Document Mb4KrG1kReOQMDnoJ4oOp8L

AR226-1030A027 Study Title Characterization Study of PFOS, Primary Standard - Test Control Reference #TCR-00017-046 Phase: Solubility of PFOS in Octanol Data Requirement 40 CFR 160.105(b) Author Mark E. Ellefson Phase Completion Date Date of signing Performing Laboratory 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Environmental Laboratory Study # FACT-TCR002 (LIMS #E00-1716) Centre Analytical Laboratories Study # 023-021 Total Number of Pages 109 BACK TO MAIN GLP Compliance Statement Study Title: Characterization Study of PFOS, Primary Standard - Test Control Reference # TCR-00017-046, PHASE: Solubility of PFOS in Octanol. Study Identification Number: FACT-TCR002, Centre Analytical Laboratories Study # 023-021 This phase of the study was conducted in compliance with Environmental Protection Agency (EPA) Good Laboratory Practice (GLP) Standards 40 CFR 160 with the exceptions in the bulleted list below. Exceptions to GLP compliance: The electronic data systems in use have not been validated and there is not an electronic audit trail of corrections currently available (40 CFR 160.130 (e)). Authenticated hardcopies of chromatograms and associated documents will be considered as the original raw data. William K. Reagen, Testing Facility Management Date FACT -TCR002 (LIMS #E00-1716), Page 2 of 109 BACK TO MAIN Quality Assurance Statement Study Title: Characterization Study of PFOS, Primary Standard - Test Control Reference # TCR-00017-046, PHASE: Solubility of PFOS in Octanol. Study Identification Number: FACT-TCR002, Centre Analytical Laboratories Study # 023-021 This phase of the study has been inspected 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 04/11/01-04/13/01 04/13/01 Phase Data Draft Phase Report Date Reported to Managem ent S tu d y D ire ctor 04/18/01 04/18/01 04/18/01 04/18/01 Date FACT -TCR002 (LIMS #E00-1716), Page 3 of 109 BACK TO MAIN Table of Contents GLP Compliance Statement............................................................................................................... 2 Quality Assurance Statement............................................................................................................. 3 Study Information................................................................................................................................6 Summary.............................................................................................................................................7 Purpose............................................................................................................................................... 7 Test Substance...................................................................................................................................7 Test System........................................................................................................................................8 Method Summaries............................................................................................................................ 8 Preparatory Methods.......................................................................................................................... 9 Sample Collection and Analysis......................................................................................................... 11 Analytical Method............................................................................................................................... 11 Analytical Results...............................................................................................................................12 Data Summary................................................................................................................................... 13 Statistical Methods............................................................................................................................. 15 Statement of Conclusion.................................................................................................................... 15 References............................................................................................................... ..........................15 List of Attachments............................................................................................................................. 16 Signature Page................................................................................................................................... 17 Attachment A: Extraction and Analytical Methods.............................................................................18 Attachment B: Data Summary Tables................................................................................................ 48 Attachment C: Sample Chromatograms............................................................................................67 Attachment D: Deviations from the Protocol.................................................................................................... 103 Attachment E: Sample Calculations...................................................................................................108 FACT -TCR002 (LIMS #E00-1716), Page 4 of 109 BACK TO MAIN List of Tables Table 1. Summary Table of Solubility of PFOS TCR-00017-046 in Octanol..................................... 