/01 11:54 D :\chem \Rush.i\R010309.b 3/10/01 14:20 D:\chem\Rush.AR010309.b 3/10/01 14:31 D:\chemVRush.i\R010309.b 3/10/01 16:57 D:\chem\Rush.i\R010309.b 3/10/01 17:08 D:\chem\Rush.i\R010309.b 3/10/01 19:00 D:\chem\Rush.i\R010309.b 3/10/01 19:11 O:\chem\Rush.iVR010309.b 3/10/01 21:36 D:\chem\Rush.i\R010309.b 3/10/01 21:48 D:\chem\Rush.i\R010309.b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAM PI F SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE RUSH0020.D RUSH0021.D RUSH0034.D R U S H 0035.0 RUSH0048.D RUSH0049.D RUSH0062.D RUSHO063 D RUSH0076.D RUSH0077.D RUSH0090.D RUSH0091.D RUSH0104.D RUSH0105.D RUSH0118.O RUSH0119.D RUSH0132.D RUSH0133.D RUSH0143.D RUSH0144.D RUSH0157.D RUSH0158D TN-A 4802 M eO H TN*A 4802 M eO H TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 MeOH TN-A 4602 MeOH TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 MeOH TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4802 M eOH TN-A 4802 M eO H TN-A 4802 M eO H TN-A 4602 M eO H Page 590 of 703 Page 4 of 4 BACK TO MAIN THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS TUpCQS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 0 0 0 0 0 0 0 n 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Q 0 0 0 PFOS 5.802 49447 0.0 0 PFOS 5.809 24769 0.0 0 PFOS 5.799 34422 0.0 0 PFOS 5.792 20717 0.0 0 PFOS 5.785 21865 0.0 0 PFOS 5.75 15324 0.0 0 PFOS 5.783 18986 0.0 0 r r 03 5.655 15124 0.0 0 PFOS 5.697 18689 0.0 0 PFOS 5.707 15833 0.0 0 PFOS 5.788 23180 0.0 0 PFOS 5.718 16806 0.0 0 PFOS 5.782 23713 0.0 0 PFOS 5.712 18643 0.0 0 PFOS 5.701 22854 0.0 0 PFOS 5.698 20038 0.0 0 PFOS 5.682 25164 0.0 0 PFOS 5.69 20930 0.0 0 PFOS 5.696 24815 0.0 Q PFOS 5.698 22446 0.0 0 PFOS 5.783 38306 0.0 0 PFOS 5.705 27663 0.0 E00-1311 PFOS Ads/Des BACK TO MAIN 3M Environmental Laboratory Sam ple Batch H010313.b, analyzed on H illary 03-13-01. PFOS Adsorb/D eaorb sam ples. M atrix: Soil/SIg/Sed. \v ' S tandard curve range used fo r calib ra tio n o f sam ples: 5-S01 ng/m L (2.5 ng/mL std n o t in cluded due to the h ig h e r sam ple conce n tra tio n range). Batch method: H010313d.m Inj Date Batch SampType File Sample Name Mise Info C om pound Name RT Area A m ount Compound Name RT Area Amount 3/13/01 12:56 3/13/01 13:07 3/13/01 13:18 3/13/01 13:30 3/13/01 13:41 3/13/01 13:52 3/13/01 14:04 3/13/01 14:15 3/13/01 14:26 3/13/01 14:38 3/13/01 14:49 3/13/01 15:01 3/13/01 17:40 3/13/01 17:51 3/14/01 9:37 3/14/01 9:48 3/14/01 12:16 3/14/01 12:28 3/14/01 14:44 3/14/01 14:56 3/14/01 15:30 3/14/01 15:41 3/14/01 15:53 3/14/01 16:04 3/14/01 16:15 3/14/01 16:27 3/14/01 16:38 3/14/01 16:49 3/14/01 17:01 3/14/01 17:12 3/14/01 17:24 3/14/01 17:35 D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry .i\H 0 1 0 3 1 3.b D :\c h e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry.i\H 0 1 0 3 1 3 .b D:\chem\Hillary.i\H0103l3.b D :\ch e m \H ilia ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry .i\H 0 1 0 3 1 3.b D :\chem \H illary.iyH 010313.b D :\ch e m \H itla ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\che m \H illa ry .i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ c h e m \H ilfa ry .i\H 0 1 0 3 1 3 b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H ilia ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D:\chem\Hiltary ,i\H010313.b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D:\chem\Hillary.i\H010313. b D :\che m \H illa ry .i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\chem \H ilta ry.i\H 010313.b D:\chemVHillary.i\H010313.b D :\chem \H i!!ary.t\H 010313.b D :\c h e m \H illa ry .i\H 0 1 0 3 1 3.b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D:\chem\Hiilary.i\H010313.b SAMPLE HILL0016.D O ng/mL PFOS in MeOH SAMPLE HILL0017.D 2 .5 ng/mL PFOS in MeOH CALIB_1 HILL0Q18.D 5 ng/mL PFOS in MeOH CALIB_2 H1LL0019.D 1 0 ng/mL PFOS in MeOH CALIB_3 HILL0020.D 2 5 ng/mL PFOS in MeOH CALIB_4 HILL0021.D 4 0 ng/mL PFOS in MeOH CALIB_5 HILL0022.D 50.1 ng/mL PFOS in MeOH CALIB_6 HILL0023.D 75.1 ng/mL PFOS in MeOH CALIB_7 HILL0024.D 100.2 ng/mL PFOS in MeOH CAL!B_8 HILL0025.D 2 5 0 .5 ng/mL PFOS in MeOH CALIB_9 HILL0026.D 400.8 ng/mL PFOS in MeOH CALIB_10 HILL0027.D 501 ng/mL PFOS in MeOH CCAL!B_1 HILL0041.D 5 ng/mL PFOS in MeOH CCALIB_1 HILL0042.D 2 5 0 .5 ng/mL PFOS in MeOH CCALIB_1 HILL0055.D 5 ng/mL PFOS in MeOH C C A L IB J HILL0056.D 2 5 0 .5 ng/mL PFOS in MeOH C C A L IB J HILL0069.D 5 ng/mL PFOS in MeOH CCALIB_1 HILL0070.D 2 5 0 .5 ng/mL PFOS in MeOH CCAL!B_1 HILL0082.D 5 ng/mL PFOS in MeOH CCALIB_1 HILL083.D 2 5 0 .5 ng/mL PFOS in MeOH SAMPLE HILL0086.D O ng/mL PFOS in MeOH SAMPLE HILL0087.D 2 .5 ng/mL PFOS in MeOH CALI B_ 11 HILL0088.D 5 ng/mL PFOS in MeOH CALIB_12 HILL0089.D 1 0 ng/mL PFOS in MeOH CALIB_13 HILL0090.D 2 5 ng/mL PFOS in MeOH C A B J 4 HILL0091.D 4 0 ng/mL PFOS in MeOH CALIB_15 HILL0092.D 5 0 .1 ng/mL PFOS in MeOH C A L IB J 6 HILL0093.D 75.1 ng/mL PFOS in MeOH CALIB_17 HILL0094.D 100.2 ng/mL PFOS in MeOH CALIB_18 HILL0095.D 250.5 ng/mL PFOS in MeOH C A L IB J 9 HILL0096.D 400.8 ng/mL PFOS in MeOH CALIB_20 HILL0097.D 501 ng/mL 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 4.99 4.99 4 .9 9 4 .9 9 4 .9 9 4.99 4.99 4.99 4 .9 9 4.99 4 .9 8 4.98 4.98 4.98 5.01 4.99 4.98 4.98 4.98 4.97 4,97 4.97 4.98 4.98 4.98 4.98 4.98 4.98 4.98 4.98 4.98 4.98 986728 1004472 1053980 999429 1025198 1022879 1010348 998419 1010291 1043376 975369 1040160 973042 965534 1293233 1084961 953043 928765 916687 906152 884570 895265 962083 913122 922984 936409 925210 908053 925726 967131 893733 968040 Average: 977950 Std Dev: 77747.7 %RSD: 8.0% 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 QC IS range (*-/-30% average): 1271335 *30%: 684565 -30%: 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 0.00 5.21 5.21 5.21 5.21 5.21 5.21 5,21 5.21 5.21 5 .2 0 6.20 5 .2 0 5.21 5.24 5.21 5 .2 0 5 .2 0 5.22 5 .2 0 0.00 5.20 5.20 5 .2 0 5.21 5.20 5.20 5.21 5,21 5,21 5.20 5,20 0 81205 141737 225923 598942 948444 1168397 1754434 2316691 5628366 8318503 10360908 154385 5687791 180636 6109094 155058 5707416 273709 5662486 0 83400 153877 221204 589951 936043 1160241 1701449 2264695 5613138 821686Q 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 6.1 263.0 5.3 250.4 6.3 275.3 11.9 280.3 0.0 3.4 6.2 9.6 26.1 41.3 52.1 78.8 103.8 258.8 429.2 511.3 %Dev 102.6% 8 9 .1 % 9 5 .3 % 9 5 .6 % 9 5 .7 % 9 8 .1 % 9 6 .9 % 9 5 .5 % 9 8 .5 % 9 3 .8 % 122.5% 105.0% 106.9% 100.0% 125.9% 109.9% 238.4% 111.9% 123.6% 9 5 .8 % 104.5% 103.2% 104.0% 104.9% 103.6% 103.3% 107.1% 102.1% Page 591 of 703 Page 1 of 3 3M Environmental Laboratory 00-1311 PFOSAds/Des Sample Batch H010313.b, analyzed on Hillary 03-13-01. PFOS Adsorb/Desorb samples. Matrix: Soil/SIg/Sed. Standard curve range used for calibration of samples: 5-501 ng/mL (2.5 na/mL std not included due to the higher sample concentration range). Batch method: H010313d.m Inj Date Batch SampType File Sample Name Mise Info Compound Name RT Area 3/13/01 15:46 3/13/01 15:57 3/13/01 16:09 3/13/01 16:20 3/13/01 16:31 3/13/01 16:43 3/13/01 16:54 3/13/01 17:06 3/13/01 17:17 3/13/01 17:28 3/13/01 16,25 3/13/01 18;37 3/13/04 18;48 3/13/04.18:50 3/13/01 19,11 3/13/01 19:22 3/13/01 19:33 3/13/01 19:45 3 /1 3 /m 19:56 3/13/01 20:08 3/14/01 10:23 3/14/01 10:34 3/14/01 10:45 3/14/01 10:57 3/14/01 11:08 3/14/0111:19 3/14/01 11:31 3/14/01 11:42 3/14/01 11:54 3/14/01 12:05 3/14/01 13:03 3/14/01 13;13 3/14/01 13;2S 3/44/01 13:36 3/14/01 13;47 3/14/01 13;SQ 3/14/01 14 ;10 3/14/01 14:22 3/14/01 14:33 D :\ch e m \H illa ry .i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry .i\H 0 1 0 3 1 3 .b D :\che m \H illa ry .i\H 0 1 0 3 1 3.b D :\c h e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa rY -i\H 0 1 0 3 1 3 .b D :\che m \H illa ry .i\H 0 1 0 3 1 3.b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D:\ffhem\HiHary,iVH010313ib D ;ti rh 6 m \H illa ryii\H 0 1 Q 3 1 3 .b &tehem\H illary.i\H010313ib D :\ c h e m \H illa ry ii\H 0 1 0 3 1 3 ib nVhsm\HiHaryii\H010313,b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry .i\H 0 1 0 3 1 3.b D :\c h e m \H illa ry .i\H 0 1 0313.b D ;\gh e m \H illa ry .i\H 0 1 0 3 13.b D :\c h e m \H illa ry .i\H 0 1 0 3 1 3.b D :\c h e m \H illa ry-i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b P WhemVHillaryi\H010313ib Q ;te h e m tH illa ry,i\H 0 1 0 3 1 3 ,b D;W hem\Hillaryj\H010313ib D ;W h e m \H illa ry ,i \H 0 1 0 3 1 3 .b DVihem\Hillary,i\H010313,b O :\c h e m \H iila ty ,ftH 010313.b &teham ^illwy.i\H010313.b D:Vchem\Hillary.i\H010313.b D iW h e m \H illa ryii\H 0 1 0 3 1 3 ib SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE gAMPI p gA^p^p SAMPLE p SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE g A f^ p ^ fi gA^RLE gA^Jp|_fi g A ^p yj yAf^P[_g gAIU|P| g CAilP | fr CAUP^g H IL L 0 0 3 1 .D H IL L 0 0 3 2 .D H IL L 0 0 3 3 .D H IL L 0 0 3 4 .D H IL L 0 0 3 5 .D H IL L 0 0 3 6 .D H IL L 0 0 3 7 .D H IL L 0 0 3 8 .D H IL L 0 0 3 9 .D H IL L 0 0 4 0 .D HILL0CM6 D H IL L 0 0 4 6 .D H IL L 0 0 4 7 .0 H1LL004B.D HILL004BiP H IL L 0 0 5 0 .D HILL0051.D H IL L 0 0 5 2 .D HILL0Q51D H IL L 0 0 5 4 .D H IL L 0 0 5 9 .D H IL L 0 0 6 0 .D HILL0061.D HILL0062.D HILL0063.D HILL0064.D HILL0065.D HILL0066.D HILLQ067.D HILL0068.D HILLX73.D W L U 0074.P HU.10075,0 HILL0076.P HILL0077.P H IL L 0 0 7 8 .D HILL0079.P m U X 8 0 .D HILL0081.P EOO-1311-5062-S2 EOO-1311-5063-S2 E 0 0 -1 311- 5 0 6 3 M S -S 2 E00-1311-5064-S2 EO0-1311-5O65-S2 E 00-1311-5066-S2 E00-1311-5066MS-S2 E00-1311-5067-S2 E00-1311-5068-S2 E00-1311-5069-S2 CQ0-1311-5060MSSa F001311 5070 S3 E X - 1311 6071 S3 600-1311.5073 S3 EOO-1311 5073MS S3 E0O-1311-5091-S2 E 00-1311- 5 0 9 2 -S 2 EOO-1311-5093-S2 50fi.1311.SM 3M S S3 E00-1311-5094-S2 EM-1311-5095-S2 EOO-1311-5096-S2 E00-1311-5096M S-S2 E00-1311-5097-S2 E00-1311-5098-S2 EM-1311-5099-S2 EOO-1311-5099MS-S2 E00-1311-51M-S2 EM-1311-5101-S2 EO0-1311-5102-S2 EX.1311.S1M M SS3 E X -1311.5103 S3 00-1311-5104 S3 EX-13U-5105-S3 E X 1311 S10SMS S3 EOQ.1311.51X S3 EX.1311.S107.S3 E0Q4311-S1M.S3 EOQ-4311-5108MSS3 Soi<2 Soil2 SoII2 Soil2 SoiI2 Soil2 Soll2 Soil2 Soil2 Soii2 SoilS Sona Soia Soia Soil3 SoI3 SoilS g Pj!3 Soil3 Soil3 Soii3 Soil3 Soil3 Soil3 Soil3 SoilS Soil3 SoilS SoilS gpjrc Soia Soia g.-.j|T g 0j!3 gpjlg Soia g^ilT THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS TUBene TuocrtQ T u p a ie THPFOS THPFOS THPFOS TUOCI-tC THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS -ruppr\g Tuocr<g THPFOS THPFQS THPFOS TUPCAC THPFOS THPFOS 4 .9 9 4 .9 8 4.99 4.99 4 .9 9 4 .9 9 4.99 4 .9 9 4 .9 9 4 .9 9 408 408 408 409 408 4 .9 8 4 .9 9 4 .9 9 409 4 .9 9 4.99 4 .9 8 4 .9 8 4 .9 8 4.98 4 .9 9 4 .9 9 4 .9 8 4.99 4 .9 8 408 408 408 408 408 408 408 408 402 909345 895204 758109 865275 860270 848747 7335M 826114 835017 8T'3A3'8O1A9 a-)CQT? faaAM 824166 786360 815722 g m o a .4 814408 878131 874013 723196 852831 841962 822196 709765 827302 824224 830977 7ig< H ` 835010 grtA-ria gQglCfi 70K770 nav220Q32 7Qg Average; 802682.15 Std Dev: 61470.3 %RSD: 7.7% Page 592 of 703 Page2 of3 BACK TO MAIN Am ount Compound Name STD perfo m a n c c co m m e n ts 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 354 W OS 254 W OS 254 W O S 254 W O S 254 W O S 254 PFOS 254 PFOS 254 PFOS ISTCU-70% 254 W O S 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 PFOS 254 W O S 254 W O S 254 W O S 254 W Q S 254 W O S 254 W O S 254 W QS 254 W O S [g TQ47Q% 254 W O S RT 5.22 5.20 5.21 5.20 5.20 5.21 5.21 5.21 5.21 5.20 500 500 500 504 500 5.20 5.21 5.21 504 5.21 5.22 5.21 5.21 5.20 5.20 5.21 500 5.20 5.20 5.20 504 500 504 500 500 500 50 540 509 Area 1448358 1150879 4304297 2329091 2422896 3659129 6555441 7748434 7494602 6105464 8538878 27175761 31535844 33732031 34739500 2640517 945552 670677 3g2335 822587 750560 736105 4068910 2533547 2481828 2597099 5483252 6079641 5936738 6228226 HQggQOO 10743365 11300416 44874136 15190691 ?5 P 9 5 7 31 34505373 36913393 Amount 66.6 53.4 252.7 114.7 120.2 188.2 415.8 438.9 417.8 333.4 5gg 3 3Q1>I g 1663.0 70.40 /\ 137.6 49.9 33 8 235,4 41.7 35.2 34.6 250.2 127.1 126.1 135.5 353.6 334.7 327 4 342.0 3 63g g 6&2A 7004 1407 3 3004.4 3045 4 3379.3 4035.0 Com m ents >501 ng/mL >501 agftwL =>501 ng/mU >501 ng/nnL . >501 ng/mL >501 ngftnL =>501 ng/mU >.S01 ng/mL >501 ng/mL >501 ng/mL =>501 ng/mL =>501 ng/mL EOO-1311 PFOSAds/Des 3M Environmental Laboratory Sample Batch HQ10313.b, analyzed on HUIary 03-13-01. PFOS Adsorb/Desorb samples. Matrix: SoiVSIg/Sed. Standard curve range used for calibration of sampfes: 5-501 ng/mL (2.5 ng/mL stdnot included due to the higher sample concentration range). Batch method: H010313d.m Inj Date Batch SampType File Sample Name Mise Info Compound Name RT Area 3/13/01 12:33 3/13/01 12:44 3/13/01 15:12 3/13/01 15:23 3/13/01 15:35 3/13/01 10:02 3/13/01 18:14 3/14/01 10:00 3/14/01 10:11 3/14/01 12:39 3/14/01 12.51 3/14/01 15:07 3/14/01 15:19 3/14/01 17:46 3/14/01 17:58 D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\chem \H iilaryj\H 0l0313.b D :\chem \H illary.i\H 0l0313.b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D:\chem\Hillary .i\H010313.b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\ch e m \H illa ryi\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry .i\H 0 l0 3 1 3 .b D :\ch e m \H illa ry.t\H 0 1 0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H M a ry .i\H 0 l0 3 1 3 .b D :\ch e m \H illa ry.i\H 0 1 0 3 1 3 .b D :\c h e m \H illa ry.i\H 0 1 0 3 1 3.b D :\c h e m \H ifia ry .i\H 0 l0 3 1 3 .b D :\c h e m \H illa ry .i\H 0 1 0 3 t3 .b SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0014.D H IL L 0 0 1 5 .D H IL L 0 0 2 8 .D HILL0029.D H IL L 0 0 3 0 .D H IL L 0 0 4 3 .D HILL0044.D HILL0057.D HLL0058.D H IL L 0 0 7 1 .D H IL L 0 0 7 2 .D HILL0084.D HILL0085.D H IL L 0 0 9 8 .0 HILL0099.D TN-A 4802 MeOH TN-A4802 MeOH TN-A4802 MeOH TN-A 4802 MeOH TN-A4802 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 THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 0 .0 0 0.00 0.00 0 .0 0 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page3of 3 Page 593 of 703 BACK TO MAIN A m ount Com pound Name RT Area 0 PFOS 5.25 23051 0 PFOS 0 .0 0 0. 0 PFOS 5.25 1B799 0 PFOS 0.00 0 0 PFOS 0.00 0 0 PFOS 5.25 8263 0 PFOS 0 .0 0 0 0 PFOS 0.00 0 0 PFOS 0 .0 0 0 0 PFOS 5.25 10516 0 PFOS 0.00 0 0 PFOS 5.25 23284 0 PFOS 5.25 12631 0 PFOS 5.25 16777 0 PFOS 0.00 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.Q 0.0 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 BACK TO MAIN TestControland Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: PFOS Purified PFOS, Perfluorooctanesulfonate (Primary Std) unknown 08/31/2001 Initials: Number/size of containers: Condition: Retain 1/ 20 m L Nalgene bottle good/ white powder 0.3480 g TCR Substance # TCR-00017-046 Received from;. George Moore Amount received (wt. or vol): Date: 05/31/2000 Shipper: unknown MSDS (y/n) Date of Retain 05/31/2000 -< c z Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) 97.9% LAC 09/19/00 N/A Recrystallized by George Moore, Bldg 236 F19, Frozen C8F17S03-K+ Standard has been moved to Freezer 19 in room 347 KJD 6/7/00 Empty container weight approximatelly 11.86g. LCG 8/16/00 tandard weighed on 9/28/00 was stored frozen at -20C+/- 10C until shippment 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(PFOS Primary Std).pdf 3M Environmental Laboratory Page 595 of 703 BACK TO MAIN Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 Phone: (814) 231-8032 Fax: (814) 231-1253 or (814) 231 -1580 t IN T E R IM C E R T IF IC A T E O F A N A L Y S IS Revision 1(9/7/00) Centre Analytical Laboratories COA Reference #: 023-021 3M Product: PFOS, Primary Standard Test Control Reference #: TCR00017-46 Purity: 97.9% Test Name Purity1 Appearance Identification NMR Metals (ICP/MS) 1. Calcium 2. Magnesium 3. Sodium 4. Potassium2 5. Nickel 6. Iron 7. Manganese Total %Impurity (NMR) Total %Impurity (LC/MS) Total %Impurity (GC/MS) RelatedCompounds- POAA Residual Solvents (TGA) Purity byDSC Inorganic Anions (IC) 1. Chloride 2. Fluoride 3. Bromide 4. Nitrate 5. Nitrite 6. Phosphate 7. Sulfate3 Organic Acids"(IC) 1. TFA 2. PFPA 3. HFBA 4. NFPA Elemental Analysis5: 1. Carbon 2. Hydrogen 3. Nitrogen 4. Sulfur 5. Fluorine . Specifications White Crystalline Powder ` ' - ' ' '... -. ' 1. TheoreticalValue= 17.8% 2. TheoreticalValue= 0% 3. TheoreticalValue= 0% 4. Theoretical Value= 5.95% 5. Theoretical Value= 60% . Result 97.9% Conforms Positive 1 . 