7 Table 2. Characterization of the Test Substance and Analytical Reference Substances................ 7 Table 3. Description of the test system used in this study...............................................................8 Table 4. Solubility Screen Test Sample Preparation........................................................................ 10 Table 5. Shake Flask Method Preparation for Study (FACT-TCR002)............................................. 10 Table 6. Sample Collection and Preparation for Study FACT-TCR002........................................... 11 Table 7. Calibration Standard Reprocessing Summary..................................................................... 13 Table 8. PFOS TCR-00017-046 Solubility in Octanol Data Summary.............................................. 14 Table 9. Summary Table of Solubility of PFOS TCR-00017-046 in Octanol.......................................15 FACT -TCR002 (LIMS #E00-1716), Page 5 of 109 BACK TO MAIN Study Information Study Director John Flaherty Centre Analytical Laboratory 3048 Research Drive State College, PA 16801 Analytical Chemistry Laboratories Solubility Testing Certificate of Analysis 3M Environmental Technology and Safety Services (ET&SS) 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Centre Analytical Laboratory 3048 Research Drive State College, PA 16801 John Flaherty, Study Director Dr. William K. Reagen, Laboratory Manager Mark E. Ellefson, Principal Analytical Investigator Kristin L. Terrell, Analytical Chemist Mark L. Anderson, Analytical Chemist Cindy M. Carlson, Analytical Chemist Sponsor 3M Environmental Laboratory 935 Bush Avenue Building 2-3E-09 St. Paul, MN 55106 Dr. William K. Reagen Experimental Dates Experimental Start Date: 29 September 2000 Experimental Termination Date: 30 March 2001 Archives Reserve samples of the reference standards will be maintained by the 3M Environmental Laboratory. All study data for this phase and a copy of the phase report are archived by the 3M Environmental Laboratory. FACT -TCR002 (LIMS #E00-1716), Page 6 of 109 BACK TO MAIN Summary The approximate solubility of PFOS in octanol was determined by performing a solubility screen test, followed by a quantitative solubility determination via Shake Flask Method. Results are presented in table 1: Table 1. Summary Table of Solubility of PFOS TCR-00017-046 in Octanol. S ampling E vent Day 1 Day 2 Day 3 Average Value PFOS S o lubility in O c ta n o l (C orrected for Purity) 56.9 pg/mL 55.7 pg/mL 55.4 pg/mL 56.0 pg/mL Standard Deviation 0.9 1.4 2.5 0.8 % CV 1.6% 2.5% 4.5% 1.4 The solubility of PFOS TCR-00017-046 in octanol was determined to be 56.0 pg/mL at 22-23 C. Purpose The purpose of this phase of the study was to determine the solubility of PFOS in octanol as part of the characterization of this test, control, and reference substance. T est S ubstance PFOS, Test Control Reference #TC R -00017-046 Table 2. Characterization of the Test Substance Test Substance PFOS Source Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity Re-crystallized by George Moore, 3M Specialty Materials, Bldg. 236-1B-10 01-01-2010 Frozen TCR-00017-046 White Powder 97.9% FACT -TCR002 (UNIS #E00-1716), Page 7 of 109 BACK TO MAIN Reference- S ubstance Table 3. Characterization of the Analytical Reference Substances Reference S ubstance PFOS THPFOS PFBS Source Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity Re-crystallized by George Moore, 3M Specialty Materials, Bldg. 236-1B-10 01-01-2010 Frozen TCR-00017-046 White Powder 97.9% SynQuest Labs Pat Savu, 3M Not Available Not Available Frozen Frozen TCR-00017047 Lot #Q7530 Primary Standard, TCR99030-23 (L-7038, F-8442); Lot 101 White Powder * White Powder * * The purity of THPFOS and PFBS (cunentiy being detennined by Centre Analytical Laboratory) will not affect any analytical findings since it is used as a reference substance only. T est System Table 4. Description of the test system used in this study Test System/Solvent Source Expiration Date Storage Conditions 3M Laboratory Identification Number P urity/G rade Octanol Screen Test S hake Flask M td . Aldrich 2005 Flammable Cabinet TN-A 3353 99+% Aldrich 11-01-05 Flammable Cabinet TN-A 4703 99.9+% HPLC Grade Method Summaries The solubility determination of PFOS TCR-00017-046 in octanol was performed according to 3M Environmental Laboratory methods ETS-8-170.0 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents;" and ETS-8-172.0 "Shake Flask Method; Solubility Determination of a Test Substance in Various Solvents" as adapted from United States Environmental Protection Agency OPPTS 830.7840, "Water Solubility; Column Elution Method; Shake Flask Method" and OECD 105, "Water Solubility" Guidelines. Methods ETS-8-170.0 and ETS-8-172.0 were subsequently revised to include additional information/clarification. The new FACT -TCR002 (LIMS #E00-1716), Page 8 of 109 BACK TO MAIN revisions, ETS-8-170.1 and ETS-8-172.1, are procedurally the same as the predecessors and shall be included in Attachment A of this report. All analyses were performed according to the 3M Environmental Laboratory method