0.006wt./wt.% 2 . 0.002 wt./wt.% 3. 1.216wt./wt.% 4. 6.685 wt./wt.% 5. <0.001 wt./wt.% 6. 0.002 wt./wt.% 7. <0.001 wt./wt.% 0.13 wt./wt.% 0.14 wt./wt.% None Detected <0.01 wt./wt.% None Detected 97.5 Mol. %. 1. <0.015 wt./wt.% 2 . 0.60 wt./wt.% 3. <0.040 wt./wt.% 4. <0.009 wt./wt.% 5. <0.006 wt./wt.% 6. <0.007 wt./wt.% 7. 7.88 wt./wt.% 1 . <0.1 wt./wt.% 2 . <0.1 wt./wt.% 3. <0.1 wt./wt.% 4. <0.25 wt./wt.% 1. 11.39wt./wt.% 2. 0.456 wt./wt.% 3. 1.51 wt./wt.% 4. 7.80 wt./wt.% 5. 58.0 wt./wt.% COA023-021 Page 1 o f 3 3M Environmental Laboratory Page 596 of 703 BACK TO MAIN Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 Phone: (814) 231-8032 Fax: (814) 231-1253 or (814) 231-1580 IN T E R IM C E R T IF IC A T E O F A N A L Y S IS Centre Analytical Laboratories COA Reference #: 023-021 Date ofLast Analysis: 08/31/00 Expiration Date: 08/31/01 Storage Conditions: Frozen <-10C Re-assessmentDate: 08/31/01 'Purity= 100%- (sumofmetal impurities, 1.226%+LC/MS impurities, 0.14%+Inorganic Fluoride, 0.60%+NMRImpurity, 0.13%). Total impurityfromall tests = 2.09% Purity = 100%- 2.09%= 97.9% 2Potassiumis expectedin this salt formandis thereforenot considered animpurity. 3Sulfurin the sample appears to be convertedto SO*andhence detectedusing the inorganic anionmethodconditions. The anionresult agrees well with the sulfur n determinationin the elemental analysis, lending confidenceto this interpretation. Based ' onthe results, the SO4 is not considered animpurity. 4TFA. HFBA NFPA PFPA Trifluoroacetic acid Heptafluorobutyric acid Nonofluoropentanoic acid Pentafluoropropanoic acid 5Theoretical value calculations based onthe empirical formula, CsFnSC^'K* (MW=538). This workwas conductedunderEPA GoodLaboratoryPractice Standards (40 CFR160). r^ COA023-021 3M Environmental Laboratory Page2of3 Page 597 of 703 BACK TO MAIN Centre Analytical Laboratories, Inc. ' Oi 3048 Research Drive PJa State College, PA 16801 S,or (814) 231-1580 Centre Analytical Laboratories COAReference #: 023-021 LC/MS PurityProfile: Impurity C4 C5 C6 C7 Total wt/wt % ND ND ND 0.14 0.14 Note: TheC7 valuewas calculatedusing the averageresponse factors fromthe C6 and C8 standardcurves. P Prepared By: ?//<>/ Dvd S. Bell Date Srierttist, Centre, lyrical Laboratories Reviewed By: L/*k ft! /ohn Flaherty ' Date ' LaboratoryManager, CentreAnalytical Laboratories COA023-021 3M Environmental Laboratory Page3of3 Page 598 of 703 BACK TO MAIN Fos urified PFOS, Perfluorooctanesulfonate (Primary Std) CR-00017-046 USE LOG Gross Wt./Vol. Amnt. Gross wt/vol Purpose (enterstandard number) Before withdrawn after withdrawal (mass or voi) withdrawal 9.9099g 0.5069 g 9.4030 g Adsorb/Oesorb Study Balance ID Initials Date 914 LCG 10/17/2000 3M Environmental Laboratory Page 599 of 703 BACK TO MAIN TestControl and ReferenceSubstance Log Substance trade name orreference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Barnes Loam "Don Uglem" 00-2404 12/31/2015 Initials: Number/size of containers: Condition: Retain LCG dried and sieved TCR Substance # Received from: [^ , r v \ r i , - S - o s t f c m c Si^s'/ I Agvise Amount received (wt. or 900 grams,Bulk vol): Date: 10/23/2000 Shipper: Fed Express MSDS (y/n) Date ofRetain jyI n Purity: Records received: Location ofsynthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Agvise Soil Characterization Report 00-2404 NA Container stored ambient inTCR-C02. LCG 12/26/00 TCR stickeradded to bottleafteroriginalweight LCG 10/25/00 d] Don Uqlem loam-0-6.pdf 3M Environmental Laboratory Page 600 of 703 BACK TO MAIN LA B O R A T O R IE S HighwayIS P.O.Box510 Northwood,ND58267 (701)587-6010 FAX(701)587-6013 emailagvisepolarcomm.com Homepageagviselabs.com AGVISE S o i l C h a r a c t e r iz a t io n R e p o r t S u b m ittin g fir m P r o to c o l o r S tu d y S am p le ID . T r ia l ID . D a te R e c e iv e d D a te R ep orted No 3M NA DON UGLEM-LOAM 0 -6 NA 1 0 -2 3 -0 0 1 0 -31-2000 AGVISE L ab N o 00- 2404 P ercen t Sand P ercent S ilt P e r c e n t C la y SDA T e x t u r a l C la ss (h y d ro m eter m ethod) 39 50 11 Loam C a tio n E x ch a n g e C a p a c ity (m eq /1 0 0 g) 23.9 P e r c e n t O rg a n ic C arbon P e r c e n t O rg a n ic M a tter pH i n 0 . 0 1 M CaC12 T o ta l N itr o g e n (%) 4 .9 8 .4 7 .4 0.358 B a se S a tu r a tio n D ata C a tio n Ess r e s s t ppm C a lciu m M agn esiu m S o d iu m P o ta ssiu m Hydrogen. 52.2 20.9 0 .7 3 .5 22.7 2500 600 38 324 54 T h ese! t e s t s w e r e c o m p le t e d i n c o m p lia n c e o f 4 0 CFR P a r t 1 6 0 . li.2 m i L ie M. J o h n s o n ly t ic a l In v e s tig a to r ID -3 1-O P D ate 3M Environmental Laboratory Agricultural Testing Page 601 of 703 BACK TO MAIN LABORATO RIES Highway15 P.O.Box510 Norlhwood,ND58267 (701)587-6010 FAX(701)587-6013 emailagvise0polarcomm.com Homepageagviselabs.com The following personnel have been duly trained to perform Plant Analysis, Soil and Water Characterizationmethods under40 CFRPart 160 Good LaboratoryPractice Standards. Technical Support Staff Anderson, LindaM. - TechnicianIE Deutsch, Robert L. - President Hart, LindaM. - TechnicianIE Hime, SherryL. - TechnicianI Johnson, Julie M. - Nutrient LaboratoryManager McNeil, Vigo (Art) - TechnicianI Moen, Lucinda S. - TechnicianEl Pollert, Garis - Nutrient Laboratory Analyst Pollock, John - TechnicianI Wall, MaryJ. - TechnicianE Wyant, LindaL. - TechnicianI Office Support Staff Berg, EileenA. - SecretaryIE Ducioame, Gail M. - Quality Control Specialist Fuglestad, Teresa S. - Secretary E Hagen, ShellyJ. - Administrative Assistant Quality Assurance Thingelstad, MaryL. - QualityAssurance Manager COPY OF ORIGINAL AGVISE Laboratories, Inc. Initialises Date 05/00 3M Environmental Laboratory Agricultural Testing Page 602 of 703 BACK TO MAIN B u lk D en sity - Disturbed bulk density is determined b y w eighing a known volum e o f dried and ground soil (N U T .0 2 .10). Core or non-disturbed bulk density is determined b y w eighing a known volum e o f an intact, dried soil core (N U T .02.02). W a ter H old in g C apacity and W ater Relations M oisture % - Determ ined b y gravim etric loss upon drying (N U T .02.36). Saturated H ydraulic C onductivity - Determined b y using th e constant head m ethod and m easuring : the rate o f flo w o f w ater through a saturated soil colum n (N U T .02.34). W ater Infiltration R ate - Determined by using the constant head method and m easuring the length o f tim e from w ater application to production o f a leachate from a soil colum n (N U T .02.35). W ater H olding T en acity - Determined b y measuring the m oisture remaining when saturated soil is placed under 1/3 or 0.1 0 bar pressure (N U T .02.08). W ater H olding C apacity - Determ ined by measuring the moisture remaining w hen saturated soil is placed under 15 bar pressure (N U T .02.13). A ll o f th e above m ethods are detailed in the current analytical SO Ps used b y AG V ISE L aboratories' Characterization testing laboratory. N U T .0 5 .0 1 . L o n e T erm S torage o f Soil and W ater C haracterization Specim ens; According to this SO P, soil characterization sam ples w ill be retained b y AG V ISE Laboratories for at least tw o years before disposal and w ater characterization sam ples w ill be retained for a period o f 60 days before disposal. A D M .0 5 .0 1 . A rchivist D uties and Archiving P rocedures: This SOP states that copies o f soil an d w a te r characterization reports, original C O C 's and original raw data w ill b e arch ived w ith in 6 0 days after the signature b y the analytical investigator. Hard copies generated b y com puter w ill b e archived w eek ly, and supplem ental data w ill be archived annually. Q A U .08.01. Q uality A ssurance Inspections o f Facilities. Studies, and P rocesses for G L P C om p lian ce; M ethod inspections w ill be performed on a regular basis at A G V ISE Laboratories, Inc. For soil characterization, tw o methods w ill be inspected per month and one water characterization inspection w ill be conducted per month. An annual facility audit w ill be perform ed b y A G V ISE Laboratories, Inc. Quality Assurance Unit. A ll o f th e a b o v e m eth od s are detailed in th e current analytical SO P 's u sed in A G V IS E L ab o ra to ries' characterization laboratory. 3M Environmental Laboratory Page 603 of 703 BACK TO MAIN C ollection Inform ation Site Id en tification D c r > \ , l A flJ js m L o i W > . ____________________________________________ Sam ple ID dfer/SF U b * d DO - 3V0V G e o g r a p h ic a l R e fe r e n c e L a titu J L . : *11` W ______________L o n g , J W , , . . - 9 7 ` V * ' D a te o f S a m p lin g l ~l al-Q&____________ ,________________________ U s e P a tte r n ( e .g . a g ricu ltu ra l, fo r e s t, e t c .) NnTixMj V ryauJjj___________________ D ep th o f Sam pling O - t o " _____________________________________________________ C o lle c t e d b y .JlnsJ* ?&<&>*___________________________________________________ ******************************************************* Site Identification j \ . f t n r s i A m . uaui- L a a s m ,_______________ Sample ID JLab* Q C i^ M O S ^ Geographical Reference _____L o n f - 9 7"V6' Date of Sampling /0 - M -0 0 __________ ______ _______________ Use Pattern(e.g. agricultural, forest, etc.) O L o X itiJ iu * * /,___________ Depthof Sampling 0 - ( o 11________ Collected by JinnL o Vr,Mi/dr._______________________________ ******************************************************** Site Identification -J imvar. o A jJ b is m iajJ l______________ Sample ID 0 0 ~ A Q o to A 6 Y I S E L a b * __________________ Geographical Reference L n iL bu L tb.: '/TVS' L o n a c h i J s , 97*37' Date of Sampling /0 - )q -OO_________________ ______________ Use Pattern(e.g. agricultural, forest, etc.) ///) l fluM^u S a ttrm ^ )_____ Depthof Sampling____ Q~ 6> 11________________________________ Collected by (\r-L DOg _______________________________ * * * * j * * * * J t ' * * * * * * * * * = f ' * )l ' * * + * + + * + :* * * * * * * * * * * : * * * * * + : * * * * * * * * * Site Identification j C d t a a t , . do- PQo m -______________________ Sample ID A b Y l S E L oJ> * 6 q 0 -A `/ 0 l ________________ Geographical Reference L aiLbuJj^t. W to 2 ' \.o^ o^ tu JjL .;-lto *89 ` Date of Sampling I D- 2lI- DO_______________________________ Use Pattern (e.g. agricultural, forest, etc.) I'ItyiLrhJLuAa/<_____ ______ Depth of Sampling____ 0 - loH_______________ ^ Collected by ("Wv^ f ______________________________ L tc iX ^rv j ^ tJJbudkU i M___ poto ^n-a-oo^fj e ^ t^ o c^ C ujdJs^ a - I m ll-A -oo jcffl 3M Environmental Laboratory Page 604 of 703 BACK TO MAIN 3M Environmental Laboratory ^ G L P Non-GLP ' Characterization Chain of Custody SEND RESULTS TO: BILLTO: r /d 2 - d JJz Contact:. Phone:. AGVISE U se Only Date received / / ^ ? ' 2 . Q ' 0 ( 0 ' Comments Purchase Order#. Protocol/Study#. Test Substance StudyDirector __ Sponsor______ inruauon u a ie AGVISELab# SpecimenI.D. Depth E jA /ik # ? A t m / ~ > fitte r fa > 'k A g v is e Laboratories,Inc. P.O.Box 510/HIghway15 Northwood,ND 58267 Telephone(701)587-6010 FAX (701)587-6013 Series1.SoilCharacterization500g sampleminimum pH,% organicmatter,cationexchangecapacity,waterholding capacity(1/3and15bar),% sand-siit-day,texture,bulk density,% totalnitrogen,phosphorus,andsolublesalts. Series2.SoilCharacterization500 g sampleminimum pH,% organicmatter,cationexchangecapacity,waterholding capacity(1/3bar),% sand-silt-clay,texture,andbulkdensity. Series3.WaterCharacterization-500ml sampleminimum pH,calcium,magnesium,sodium,hardness,conductivity, sodiumabsorptionratio,totaldissolvedsolids,andtuibidity. Series4.Water Characterization-500 ml sampleminimum pH,calcium,magnesium,sodium,hardness,sodiumabsorp tionratio,andconductivity. StudyDirector'sManagement. NatureofStudy_________ .TestSystem:Soil/Water RequestedTest(s) METHOD OF SHIPMENT: Shipment I.D. #(3) A A A ^ ^ 2% / '/ Fed Express UPS USPS . y OtherjQ^f .^------- -------------------------------------------- ----- Aconv of this COC will be mailed to vou when soerimens are received bv Lab. COPY OF ORIGINAL AGVISE laboratories, Inc. Initial ,, Dato/rO-^^rvOC?- 19AQB Page 605 of 703 BACK TO MAIN 3arnes Loam 1 rCR-00065-058 USE LOG Gross Wt./Vol. Amnt. Gross wt/vol Purpose (enterstandard number) Before withdrawn after withdrawal (mass orvoi) withdrawal 954.7g 60.1 g 894.6 g EOO-1311SuitableAn Study Balance ID Initials Date 904 LCG 10/25/2000 3M Environmental Laboratory Page 606 of 703 BACK TO MAIN 3arnes Loam 1 rCR-00065-058 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 834.6g 60.2g Gross wt/vol after withdrawal 774.4g 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 T est C ontrol and R eferen ce S u b sta n ce Log Substance trade name or reference # Substance/chemicai name: Lot/batch #: 3M # Expiration date: Clay soil Kittson Co. 00-2407 NA 12/31/2015 Initials: Number/size of containers: Condition: Retain LCG 1L Nalgene dried and sieved TCR Substance # Received from: tcrJ H H H r n 'C 'S 'c r : C M C i 12--+I < Agvise Amount received (wt. or Bulk vol): Date: 10/25/2000 Shipper: FedEx X -< z MSDS (y/n) Date of Retain Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Agvise Soil Characterization Report 00-2407 NA Container stored ambient in TCR-C02. LCG 12/26/00 1363.9g-original weight and container LCG 10/25/00 H kittson co clay-0-6.pdf 3M Environmental Laboratory Page 608 of 703 BACK TO MAIN LABORATORI ES AGVISE S o il C haracterization Report Highway 15 P.O. Box 510 Northwood, ND 58267 (701) 587-6010 FAX (701) 587-6013 _ email; agvise@polarcomm.com Homepage: agviselabs.com Submitting firm P rotocol or Study No Sample ID. T rial ID. Date Received Date Reported 3M NA KITTSON CO CLAY 0-6 NA 10- 23-00 11- 02-2000 AGVISE Lab No 00- 2407 Percent Sand 16 Percent S ilt 22 Percent Clay 62 USDA T extural Class (hydrometer method) Clay Cation Exchange Capacity (meq/100 g) 54.5 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 T otal N itrogen (%) 2.6 4.5 7.2 0.223 Base Saturation Data Cation Calcium Magnesium Sodium Potassium Hydrogen Percent 54.2 34.6 0.9 3.6 6.8 ppm 5900 2260 110 771 37 Thes^: t e s t s were completed in compliance of 40 CFR Part 160. //-> a ~ o o Robert Deutsch u Date Soil Scientist/A nalytical Investigator A gricu ltu ral Testing 3M Environmental Laboratory Page 609 of 703 BACK TO MAIN LABORATORI ES Highway 15 P.O. Box 510 Northwood. ND 58267 (701) 587-6010 FAX (70 587-6013 email: agvisepo!arcomm.com Homepage agviselabs.com T h e fo llo w in g p erson n el h ave b een duly trained to perform P lant A nalysis, S o il and W ater C h aracterization m eth od s under 4 0 C F R Part 160 G o o d L aboratory Practice Standards. Technical Support Staff A n derson, L inda M . - T ech nician HI D eu tsch , R obert L . - President H art, L inda M . - T echnician III H im e, Sherry L . - T echnician I Johnson, Julie M . - N utrient L aboratory M anager M cN eil, V igo (A rt) - T echnician I M oen , Lucinda S . - T echnician HI P ollert, G aris - N utrient L aboratory A nalyst P ollock, John - T echnician I W all, M ary J. - T ech nician H W yant, L inda L. - T echnician I O ffice Support S ta ff inB e r g , E ile e n A . - S e c r e ta r y D u cioam e, G ail M . - Q uality C on trol Sp ecialist F uglestad, T eresa S. - Secretary H H agen , Shelly J. - A dm inistrative A ssistant Q uality A ssurance T hin gelstad, M ary L . - Q uality A ssurance M anager C O P Y O F O R IG IN A L A G V IS E L a b o ra to rie s , In c . InitiaW^S Date /O 'Z X 'z** 0 5 /0 0 3M Environmental Laboratory A gricu ltu ral Testing Page 610 of 703 BACK TO MAIN B u lk D en sity - Disturbed bulk density is determined b y w eighing a known volum e o f dried and ground soil (N U T .0 2 .10). Core or non-disturbed bulk density is determined b y w eighing a known volum e o f an intact, dried soil core (N U T .02.02). W a ter H old in g C apacity and W ater Relations M oisture % - Determ ined b y gravim etric loss upon drying (N U T .02.36). Saturated H ydraulic Conductivity - Determined b y using the constant head method and m easuring the rate o f flo w o f w ater through a saturated soil colum n (N U T .02.34). W ater Infiltration R ate - Determ ined b y using the constant head method and m easuring the length o f tim e from w ater ap p lication t o production o f a leach ate from a soil, colu m n ( N U T .0 2 .3 5 ). .. W ater H olding C apacity - Determ ined by measuring the moisture remaining when saturated soil is placed under 1/3 or 0.10 bar pressure (N U T .02.08). W ater H olding C anacitv - Determined by measuring the moisture remaining when saturated soil is placed under 15 bar pressure (N U T .02.13). A ll o f th e above m ethods are detailed in the current analytical SO Ps used b y AG V ISE L aboratories' Characterization testing laboratory. N U T .0 S .0 1 . L on g T erm Storage of Soil and W ater C haracterization Specim ens: According to this S O P , so il characterization sam ples w ill be retained by AG V ISE Laboratories for at least tw o years before disposal and w ater characterization sam ples w ill be retained for a period o f 60 days before disposal. A D M .0 5 .0 1 . A rchivist D uties and Archiving Procedures: This SOP states that copies o f soil and w ater characterization reports, original CO C's and original raw data w ill be archived within 6 0 days after the signature b y th e analytical investigator. Hard copies generated b y com puter w ill b e archived w eekly, and supplem ental data w ill be archived annually. Q A U .0 8 .0 1 . Q uality A ssu ran ce Inspections o f F acilities. Stu dies, a n d P rocesses for RT.P C om p li ance: M ethod inspections w ill be performed on a regular basis at A G V ISE Laboratories, Inc. For so il characterization, tw o methods w ill be inspected per month and one w ater characterization inspection w ill b e conducted per month. An annual facility audit w ill be perform ed b y A G V ISE Laboratories, Inc. Quality Assurance Unit. All of the above methods are detailedinthe current analytical SOP's used inAGVISE 3M Environmental Laboratory Page 611 of 703 BACK TO MAIN Collection Information SSiatme pIdleenIDtificatioAnh VDI &cFr ^ UftvLb-rw L>b* L o c u m .___________________ Geographical Reference L a J i t u .; V7 *1 1 1________ L-oncyl,tJ*.:-c) l `W Date of Sampling / - H -OP___________ __________ 0 ________ Use Pattern(e.g. agricultural, forest, etc.) N n ttu ^ Vr\aW xt>____________ Depth of Sampling Q -to" ____________________________________ Collected by _________________________________ ******************************************************** Site Identification f\ . rJtsuur^ CliW Loa^m._______________ Sample ID AfiV'/fiE L a h * O r)U j05 Geographical Reference LentjfjidUj 97*V6' Date of Sampling /0 - /6 - 0 0 ^ Use Pattern(e.g. agricultural, forest, etc.) d g A i ^ J A u A f l / ___________ Depthof Sampling 0 - ( o 11___________ Q_____________________ Collected by A/iZn__? c J & d t_______________________________ ******************************************************** Site Identification J in c x u L i l m ^ u d u M s m i ~ ______________ Sample ID D O - J k l o l o A 6 r /< ,E L i b * __________________ Geographical Reference L n u J j . : 1 V 1 S ' L o ^ a c h j J / . 97<'37' Date of Sampling /0 - lq - OO________________ _ _______ ______ Use Pattern(e.g. agricultural forest, etc.l \J f\ l (ILou^ BntbmrC) Depth of Sampling____O - >"________________________________ Collected by A r -t PHc.b J jJ ,_______________________________ ***********************************>******************** Site Identification C itt o u ,. o . CGo m .______________________ SampieID A b Y l S E L * h * pO- 3.1o~______________ _ Geographical Reference L .alibujL ^ t 1 8 ' Lov^oAtudiL,!-)to *S T DateofSampling I D - A l - DO_____________________________ Use Pattern (e.g. agricultural, foresi, etc.) d y f J l u j ^ / , ___________ Depili of Sampling____ 0 - lo*_______________ * _________________________ Collected by rwL^. ) .*/.______________________________ UMX t t M j u M , d ^ u L O ^ A . o p sn ^ L U. ^ _ _ c ^ u s v J j^ u s c t L ^ ImamActoO. Il-5-oo jqffl 3M Environmental Laboratory Page 612 of 703 BACK TO MAIN Co ^ GLP Non-GLP ' sS' C h a ra c te riza tio n C h a in o f C u s to d y S' 3 SEND RESULTS TO: C3D r~ CoD* o BILL TO: Contact: Phone:. AGVISE Use Only Date received / / ? ' 7 ,0 ' (D rO , <\ Purchase Order# Protocol/Study#. Test Substance StudyDirector __ Sponsor______ Initiation Date___ A g v is e Laboratories, Inc. P.O. Box 510/Highway 15 Noithwood, ND 58267 Telephone (701) 587-6010 FAX (701) 587-6013 Series 1. Soil Characterization 500 g sample minimum pH, % organic matter, cation exchange capacity, water holding capacity(1/3 and 15 bar), % sand-silt-day, texture, bulk density, % total nitrogen, phosphorus, and soluble salts. Series 2. Soil Characterization - 500 g sample minimum pH, % organic matter, cation exchange capacity, water hotdng capacity (1/3 bar), % sand-sitt-day, texture, and bulkdensity. Series 3. Water Characterization - 500 ml sample minimum pH, calcium, magnesium, sodium, hardness, conductivity, sodiumabsorption ratio, total dissolvedsolids, and turbidity. Series 4. Water Characterization - 500 ml sample minimum pH, calcium, magnesium, sodium, hardness, sodiumabsorp tion ratio, and conductivity. Study Director's Management. Natureof Study___________ _ Test System: So#/Water CmteOno Com m ents AGVISE Lab# S p e c im e n I.D. Depth R equested Test(s) ' > m o (o Tl ' (CQD CD O METHOD OF SHIPMENT: Fed Express CO O--h Shipment I.D. #(S) UPS Sent bv -- - -- o -.. - f a i / //u Z & y y L 'Other instructions: OC"-OJ Fax: USPS / Z Q/ J r 0 C O P Y O F O R IG IN A L Other Date: A G V IS E L ab o rato ries, In c . Initia): -Dato//9-?'?? -,o O A conv of this COC will be mailed to vou when soecimens are received bv Lab. 19AW BACK TO MAIN Eii \ oil rCR-00065-077 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 1243.7 g 60.1 g Gross wt/vol after withdrawal 1183.6 g Purpose (enter standard number) EOO-1311 Sorption Balance ID Initials Date 904 LCG 11/13/2000 3M Environmental Laboratory Page 614 of 703 BACK TO MAIN 2lay soil rCR-00065-077 USE LOG Gross Wt./Vol. Before withdrawal 696.0 g Amnt. withdrawn (mass or voi) 255.76g Gross wt/vol after withdrawal 440.24g Purpose (enter standard number) E00-1311 Sorption Study Balance ID Initials Date 904/916 LCG 11/28/2000 3M Environmental Laboratory Page 615 of 703 BACK TO MAIN -lay ^ oil rCR-00065-077 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 390.82 g 22.44 g Gross wt/vol after withdrawal 368.38 g Purpose (enter standard number) E00-1311 PFOS Adsorb/Desorb Balance ID Initials Date 904/916 CMC 01/22/2001 3M Environmental Laboratory Page 616 of 703 BACK TO MAIN -lay ^ oil rCR-00065-077 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 368.37 g 75.27 g Gross wt/vol after withdrawal 293.1 g Purpose (enter standard number) E00-1311 PFOS Ads/Des Balance ID Initials Date 904/914 CMC 01/25/2001 3M Environmental Laboratory Page 617 of 703 BACK TO MAIN Hay oil CR-00065-077 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 293.01 g 97.54 g Gross wt/vol after withdrawal 195.47 g Purpose (enter standard number) EOO-1311 PFOS Ads/Des Balance ID Initials Date 904/916 CMC 01/29/2001 3M Environmental Laboratory Page 618 of 703 BACK TO MAIN 3lay oil rC R -00065-77 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 1363.9 g 60.2 g Gross wt/vol after withdrawal 1303.7 g Purpose (enter standard number) E00-1311 Suitable Analytical Balance ID Initials Date 904 LCG 10/25/2000 3M Environmental Laboratory Page 619 of 703 BACK TO MAIN TestControland ReferenceSubstance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Clay Loam K. Broeren 00-2405 NA 12/31/2015 Initials: Number/size of containers: Condition: Retain LCG Dried and Sieved TCR Substance # Received from: tcr- H B M I (,+t) r ) l . b ~ n /.< 4 O n e S l-W I o \ Agvise Amount received (wt. or Bulk vol): Date: Shipper: 10/23/2000 Fed Ex MSDS (y/n) Date of Retain 3 Y N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Agvise Soil Characterization Report 00-2405 NA Container stored ambient in TCR-C02. LCG 12/26/00 TCR sticker added after original weight taken. LCG 10/25/00 H K Broeren clay loam-0-6.pdf 3M Environmental Laboratory Page 620 of 703 BACK TO MAIN LA B O R A T O R IE S Highway IS P.o. Box 510 Northwood, ND 58267 (701) 587-6010 FAX (701) 587-6013 email; agviseapolarcom m .com Homepage; agviselabs.com AGVISS S o i l C h a r a c t e r i z a t i o n R ep o rt Subm itting firm P r o t o c o l o r S tu d y No Sample ID. T rial. ID. Date R eceived Date Reported 3M NA K BROEREN-CLAY LOAM 0 - 6 NA 10-23-00 10-31-2000 AGVISE Lab No 00- 2405 P ercen t Sand Percent S ilt P ercen t Clay USDA T e x t u r a l C la s s (hydrom eter method) 21 46 33 C la y Loam C ation Exchange C ap acity (meq/100 g) 24.7 P ercen t O rganic Carbon P ercen t O rganic M atter pH i n 0 . 0 1 M CaC12 T otal N itrogen (%) 2.6 4 .4 6.0 0.216 Base S a tu ra tio n Data C ation Percent BBm C a lciu m M agnesium Sodium P o ta ssiu m Hydrogen 52.7 24.3 0 .7 5 .8 16.5 2600 720 39 557 41 T h e se t e s t s w ere c o m p le te d i n com p i a n c e o f 40 CFR : CY<0 / 07 Y Y . O v v iv ir\y p t/U J/iklie M. J o h n so n ia ly tic a l In vestigator /0-3/-O D ate Agricultural Testing 3M Environmental Laboratory Page 621 of 703 BACK TO MAIN L A B O R A T O R IE S t Highway IS P.O. Box 510 Northwood, ND 58267 (701) 587-5010 FAX (701) 587-6013 email: agvisepolarcomm.com Homepage agviselabs.com T h e fo llo w in g p e r so n n e l h a v e b e e n d u ly tra in ed to p erfo rm P la n t A n a ly sis, S o il a n d W a ter C h a ra cteriza tio n m eth o d s u n d er 4 0 C F R P art 1 6 0 G o o d L ab oratory P ra ctice Stan d ard s. T ech n ica l S u p p ort S ta ff A n d erso n , L in d a M . - T e ch n icia n m D e u tsch , R o b ert L . - P resid en t H art, L in d a M . - T ech n icia n H I H im e, S h erry L . - T ech n icia n I J o h n so n , Ju lie M . - N u trien t L a b oratory M an ager M cN eil, V ig o (A rt) - T ech n icia n I M o en , L u cin d a S . - T ech n icia n H I P o lle r t, G aris - N u trien t L a b o ra to ry A n a ly st P o llo c k , John - T ech n icia n I W a ll, M ary J. - T e ch n icia n U W yant, L in d a L . - T ech n icia n I O ffice S u p p ort S ta ff B erg , E ileen A . - S ecreta ry H I D u cio a m e, G a il M . - Q u a lity C o n tro l S p ec ia list F u g lesta d , T eresa S . - S ecreta ry II H a g en , S h elly J. - A d m in istra tiv e A ssista n t Q u a lity A ssu ra n ce T b in g elsta d , M ary L . - Q u a lity A ssu ra n ce M an ager COPY OF ORIGINAL AGVISE Laboratories, Inc. Initial e s Dal 0 5 /0 0 3M Environmental Laboratory Agricultural Testing Page 622 of 703 BACK TO MAIN Bulk Density - Disturbed bulk density is determined by weighing a known volume o f dried and ground soil (NUT.02.10). Core or non-disturbed bulk density is determined by weighing a known volume o f an intact, dried soil core (NUT.02.02). W ater Holding Capacity and W ater Relations Moisture % - Determined by gravimetric loss upon drying (NUT.02.36). Saturated Hydraulic Conductivity - Determined by using the constant head method and measuring . the rate o f flow o f water through a saturated soil column (NUT.02.34). W ater Infiltration Rate - Determined by using the constant head method and measuring the length > o f time from water application to production o f a leachate from a soil column (NUT.02.35). -.. W ater Holding Capacity - Determined by measuring the moisture remaining when saturated soil is placed imder 1/3 or 0.10 bar pressure (NUT.02.08). W ater Holding Capacity - Determined by measuring the moisture remaining when saturated soil is placed imder 15 bar pressure (NUT.02.13). All o f die above methods are detailed in the current analytical SOPs used by AGVISE Laboratories' Characterization testing laboratoiy. NUT.05.01. Long Term Storage of Soil and W ater Characterization Specimens: According to this SOP, soil characterization samples will be retained by AGVISE Laboratories for at least two years before disposal and water characterization samples will be retained for a period o f 60 days before disposal. ADM.05.01. Archivist Duties and Archiving Procedures; This SOP states that copies o f soil and water characterization 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. QAU.08.01. Quality Assurance Inspections of Facilities. Studies, and Processes for GLP Compliance; Method inspections will be performed on a regular basis at AGVISE Laboratories, Inc. For soil characterization, two methods will be inspected per month and one water characterization inspection will be conducted per month. An annual facility audit will be performed by AGVISE Laboratories, Inc. Quality Assurance Unit. . All of the above methods are detailed in the current analytical SOP's used in AGVISE Laboratories' characterization laboratory. 3M Environmental Laboratory Page 623 of 703 BACK TO MAIN Collection Information Site Identification D Cr*v, Ujklxm^ Loasrr^_____________________ Sample ID AbYISE bh* d p O - a V V . Geographical Reference LatdLiJ*. V7* W __________Longrf,<*/*,;-97 Wx' Date o f Sampling I-M -0Q_____________________________________ Use Pattern (e.g. agricultural, forest, etc.) Native, VahWai^_____________ Depth o f Sampling 0~>"_______________________________________ Collected by J it ________________________________________________________________________ ************ ******************************************* Site Identification f(. fin ajisuisn. C&ui Looum,________________ Sample ID Ae>Yl<,F. Lah* 05 , ( Geographical Reference LoiJfjiaU^ VI *VA_____ Lontu+t.J*-,t- 97*V0` Date o f Sampling / 0 - 14 -frO ^ ____________ Use Pattern (e.g. agricultural, forest, etc.) OfWttJuJiuA*!,____________ Depth o f Sampling O-b 11____________ i ________________________ Collected by JianLa PaMixt.__________________________________ ******************************************************** Site Identification J jo & c u L 1 iu \ t A - > d - t J i s m t s u J . _______________________________ Sample ID O Q -^ ^ o fe A6rr*E U b* _____________ Geographical Reference LniJbuJj,: *iTVS' Lor\atJj,*/s. t- 97*37* Date o f Sampling 10- li- 00___________________ ________________ Use Pattern (e.g. agricultural, forest, etc.). ///) C(luue, 6 ottcmO_____ Depth o f Sampling O - 6 11___________________________ ,_______ Collected by A rt PHe.NjU.__________________________________ ******************************************************** Site Identification ICiOon* . C,o. i& U A . Sample ID . oA b Y i s F u h * o i i n GeographicalReference Laiikujlt^i `i 'la3' Loir\agJiAallu! t SV Datte oif Soaammppulinngg //Du --*ut-- 0v0u _____________________ ______________________ ; Pattern (e.g. agricultural, forest, etc.) doyj-jJV-u^a/, ______________ pth o f Sampling____ 0~ io*___________ ___________________________ illected by _____________________________________ io ^ A . u , iM t M , TT n n tn ex ll--oo jcff 3M Environmental Laboratory Page 624 of 703 BACK TO MAIN ^ GLP Non-GLP ' Characterization Chain of Custody SEND RESULTS TO: BILL TO: f c J& M Contact. Phone: 4 P- AGVISE Use Only Date received //* ? ' 7 -0 ' O r t J q _ IN Comments Purchase Order#. Protocol/Study#. TestSubstance _ StudyDirector __ Sponsor______ Initiation Date AGVISELab# Specimen I.D. Her Depth -i V>L '> A g v is e Laboratories; Inc. P.O. Box510/Highway 15 Northwood, ND 58267 Telephone (701) 587-6010 FAX (701) 587-6013 Series 1. Soil Characterization - 500 g sample minimum pH, % organic matter, cation exchange capacity, water holding capacity (1/3 and 15 bar), % sand-st-day, texture, bulk density, % total nitiogen, phosphorus, and soluble salts. Series 2. Soil Characterization - 500 g sample minimum pH, % organicmatter, cationexchange capacity, water holding capacity (1/3 bar), % sand-st-day, texture, and bulkdensity. Series 3. Water Characterization -500 ml sample minimum pH, calcium, magnesium, sodium, hardness, conductivity, sodiumabsoiption ratio, total dissolved solids, and tuibidity. Series 4. Water Characterization - 500 ml sample minimum pH, calcium, magnesium, sodium, hardness, sodium absorp tion ratio, and conductivity. Study Director's Management. Nature of Study___________ .Test System: Soil/ Water CirdeOne RequestedTest(s) to, ' ^ ___ a.