ETS-8-155.0 "Analysis of Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry". The Solubility Screen Test Method (ETS-8-170.0) was used to determine the solubility range of PFOS TCR-00017-046 in octanol. Incremental amounts of octanol were added to PFOS neat material and a qualitative determination of the solubility point was made. The screen test indicated a solubility of PFOS in octanol of less than 10 pg/mL at 23 C. It is recommended that the solubility of substances having a solubility of less than 10 pg/mL be determined via the Column Elution Method. However, the Shake Flask Method was used for the quantitative determination of PFOS solubility because of the difficulty in finding compatible tubing (preliminary results demonstrated that the tubing swelled and cracked when in contact with octanol for extended periods of time) and the possible explosion hazard of containing a non-sealed container of a flammable solvent in an incubator equipped with electrical outlets on the inside. Detailed descriptions of the Solubility Screen Test Method and Shake Flask methods used in this study are located in Attachment A. Preparatory Methods ETS-8-170.0 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents." This method is a prerequisite to the shake flask and column elution methods and gives an estimate of the solubility point of the test substance in the solvent of choice. Approximately ten milligrams of PFOS was weighed into a glass vial, and varying amounts of octanol were added in a step-wise fashion. After each octanol addition, the vial was shaken, sonicated, and observed for particulate. When particulate was observed in a final volume of 2 mL of octanol (approximately 5000 pg/mL), the final step of the screen test was initiated. Fourteen point one mg PFOS was placed into a 100 mL volumetric flask and octanol was added in a step-wise fashion up to 100 mL (with shaking, vortex-mixing, sonicating, and observations for particulate in between). Particulate was still observed at 140 jjg/mL, therefore 2.48 mg was weighed into a 250 mL flask and filled to the mark with octanol for a final concentration of approximately 10 pg/mL. The particulate did not dissolve after more than 24 hours of contact at 23 C. The screen test estimated the solubility of PFOS in octanol to be less than 10 pg/mL. This concentration estimation was used as a starting point for the shake flask method, and as a guide to determine the amount of dilution necessary to bring the final sample concentration into the analytical range of method ETS-8155.0 (2.5 - 1002 ng PFOS/mL). FACT -TCR002 (LIMS #E00-1716), Page 9 of 109 BACK TO MAIN Table 4. Solubility Screen Test Sample Preparation S tep 1 2 3 4 5 6 7 8 C en tr ifu g e T u bes P repa r a tio n 10 mg test substance weighed into tared 4.0 mL glass screw-capped vial 0.1 mL of octanol added to glass screw-capped vial Following the addition of octanol, vial was capped, shaken vigorously and vortexed, and sonicated. Mixing and sonication times recorded on the worksheet. Sample checked visually for undissolved particles of the test substance. (If all of the test substance is dissolved, the solubility is determined to be greater than 10% (mass/volume) and no additional solubility testing is required. If a portion of the test substance remains undissolved, additional dilutions are performed using the appropriate solvent.) Observation made: undissolved particles present... continue to step 5. Step 2 repeated with total volume of octanol of 0.5,1, and 2 mL, respectively. Following octanol addition, vial was shaken, sonicated, and observed for particulate. Following the final octanol addition to bring the volume of octanol to 2 mL, there was still undissolved PFOS. The shake flask method would therefore be continued to step 7. 14 mg were weighed into a 100 mL volumetric flask and octanol was added stepwise up to 100 mL. Following each addition of octanol the flask was capped, vortex-mixed, sonicated, and allowed to settle. Particulate still remained. Therefore 2.5 mg PFOS were diluted in 250 mL octanol. The flask was vortex-mixed, sonicated, and allowed to settle for >24 hours. The concentration of octanol was approximately 10 pg/mL and there was still particulate. A solubility < 10 pg/mL would require the column elution method to quantitatively determine the solubility. However due to difficulties with tubing selection and the potentially dangerous solvent conditions of having a non-sealed container of flammable solvent in an incubator equipped with electrical outlets on the inside, it was decided that the shake flask method shall be used for the solubility determination. ETS-8-172.0 " Shake Flask Method: Solubility Determination of a Test Substance in Various Solvents." Approximately 0.01 Og PFOS was weighed into a tared 15 ml. plastic centrifuge tube. Octanol was added gravimetrically to approximately 8.5 g (approximately 10 ml_). Nine centrifuge tubes w ere prepared, along with three method blanks (tubes w ith 8.5 g 0.5 g octanol only). The centrifuge tubes were placed in a temperature-controlled orbital shaker set at approximately 30C. See the following table documenting the shake flask method preparation: Table 5. Shake Flask Method Preparation for Study (FACT-TCR002) S tep C en tr ifu g e T ube P r epa r a tio n R eplic a tes 1 * 0.010 g PFOS weighed into tared 15 mL centrifuge tube g 2 Octanol added to centrifuge tube such that total weight of PFOS g and octanol is approximately 8.5 g. 3 Method Blank Preparation- Approximately 8.5 g octanol added to a 3 tared centrifuge tube gravimetrically. 