__ --------- A conv o f th is CO C w ill be m ailed to vou when specim ens are received bv Lab. BACK TO MAIN Ulay Loam rC R -00065-065 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) Balance ID 1 Balance ID 2 1188.0 g 79.2 g Gross wt/vol after withdrawal Balance ID 1 1108.8 g Purpose (enter standard number or reason for removal) E00-1311 PFOS Adsorb/Desorb Balance Balance ID ID 12 Initials Date 904/914 CIVIC 01/20/2001 3M Environmental Laboratory Page 626 of 703 BACK TO MAIN 3lay Loam i rC R -00065-064 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) Balance ID 1 Balance ID 2 1055.7g 60.2g Gross wt/vol after withdrawal Balance ID 1 995.5g Purpose (enter standard number or reason for removal) E00-1311 Sorption Balance Balance ID ID 12 Initials Date 904 LCG 11/13/2000 3M Environmental Laboratory Page 627 of 703 BACK TO MAIN 3lay Loam rC R -00065-065 USE LOG Gross Wt.A/ol. Before withdrawal Balance ID 1 Amnt. withdrawn (mass or voi) Balance ID 2 1108.8 g 97.3 g Gross wt/vol after withdrawal Balance ID 1 1011.5 g Purpose (enter standard number or reason for removal) E00-1311 PFOS Ads/Desorb Balance Balance ID ID 12 Initials Date 904/916 CMC 01/30/2001 3M Environmental Laboratory Page 628 of 703 BACK TO MAIN :iay'Loam rCR-00065-064 USE LOG GrossWt./Vol. Amnt. Grosswt/vol Purpose(enterstandardnumber) Before withdrawn after withdrawal (massorvoi) withdrawal 1175.7g 60.0g 1115.7g EOO=124+-SuitrNalyStOBy-' o - 1 i ( SuH fWJ 5 1 ^ 4 *oV BalanceID Initials Date 904 LCG 10/25/2000 3M Environmental Laboratory Page 629 of 703 BACK TO MAIN 3layLoam 1 rCR-00065-064 USE LOG GrossWt./Vol. Amnt. Grosswf/vol Purpose(enterstandardnumber) BalanceID Initials Before withdrawn after Date withdrawal (massorvoi) withdrawal 1055.7g 60.2g 995.5g EOO-1311Sorption 904 LCG 11/13/2000 3M Environmental Laboratory Page 630 of 703 BACK TO MAIN Test Control and Reference Substance Log Substancetradename ClayLoam orreference# Substance/chemical name: Lot/batch#: "K. Broeren" 00-2405 3M# NA Expirationdate: 12/31/2015 Initials: Number/sizeof containers: Condition: Retain LCG DriedandSieved TCRSubstance# Receivedfrom: tcr-BHUB A Cr/Ytf^ T/VaC 5 -/^ /O \ . Agvise Amountreceived(wt. or bulk vol): Date: 10/23/2000 Shipper: FedEx MSDS(y/n) DateofRetain JYN Purity: Recordsreceived: Locationofsynthesis, fabrication, orderivation records: StdLocation/Storage: MolecularFormula: Comments Attachment(s) NA AgviseSoil CharacterizationReport 00-2405 NA ContainerstoredambientinTCR-C02. LCG12/26/00 H KBroeren clay loam-0-6.pdf . 3M Environmental Laboratory Page 631 of 703 BACK TO MAIN SlayLoam 1 rCR-00065-065 USE LOG GrossWt./Vol. Amnt. Grosswt/vol Purpose(enterstandardnumber) Before withdrawn after withdrawal (massorvoi) withdrawal 1188.0g 79.2g 1108.8g E00-1311PFOSAdsorb/Desorb BalanceID Initials Date 904/914 CMC 01/20/2001 3M Environmental Laboratory Page 632 of 703 BACK TO MAIN 3layLoam ______________________________ USE LOG 1 rCR-00065-065 _______ GrossWt./Vol. Amnt. Grosswt/vol Purpose(enterstandardnumber) Before withdrawn after withdrawal (massorvoi) withdrawal 1108.8g 97.3g 1011.5g E00-1311PFOSAds/Desorb BalanceID Initials Date 904/916 CMC 01/30/2001 3M Environmental Laboratory Page 633 of 703 BACK TO MAIN TestControland Reference Substance Log Substancetradename RiverSediment orreference# Substance/chemical name: Lot/batch#: 3M# Expirationdate: 12/31/2015 Initials: Number/sizeof containers: Condition: Retain LCG DriedandSieved TCRSubstance# Receivedfrom: tcrJ M -H ) / ( . -(> n O c m c . s /,-y-i ( o \ Agvise Amountreceived(wt. or Bulk vol): Date: 10/23/2000 Shipper: FedEx MSDS(y/n) Date of Retain OY N Purity: Records received: Locationofsynthesis, fabrication, orderivation records: StdLocation/Storage: MolecularFormula: Comments Attachment(s) NA AgviseSoil CharacterizationReport 00-2406 NA ContainerstoredambientinTCR-C02. LCG12/26/00 TCRstickeraddedafteroriginalweightwastaken. LCG10/25/00 3M Environmental Laboratory Page 634 of 703 BACK TO MAIN LABORATORIES Highway15 P.O.Box510 Northwood, ND58267 (701)587-6010 FAX(701)587-6013 email:agvise@polarcomm.com Homepage:agviselabs.com AGVISE S o i l C h a r a c t e r i z a t i o n R e p o r t Subm itting firm = 3M P r o t o c o l o r S tu d y No = NA Sample ID. = GOOSE RIVER-SEDIMENT 0 - 6 T ria l ID. = NA D ate R eceived = 10-23-00 Date Reported = 10-31-2000 AGVISE Lab No . 00- 2406 P ercent Sand 39 Percent S ilt 42 P ercent C lay 19 USDA T e x t u r a l C la s s (h y d ro m eterm ethod) Loam C ation ExchangeC ap acity (meq/100 g) 17.5 P ercen t O rganic Carbon P ercen t O rganic M atter pH i n 0 . 0 1 M CaC12 T otal N itrogen (%) 1 .3 2 .3 7.7 0.101 Base S a tu ra tio n Data Cfotipn, C a lciu m M agnesium Sodium P o ta ssiu m Hydrogen P ercer 57.2 28.6 4.8 3 .4 6 .0 ppm 2000 600 193 232 10 T h ese t e s t s w ere c o m p le te d i n c o m p lia n c e o f 40 CFR P a r t 1 6 0 . A n alytical In vestigator IQ -< 3 1 -0 0 D ate 3M Environmental Laboratory A gricu ltu ra l T estin g Page 635 of 703 BACK TO MAIN LABORATORIES HighwayIS P.O.Box510 Northwood, ND58267 (701)587-6010 FAX(701)587-6013 email:agvisepolarcomm.com Homepageagviselabs.com ft The following personnel have been duty trained to perform Plant Analysis, Soil and Water Characterization methods under 40 CFR Part 160 Good Laboratory Practice Standards. Technical Support Staff Anderson, Linda M. - Technician in Deutsch, Robert L. - President Hart, Linda M. - Technician HI Hime, Sherry L. - Technician I Johnson, Julie M. - Nutrient Laboratory Manager McNeil, Vigo (Art) - Technician I . Moen, Lucinda S. - Technician HI Pollert, Garis - Nutrient Laboratory Analyst Pollock, John - Technician I WaD, Mary J. - Technician H Wyant, Linda L. - Technician I Office Support Staff Berg, Eileen A. - Secretary IU Ducioame, Gail M. - Quality Control Specialist Fuglestad, Teresa S. - Secretary n Hagen, Shelly J. - Administrative Assistant Quality Assurance Thingelstad, Mary L. - Quality Assurance Manager C O PY O F ORIGINAL AGVISE Laboratories, Inc. Initial ^ DateJ2 r21 ^ 05/00 3M Environmental Laboratory A g ricu ltu ra l T estin g Page 636 of 703 BACK TO MAIN B u lk D en sity - D isturbed bulk d ensity is determ ined b y w eighing a known volum e o f dried and ground so il (N U T .0 2 .10). C ore or non-disturbed bulk density is determ ined by w eighing a know n volu m e o f an intact, dried soil core (N U T .0 2 .02). W a te r H o ld in g C ap acity and W a ter R elations M oisture % - D eterm ined b y gravim etric lo ss upon drying (N U T .02.36). Saturated H ydraulic C onductivity - Determ ined b y using th e constant head m ethod and m easuring th e rate o f flo w o f w ater through a saturated soil colum n (N U T .02.34). W ater Infiltration R ate - D eterm ined b y using the constant head m ethod and m easuring th e length o f tim e fro m w a ter app lication to production o f a leach ate from a soil colu m n (N U T .0 2 .3 5 ). ... W ater H old in g C apacity - D eterm ined b y m easuring th e m oisture rem aining w hen saturated soil is p laced under 1/3 or 0 .1 0 bar pressure (N U T .02.08). W ater H old in g C apacity - D eterm ined b y m easuring th e m oisture rem aining w h en saturated soil is placed under 15 bar pressure (N U T .0 2 .13). A ll o f th e a b ove m ethods are detailed in the current analytical S O P s used b y A G V ISE L aboratories' C haracterization testing laboratory. N U T .0 5 .0 1 . L o n g T erm S to ra g e o f S oil and W a ter C h aracterization Sp ecim en s: A ccording to th is S O P , so il characterization sam ples w ill be retained b y A G V ISE L aboratories for at least tw o years before disposal and w ater characterization sam ples w ill be retained fo r a period o f 60 days before disposal. A D M .0 5 .0 1 . A rch ivist D u ties and A rch ivin g P roced u res: T his SO P states that copies o f soil and w ater characterization reports, original C O C 's and original raw data w ill b e archived w ith in 60 days after the signature b y th e analytical investigator. H ard copies generated b y com puter w ill b e archived w eek ly, and supplem ental data w ill b e archived annually. Q A U .0 8 .0 1 . Q u ality A ssu ran ce Insp ection s o f F acilities. S tu dies, and P rocesses for G L P C o m p lia n ce: M ethod inspections w ill b e perform ed on a regular basis at A G V ISE L aboratories, Inc. F or soil characterization, tw o m ethods w ill be inspected p er m onth and one w ater characterization inspection w ill b e conducted per m onth. A n annual facility audit w ill be perform ed b y A G V ISE L aboratories, Inc. Q uality A ssurance U nit. All of the above methods are detailed in the current analytical SOP's used in AGVISE Laboratories' characterization laboratory. 3M Environmental Laboratory Page 637 of 703 BACK TO MAIN C ollection Inform ation Site Id en tification D c n ^ l l a J j s m L o a - r r i _______________________ _________ S am p le ID AhVlSF h* 6 DO ~ 3V 0V G e o g r a p h ic a l R e f e r e n c e Lafj&uJU, : V 7 * V V '_______________ Long rt,, */*.:-<!1 W x 1 D a te o f S am p lin g l b - l l - 0 Q _________________ ._________________ ___________________ U s e P a t t e r n ( e . g . a g r ic u lt u r a l, f o r e s t , e t c . ) N o tu o C VnauuLt;___________ :_______ D ep th o f S am p lin g O - t o " _____________________________ _______ C o l l e c t e d b y ____ ____________ ? U k d z ___________________________________________________ __ ******************************************************** S i t e I d e n t if i c a t io n f \ . P>/i C&tu. L o a ^ m __________________ S am p le ID A feZ /sE Luh# O ftU w S ^ G e o g r a p h ic a l R e f e r e n c e Lcrt '.in d ^ . V 7 , V ^ ' ______L o n c , , ? / , , ! - I l ' Y ' D a te o f S am p lin g /O - - 0 0 ________________ __________ : ___________________________ U s e P a t t e r n ( e . g . a g r ic u lt u r a l, f o r e s t , e t c .) O tW iiLA iJttuA f/,______________________ D ep th o f S am p lin g 0 ~ ( o "____________________ Q _______________________________' C o l l e c t e d b y J in ^L r. P n lA x f,______________________________________________________ ******************************************************** S i t e I d e n t if i c a t io n ~MQ rw L f. _______________________ S am p le ID O O -ilV ofa A & Y t ^ E L<tb*_____________________________ G e o g r a p h ic a l R e f e r e n c e L n -td b v J u t.: `i T V S 1______A o n a ^ v ' / . 9 7 * 3 7 ' D a te o f S a m p lin g 10 - )q - 06 __________________ 5______________ U s e P a t t e r n ( e . g . a g r ic u ltu r a l, f o r e s t , e t c . ) f J A C &L*m ^ QotbrmC)________ D e p t h o f S a m p lin g ________<0- L 11__________________________________ C ollected b y f l r - f r D t b J j U . ____________________________________________________ ******************************************************** S ite Id en tification . C o. C&lm.________________________ S am p le ID A b Y l S F L * h * OoQ 4 0 1 G e o g r a p h ic a l R e f e r e n c e LcdLbujLi^i 4 $ ' h i Larvy^tuaU^ D a t e o f S a m p lin g ID-!- D O _____________________________ U s e P a t t e r n ( e . g . a g r ic u lt u r a l, f o r e s t , e t c .) (laALrljJJ-uA/,__________________ D ep th o f Sam p lin g 0 - (o11________________ "___ _______________________________ C o l l e c t e d b y _______ ( " W ^ ] >t.__________________________________________________ urn cU ^L __r<t>1 M ^U-wAi/V-J ^ll-a-oo jq ft I 'rv-im < f*u svL ll--oo jfi 3M Environmental Laboratory Page 638 of 703 3M Environm ental Laboratory BACK TO MAIN GLP Non-GLP ' C h a ra c te riza tio n C h a in o f C u s to d y SEND RESULTS TO: BILL TO: AGVISE U se Only Date received //* ? ' 7,> ' 0 ( 0 Protocol/Study#. Test Substance _ Study Director __ Sponsor______ Comments AGVISE Lab# Specimen I.D. Depth IDAHOS v c y ^ LiO(p D u / A sk A ut/ 6 - 6 fa /> A * * * fitter A g v is e Laboratories, Inc. P.0.Box510/Highway15 Northwood,NO58267 Telephone(701)587-6010 %FAX(701)587-6013 Series1.SoilCharacterization-500gsampleminimum pH,%organicmatter,cationexchangecapacity,waterholding capacity(1/3and15bar),%sand-silt-clay,texture,bulk density,%totalnitrogen,phosphorus,andsolublesalts. Series2.SoilCharacterization-500gsampleminimum pH,%organicmatter,cationexchangecapacity,waterholding capacity(1/3bar),%sand-silt-clay,texture,andbulkdensity. Series3.WaterCharacterization-500mlsampleminimum pH,calcium,magnesium,sodium,hardness,conductivity, sodiumabsorptionratio,totaldissolvedsolids, andturbidity. Series4.WaterCharacterization-500mlsampleminimum pH,calcium,magnesium,sodium,hardness,sodiumabsorp tionratio,andconductivity. StudyDirector'sManagement. NatureofStudy_______ . TestSystem:Soil/ Water RequestedTest(s) Page 639 of 703 '* METHOD OF SHIPMENT: Shipment I.D. #(s) Fed Express UPS Other Sent hv Fax: ^ / 1--------------------------- -- 'Other instructions: CO PY OF ORIGINAL AGVISE Laboratories, Inc. -- Initial , h s -Date/O'? f -nc) BACK TO MAIN River Sediment * rCR-00065-070 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 1191.4 g 60.1 g Gross wt/vol after withdrawal 1131.3 g Purpose (enter standard number) E00-1311 Suitable Analytical Balance ID Initials Date 904 LCG 10/25/2000 3M Environmental Laboratory Page 640 of 703 BACK TO MAIN *iver Sediment 4 rCR-00065-070 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 1131.3g 60.0 g Gross wt/vol after withdrawal 1071.3 g Purpose (enter standard number) E00-1311 Sorption Balance ID Initials Date 904 LOG 11/13/2000 3M Environmental Laboratory Page 641 of 703 BACK TO MAIN River Sediment rCR-00065-070 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 592.9g 256.16g Gross wt/vol after withdrawal 336.74g Purpose (enter standard number) E00-1311 Sorption Studies Balance ID Initials Date 904 LCG 11/28/2000 3M Environmental Laboratory Page 642 of 703 BACK TO MAIN 3iver Sediment 1 rCR-00065-070 USE LOG Gross Wt./Vol. Before withdrawal 287.20 g Amnt. withdrawn (mass or voi) 23.9 g Gross wt/vol after withdrawal 263.3 g Purpose (enter standard number) EOO-1311 PFOS Adsorb/Desorb Balance ID Initials Date 904/916 CMC 01/22/2001 3M Environmental Laboratory Page 643 of 703 BACK TO MAIN 3iver Sediment 1 rCR-00065-070 USE LOG ____________ Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 263.23 g 75.54 g Gross wt/vol after withdrawal 187.69 g Purpose (enter standard number) E00-1311 PFOS Adsorb/Desorb Balance ID Initials Date 904/914 CMC 01/24/2001 3M Environmental Laboratory Page 644 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic Sludge 2781 NA 10/31/2005 Initials: Number/size of containers: Condition: Retain LCG 1 of 15 freeze- dried TCR Substance # TCR-00065-025 Received from: NIST Amount received (wt. or 40 g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (y/n) Date of Retain O Y N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA certificate of analysis SRM 2781 NA Container stored ambient (10-30C) in TCR-C02. LCG 12726/00 domestic sludge.pdf 3M Environmental Laboratory Page 645 of 703 BACK TO MAIN lomestic Sludge lomestic Sludge CR-00065-025 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 164.58 g 40.92 g Gross wt/vol after withdrawal 423.66 g Purpose (enter standard number) E00-1311 Suitable Analytical Balance ID Initials Date 904 LCG 10/25/2000 3M Environmental Laboratory Page 646 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic Sludge 2781 NA 10/31/2005 Initials: Number/size of containers: Condition: Retain LCG 2 of 15 freeze-dried TCR Substance # TCR-00065-026 Received from: NIST Amount received (wt. or 40 g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (y/n) Date of Retain 3 Y N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Certificate of Analysis SRM 2781 NA Container stored ambient (10-30C) in TCR-C02. LCG 12/26/00 domestic sludqe.pdf 3M Environmental Laboratory Page 647 of 703 BACK TO MAIN I bomestic Sludge / Domestic Sludge [TCR' 00065-026 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 164.61 g 19.12 g Gross wt/vol after withdrawal 145.49 g Purpose (enter standard number) E00-1311 gSuitable Analytical Balance ID Initials Date 904 LCG 10/25/2000 3M Environmental Laboratory Page 648 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic sludge 2781 NA 10/31/2005 Initials: Number/size of containers: Condition: Retain LCG 3 of 15 freeze-dried TCR Substance # TCR-00065-027 Received from: NIST Amount received (wt. or 40 g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (y/n) Date of Retain O Y N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) certificate of analysis SRM 2781 NA container was stored am bient LCG 12/26/00 m domestic sludqe.pdf 3M Environmental Laboratory Page 649 of 703 BACK TO MAIN lomestic Sludge lomestic sludge CR-00065-027 USE LOG Gross Wt./Vol. Amnt. Before withdrawal withdrawn (mass or voi) 125.38g 3.50g Gross wt/vol after withdrawal 121.88g Purpose (enter standard number) Sorption E00-1311 Balance ID Initials Date 904 LCG 11/13/2000 3M Environmental Laboratory Page 650 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic Sludge 2781 NA 10/31/2005 Initials: Number/size of containers: Condition: Retain LCG of 15 freeze-dried TCR Substance # TCR-00065-028 Received from: NIST Amount received (wt. or 40 g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (y/n) Date of Retain JV#N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Certificate of analysis SRM 2781 NA Container was stored ambient. LCG 12/26/00 g domestic sludqe.pdf 3M Environmental Laboratory Page 651 of 703 BACK TO MAIN >omestic Sludge >omestic Sludge CR-00065-028 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 164.74g 41.56g Gross wtyvol after withdrawal 123.18g Purpose (enter standard number) E00-1311 Sorption Study Balance ID Initials Date 904 LOG 11/13/2000 3M Environmental Laboratory Page 652 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic Sludge 2781 NA 10/31/2005 Initials: Number/size of containers: Condition: Retain LCG 5 of 15 freeze-dried TCR Substance # fCR-00065-029 Received from: NIST Amount received (wt. or 40 g(per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (y/n) Date of Retain O Y N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Certificate of analysis SRM 2781 NA Container stored ambient (10-30C) in TCR-C02. LCG 12/26/00 ni domestic sludqe.pdf 3M Environmental Laboratory Page 653 of 703 BACK TO MAIN I Domestic Sludge / Domestic Sludge TCR-00065-029 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 162.69g 15.38g Gross wt/vol after withdrawal 147.31 g Purpose (enter standard number) E00-1311 Sorption Study Balance ID Initials Date 904 LCG 11/13/2000 3M Environmental Laboratory Page 654 of 703 BACK TO MAIN I Domestic Sludge i Domestic Sludge TCR-00065-029 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 147.06 g 25.06 g Gross wt/vol after withdrawal 122.00 g Purpose (enter standard number) E00-1311 Sorption Study Balance ID Initials Date 904 CMC 01/24/2001 3M Environmental Laboratory Page 655 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic Sludge 2781 NA 1013112005 Initials: Number/size of containers: Condition: Retain LCG 6 of 15 Freeze-dried TCR Substance # TCR-00065-030 Received from: NIST Amount received (wt. or 40g (per vendor) vol): Date: 10/03/2000 Shipper: UPS z >Q_ MSDS (y/n) Date of Retain Purity: Records received:: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA certificate of analysis SRM 2781 NA Container stored ambient (10-30C) in TCR-C02. LCG 12/26/00 H domestic sludge.pdf 3M Environmental Laboratory Page 656 of 703 BACK TO MAIN Jomestic Sludge lomestic Sludge CR-00065-030 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 165.67 g 42.27 g Gross wt/vol after withdrawal 123.400 g Purpose (enter standard number) E00-1311 Adsrb/Desorb Balance ID Initials Date 914 CMC 01/24/2001 3M Environmental Laboratory Page 657 of 703 BACK TO MAIN Test Control and Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Domestic Sludge Domestic Sludge 2781 NA 10/31/2005 Initials: Number/size of containers: Condition: Retain LCG 7 of 15 freeze-dried TCR Substance # TCR-00065-031 Received from: NIST Amount received (wt. or 40g (per vendor) vol): Date: 10/03/2000 Shipper: UPS MSDS (y/n) Date of Retain C T y f ' N ----------------------------------------- Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA Certificate o f analysis SRM 2718 NA Container stored ambient (10-30C) in TCR-C02. LCG 12/26/00 n domestic sludqe.pdf 3M Environmental Laboratory Page 658 of 703 BACK TO MAIN lomestic Sludge Jomestic Sludge CR-00065-031 USE LOG ____ Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 163.78 g 7.82 g Gross wt/vol after withdrawal 155.96 g Purpose (enter standard number) E00-1311 PFOS Adsorb/Disorb Balance ID Initials Date 914 CMC 01/24/2001 3M Environmental Laboratory Page 659 of 703 BACK TO MAIN ^iattjcmal i n s t i t u t e a t JB>fcmrars S c ^ l e c t ^ n a t a Q ^ a f Amtlgsts 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 similar matrix. SRM 27S1 is a dried and pulverized domestic sludge. A unit of SRM 2781 consists of 40 g of the dried material. Certified Values: The certified values for 10 elements are listed in Table 1and are based on concordant results from two or more analytical methods. Analytical methods used for the characterization of this SRM are given in Table 3. All values are reported as mass fractions [1], on 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 combination of results from NIST and collaborating laboratories. These results may have sources of bias yet to be investigated and do not meet NIST criteria for certification. Expiration of Certification: This certification is valid for five years from the date of shipment from NIST. However, the certification will be nullified if the SRM is contaminated or modified. Should any of the values change before the expiration of the certification, purchasers will be notified by NIST. Return of the attached registration card will facilitate notification. Stability: This material is considered to be stable; however, its stability has not been rigorously assessed. NIST will continuously monitor this material and report any 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 complete dissolution for analytical determinations to be related io the certified values provided. Instructions for Drying: When nonvolatile elements are to be determined, samples should be vacuum dried at room temperature for 24 h or oven dried for 2 h at 110 C. Volatile elements (e.g., arsenic, mercury, and selenium) should be determined on samples as received; separate samples should be dried according to these instructions to obtain a correction factor for moisture. Moisture corrections are then made to measurement values before comparing them to the certified values. [Note that the mass loss on drying at the time of certification was found to be in the range of 4.7 % to 6.6 % when using the recommended drying procedures.] Statistical consultation was provided by L.M, Gill of the NIST Statistical Engineering Division. The overall direction and coordination of the analyses were under the chairmanship of I.D. Fassett of the NIST Analytical Chemistry Division. The technical and support aspects 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 through the Standard Reference Materials Program by B.S. MacDonald. Gaithersburg, MD 20899 Certificate Issue Date: October 25, 1996 (Revision of certificate dated 6-22-95 to include addendum) Thomas E. Gills, Chief Standard Reference Materials Program Page 1 o f 4 3M Environmental Laboratory Page 660 of 703 BACK TO MAIN Source and Preparation of Material: The U.S. Geological Survey (USGS), under contract to NIST, obtained partially dehydrated sewage cake material from the Metropolitan Denver Sewage Disposal District No. 1. The material (approximately 182 kg) was placed in plastic-lined drams and transported to the USGS facilities in Lakewood, CO for processing. It was dried at ambient temperature in a forced air chamber, ground to pass a 74 m. (200 mesh) sieve, blended for 24 h to assure homogeneity of the pulverized material after which test samples were taken from the blender for preliminary homogeneity analyses. The material was then radiation sterilized. The sterilized material was shipped in bulk to NIST, where the material was bottled in 40 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) and/or inductively coupled plasma atomic emission spectrometry (ICP-AES). Homogeneity was further assessed during certification analysis; at sample sizes of 100 mg or greater. No sample-tosample variations in excess of those expected from the analytical measurements were detected. Certified Values and Uncertainties: The certified values are the means of the results from two or more independent analytical methods as described by Schiller and Eberhardt [2], The uncertainty is based on a 95 % confidence interval for the true value, and includes an allowance for differences between the analytical methods used [3], Table 1. Certified Mass Fractions Element Mass Fraction (in mg/kg) Element Mass Fraction (in %) Arsenic Cadmium Copper Lead Mercury Molybdenum Nickel Selenium Zinc 7.82 0.28 12.78 0.72 627.4 13.5 202.1 6-5 3.64 0.25 46.7 3.2 80.2 2.3 16.0 1.6 1273 5 3 Nitrogen 4.78 0 . 1 1 Noncertified Values and Uncertainties: The noncertified values are the means of the results from two or more independent analytical methods as described by Schiller and Eberhardt [2]. The uncertainty is based on a 95 % confidence interval for the mean, and includes an allowance for differences between the analytical methods used (3). As the accuracy of the measurements could not be assessed from the data, the uncertainty associated with a noncertified value may fail to include all sources of uncertainties and may represent only a measure of the precision of the measurement methods. Element Table 2. Noncertified Mass Fractions Mass Fraction (in mg/kg) Element Mass Fraction (in %) Chromium Silver 202 9 98 8 Aluminum Calcium Iron Magnesium Phosphorus Potassium Silicon Sodium Titanium 1.6 0.1 3.9 0.1 2.8 0.1 0.59 0.04 2.42 0.09 0.49 0.03 5.1 0.2 0.21 0.02 0.32 0.03 Page 2 of 4 3M Environmental Laboratory Page 661 of 703 B A C K T O M A IN Table 3. Methods used for the Analysis of SRM 2781" Aluminum Arsenic Cadmium Calcium Chromium Copper Iron Lead Magnesium Mercury Molybdenum Nickel Nitrogen Phosphorus Potassium Selenium Silicon Silver Sodium Titanium Zinc . INAA, ICP-AES, XRF RNAA, Hyd. AAS, INAA ID-ICPMS, PGAA, RNAA, INAA, TXRF INAA, TXRF, ICP-AES, XRF INAA. TXRF, ICP-AES ID-ICPMS, RNAA, INAA, TXRF INAA. TXRF, ICP-AES, XRF ICP-AES, ID-ICPMS, TXRF INAA. ICP-AES, XRF FIA-CV-AAS, RNAA, INAA ID-ICPMS, ICP-AES, TXRF, INAA ICP-AES, ID-ICPMS, INAA, TXRF Kjeldahl, PGAA Color, ICP-AES, XRF INAA, TXRF, ICP-AES Hyd. AAS, RNAA, INAA, TXRF XRF RNAA, INAA, TXRF INAA, ICP-AES, XRF INAA, TXRF, XRF ICP-AES, ID-ICPMS, INAA, TXRF M e th o d s used fo r establishm ent o f ce rtifie d values are show n in bold-face type; methods used fo r inform ation o n ly values o r to corroborate c e rtifie d values are not in bold. M ethods FIA-CV-AAS Hyd. AAS ICP-AES ID-ICPMS INAA PGAA RNAA TXRF XRF Flow injection analysis cold vapor atomic absorption spectrometry Hydride generation atomic absorption spectrometry Inductively coupled plasma atomic emission spectrometry Isotope dilution inductively coupled plasma mass spectrometry Instrumental neutron activation analysis Prompt gamma activation analysis Radiochemical neutron activation analysis Total reflectance x-ray fluorescence Wavelength dispersive x-ray fluorescence N IS T Analysts M.H. Ahsan E.S. Beary C . M. Beck II D. A. Becker M.S. Epstein K. Garricy R.R. Greenberg R.M. Lindstrom E.A. Mackey J.R. Moody B.R. Norman P.J. Paulsen M.S. Rearick T.A. Rush R. Saraswati J.M. Smeller R.L. Watters, Jr. L.J. Wood Page 3 o f 4 3M Environmental Laboratory Page 662 of 703 B A C K T O M A IN Cooperating Analysts and Laboratories: - f, S. Landsberger and D. Wu; University of Illinois, Nuclear Engineering Department, Champaign, IL ' S.A. Wilson, D. Siems, and P. Briggs; USGS, Lakewood, CO , A. Prange, U. Reus, and R. Neidergesiss; GKSS Research Center. Institute of Physical and Chemical Analytics, t Geesthacht, Germany REFERENCES [1] Taylor, B.N., `Guide for the Use of the International System of Units (SI),` NIST Special Publication 811, 1995 Ed., (April 1995). [2] Schiller, S.B. and Eberhardt, K.R., Combining Data from Independent Chemical Analysis Methods, Spectrochimical Acta, 46B (12). pp 1607-1613, (1991). [3] Guide to the Expression o f Uncertainty in Measurement, ISBN 92-67-10188-9, 1st Ed. ISO, Geneva. Switzerland, (1993): see also Taylor, B.N. and Kuyatt, C.E., `Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results,* NIST Technical Note, 1297, U.S. Government Printing Office. Washington D.C., (1994). Page 4 o f 4 3M Environmental Laboratory Page 663 of 703 B A C K T O M A IN A d d e n d u m to S ta n d a rd R e fe re n c e M aterial 2 7 8 1 Domestic Sludge L e a c h a b le M a s s F ra c tio n s U s in g U .S . E P A a n d N J D E P M e th o d s f o r F la m e A t o m ic A b s o r p t io n S p e c tr o m e tr y a n d I n d u c t iv e ly C o u p le d P la s m a A t o m ic E m is s io n S p e c tr o m e tr y The certified concentration values of constituent elements in this certificate are given as total mass fractions. To obtain total mass fractions, either subsamples of the SRM must be completely decomposed, or the sample must be analyzed directly in its solid form. For mixed acid dissolution, hydrofluoric acid must be included in the acid mixture to totally dissolve siliceous material present in sludge. For a number of environmental monitoring purposes, acid extractable mass fractions of elements are often used 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 reports as total results. However, reported acid labile or extractable mass fractions of elements are generally lower than total mass fractions. Results are often presented as measured mass fractions in the leachate in comparison to the total or certified mass fractions. The recovery of an element as a percent of total is a function of several factors such as the mode of occurrence in the sample, leach medium, leach time, temperature conditions, and pH of the sample-leach medium mixture (1]. In its monitoring programs, the U.S.. Environmental Protection Agency (U.S. EPA) has established a number of leach methods, such as Methods 3015, 3050, and 3051 [2,3] for the determination of acid labile or extractable mass fractions of elements. The New Jersey Department of the Environment (NJDEP) has developed its own leach method, NJDEP 100 for state use [4]. The NJDEP and die U.S. EPA prepared samples of SRM 2781 using the NJDEP 100 method and EPA Methods 3050 and 3051 and analyzed the resulting leachates by flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Reference values have been established for the acid-leachable mass fractions of several elements in SRM "2781. These values are the means of all results from the different leach measurement methods and combinations used. The reference values are listed in Table 1, alaig with their uncertainties which are based on 95 %confidence intervals of the means of results. For some of the elements (copper, iron, silver, vanadium), no statistically significant differences were found among results from the two laboratories using three or four combinations of sample preparation and instrumental measurement techniques (NJDEP 100 - FAAS; NJDEP 100 - 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 the stated uncertainties. 