4 Samples sealed with tape, vortex-mixed, and placed in a 12 temperature-controlled orbital shaker set at approximately 30.0 C, rotation speed set at approximately 150 rpm. Da te (s ) Performed 01-22-01 01-22-01 01-22-01 01-22-01 FACT -TCR002 (LIMS #E00-1716), Page 10 of 109 BACK TO MAIN Sample Collection and A nalysis On each of Days 1, 2, and 3 (approximately 24, 48 and 72 hours after initial sample preparation) three centrifuge tubes (containing PFOS) and a method blank were removed for analysis. The centrifuge tubes with PFOS and method blanks were allowed to equilibrate at 22-23 C for 24 hours, centrifuged, and aliquots of supernatant were collected. The aliquots were diluted 100X (990 pL methanol: 10 pL sample) and spiked with internal standard (17 pL of 15 pg THPFOS and PFBS/mL) and analyzed via HPLC/ES/MS according to analytical method ETS-8-155.0. Four injections of each final diluted sample were performed. The following table describes the sample collection and preparation regimen: Table 6. Sample Collection and Preparation for Study FACT-TCR002 S tep 1 P rocedure At 24,43, and 72 hours, 3 PFOS+ odanol, and 1 octanol (method blank) centrifuge tubes are removed from the incubator and equilibrated at 4-25 C for approximately 24 hours. R eplic a tes 4 centri fuge tubes per day Day1 Day2 Day3 2 Aliquots of the supernatant (octanol containing 4 per Day1 dissolved PFOS or octanol only from the method blanks) were collected and dispensed into autovials. centrifuge tube Day2 Day3 3 The aliquots were diluted 100X with methanol (using a dual syringe diluter). Day 1 Day 2 Day 3 4 Internal Standard was added to the 100X sample dilutions (17 (xL THPFOS and PFBS solution at 15 |xg /mL in methanol). 5 Samples were analyzed via HPLC/ES/MS on HP 1100 LC/MSD Day 1 Day 2 Day 3 Day 1 Day 2 Day 3 D a t e (s ) P er fo r m ed 01-23-01 01-24-01 01-25-01 01-24-01 01-25-01 01-26-01 01-24-01 01-25-01 01-26-01 01-24-01 01-26-01 01-26-01 through 01-27-01 01-27-01 01-30-01 Analytical Method ETS-8-155.0 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry". Diluted samples (i.e. diluted supernatants) were analyzed using HPLC/ES/MS in the negative ion mode. PFOS levels were evaluated versus calibration standards ranging in concentration from 2.5-1002 ng PFOS/mL. Internal Standard quantification was used to normalize the data. Target ions were 499 m/z (PFOS anion), 427 m/z (deprotonated THPFOS), and 299 m/z (PFBS anion). Analytical Equipment FACT -TCR002 (LIMS #E00-1716), Page 11 of 109 BACK TO MAIN Liquid Chromatograph: Hewlett-Packard Series 1100 Liquid Chromatograph system Analytical column: Keystone BetasilTM C182x50mm, 5pm particle size Column temperature: Ambient Cycle Time: 10 minutes Flow rate: 300pL/min Injection volume: 10pL Mobile phase components: Solvent A: 2.0 mM ammonium acetate in water Solvent C: Methanol Solvent Gradient: Time 0.00 0.50 0.80 3.50 6.50 7.00 9.75 10.00 %C 15% 15% 60% 100% 100 % 15% 15% Stop Mass Spectrometer: Hewlett-Packard Series 1100 API/Mass Spectrometer Detector Software: HP ChemStation" 6.0 Fragmentar Voltage: m/z 299=100 V; m/z 427=100 V; m/z 499= 140 V Capillary Voltage: 3500 V Gain = 2.0 EMV Mode: Electrospray Negative Gas Temperature: 350 C Drying Gas: 10.0 L /min. Nebulizer Pressure: 25 psig Analysis Type: Single Ion Monitoring (SIM) Analytical Results Data quality objectives outlined in the 3M Environmental Laboratory method were met (see Appendix A). Regressions. Quadratic curve fit was applied to calibration standards and sample data to improve quantitation over the concentration range appropriate to the data. All calibration curves had least-square fits of 0.980 or greater (R2 values ranged from 0.9994-0.9997). Calibration Standards. Twelve standards ranging in concentration from approximately 2.5 to 1002 ng PFOS/mL methanol were used for the calibration curves. Calibration curves were run before and after every analytical sequence. Calibration standards were also evaluated for accuracy, and were consistently < 15% difference from the expected value. Sample Replicates. Samples were within the 15% precision requirement. FACT -TCR002 (LIMS #E00-1716), Page 12 of 109 BACK TO MAIN Continuing Calibration Verification. For quantitative determinations, a mid-level matrix calibration check was analyzed every ten samples to monitor instrumental drift, with a limit of 15% deviation of the target concentrations. (Note: the method states a 30% deviation of the target concentrations, but to be consistent with the more stringent sample requirements of 15% precision, the accuracy requirement of the CCVs was reprocessed as 15%). Limit of Quantitation (LOQ). The LOQ is equal to the lowest standard in the calibration curve (25 ng/mL). Table 7. Calibration Standard Reprocessing Summary Data S ub Ba tc h , A nalysis Date C alibration S tandards Day 1 data: 01-26-01 25-1002 ng/mL Day 2 and 3 data: 01-26-00, 01-29-00 25-1002 ng/mL S tandards not u sed , reason for exclusion Std 1 (2.5 ng/mL), Std 2 (5 ng/mL), and Std 3 (10 ng/mL) were excluded to betterfit the data at the low end of the curve and because the hlgh/lowstandards did not meet the <15% deviation criteria. Std 1 (2.5 ng/mL), Std 2 (5 ng/mL), and Std 3 (10 ng/mL) were excluded to be consistent with Day 1 data work up. Blanks. Method blanks (octanol 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). Solvent blanks (methanol injections) provided a measure of instrument contamination. Acceptable solvent blanks must contain levels of target analyte less than 50% of the limit of quantitation (LOQ). Acceptable solvent blanks were analyzed before each calibration curve. Specificity (according to OPPTS 830.7840): The solubility determination as stated in the EPA Guidelines follows. This method should only be applied to: Pure substance. This study shows a purity of 97.9%. Substances that are stable in water. Hydrolytic studies have been conducted at the 3M Environmental Laboratory showing stability (Report # W1878). Data Summary Table 8 summarizes individual sample data. Representative chromatograms are presented in Attachment C. The table displays PFOS concentrations for individual injections. Also included are the average concentrations for each Centrifuge Tube replicate, standard deviation, and % coefficient of variation. FACT -TCR002 (LIMS #E00-1716), Page 13 of 109 BACK TO MAIN Table 8. PFOS TCR-00017-046 Solubility in Octanol Data Summary S a m p le ID TCR-00017-046 PFOS ug/m L C orrected for P urity Day 1 Centrifuge Tube#1 Day 1 Centrifuge Tube #2 Day 1 Centrifuge Tube #3 Day 2 Centrifuge Tube#l Day 2 Centrifuge Tube #2 Day 2 Centrifuge Tube #3 Day 3 Centrifuge Tube#1 Day 3 Centrifuge Tube #2 Day 3 Centrifuge Tube #3 Rep 1: 012201-oPFOS-1.1.1 Rep 2:012201-oPFOS -1.1.2 Rep 3:012201-oPFOS-1.1.3 Rep 4:012201-oPFOS -1.1.4 Rep 1:012201-oPFOS-1.2.1 Rep 2:012201-oPFOS -1.2.2 Rep 3:012201-oPFOS -1.2.3 Rep 4:012201-oPFOS-1.2.4 Rep 1:012201-oPFOS-1.3.1 Rep 2:012201-oPFOS -1.3.2 Rep 3:012201-oPFOS -1.3.3 Rep 4: 012201-oPFOS -1.3.4 Rep 1:012201-oPFOS -2.1.1 Rep 2:012201-oPFOS -2.1.2 Rep 3:012201-oPFOS -2.1.3 Rep 4:012201-oPFOS -2.1.4 Rep 1:012201-oPFOS -2.2.1 Rep 2:012201-oPFOS -2.2.2 Rep 3:012201-oPFOS -2.2.3 Rep 4:012201-oPFOS -2.2.4 Rep 1:012201-oPFOS-2.3.1 Rep 2:012201-oPFOS -2.3.2 R e p 3: 0 1 2 2 0 1 -o P F O S -2 .3 .3 Rep 4:012201-oPFOS -2.3.4 Rep 1:012201-oPFOS-3.1.1 Rep 2:012201-oPFOS -3.1.2 Rep 3:012201-oPFOS -3.1.3 Rep 4:012201-oPFOS -3.1.4 Rep 1:012201-oPFOS-3.2.1 Rep 2:012201-oPFOS -3.2.2 Rep 3:012201-oPFOS -3.2.3 Rep 4:012201-oPFOS -3.2.4 Rep 1:012201-oPFOS -3.3.1 Rep 2:012201-oPFOS -3.3.2 Rep 3:012201-oPFOS-3.3.3 Rep 4:012201-oPFOS -3.3.4 59.1 57.4 57.6 57.1 59.1 55.7 57.7 55.0 55.7 55.7 56.9 55.5 55.2 56.5 54.6 56.8 54.9 53.8 54.2 54.1 57.3 57.0 5 5 .5 58.3 54.7 55.4 57.1 54.2 53.4 52.9 52.7 52.7 59.3 57.2 57.7 57.7 A verage ug/mL S td Dev "/Co e ffic ien t o f v a riatio n 57.8 0.9 1.5% 56.9 1.9 3.3% 56.0 0.7 1.2% 55.8 1.0 . 1.9% 54.2 0.5 0.9% 57.1 1.2 2 .1 % 55.4 1.2 2.2% 53.0 0.3 0.6% 58.0 0.9 1.6% FACT -TCR002 (LIMS #E00-1716), Page 14 of 109 BACK TO MAIN The average PFOS concentration and standard deviation for each day, as well as the final overall average for all non-excluded replicates and time points were as follows: Table 9. Summary Table of Solubility of PFOS TCR-00017-046 in Octanol. S ampling Event Day 1 Day 2 Day 3 P F O S S o lub ility in O ctanol (C orrected for P urity) 56.9 pg/mL 55.7 pg/mL 55.4 pg/mL S tandard D eviation 0.9 1.4 2.5 Average Value 56.0 pg/mL 0.8 % CV 1.6% 2.5% 4.5% 1.4% The solubility of PFOS TCR-00017-046 in octanol is 56.0 pg/mL at 22-23 C. Attachment B contains data summary tables. Statistical Methods Statistical methods were limited to calculating means and standard deviations. Refer to Attachment E for formulas and example calculations. Statement of Conclusion Under the conditions of the present study, the solubility of PFOS TCR-00017-046 in octanol is 56.0 pg/mL at 22-23 C. References 1. Fate, Transport and Transformation Test Guidelines Office of Prevention, Pesticides and Toxic Substances (OPPTS) 830.7840 Water Solubility: Column Elution Method; Shake Flask Method. EPA 712-C-96-041, August 1996. 2. OECD 105: Water Solubility. Adopted 27July, 1995. FACT -TCR002 (LIMS #E00-1716), Page 15 of 109 List of Attachments Attachment A: Extraction and Analytical Methods Attachment B: Data Summary Tables Attachment C: Sample Chromatograms Attachment D: Deviations from the Protocol Attachment E: Sample Calculations BACK TO MAIN FACT -TCR002 (LIMS #E00-1716), Page 16 of 109 BACK TO MAIN S ignature Page We certify that this report is a true and complete representation of the data for this phase of the study: Mark E. Ellefson Principal Analytical Investigator William K. Reagen Laboratory Manager Date FACT -TCR002 (LIMS #E00-1716), Page 17 of 109 BACK TO MAIN Attachment A: Extraction and A nalytical Methods (ETS-8-170.0 and ETS-8-172.0, the methods used in this study, were not included as an attachment. ETS-8-170.1 and ETS-8-172.1, which are procedurally the same, will be included for confidentiality reasons and further clarification of the procedures followed.) FACT -TCR002 (LIMS #E00-1716), Page 18 of 109 BACK TO MAIN 3M Environmental