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 Uncertainties: The reference values given in Table 1are not NIST certified but are provided as a reference for U.S. EPA 3050 and 3051, and NJDEP 100 methods. The uncertainties are based on a 95 % confidence interval for the mean and include an allowance for differences between the analytical methods used. Gaithersburg, MD 20899 Addendum Issue Date: October 25, 1996 Thomas E. Gills, Chief Standard Reference Material Program Page 1 o f 2 3M Environmental Laboratory Page 664 of 703 B A C K T O M A IN Element Aluminum Barium Cadmium Calcium Chromium Copper Iron Lead Magnesium Manganese Nickel Silver Vanadium Zinc Table 1. Reference Leach Values for SRM 2781 Leachable mass fraction (in mg/kg) 8040 980 570 65 11 2 36 440 1 830 143 14 601 16 24 300 2100 183 15 4 850 290 745 33 72.3 6.3 86.3 . 1.7 81.9 3.8 1 120 34 % Leach Recovery* 50 86 93 71 96 87 91 82 -- 90 88 ... 88 %Leach Recovery = 100 or ________Leach Value________ Certified or Noncertified Value C oop eratin g A n a ly sts an d L ab oratories: S.J. Nagoumey; New Jersey Department of the Environment, Trenton, NJ. J. Birri, K. Peist; U.S. Environmental Protection Agency, Edison, NJ. REFERENCES [1] Kane, J.S., Leach Data vs Total: Which is Relevant for SRMs, Fresenius J. Anal. Chem. 352: pp 209-213, (1995). [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 Administrative Code, 1994. N.J.A.C. 7:14-4. Page 2 o f 2 3M Environmental Laboratory Page 665 of 703 B A C K T O M A IN Test Controland Reference Substance Log Substance trade name or reference # Substance/chemical name: Lot/batch #: 3M # Expiration date: Soil: Sandy Loam Soil: Sandy Loam 99-2564 TNA-4621 08/01/2015 Initials: Number/size of containers: Condition: Retain LCG 1-500ml (2 of 3) Dried and sieved TCR Substance # rCR-00065-009 Received from: Agvise Amount received (wt. or 448 g net weight vol): Date: 09/14/2000 Shipper: MSDS (y/n) Date of Retain D Y N Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) NA NA container stored ambient in cabinet TCR-C02. LCG 12/26/00 weight of container w/cap 66.4g LCG 9/14/00 3M Environmental Laboratory Page 666 of 703 B A C K T O M A IN oil: Sandy Loam oil: Sandy Loarn CR-00065-009 USE LOG Gross Wt./Vol. Amnt. Before withdrawn withdrawal (mass or voi) 514.81 g 166.61 g Gross wt/vol after withdrawal 348.20 g Purpose (enter standard number) E00-1311 PFOS ads/des Balance ID Initials Date 904 CMC 01/31/2001 3M Environmental Laboratory Page 667 of 703 B A C K T O M A IN 05/23/01 WED 15:19 FAI 1 701 587 8013 AGVISE LABORATORIES LABORATORIES May 23,2001 @ 002 Highway IS P.O. Box 510 Northwood, ND 58267 (701) 587-6010 FAX (701) 337-5013 email: agvisepolarcomrocom Homepage: agviselabs.com Mr. Mark Ellefson 3M Corporation Re SoilCharacterizationforAgviseSouth SoilcollectedfromthesiteAgvise South hastestedasfollows: PercentSand Percent Silt Percent Clay USDA TexturalClass (Hydrometermethod) 58 22 20 Sandy Loam Bulk Density(disturbed) gm/cc Cation Exchange Capacity(meq/100g) 1.05 23.3 % Moistureat1/3Bar 27.9 Percent Organic Matter 4.8 pH in1;1 soi|;waterratio 7.8 Extractable Iron (ppm) ExtractableZinc(ppm) ExtractableManganese(ppm) ExtractableCopper(ppm) Base Saturation Data Cation Percent 10.3 1.59 11.9 0.24 Calcium Magnesium Sodium Potassium Hydrogen 79.5 10.0 0.8 2.5 7.2 ppm 3700 280 41 231 17 Robert Deutsch SoilScientist 3M Environmental Laboratory A g ricu ltu ra l Testing Page 668 of 703 B A C K T O M A IN AGVISE LABORATORIES @001 H ighw ay is P.O. BOX 510 Northwood, ND S8267 % LABORATORIES (701) 587-6010 FAX (701) 567-6013 A G V IS E S o i l C h a r a c t e r i z a t i o n R e p o r t email-, agviseSpolarcommoom Homepage agviselabs.com S u b m itte d B y : BO B D EU TSC H P .O . BOX 316 111 1S T AVENUE NO R TH W O O D ND P r o tO C O l/S tu d y S p e c im e n I D P u rc h a s e O rd e r No T r ia l o r T e s t N o = = = = 58267 A G V IS E S O U T H R e s u lt s R e p o r te d BO B DEU TSC H P .O . BOX 316 111 1S T AVENUE NO RTHW O O D ND T o: D e p th = 58267 D a te D a te R e c e iv e d R e p o r te d = = 9 /2 0 /0 0 9 /2 2 /0 0 A G V IS E A G V IS E Lab R ef No No = = 2 7 ,7 6 7 6 ,6 3 3 ,3 5 7 P e rc e n t S a n d P e rc e n t S i l t P e r c e n t C la y U S D A T e x t u r a l C la s s ( h y d r o m e te r m e th o d ) % O r g a n ic M a t t e r ( W a lk le y - B la c k ) 58 22 20 SANDY 4 .9 LO AM p H (W a te r) 7 .8 /U .'K 3~ //a F *~ K .J A gricultural Testing 3M Environmental Laboratory Page 669 of 703 B A C K T O M A IN 1 2 / 1 1 / 0 0 MON 15: 18 FAX 1 701 587 6013 AGVISE LABORATORIES 0002 AGUISE S o il. C h a r a c t e r i z a t i o n R e p o r t Subm itting firm P ro to c o l or Study Sam ple ID. Tri,-]. II). D ate Received Da t e ft e p o r t e d = No -- = AGUISE SOUTH " SANDY LOAI1 * 11-9-00 = 1 2 -1 1 -2 0 0 0 A GUI SE L a b No 00" 2484 P e rc e n t Sand P ercen t Silt. P erce n t Clay IJSDA T e x t u r a l C lass (hydrom eter method) 58 ee 20 Sandy Loam Bulk D en sity (d is tu rb e d ) gm/ec C a t i o n E x c h a n g e C a p a c i t y (m ec|/100 g) 1.03 23. 3 * M oisture a t 1/3 Bar 27.. 3 P ercen t O rganic M atter 4.8 pH i n 1 s 1 s o i l s w a t e r r a t i o 7.8 E xtractable E xtractable E xtractable E xtractable I r o n (ppm) Z in c (ppm) M a n g a n e se (ppm) C o p p e r (ppm) 10.3 1.59 11.9 0. 24 Base S a tu r a tio n Data C ation Percent ppm C alciu m M agnesium Sod iurn Potass!urn H ydrogen 79.5 10. 0 0.8 2. 5 7.2 3700 280 41 231 17 T h e s e t e s t s w e r e c o m p l e t e d i n c o m p l i a n c e o f 4 0 CFR P a r t 1 6 0 . ** R obert Deutsch D ate Soil S c ie n tist/A n a ly tie a l In v estig ato r 3M Environmental Laboratory Page 670 of 703 B A C K T O M A IN TestControland ReferenceSubstance Log Substance trade name or reference # Substance/chemica) name: Lot/batch #: 3M # Expiration date: 1H, 1H, 2H, 2Hperfluorooctanesulfonic Acid Q-7S-30 N/A Initials: Number/size of containers: Condition: Retain PMR 1/ 250 mL jar good/ white powder 0.2762 g TCR Substance # TCR-00017-047 Received from: SynQuest Labs Amount received (wt. or 80 g, 428.04 g gross wt. vol): Date: 05/15/2000 Shipper: UPS MSDS (y/n) Date of Retain vO n 05/17/2000 Purity: Records received: Location of synthesis, fabrication, or derivation records: Std Location/Storage: Molecular Formula: Comments Attachment(s) TBD USDS SynQuest Labs F19, Frozen C8H5F1303S TN-A-444B, PUR 5/15/00 Standard has been moved to Freezer 19 in room 347 KJD 6/67/00 Standard was stored at room temperature prior to 6/7/00 LAC 12/21/00 3U Transit Number FC-SOOO-0179-4; CORROSIVE tcr00017-47msds.pdf 3M Environmental Laboratory Page 671 of 703 B A C K T O M A IN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log {Standard ID# 101001-03-07 {Description 1500 mg/L ' Stock ID# TCR-00014-046 I T Cone or Purity neat Weight or Volume Balance ID 0.500 g 914 Book No. 001 Page No. 03 IDate Prepared 02/01/2001 Analyst fCMCf | I Final Volume 1000 ml TN-A Solvent 0.01 M CaCI2 00001-34-12 I Final Cone |500 mg/L { Storage Location \ Expiration Date |3rd Floor 108/01/2001 | I Comments: ' I Reviewed By: Cindy M. Carlson 02/06/2001 .. | 'I | 3M Environmental Laboratory Page 672 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001-19-01 Stock ID# ITCR-00017-47 Cone or Purity neat Description THPFOS Book No. 001 Page No. 19 Date Prepared Analyst 07/05/2000 " Iklt | I Weight or Volume 0.0111 g Balance ID Final Volume 1118172181 (914) 25 ml TN-A Solvent TN-A-4464 Methanol { Final Cone 444 ppm | Storage Location | Expiration Date 3rd Floor 01/31/2001 Comments: Added Meoh TN-A per KLT on 1/30/01 OK. Updated Balance ID on 2/16/01 per KLT. OK Reviewed By: Ognjenka Krupljanin 02/16/2001______________________________________ 3M Environmental Laboratory Page 673 of 703 BACK TO MAIN [Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001-24-03 Description ITHPFOS Book No. 001 Page No. 24 Date Prepared 09/13/2000 o 3 O Analyst | Stock ID# 00001-19-01 Cone or Purity 444 ug/ml I ______________________________________________________________________________________ Weight or Volume Balance ID 0.5 ml Final Volume 10 ml TN-A Solvent tn-a-4639 Methanol I Final Cone 22.2 ug/ml | Storage Location I Expiration Date 3rd Floor 03/31/2001 | I I Comments: Reviewed By: Cindy M. Carlson 10/19/2000 3M Environmental Laboratory Page 674 of 703 BACK TO MAIN SINGLE COMPONENT STANDARD PREPARATION LOG Book No. K)0 001 Co Page No. 25 S' s 3' I 3 0} Cr O 3 '3 ^ , 7 u f i* o Q> to (D o> M cn o S ta n d a rd ID # D e s c rip tio n ^<x>i -- 5s " - cm Pf &s Q m -M x S d in / D a te P re p a re d `T - n - c o r -fy O D A n a ly s t S to c k ID # e rre - coto i -D M - 15 Iter C O M l- ^ -- IM C one or P u rity W e ig h t o r V o lu m e r s c o .^ l.e L fO O u L t ill F in a l V o lu m e 5 (3 2 *1 c jO v h L S o lv e n t/ TN A# F in a l C o n c S to ra g e L o c a tio n > ''V O + 4 ie r tm o w U (p p 1 l^ j / L S ^L i A V /i^ .in it'K M v ; 3 E xp. D a te C io O O O O r ^ F (L M U 3 0 \ jjo r U / ^ O c d i- - t f 't y J1 S 7 C W C 'l- f r c s ;. p e c c a i C n 7e$ % y \ ) i M W iijtV cooc \ > - 1 OCOG 1 te w l e z e i uo A T c*e c> H )' ,* (.S tO 3 .'S - f i ceco i " S -- c 1-- tx M T P r ^ AJU * ? r S C ^ T - Z D JCCL> * - _ a s -a rT necci ~ a s - i< 3 \X O l- P fo S P FS P fb s o '( 3 OoOCi - P ro s //> p B S t .s . t t 'H e cca - V r j- K H ^ - `r - o ' o fta J f / l? / c v f lc J J \ alT q 2 1 - c o >KJ o f-C fa jo o onC c '( < 9 J / 0 q a r\C ` / M / a O ld '\ ia t / Cw C. flt o / 0 c* n c. _ J __________ i \ A & V ^ i/ f/ ,7 ' ' / ' / M t C e c o 3>-- l^ q . 1 . OC ffV -> CtM C-'C P' / V C iO C O i - \o > TP& > fir c O .tv j/ L S O -c d T c e c o io S -fD CCW * ' a s -a VOCOi - 3 s -n ( \ d .J r S 'r - jj^ . U P a / A- V c i c c i I u IH m L i i'h L P - J c j % ~ l J ll^ ZL _ 2 . 5 ' /L u i . Z ju o X fM W ltV ) O .& _________ uZi . ju L ffs p fj t - S C7 f (P jfj? /? p H \ M c i/ J p f - s 9 X l'K r H c o rt 4 C ,4 j a . c , /n ' M JV 0 (2 f f G P - S jCj u J I J I S a j u I O .( c 'f > { > & ' i t is L f '0 / y /. O m L- ^ T ( iO U .n L . O .C D D 'C Q 'A C l0 i\* L * O O .H C tA C iX -'C i -- M - q T*J - f t - 'J u , I ty ic tjiJ % Sr `f O > " j L r iO - r t S , r t i. y f a t f v u t . f o t f u a it - 1 ? 5 yrA U o .c i WC M / V J C ix c 'i " - M - - S C O r ^ j U cm -0 ia L -rStU -- u U P p 0v R . . 6 b ~ - / > P * is ! y* T y ic U 3 n C i7 3d ^ - `7 j- 1 | 13 S j L \ S /tc ^ ja i \> VRwV V S j i L l j u if ll- if f l sH i ^ h fs *L H A c * V i% C TJ % ?/ d V o CO Review ed B y :. *Z id Date: / - BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001 -31-10 Description 10.01 M CaCI2 |Stock ID# ITN-A-4000 Cone or Purity neat | Weight or Volume Balance ID 6.7015g Book No. 001 Page No. 31 Date Prepared 11/01/2000 Analyst CMC | Final Volume 6.0L TN-A Solvent milli-q ] I Final Cone 0.01 M Storage Location I Expiration Date 3rd Floor 02/08/2001 Comments: Reviewed By: Ognjenka Krupljanin 11/21/2000 3M Environmental Laboratory Page 676 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log |Standard ID# 100001-31-11 {Description |500mg/L PFOS Stock ID# ITCR-00017-046 I | Cone or Purity neat Weight or Volume Balance ID 0.0500g Book No. 001 Page No. 31 Date Prepared 111/01/2000 {Analyst |CMC Final Volume 100ml TN-A Solvent 00001-31-10 0.01 M CaCI2 I Final Cone |500mg/L I Storage Location 3rd Floor Expiration Date 12/06/2000 | I Comments: Reviewed By: Ognjenka Krupljanln 05/23/2001 3M Environmental Laboratory Page 677 of 703 BACK TO MAIN 3M Environmental Laboratory SINGLE COMPONENT STANDARD PREPARATION LOG Book No. <**- 00 001 Page No. 32 Standard ID# Description o c c o I ? > 2 -o I f\^WVV.f'Al' - 3 a -a a . C f^oi - 32 -o 3 c2rv\l"\ P\mOlLc"i /aopj)x> ffi ^rg p p ,-^ P f c s >F5> Date Prepared Wo / O0 y lM o O it/? / >0 Analyst Stock ID# Cone or Purity Weight or Volume TN-A - One one. U.o.JiJ TCfi-- Cecil - C|Cfl CCCCi " -1--.-3- 5--3-SV-yi o .coya, O i l 3 ^ - 0 > /OQiprrs /D Oml Final Solvent/ Volume TNA# Final Cone ex7i S D in L M//A -& - 3--<tr M ciLm H io 0 ( f , v \ (D HSctTip/n (3.0 (S> Storage Exp. Location Date 7 r/i 3 cd J /" i dM' s / a o D to rP ____ =CUl . CJOOO t - 3J- "07 /0Om ^/i. ?f Of, acco i - ?Jt, -O S i.O O rxu-lL PFOS Of i - 3 L -0 7 VcW - O I D ^ / l PPC' S J l'lD cU ? cC ')- JX ~ (( Xit'O 1- T //f/^ r A C* t tl/i/tv v /t/to w k llQ / i'/i.?/ GO u/'3/0O \\/\b h > e tt//3 /c o l* h . U f i / o 0 Et Her * c*nc CmC Cm c TVflvPlI W -ttW l . y f . -5 'i - 13, S 0 (& jrr-fMc Sl.tt (aIsCvfikfiCi 25DinL WA 2j g $ / ) U - r m > 5 fa lo & lfr Ulfl-Cf ft fh ii7 P 'S O f f i K - > / ' ~ FTCi2 -Cecil `/l (X1M- -JJb -o~1 neat ,oCU%. OCXT*i * - a/ too rofj L A v^/y/ -o S / XXMUM O tin l `-- 7 iO O O 0 . / >0O(J ,n L <3S0mL 5 0 > iL ?5CVviL 7.3JL , / U tfk r Ot-i-fll'H-tO C*C htti6\ o o c c t-/| - 1o Cc-Ch (G\ to O-Cljtau) rd A -''i7 1 lO O m ijlL |, (XJ t'-cvcjlL_ 0 ( 0 r.itj 1(- y ti 3je s iX ncP j fU \J T H '/\2 a ? / W 6 J (7 5 ~ j 2 L a /f,6 ( M Jref 5 /c 1'' y /c 'i 5 /o i 5 /cl ^ -/ J '/c \ ccD o i- -11 / k / O 3 3 - /3 T t ' P f o S ____________________ ~5.2-/'-i <9ete*=*? ii) (SPZ^ ' o X V P r A T H p ' R j J C X C O '? ^ ' /S ' 5 C ffr* P Foi ll/'T /o O y/ts~(0O X 4iaC-- cmC Cmc CivvC -m ou.O/ 3 3 -- f3 ccx\?i " 3 3 -0 '/ neal 5H$ ffvr i&o 0 - 0 iMT^ MfC'if Qrt .0?\L 5 3 ^ |o TN.V-Cjt'OU Ci3^/vi\ fi'.K t ,-lfrr * Q . tX - l BC -il-lC lO/.vO c>riH 3> m n 3^ 5(o f -J------ 5 /fc l 3 ^ 5/cl q ) a t * i <s i m t x - ' t ^ m t il'd d a * c Reviewed By:______________________ Date: in Page 678 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001-32-03 |StOck ID# (00001 -32-02 Cone or Purity 100ppm Description 10ppm PFOS Weight or Volume Balance ID 10.0mL Book No. 001 Page No. 32 Date Prepared 11/08/2000 Analyst CMC Final Volume lOO.OmL TN-A Solvent 00001-31-10 0.01 M CaCI2 Final Cone 10ppm Storage Location 3rd Floor Expiration Date 05/31/2001 Comments: Reviewed By: Ognjenka Krupljanin 11/21/2000 3M Environmental Laboratory Page 679 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log {Standard ID# 100001-32-07 Description 100mg/L PFOS Stock ID# TCR-00017-046 Cone o r Purity neat Weight or Volume 0.1000g Balance ID Book No. 001 Page No. 32 Date Prepared 11/13/2000 {Analyst |CMC Final Volume 1000mL TN-A Solvent 00001-31-10 0.01M CaCI2 Final Cone 100mg/L { Storage Location 3rd Floor Expiration Date 05/31/2001 I Comments: ~ ~~ I I Reviewed By: Ognjenka Krupljanin 11/21/2000________________________________________ I I 3M Environmental Laboratory Page 680 of 703 BACK TO MAIN [Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001-32-09 |Stock ID# |00001-32-07' Cone or Purity 100mg/L Description 0.10mg/L PFOS Weight or Volume 250uL Balance ID Book No. 001 Page No. 32 Date Prepared 11/13/2000 Analyst CMC Final Volume 250mL TN-A Solvent 00001-31-10 0.01 M CaCI2 Final Cone 0.10mg/L Storage Location | Expiration Date 3rd Floor 05/31/2001 Comments: Reviewed By: Ognjenka Krupljanin 11/21/2000 3M Environmental Laboratory Page 681 of 703 BACK TO MAIN EEnvironmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log {Standard ID# 100001-32-10 Description THPFOS Book No. 001 Page No. 32 Date Prepared 1 /1 3/2000 Analyst RWW Stock ID# 00001-21-03 Cone or Purity 1000ppm Weight or Volume Balance ID 0.25mL Final Volume 500mL TN-A Solvent TN-A-4672 methanol 1 Final Cone |500ppb 1 Storage Location |2nd Floor Expiration Date 03/30/2001 I Comments: Reviewed By: Ognjenka Krupljanin 11/21/2000 3M Environmenteil Laboratory Page 682 of 703 BACK TO MAIN [Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001-32-14 Description 20 ppm THPFOS Book No. 001 Page No. 32 Date Prepared 11/15/2000 Analyst CMC Stock ID# 00001-32-13 Cone or Purity 588 ppm Weight or Volume Balance ID 850 ul Final Volume 25 ml TN-A Solvent tn-a-4604 Methanol Final Cone 20 ppm Storage Location 3rd Floor Expiration Date 05/15/2001 Comments: Reviewed By: Ognjenka Krupljanin 11/27/2000 | I 3M Environmental Laboratory Page 683 of 703 BACK TO MAIN {Environmental Laboratory Standards Database SCS PL Single Component Standard Preparation Log Standard ID# 00001-32-15 Stock ID# 00001-32-07 Cone or Purity 100 ppm Description 50 ppm PFOS Weight or Volume 5 ml Balance ID Book No. 001 Page No. 32 Date Prepared 11/15/2000 Analyst CMC Final Volume 10 ml TN-A Solvent 00001-31-10 0.01 MCaCI2 I Final Cone 50 ppm I Storage Location I Expiration Date 3rd Floor 05/15/2001 | 1 Comments: Reviewed By: Ognjenka Krupljanin 11/27/2000 3M Environmental Laboratory Page 684 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 00001-33-07 Description 0.01 M CaCI2 (aq) Stock ID# tn-a-4000 Cone or Purity neat | Weight or Volume 6.7310 g Balance ID - Book No. 001 Page No. 33 Date Prepared 11/21/2000 o 3 O jAnalyst | | Final Volume 6L TN-A Solvent milll-q I Final Com; |0.01 M I Storage Location I Expiration Date {3rd Floor 103/01/2001 Comments: Reviewed By: Ognjenka Krupljanin 11/27/2000 3M Environmental Laboratory Page 685 of 703 BACK TO MAIN EEnvironmental Laboratory Standards Database SCS PL Single Component Standard Preparation Log Standard ID# 100001-34-12 Description 0.01 M CaCI2 (aq) Stock ID# |tn-a-4000 Cone or Purity neat Weight or Volume 6.7142 g Balance ID NA Book No. 001 Page No. 34 Date Prepared 12/04/2000 Analyst CMC | I Final Volume 6 Liters TN-A Solvent m illi-q I Final Cono 0.01 M Storage Location { Expiration Date 3rd Floor 03/14/2001 Comments: Reviewed By: Cindy M. Carlson 12/14/2000 3M Environmental Laboratory Page 686 of 703 BACK TO MAIN 3MEnvironmental Laboratory SINGLE COMPONENT STANDARD PREPARATION LOG Book No. _ 00 001 Page No. 34 S ta n d a rd ID # D e s c rip tio n D a te P re p a re d A n a ly s t S to c k ID # C one or P u rity W e ig h t o r V o lu m e F in a l V o lu m e S o lv e n t/ TN A # F in a l C o n e S to ra g e L o c a tio n E xp. D a te C V CO | 54- 1 f/.-t-r - o o tX > \ - 3 M -3 C e to * - 3 1 - *4 X 1- 3M - 5 " OCCC.*i ' 3W -( c X 'j o c i - 3 /' T ( 4 d h i t U 6k ' j ` l o K li,, f ^ 4- 5 0 n i.) A - 5> - U 6 iy \C - D ' io 5 0 r r l _ p r | 4 3 (I/b d / oo c t o C . SE' o3D 5 0 ,- r ^ lL P f o P i 5 " o * ^ /_ P P o a U / 3 o / oc> Cm C ! '/?)C SCKO c *n c o i m H A i A j v i c i ' . t i < n f ) c i Ll~ i t U / t / ` 0 CM c o l r r > M A<Vj/t76*:<iAir> W /1 / oc t' R S io c 30 P R o S 'o 30 - u s a -/ rru A - S4 I 'u V l/ ' neoV nm + 0 .0 ^ 5t> iA 't L M & O F - l - 'i ! ^ ) / h i U Q. 00703=} Q c X fC 'ii'C 7 to o O m U C-.AS c . U X i 'It H eoH O O .O .a I rro /l ' / m v-A j SC 'w tjJ L C ' . c 3 < 3 5 b i CJ Oc -<j - 3 j t ( O O - O v ^ U O w M O c l j . J m . ^ I>U fp ;" 33 -^ 3 '^ 0 i? C L E O -O O S o S ^ T fy }A 5 0 rTM j ^ r< j n ra i 0 3 0 9 / fj 5L M a h -Q 2 lV \ M 3^ t\e a i 0 . 3 /o O g 2 L H u ll -C i y v \ (^1 3oi V o, V -i b> ^ 5 /< = i ii / c i u f O', D o a < ? y. y O eC O | 3 V -9 S 6D o ( ? / - / <S> C b > C ( ocxx'i .3 " /' qv< - > 1 ' /3 .X -'C K ji ' OCOOf ^ -O f . _ "W - /5 s f ^ y J j4 < t x - J t_ ^ L n ^ / ^ / / /* > V - S 1 * 1& Q A * . -( 1 T *M - 3S u S l OO O 0 i. N O O J a . i o ? L f la ^ J L /* ,3 u f K j/ l, L . J S li. '3 t a 9 1^ ^ - 1* J - -? rc / / y ^ /L l 1 S fi - 2 > o .A 5 +/ - 3 (J) O / C a C i j C a f) o c " - j / <- f - o f i 50 .^ /L F<?54 L -F )5 O - S 'O i- . L 1i 1 5o J t h / c6 U lf lo o S - ls jc ' anc O ne am c I T fliA H 0C lt d W lJ i- t f ne' m it i'* # i / .O O l* , l J / n e a -f n & Jrm L (j> . 7 i 6 / y C C r ^ 'f j^ C .c 'o V C ' i ^ (p l-- lO C ^ L - a u lii 0 7 .0 / M G -c- i H _ : (L<iC ij.t c s j) H c -O H ^ r td B H c lf/ . ^ J l ^ h '/ o OC JC ' 03S e .e o v c ^ $ 't&>'jv U U , S i H |p ? //j J M h l(X > .r\U A ie o lf ^ "7 7 o Qk //d 1 S > 5 /3 ^ rd "D O o /* > i i/ '* lo \ V o, 6 /01 R e v i e w e d B y : _________________________________________ D a t e : f j t O S i ) L j ~ ~ J M 0 o r n i t <? i 5 1 C & Page 687 of 703 BACK TO MAIN [Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 01001-02-01 Description 20 mg/L THPFOS IS Book No. 001 Page No. 02 IDate Prepared 01/08/2001 Analyst CMC Stock ID# 00001-32-13 Cone or Purity 588 mg/L Weight or Volume Balance ID 850 ul NA Final Volume 25 ml TN-A Solvent TN-A-4715 Methanol Final Cone 20 mg/L Storage Location | Expiration Date 3rd Floor 05/08/2001 Comments: I Reviewed By: Cindy M. Carlson 02/06/2001 3M Environmental Laboratory Page 688 of 703 BACK TO MAIN EEnvironmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 01001-02-02 Description IPFOS Stock Book No. 001 Page No. 02 Date Prepared 01/09/2001 Analyst NILA |Stock ID# ITCR-00017-046 Cone or Purity neat Weight or Volume Balance ID 0.1278 g 914 Final Volume 10 ml TN-A Solvent tn-a-4755 Methanol | Final Cone 112780 ug/ml | Storage Location | Expiration Date |3rd Floor [01/09/2002 | | | Comments: I ................ ~ ..................................... ~ ~ | Reviewed By: Cindy M. Carlson 02/06/2001 | I 3M Environmental Laboratory Page 689 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 01001-02-03 Description ITHPFOS Stock Book No. 001 Page No. 02 Date Prepared 01/09/2001 Analyst MLA Stock ID# TCR-00017-047 Cone or Purity neat Weight or Volume Balance ID 0.0053 g 914 Final Volume 10 ml TN-A Solvent TN-A-4755 Methanol I Final Con; 530 ug/ml I Storage Location I Expiration Date 3rd Floor 01/09/2002 I Comments: Reviewed By: Cindy M. Carlson 02/06/2001 3M Environmental Laboratory Page 690 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log [Standard ID# 01001-02-04 [Description jpFBS Stock Book No. 001 Page No. 02 [Date Prepared [01/09/2001 [Analyst |MLA Stock ID# TCR-99030-023 Cone or Purity neat Weight or Volume 0.0127 g Balance ID 914 Final Volume 10 ml TN-A Solvent TN-A-4755 Methanol [ Final Cone |1270 ug/ml [ Storage Location [ Expiration Date |3rd Floor 101/09/2002 | I I Comments: I' I Reviewed By: Cindy M. Carlson 02/06/2001 [ I I [ I 3M Environmental Laboratory Page 691 of 703 BACK TO MAIN Environmental Standards Database Laboratory SCSPL Single Component Standard Preparation Log t Standard ID# 101001 02-05 [Description |25 ppm (ug/ml) PFOS Book No. 001 Page No. 02 Date Prepared 1/09/2001 |Analyst [m l a |Stock ID# [0 1 0 0 1 -0 2 -0 2 Cone or Purity 12780 ug/ml Weight or Volume Balance ID 49 ul NA Final Volume 25 ml TN-A Solvent TN-A-4755 Methanol I Final Cone I25.048 ug/ml I Storage Location I Expiration Date [3rd Floor 101/09/2002 | I { Comments: I----------------------- " - '' I Reviewed By: Cindy M. Carlson 02/06/2001 | I 3M Environmental Laboratory Page 692 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log |Standard ID# 101001-03-08 Description 50 mg/L PFOS Book No. 001 Page No. 03 Date Prepared 02/01/2001 Analyst CMC Stock ID# 01001-03-07 Cone or Purity 500 mg/L I ______________________________________________________________________________________I Weight or Volume Balance ID 10 ml NA Final Volume 100 ml TN-A Solvent 0.01 M CaCI2 00001-34-12 I Final Cone (50 mg/L Storage Location I Expiration Date 3rd Floor 08/01/2001 I Comments: Reviewed By: Cindy M. Carlson 02/06/2001 3M Environmental Laboratory Page 693 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 01001-03-15 Description 0.01 M CaCI2 Stock ID# TN-A-4000 Cone or Purity neat | Weight or Volume |BalancelD 6.6723g 914 Book No. 001 Page No. 03 Date Prepared 2/12/2001 Analyst CMC | I Final Volume 6 liters TN-A Solvent milli-q j I Final Cone 0.01 M I Storage Location j Expiration Date 3rd Floor 08/12/2001 | I Comments: Reviewed By: Cindy M. Carlson 02/28/2001 3M Environmental Laboratory Page 694 of 703 BACK TO MAIN Environmental Laboratory Standards Database SCSPL Single Component Standard Preparation Log Standard ID# 01001-04-05 Description 10 mg/L THPFOS IS Book No. 001 Page No. 04 I Date Prepared Analyst I 02/21/2001 CMC | I Stock ID# 00001-32-13 Cone or Purity 588 mg/L Weight orVolume Balance ID 850 ul NA Final Volume 50 ml TN-A Solvent TN-A-4755 Methanol Pinal Cone 10 mg/L Storage Location Expiration Date 3rd Floor 05/31/2001 Comments: Reviewed By: Cindy M. Carlson 02/28/2001 3M Environm ental Laboratory Page 695 of 703 Description: JV.svb Date Prepared: g / g . j oo Prepared By: Storage Location: ^ Expiration Date: , / qi C u roV BACK TO MAIN 3MEnvironmental Laboratory (uQo CD CD CcnO -QO4J Reviewed By: BACK TO MAIN 3MEnvironmental Laboratory MULTI-LEVEL PREPARATION LOG Book No.01 003 Page Nor" 7 Description: Date Prepared: Prepared By: Storage Location: Expiration Date: Pfto5 fWe. Mlo^tDl /*!AV - _______ Solvent: 3M Trace#: ^7^5 Standard ID# 01 003-7-1 01 003-7-2 01 003-7-3 01 003-7-4 01 003-7-5 01 003-7-6 01 003-7-7 01 003-7-8 Description Component Standards ___ SL____ m ____ 90 2___ 21___ '' Amount ofComponent Standard Added Expiration Description ID# Cone Date Std 1 Std2 Std 3 Std4 Std5 Std6 Std7 Std 8 lm-x-s Voi ,7U <.S,,l uL 10L $i;(_ iJt/L <>QU 7SvL THPfoS QlOOt-i.-'} f/o u Zoi AvL L I3,,L l)i,L ILL \,L luL ws Ol0e(-2-ll Zoi - 5S/L 9uL *>vL W , 5uL Sub 9j L M'V - FinalVolume O U I a5-,c. c>57>f-: cJ/rrL 09L U L J U L Final Concentration 6 P.9 5 to Vi) n Standard ID# 01 003-7 01 003-7 01 003-7 01 003-7 01 003-7 01 003-7 01 003-7 01 003-7-9 10 11 12 13 14 15 16 Description ide x rc i w/ S /m r te w / [ Component Standards Amount ofComponent StandardAdded Expiration Description ID# Cone Date Std 9 Std 10 Std 11 Std 12 Std 13 Std 14 Std 15 Std 16 ?F O S m m - i - x w Z t Vox tOO,,L 5 0 0 , F if0 0 A 0 O .A ( n v u , ( \t H P F 0 5 \?Ffy> 0 V I - 1- y 0/00 - J-if s w ^ r A t Voh ( r h ) p Z , L Vox D uL % l IO u L O vL I3*L 9ui iiv i 5v L fu ~ ----------- :---------------- ____ 4 l ______ F nalVolume Final Concentration L too V *L P ro U fVoO OU. foo )U L 1 <)Oc> Page 697 of 703 BACK TO MAIN 3MEnvironmental Laboratory Exact concentration of every point of every analyte Prep date: Analyst: Type of the curve: Target analytes: 0 fJ q * i M ________ - d ____ __ ____ PPOS Shd O " * Y T p y iHPFDiC2 5 ) sf f Sf* V Book No: Page No: 01 oo3 7 Solvent & TN-A #: /*#>//. 7M-4-'`i'rSS Final Volume of each point: Standard mix used for preparing the curve: 101 -J - 5 C^0 *^ )^ / / * Amount MLL Curve point number ofmix { e,b / used w o * Analyte concentration in every point ------- 01003-7-1 01003-7-2 01003-7-3 00 V 5,5/ 3 h.0/ 01003-7-4 !0 01003-7-5 01003-7-6 .aJF... 15.05 H0 01003-7-7 01003-7-8 5 0 50J 9 75 01003-7-9 01003-7-10 Wtn xa 1 0 0 .1 0 iW So \A r 01003-7-11 W 01003-7-12 S 9 0 50/^0 01003-7-13 1049 to&'to 01003-7-14 01003-7-15 01003-7-16 ..(pi... Internal Standards T H F f O i P P 13 S standard concentration r'/c IW<L amount used 1 ~SA concentration in curve / J Jr--. J Same am ount o f Internal standard used in all points, leading to same concentration in every point. Page 698 of 703 BACK TO MAIN MULTI-COMPONENT STANDARD PREPARATION LOG Book No. 00 003 Page No. 147 Sk-PO iG Description: p ro s /P P o fl f p p H S / F a s i t f ^ iX Date Prepared: 4- / 0 0 .. . . . . . . Prepared By: C -m ( Storage Location: 3 * -^ Expiration Date: ie / o 1 Solvent: H & Q 1 4 Source: M . -AtJ2_ Lot#: 3M Trace#: TW|A - *-f"14 0 Expiration Date: 5 0 d K" ' Standard ID # 0 0 0 0 3 - 1 ^ 7 [ Component Standard Description ID# ooooi - Cone, or Purity S b a f a i PFH-S U MgoM- 3<V-03> S O p rr \ DCOOI - t 50 ppm E ohA * ' * \ ?R) ; S0Dpj)w> ? F c * !.. ' ' r 5a M e51+ VteoH 3 4 - IS" S D f O m OOOOI 3 4 -+ 3 0 (7000 1- 3M -05 OOOOI - S b ffrr\ 1 T - i S C O p m Expiration Date Weight or Volume S jo l L*j o l lO im L - JO k /o l IO *> L . fT/l 3 / ol Id *>l. 1 ,0 ^ L. Corr. Weight Final Cone. -- )OpTfrl/Vs* ------------1-C--?[0j/rt /:r \1---------- 1 0 pj0mr\ fi- -_ ^ 1 <n 1 yr -- m I S By '-- ---------------- 1 Final Volume Date:. 3M Environm ental Laboratory j S D -O ^L . ^ e )c m o ia -/iV 00 Page 699 of 703 M t ET&S Chemical Inventory System Chemical Status G Available Discarded Trace #: Chemical Sort Prefix: Chemical Name: CAS/ID #: Manufacturer: CAT/Study #: Lot#: Size: Qty Recorded: Date Recorded: Date Expired: Storage Requirrnents: Chemical Hazard Class TN-A-4451 methanol 67-56-1 EM MX0475-1 40104 4L 12 5/17/00 2005 Flammable 3 BACK TO MAIN 3M Environm ental Laboratory Page 700 of 703 ET&S Chemical Inventory System Chemical Status # Available .O Discarded Trace #: Chemical Sort Prefix: Chemical Name: CAS/IO #: Manufacturer: CAT/Study #: Lot#: Size: Qty Recorded: Date Recorded: Date Expired: Storage Requinnents: Chemical Hazard Class TN-A-4715 Methanol 67-56-1 EM MX0475-1 40276 4L 12 11/10/00 11/10/05 Flammable 3 BACK TO MAIN 3M Environm ental Laboratory Page 701 of 703 BACK TO MAIN ET&S Chemical Inventory System Chemical Status # Available O Discarded - Trace #: Chemical Sort Prefix: Chemical Name: CAS/ID #: Manufacturer: CAT/Study #: lot#: Size: Qty Recorded: Date Recorded: Date Expired: Storage Requirments: Chemical Hazard Class TN-A-4740 methanol 67-56-1 EM MX0475-1 40276 4L 12 11/27/00 11/27/05 flammable 3 " 3M Environm ental Laboratory Page 702 of 703 ET&S Chemical Inventory System t Chemical Status # Available O Discarded Trace #: Chemical Sort Prefix: Chemical Name: CAS/ID #: Manufacturer: CAT/Study #: Lot#: Size: Qty Recorded: Date Recorded: Date Expired: Storage Requirments: Chemical Hazard Class TN-A-4755 Methanol 67-56-1 EM MX0475-1 4L 12 12/11/00 12/11/05 flammable 3 BACK TO MAIN 3M Environm ental Laboratory Page 703 of 703 BACK TO MAIN C ollection Inform ation Site Identification D o w , Loasm ^______________________ Sample ID ____ flbV7SC U b * ^ O Q -. A U M --------------------- :____________ Geographical Reference L a t d L . J * , V7* H '__________ W x' Date o f Sampling t d - I H - O Q _____________________ t _____________ _ Use Pattern (e.g. agricultural, forest, etc.) N n rtijjL> Vamjjuli^_____________ Depth o f Sampling Q~(o"____________________________________ _____ Collected by t --------------- ------------------------------------------- ******************************************************** Site Identification f \ . B a /sLa ^ v. dfiam - L o a s r^ ,_________________ Sample ID A f t / / s E L ah* ____ _______________ Geographical Reference LartX jxtU z _____ L o n s- 9.1*A Q ' Date o f Sampling / 0 -1 * 1 - 0 0 ___________________ _________________ Use Pattern (e.g. agricultural, forest, etc.) _____________ Depth ofSampling 0 ~ 6 >11__________ d _______________________ Collected by __ 'P cdJkAf,------------------------------------------------------ ******************************************************** Site Identification J in c x u L f t jjj& u A j J x r c n t ^ ________________ Sample ID D O - A V o (o A6Yi?> L i b * _____ _______________ Geographical Reference Ln-L+ixJj t , : H T H S ' ____ L & n a ftu J z .i- <1T ..3 .T . Date o f Sampling /0 - 1 ^ -0 0 ______________ _______________ _______ Use Pattern (e.g. agricuhuraL forest, etc.l fL f\ L ilc u u ^ S a tb rn C )_____ Depth o f Sampling Q~ (o 11 _________________________________ Collected by A r - t P D ahJsU .___________________________________ ******************************************************** She Identification , fo f&M. Sample ID AbYlSE U J ) * 0O a J 4 L Geographical Reference LaJbu^L >-, W to 2 ' lj> )r* u M > : - `j b ' Z V Date o f Sampling I D - A l - DO Use Pattern (e.g. agricultural, forest, etc.) Q a A u -h liu A */, Depth o f Sampling 0 - <b11______ "__________ Collected by --------------------------------- ^oury*j^HjU> U K l e U v M , ^ __Vfr*\ M <S>n-a-oo^ u t rv"'m \-A -o o jqffi BACK TO MAIN LABORATORIES AGVISE Soil Characterization Report Highway IS P.O. Box 510 Northwood, ND 68267 (701) 587-6010 FAX (701) 587-6013 email agvisepolarcomnuam Homepage agviselabsxom Submitting firm Protocol or Study No Sample ID. Trial ID. Date Received Date Reported 3M NA KITTSON CO CLAY 0 -6 NA 10- 23-00 1 1 - 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/100 g) 54.5 Percent Organic Carbon Percent Organic Matter pH in 0.01 M CaC12 Total Nitrogen (%) Base Saturation Data Cation Calcium Magnesium Sodium Potassium Hydrogen These tests were cpmple 2.6 4.5 7.2 0.223 Percent ppm 54.2 34.6 0.9 3.6 6.8 5900 2260 110 771 37 in compliance of 40 CFR Part 160. //- -o o Robert Deutsch Date Soil Scientist/Analytical Investigator A g ric u ltu ra l T estin g BACK TO MAIN LABORATORIES Highway IS PO Box 5 Northwood, ND 58267 (701) 587-6010 FAX (70) 687-6013 email agviseSpolarcommjGom Hom epage agvisdabs.com AGVISE S o i l C h a r a c t e r iz a t io n R ep o rt Subm itting firm = 3M P r o t o c o l o r S tu d y No = NA Sample ID. - don UGLEM-LOAM 0 -6 T r ia l ID. = NA Date R eceived = 10-23-00 Date R eported = 10-31-2000 AGVISE Lab NO 00- 2404 P ercent Sand 39 Percent S ilt 50 P ercent C lay 11 USDA T e x t u r a l C la s s (h y d ro m eter m ethod) Loam C ation Exchange C apacity (m eg/100 g) 23.9 P ercent O rganic Carbon P ercent O rganic M atter pH i n 0 . 