Laboratory Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents Method Number: ETS-8-170.1 Adoption Date: 09/08/00 Effective Date: 03/14/01 Approved By: 1.0 Scope and Application______________________ ;________________________ ;_________ 1.1 APtp(Tdh(fionOoEpeiuhggrtmpTEtereehhcpeSnCr)Eleormoyc-fDmtP8ssyohisoeA)-nrpeo(1lm.aoaUvlC7autueiAi2pSnbnoonn.rdclgl0ndteEeuc)lsOoPtsmoiieimofnhrAEssndliaituCpnt)invoEnibatDaainelgrinbnrudrltygieeidsttitcoiscoyusosuttalh.tomsnulttuaeeeelbdAueMrsdsiOyttb.lsdihai,einortdolItgwyslgihidfvtoatyhotispevnleoiudnriigsscnaezbtterh(salaiiettEin,llthmwailfigTntyeotoyieioS,nrlgnCrlt-oduafhf8tbouufriho-dlebyre>ra1uteynoh7mtttleh1oiue1tns1h0nert.tte0l0'ehi2sEiEsn%)neogUclgeswlu/otutndL(etiainmbiinnltoitol(iednedal1nmbiidest0tctehMsnyhiaS/capciutvdtsetepyaCsoetsimmethlotfoeudeao)setfomrh,dttspcmEhoetoeeehaoni)lrrpdnenu.dtvareadab,tieStiirtienlsoiSholioerinmanhtcmrnykmavoaiiewknemnoneesaFdiefnplrFal<tlyDotaashlbuslase1eaeknsoP0vkdsp*lnreMu2oosrelMebolgtcetueripo/eteelbLchmistqbttihosiylu(eeaoiod1tinrndys0ytist.e 1.2 Compatible Analytes. Test substance and degradation products for solubility testing. ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 19 of 109 Page 1 of 9 BACK TO MAIN 1.3 oAtchceerpstoalbvelentM(s)atorficienste.reAstq.ueous (e.g. Milli-Q water, 0.01M CaCl2), Acetone, Methanol, or 2.0 Summary of Method__________________________________________ ;_____________ 2.1 hhmtgltddodpaasiaP1oehnulpneaiirig2rrsligsgescabtspdoe/nntssehrbdhmsrvlwuoeoborsosoiulotimmtluelyaLmtouaoaxevvfnebpnl.rtskieioesei,necnssmia.nno.ssrct,edwIertalaaaamftAisatuOniicecnthttrftncbheehyiactdyhtenlgotleel1xeildeeo2ceyeihrcSisnte,Ls-vamosthtao5o1dean1ohaele1ol0lsea2unr0ddlemuu0eturrl.mdv.pbb50m.tfbsidlippriniinaenoRiarlmimlgArmlulsoisslien.ietevtsstttLdLyos)yseclfyoe.seAodf.uuf-sonloesnD4l.tufrtrfTttioriltetdettmosv;ehmliMihetsosvnneooteitareitelLtnentralvsmaearslmntc.khutemoagooetseaea1nbcallItsbnhdtsviatsehyfhLton,stadtsiepnatobaensasstbinhwgiohnotrdsgtentebisvrieetclioeocauevwsiarneuynsrrsdveenneteneiehiinusanrtloconftwdilaeihtataelnntfbriikqboto-sosesasvee1eucheusssadnidea0aiaoooilcsfdsrunopd0rlunllhce1iytavovnptyadeiab0psiaeleeflldcot.ukei0Ldiodnztshc,nnph,tsIetmmoip,tvda.aeoefdhttnalivenhoeLvntelaWsrfrho(odteeilito/h2Ec.gaeirrwadvtlcoetmarplrTe,umoelaeAiddtptsexgtwSleashiLiutrsdahdszt(o-oemeimsrE.8denaosiexuaad-sgTritnetIipnb1xoaeosemhtSfpdpsn7trlopssitfutr-iraa1dtlphaftoce8aolttip.nseeipltr-el0vxufolhpolr1ca)oliaisnecnerla.eo7smrwpuvododuas2btspbesxIkaniteoa.suvhsifnrs0itdcleoboomse(taltst)eracyonhlsxllitvinyaulntoowtlneiceasvttmmcbnfreih1donstoeveaecleli0aeencldraytetasftetecifbrnmuteurofopityo1ietrltpdlvsnaceoiynr0gmluineyraurrstsiftbmgroto1ssisislwindscea5oiofga5titelsdhlntagtetskureieonsheent1istotccofsditgth0io.enrt0,eno>r 33..10 TsoDelsvetefsniutnbwitsitilaolnbncese_d._e_At_er_lmi_q_iun_ie_dd_.o__r_s_o_li_d__m_a_t_e_ri_a_l_f_o_r_w__h_ic_h__t_h_e_r_e_la_t_i_v_e_s_o_l_u_b_i_li_ty__i_n_a__s_p_e_c_if_i_e_d__ 3.2 Tmsaeonesldvtthvesanaonrtloivmole,uanasytn.sidanTlcathlcmueedtamoetnrabietcur.eitxsis(teon.gow.th0lii.cm0h1itMtehdeCttoeasCatqls2u(uaeqb)o)su;tasannmcdeaotorrifgciaennst,iecrinescsotlluvisdeininntgtmroAadSturTciceMeds.,TTiynhpceelutIedsWint gater 44..10 WHaeranltihngasnadnSdafCeatyuWtioanrnsi_n_g_s_:____________________________ ._________________ .______ 4.1.1 pWroetaerctthioenparot paellrtliambeas.ttire for all parts of these procedures. Wear gloves and eye 4.1.2 Hpraoncdeldeuarell. solvents in a hood for all parts of the described sample preparation 4.1.3 Fpaocrkpiontgenmtiaatlerhiaazlsa,rdansdof3MeacEhncvhieromnimcaelnutasel dL,arbeoferarttoorym'satCerhieaml siacfaeltyHadzaatardshReeevtsie,w. 4.1.4 No mouth pipetting is allowed. ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 20 of 109 Page 2 of 9 BACK TO MAIN 4.2 Cautions: 4.2.1 mGleatshsawnoarletoinrewdhuiccehtshteanpdoasrsdibsialirteyporfepacacreiddesnhtaolucldonbteamtriipnlaetiroinn.sed with acetone and 55..10 IntIetmseptrusfureibtrisetesannmcceaeyss_hs_oig_un_ldi_f_ibc_ea_nk_tn_lyo_w_a_fnf_ea_cn_td_th_d_eo_cs_ou_lmu_be_ni_lt_iet_yd_op_rf_it_oh_re_to_te_ss_tta_sr_ut_ibn_sg_ta_tnh_ce_e_.s_cT_reh__een_i_pn_ug_ri_pt_yro_oc_ef_dt_hu_er_e. 6.0 Equipment____________________ ;________ '________ '__________________________ 6.1 Analytical balance sensitive to 0.1 mg. 6.2 Vortex mixer. 6.3 Sonicating device. 7.0 Supplies and Materials______________________________________________________ 7.1 Disposable glass graduated pipettes, 1 mL to 100 mL. 7.2 Disposable glass Pasteur pipettes and rubber bulbs. 7.3 Glass beakers, various sizes. 7.4 2.5 mL-4 mL glass screw-top vial. 7.5 Glass volumetric flasks, 10 mL to 1000 mL. 7.6 10 pL-1000 pL PipettemanTM manual pipettor and plastic pipette tips, or equivalent. 8.0 Reagents and Standards_____________________________________________________ 8.1 Methanol (MeOH), HPLC/SPEC/GC grade from EM Science, or equivalent. 8.2 Acetone, HPLC/SPEC/GC grade from EM Science or equivalent. 8.3 Water, ASTM Type I, or equivalent. 8.4 Calcium Chloride Dihydrate, Approximately 99% or better, from Sigma or equivalent. 8.5 Dm0.0iah1rykdMwraiCttehaiMCnlia2l,lwiA-Qei0TMg.0h1wbaMotaetrC.aanCdlt2rsatnoscfkersroinlugtitoonais1pLrevpoaluremdebtryicwfelaigshkianngd1d.5ilugtiCnagCtlo2the 8.6 Test substance of known purity. 9.0 Sample Handling______________________________________^______________________ 9.1 Record times of initial preparation and dilution on a sample preparation sheet or logbook. 9.2 eOxntrcaectthede,ptrheelismcirneaenrytetessttsinamg hpalessbseheonucldombepldeitsepdoasendd itnhteoatphperporporpiaetrewinafsotermstarteiaomn .is ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 21 of 109 Page 3 of 9 BACK TO MAIN 10.0 Quality Control____________________________________________________________ 10.1 Not applicable. 11.0 Calibration and Standardization____________________________________________ 11.1 Tspheecicfoicmatpioounns.ds of interest must be of known characterization according to laboratory 11.2 All equipment used, such as the analytical balance, should be calibrated daily prior to use. 12.0 Procedures__________________________________________________________________ 12.1 Solubility screen. 12.1.1 eWstqaueniidgvaharlde1ni0zte.mdRgperceop1rmdshgteheoet)fw.teesigt hsutb(rsetafenrcteoinattotacah4mmenLtgAlafsosrsacnreewx-atmopplveiaolfoar 12.1.2 Asudbdstsaonlcvee.nt (e.g. water, methanol, acetone) according to the table below to the test 4 mL vial or equivalent Total vaodludmede(smolLv)e.n..t Approximate Solubility (pg/mL)... adSdoiltvioennt1 0.1 100000 adSdoiltvioennt2 0.5 20000 adSdoiltvioennt3 1 adSdoilt2vioennt4 10000 5000 12.1.3 FmrtRoeoeimlnacllouaolritownedwssin.,otgbchVoseaenidsrstudvionaialtuultilioetyoinonacndsohdftoeoincsnoksgtlehvftsoeetolrneslvtut,faenonvndrdotiusaratsprceodcxtlioovzmree5dddiixmnppgraaienprtptupoitcrsetolhhsexeesibe.mateI.bfafooturevenleydmci1sha5sakorisltnev.gceoIdotnbtmdesssea,trysvsobauntebiioscntnaeastcne.ecs2es-a5ry 12.1.4 Icd(d"fEohieeanTtieglctSlrheemp-sln8yatti-rrns1staueio7tcbdil2louse.tntb0osa.l)ndebwcB,ie"seies>ladcol1nailb0svdues%esno,euoltvs(thmehfeeudesanrtsatcohesfo/stenvdetricroemtetlteeuhnasrmetttmreifaneiittgr)nhi.soeeitnsTtashrihposeeeplqv>artueo1ceincxs0retutimdparsa.gduat/bdetmesitstLisaooon,lnulctuhbeobeifsliilhs1tihyta0yal0lpkaobpenieLdnflrtatde.hsgoekHacrusmodomweeludteehbnvaoietsldrti,htyeifis 12.1.5 twIefsettihgsehuttbe(ssrtteafnseucrbetsoitnaatnotctaeacdh1i0md0enmnotLtAdgifsloassorslavvneoeilxnuamtmheeptrl2iecmoflfLaasoksftoasrnodlevaqerunditiv,zaewldeenpitgr.hepR1es0hcmoeergdt)+.the1 mg of 12.1.6 Apaaplrdlepodprwaosrpotahrltiveiaoettnenetsastahmcsecooeoltuu.rndttiionongftstooolsvtehetetnltet.a.bARlesebcdeoelrsodcwraibltloeodtbhisenetr1ev2sat.t1is.ou3nb,ssvtaoanrntdceexprtmoocidxeed,lusivoreensrictoahnteet,haend ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 22 of 109 Page 4 of 9 BACK TO MAIN 1fl0a0skmoLrveoqluuimvaelternict Solvent addition 1 Solvent addition 2 Solvent addition 3 Total volume solvent added (mL)... 10 50 100 Approximate Solubility (pg/mL)... 1000 200 100 12.1.7 Icafontndhcesehnsaotlrllaubtbieoilnuitsyeesdptiomaisnaattiiosstnarerataticnwhghepdicoahintttohfreopsrrutihobersttsaohnatchkeeeiscfolsamoslkpulbmelteeetshahododdui(ltEdioTbnSeo-d8fo-11c0u70m2m.0en)L.t,etdhe 12.1.8 If the 100 mL solvent level has been reached without complete dissolution of test fsluabsskt,agnrcaed,uwaeteigdhcyoluint d1e0rm, ogr eq1uimvagletenst.t sDubilsuttaentcoe 1anLdwtriatnhstfeesrttsooalv1enLt.voTlhuemetric paa11pla77lrpo21tr.wi.0o0ce)xl)edissmh.taoaaIrltfelseinbstcoeto1ilvun2lisc-os2eeib4dnbstlhetreoarovptudieaoredrsntt,eitcortohmufealtialencltsoeeotwsltsuhaumferboenssrotomaelbnluasucbexteiirilovmiitnseyadma.l,tdet1hits0hesoopsdhlguaw/tmkiioelLnlf..blaeTIsfkuhttemhilefielzautehsndkodd(isEsh(sToEoSuTlvl-Sd8e--db8e- 13.0 Data Analysis and Calculations___________________________________________ 13.1 The solubility determination in this method is qualitative/semi-quantitative. 13.2 pTohienpt oisinthtetorewfohriecha qthuealsiutabtsivtaendceetedrimssionlavteisonin. solvent is confirmed visually. The solubility 13.3 Tcahlecucloantecdenbtyratthioenfoelsltoimwiantigoneqiusasteiomni:-quantitative in that the approximate concentration is c"W=hae/rbe: c= the semi-quantitative concentration pg/mL, ba== athmeoaupnptroofxismubastetaanmceowunetigohfesdolovuetn(tpagd)d,eadnd(mL). 14.0 Method Performance______;________ ' _________ :________________________ 14.1 Llmlaairrumggseetitbmaanetaidcrogonvinanosryiofdifdneeargertrdaino.wcrrTdheuhemeenetarnoectpscthouoerrftawicsnoyaglytvtoheinnewtwchaoihrcneihccbhetenhtiethnreagstosialooudnldbveieeldsnitttiytmoisiastahtdideoednsteeo.drlmuttoien,tehtdheiisssoeslruurtboejr.emcStaitnrogceian 14.2 Tquhaelidtaattiavoebetsatiinmeadtitohnrooufgthhethsisolsutbuidlyityisoafnteessttismubatsitoanncoenilny aangdivsehnousoldlvbeentt.reated as a ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 23 of 109 Page 5 of 9 BACK TO MAIN 14.3 mFoerthaond,acocrucroaltuemmneaesluutrieomnemntetohfotdhewsiullbbsetaunsceeds.olubility concentration, the shake flask 15.0 Pollution Prevention and Waste Management_____________ ____________ __ 15.1 bDrioskpeonsegolafsssacmopnlteaiwnearsstetobydipsplaocsiengofinglhaisgshpoipreltotews.BTU containers as appropriate. Use 16.0 Records____________________________________________________________ ________ 16.1 Sign and date all observations and calculations. 