0 1 M CaC12 T otal N itrogen (%) 4 .9 8 .4 7 .4 0.358 Base S a tu ra tio n Data c a tio n Percent ppm C alciu m M agnesium Sodium P o ta ssiu m Hydrogen 52.2 20.9 0 .7 3 .5 22.7 2500 600 38 324 54 T h e se t e s t s w ere c o m p le te d i n c o m p lia n c e o f 40 CFR P a r t 1 6 0 . _ie M. Jo h n so n A rihlytical In v estig a to r 1 0 - 3 / - O D ate A g ric u ltu ra l Testing BACK TO MAIN LABORATORIES Highway IS P.O. Box 510 Northwood, ND 58267 (701)887-6010 FAX <701)587-6013 em ail agviscpolarcom ntcom Hom epage agvisdab&com AGVISS S o i l C h a r a c t e r iz a t io n R ep o rt Subm itting firm * 3M P r o t o c o l o r S tu d y No = NA Sample ID . = K BROEREN-CLAY LOAM 0 -6 T r ia l ID. * NA Date R eceived = 10-23-00 Date Reported - 10-31-2000 AGVISB Lab NO 00- 2405 P ercen t Sand 21 Percent S ilt 46 P ercent Clay 33 USDA T e x t u r a l C la s s (h y d ro m eter m ethod} C la y Loam C a tio n Exchange C a p a c ity (meq/lOO g) 24.7 P ercen t O rganic Carbon P ercent O rganic M atter pH i n 0 . 0 1 M CaC12 T otal N itrogen (%) 2 .6 4 .4 6 .0 0.216 Base S a tu ra tio n Data C ation B ercen t. ppm C alciu m M agnesium Sodium P o ta ssiu m Hydrogen 52.7 24.3 0 .7 5 .8 16.5 2600 720 39 557 41 T h ese t e s t s w ere c o m p le te d i n c o m p lia n c e o f 40 CFR P a r t 1 6 0 . )u $ iq 7YY)<L O L jQ2V L lie M. JJoolhnson la ly tic a l In vestigator / -3 /-0 0 D ate A g ric u ltu ra l Testing 0 5 / 2 3 / 0 1 WED 1 5 : 1 9 FAX 1 7 0 1 5 8 7 6 0 1 3 AGVISE LABORATORIES LABORATORI ES May 23, 2001 BACK TO MAIN Highway IS P.O. Box 510 Northwood, ND S8267 (701) 507-6010 FA X (701) 587-6013 em ail: agvise8polarcom rn.com H om epage agviselabs.com Mr. Mark Ellefson 3M Corporation Re Soil Characterization forAgvise South Soil collected from 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) gm/cc Cation Exchange Capacity (meq/100 g) 1.05 23.3 % Moisture at 1/3 Bar 27.9 Percent Organic Matter pH in 1:1 soihwater ratio 4.8 % c a c = ^ / 7 J 7.8 Extractable Iron (ppm) Extractable Zinc (ppm) Extractable Manganese (ppm) Extractable Copper (ppm) 10.3 1.59 11.9 0.24 Base Saturation Data Cation Calcium Magnesium Sodium Potassium Hydrogen Percent 79.5 10.0 0.8 2.5 7.2 ppm 3700 280 41 231 17 Vo Robert Deutsch Soil Scientist A g ric u ltu ra l T esting LABORATORIES BACK TO MAIN Highway 15 P.O. Box 510 Northwood, ND 58267 (701) 587-6010 FAX (701) 587-6013 email: agvise@polarcomm.com Homepage agviselabs.com AGVISE S o i l C h a r a c t e r i z a t i o n R e p o r t S u bm itting firm P r o to c o l o r Study No Sam ple ID. T r ia l ID. D ate R eceived D ate R eported 3M NA GOOSE RIVER-SEDIMENT 0 - 6 NA 10-23-00 10-31-2000 AGVISE Lab NO 00- 2406 P ercen t Sand Percent S ilt P ercen t C lay USDA T e x t u r a l C l a s s (h y d r o m e t e r m e th o d ) 39 42 19 Loam C a tio n ExchangeC a p a c ity (m eq/100 g) 17.5 P ercen t O rganic Carbon P ercen t O rganic M atter pH i n 0 . 0 1 M CaC12 T otal N itrogen (%) 1 .3 2 .3 7 .7 0.101 Base S a tu ra tio n D ata C ation Percent ppm C alcium M agnesium Sodium P otassium H ydrogen 57.2 28.6 4 .8 3 .4 6 .0 2000 600 193 232 10 T h e s e t e s t s w e r e c o m p l e t e d i n c o m p li a n c e o f 4 0 CFR P a r t 1 6 0 . A n a ly tica l In v e stig a to r IQ - 3 1 - 0 0 D ate A g ric u ltu ra l T estin g BACK TO MAIN R a t i o n a l i n s t i t u t e -of J ^ ta n im r s S c f& z th p iB ltx g Q **"* ( E t r t x i i t n t t a i S ta n d a rd R e fe r e n c e M aterial 2 7 8 1 Domestic Sludge This Standard Reference Material (SRM) is intended primarily for use in the evaluation of martin^ used for the analysis of sludges and other materials of a similar matrix. SRM 2781 is a dried and pulverized domestic sludge. A unit of SRM 2781 consists of 40 g of the dried material. Certified Values: The certified values for 10 elements are listed in Table 1 end are based on concordant results from two or more analytical methods. Analytical methods used for the characterization of this SRM are given in Table 3. All values are reported as m? fractions [1], on a dry mass basis and are based on measurements using a sample m of at least 100 mg. Noocertifled Values: Noncertified values for eleven additional elements are listed in Table 2 and were derived from a combination of results from NIST and collaborating laboratories. These results may have sources of bias yet to be investigated and do not meet NIST criteria for certification. Expiration of Certification: This certification is valid for five years from the date of shipment from NIST. However, the certification will be nullified if the SRM is contaminated or modified. Should any of the values change before the expiration of the certification, purchasers will be notified by NIST. Return of the attached registration card will facilitate notification. Stability: This material is considered to be stable; however, its stability has not been rigorously assessed. NIST will continuously monitor this material and report any 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 complete dissolution for analytical determinations to be related to the certified values provided. Instructions for Drying: When nonvolatile elements are to be determined, samples should be vacuum dried at room temperature for 24 h or oven dried for 2 h at 110 *C. Volatile elements (e.g., arsenic, mercury, and selenium) should be determined on samples as received; separate samples should be dried according to these instructions to obtain a correction factor for moisture. Moisture corrections are then made to measurement values before comparing them to the certified values. [Note that die mass loss on drying at the time of certification was found to be in the range of 4.7 %to 6.6 % when using the recommended drying procedures.] Statistical consultation was provided by L.M, Gill of the NIST Statistical Engineering Division. The overall direction and coordination of the analyses were under the chairmanship of J.D. Fassett of the NIST Analytical Chemistry Division. The technical and support aspects 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 through the Standard Reference Materials Program by B.S. MacDonald. Gaithersburg, MD 20899 Certificate Issue Date: October 25, 1996 (Revision of certificate dated 6-22-95 to include addendum) Thomas E. Gills, Chief Standard Reference Materials Program Page 1 o f 4 BACK TO MAIN Source and Preparation of Material: The U S. Geological Survey (USGS), under contract to NIST, obtained partially dehydrated sewage cake material from the Metropolitan Denver Sewage Disposal District No. 1. The material (approximately 182 kg) was placed in plastic-lined drams and transponedto the USGS facilities in Lakewood, CO for processing. It was dried at ambient temperature in a forced air chamber, ground to pass a 74 m. (200 mesh) sieve, blended for 24 h to assure homogeneity of the pulverized material after which test samples were taken from the blender for preliminary homogeneity analyses. The material was then radiation sterilized. The sterilized material was shipped in bulk to NIST, where the material was bottled in 40 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) and/or inductively coupled plasma atomic emission spectrometry (ICP-AES). Homogereity was further assessedduring certification analysis; at sample sizes of 100 mg or greater. No sample-tosample variations in excess of those expected from the analytical measurements were detected. Certified Values and Uncertainties: The certified values are die means of de results from two or more independen analytical methods as described by Schiller and Eberhaidt [2]. The uncertainty is based on a 95 %confidence interval for die true value, and includes an allowance for differences between the analytical methods used [3]. Table 1. Certified Mass Fractions Element Mass Fraction (inmg/kg) Element Mass Fraction (in %) Arsenic Cadmium Copper Lead Mercury Molybdenum Nickel Selenium Zinc 7.82 0.28 12.78 0.72 627.4 13.5 202.1 6.5 3.64 0.25 46.7 3.2 80.2 2.3 16.0 1.6 1273 53 Nitrogen 4.78 0.11 Noncertifled Value and Uncertainties: The noncertified values are the means of the results from two or more inHop^rwfUiv analytical methods as described by Schiller and Ebeihardt [2]. The uncertainty is based on a 95 % interval for die mean, and includes an allowance for differences between the analytical methods used [3]. As the accuracy of the measurements could not be assessed from the data, the uncertainty associated with a prwrnjffrd value may fail to include all sources of uncertainties and may represent only a measure of the precision of the measurement methods. Table 2. Noncertified Mass Fractions Element Mass Fraction (in mg/kg) Element Mass Fraction (in * ) Chromium Silver 202 9 98 8 Aluminum Calcium Iron Magnesium Phosphorus Potassium Silicon Sodium Titanium 1.6 0.1 3.9 0 .1 2.8 0.1 0.59 0.04 2.42 0.09 0.49 0.03 5.1 0.2 0.21 0.02 0.32 0.03 .. > Page 2 o f 4 BACK TO MAIN A d d en d u m to S tan d ard R e fe r e n c e M aterial 2 7 8 1 Domestic Sludge Leachable Mass Fractions Using U.S. EPA and NJDEP Methods for Flame Atomic Absorption Spectrometry and Inductively Coupled Plasma Atomic Emission Spectrometry The certified concentration values of constituent elements in this certificate are given as total mass fractions. To obtain total mass fractions, either subsamples of the SRM must be completely decomposed, or the sample must be analyzed directly in its solid form. For mixed acid dissolution, hydrofluoric acid must be included in the acid mixture to totally dissolve siliceous material present in sludge. For a number of environmental monitoring purposes, acid extractable mass fractions of elements are often used 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 reports as loud results. However, reported acid labile or extractable fractions of elements are generally lower than total mass fractions. Results are often presented as measured mass fractions in the leachate in comparison to die total or certified mass fractions. The recovery of an element as a percent of total is a function of several factors such as the mode of occurrence in the sample, leach medium, leach time, temperature conditions, and pH of the sample-leach medium mixture [1], ' In its monitoring programs, the U.S..Environmental Protection Agency (U.S. EPA) has established a number of leach methods, such as Methods 3015, 3050, and 3051 [2,3] fen' the determination of acid labile or extractable mass fractions of elements. The New Jersey Department of the Environment (NJDEP) has developed its own leach method, NJDEP 100 for state use [4]. The NJDEP and the U.S. EPA prepared samples of SRM 2781 using the NJDEP 100 method and EPA Methods 3050 and 3051 and analyzed the resulting leachates by flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Reference values have been established for the acid-teachable mass fractions of several elements in SRM2781. These values are the means of all results from the different leach measurement methods and combinations used. The reference values are listed in Table 1, along wahtbsiruncertainties which ate basedon 95 %confidence intervalsof the meats of results. For some of the elements (copper, iron, silver, vanadium), no statistically significant differences were found among results from the two laboratories using three or four combinations of sample preparation and instrumental measurement techniques (NJDEP 100 - FAAS; NJDEP 100 - 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 the stated uncertainties. 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 Uncertainties: The reference values given in Table l are not NIST certified but are provided as a reference for U.S. EPA 3050 and 3051. and NJDEP 100 methods. The uncertainties are based on a 95 % confidence interval for the mean and include an allowance for differences between the analytical methods used. Gaithersburg, MD 20899 Addendum Issue Date: October 25, 1996 Thomas E. Gills, Chief Standard Reference Material Program Page 1 of 2 BACK TO MAIN Element Aluminum Barium Cadmium Calcium Chromium Copper Iron Lead Magnesium Manganese Nickel Silver Vanadium Zinc Table 1. Reference Leach Values for SRM 2781 Leachable mass fraction (in mg/kg) 8 040 570 11 36 440 143 601 24 300 183 4 850 745 72.3 86.3 81.9 1 120 980 65 2 1830 14 16 2 100 15 290 33 6.3 1.7 3.8 34 %Leach Recovery* 50 _ 86 93 71 96 87 91 82 -- 90 88 -- 88 %Leach Recovery * 100 * _______ Leach Value_______ Certified or Noncertified Value Cooperatine Analysts and Laboratories: S.J. Nagoumey; New Jersey Department of the Environment, Trenton. NJ. J. Birri, K. Peist; U.S. Environmental Protection Agency, Edison, NJ. REFERENCES [1] Kane, J.S., Leach Data vs Total: Which is {levant for SRMs, Fresenius J. Anal. Chem. 352: pp 209-213, (1995). [2] U.S. EPA 1991 Code of Federal Regulations, Tide 40, Pan 136, Paragraph 33. [3] Federal Register 1-13-95 SW-846 update #2, Final. [4] New Jersey Administrative Code, 1994. N.J.A.C. 7:14-4. > Page 2 of 2 BACK TO MAIN * *j Table 3. Methods used for the Analysis of SRM 2781* Aluminum Arsenic Cadmium Calcium Chromium Copper Iron Lead Magnesium Mercury Molybdenum Nickel Nitrogen Phosphorus Potassium Selenium Silicon Silver Sodium Titanium Zinc INAA, ICP-AES, XRF RNAA, Hyd. AAS, INAA ID-ICPMS, PGAA, RNAA. INAA, TXRF INAA, TXRF, ICP-AES, XRF INAA. TXRF, ICP-AES ID-ICPMS, RNAA, INAA, TXRF INAA. TXRF, ICP-AES, XRF ICP-AES, ID-ICPMS, TXRF INAA. ICP-AES, XRF FIA-CV-AAS, RNAA, INAA ID-ICPMS, ICP-AES, TXRF, INAA ICP-AES, ID-ICPMS, INAA. TXRF KjeldaM, PGAA Color, ICP-AES. XRF INAA, TXRF. ICP-AES Hyd. AAS, RNAA, INAA, TXRF XRF RNAA, INAA, TXRF INAA, ICP-AES, XRF INAA. TXRF, XRF ICP-AES, ID-ICPMS, INAA, TXRF "Methods used for esabiisfamenofcertified values are shown in bold-face type; methodsusedfor information only values or to corroborate certified valuesare not in bold. Methods FIA-CV-AAS Hyd. AAS ICP-AES ID-ICPMS (NAA PGAA RNAA TXRF XRF How infection analysis cold vapor atomic absorption spectrometry Hydride generation atomic absorption spectrometry Inductively coupled plasma atomic emission spectrometry Isotope dilution inductively coupled plasma mass spectrometry Instrumental neutron activation analysis Prompt gamma activation analysis Radiochemical neutron activation analysis Total reflectance x-ray fluorescence Wavelength dispersive x-ray fluorescence NIST Analysts M.H. Ahsan E.S. Beary C. M. Beck II D. A. Becker M S. Epstein K. Garrity R.R. Greenberg R.M. Lindstrom E.A. Mackey J.R. Moody B.R. Norman P.J. Paulsen M.S. Rearick T.A. Rush R. Saraswati J.M. Smeller R.L. Watters, Jr. L.J. Wood Page 3 o f 4 BACK TO MAIN Cooperating Analysts and Laboratories: - S. Landsberger and D. Wu; University of Illinois, Nuclear Engineering Department, Champaign. IL S.A. Wilson, D. Stems, and P. Briggs; USGS, Lakewood, CO A. Prange. U. Reus, and R. Neidergesiss; GKSS Research Center, Institute of Physical and Chemical Analytics. Geesthacht, Germany REFERENCES [1] Taylor, B.N., 'Guide for the Use of the International System of Units (SI).' NIST Special Publication 811, 1995 Ed., (April 1995). [2] Schiller, S.B. and Eberhardt, K.R., Combining Data from Independent Chemical Analysis Methods, Spectrochimkal Acta, 46B (12), pp 1607-1613, (1991). [3] Guide to the Expression of Uncertainty in Measurement. ISBN 92-67-10188-9, 1st Ed. ISO, Geneva, Switzerland, (1993): see also Taylor, B.N. and Kuyatt, C.E.. 'Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results,* NIST Technical Note, 1297, U.S. Government Printing Office, Washington D.C.. (1994). f, ' Page 4 o f 4