17.0 Attachments________;_______________________________________________ _ 17.1 PArtetpacShhmeeetn. t A-Example of a Standardized Sample Preparation Sheet: Solubility Screen 18.0 References_________________________________________________________ _ 18.1 OChrgeamniiczaaltsi.onWfoarteErcSoonloumbiilcityCo-OopEeCraDtioGnuaidnedliDneev1e0l5o:ppmpe.n1t.-7O,EACdDopGteudid1e9l9in5e for Testing of 18.2 U(aGnndeitnTeedrraaSntotsafrtoeCrsmoElauntmivoinnroMTnemesttehnoGtdau)li.dPPerrloientveeecsnt.itoEionPnAA, Pg7ee1ns2tci-ycCi.d-O9e6sP-Pa0nT4dS2:T8op3xp0i..c718S-6u10b7sW,t1a9ant9cee6rs:SoFlauteb,ilTitryansport 18.3 UCS1u-on1bli2utset,mad1nnS9cE9tea6sltu:etFsioaEntne,MvTirerotahnnomsdpe;onSrttahlaanPkderoFTtelracastniksofMnorAemtghaeotnidoc.nyP.TrOeevPsetPnGTtiuSoind8,e3Pl0ien.7set8si.4ciE0dPWeAsaat7ne1dr2ST-oColx-u9ibc6il-i0ty4:1: pp. 18.4 D3MeteErmnviinraotniomneontfaTl eLsatbSourbastotarnycMe einthVoadrEioTuSs-S8o-1lv7e1n.0ts,.""Column Elution Method: Solubility 18.5 D3MeteErmnviinraotniomnenotfaTl eLsatbSourbastotarnycMe einthVodarEioTusS-S8o-1lv7e2n.0ts,.""Shake Fl.ask Method: Solubility 19.0 Affected Documents____________________________________________________ 19.1 VETarSi-o8u-s17S1o.l0v,e"nCtso."lumn Elution Method: Solubility Determination of Test Substance in 19.2 VETarSi-o8u-s17S2o.l0v,e"nStsh."ake Flask Method: Solubility Determination of Test Substance in ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 24 of 109 Page 6 of 9 BACK TO MAIN 20.0 R evisions_______________________ _______________________________________________________ RNeuvmisbioenr Reason For Revision ReDvaisteion 1 Irtemwoasvidnegsirreafbelreentocems atokesptheecimficettheostdsmubosrteanucneivs.ersally applicable by 03/13/01 ETS-8-170.1 Solubility Determination: Screen Test Method FACT -TCR002 (LIMS #E00-1716), Page 25 of 109 Page 7 of 9 Attachment A: Example Preparation Worksheet, page 1 of2 BACK TO MAIN GLP Study Number: Test Substance: 3M Envirnnmentnl I ahoratory SOLUBILITY SCREEN _______________________________________________ _ ID#:------ ------ Sample preparation worksheet Date: . Source: Solvent: ID#: Source: Step 1 Weigh approximately 10mg1 mg of test substance into a 2.5 mL-4 mL glass screw-top vial. Weight of test substance: __________ mg Balance ID:-------------------- Date/lnitials: 2nd replicate optional:_ _mg Thermometer ID: 2 Add test solvent according to the table below. Following each addition of solvent, shake vigorously/vortex, and sonicate the mixture and visually check for undlssolved particles. Analyst Analyst Analyst Analyst volume added (mL)/ approx cone, after Solubility data addition (ug/mL) Dale/Time- J-- Step 2-1 Total volume solvent added (mL) Q.1 Approximate Solubility (ug/mL) 100,000 Sample Prep OBSERVATIONS/NOTES !cFlask vortex-mixed? Yes/No Room Temp------- Is there solute still presentYescontinue to step 2-2 Flask sonicated? Yes/No Time-------- -------- min NO- The solution Is at 10%, and is considered "infinitely soluble." N 3 Flask allowed to settle? Yes/No Time---------min further solubility testing is required. Date/TIme- -X- Step 2-2 Total volume solvent added (mL) Q.5 Approximate Solubility fuq/mLI 20.000 1Date/Time- Step 2-3 Total volume solvent added (mL) Approximate Solubility /uo/mLI 10,000 Date/Time- Step 2-4 2Total volume solvent added (mL) Approximate Solubility /uo/mLI 5.000 Flask vortex-mixed? Yes/No Room 1 Flask sonicated? Yes/No Time--------Flask allowed to settle? Yes/No Tima. Is there solute still present? Yes/No .min Flask vortex-mixed? Yes/No Room 1 Flask sonicated? Yes/No Time--------Flask allowed to settle? Yes/No Time. Is there solute still present? Yes/No Flask vortex-mixed? Yes/No Room TempFlask sonicated? Yes/No Time-----------Flask allowed to settle? Yes/No Time-- JC Is there solute still present? Yes/No Conclusions: ' Did the substance dissolve in 2 mL or less of solvent? Yes -Approximate concentration at which the test substance is soluble in solvent:_______ ug/ml The solubility of the test substance is to be determined via the shake flask method. or No Continue to page two for further testing. Notes/ additional comments: FACT -TCR002 (LIMS #E00-1716), Page 26 of 109 ETS-8-170.1 Solubility Determination: Screen Test Method Page 8 of 9 Attachment A Coni.: Example Preparation Worksheet, page 2 of2 BACK TO MAIN 3M Environmental Laboratory SOLUBILITY SCREEN GLP Study Num ber:___________________________ Sample preparation worksheet Test Substance:_____________________ lQfi_____________ Source: Date:___________________ Solvent: ID#: Source:_____________ Step (continued from page 1) ***Dld the test substance dissolve in 2 mL? Yes/No If YES, the test Is complete, and there Is no need to continue with the screen test. If NO, continue to step 3 to determine the approximate solubility of the substance. 3 Weigh approximately 10 mg 1 mg of test substance intoa 100 mL graduated stoppered cylinder/volumetric flask. Weight of test substance: ___________ mg Balance ID:______________ t Date/lnitials:. 2ndreplicateoptional:____________ mg Thermometer ID:___________ ^ 4 Add test solvent according to the tattle below. Following each addition of solvent, shake vlgorously/vortex, and sonicate the mixture and visually check for undissolved particles._____________________________________________________ A n a ly s t A n a ly s t A n a ly s t A n a ly s t volume added (mL)/ approx cone, after Solubllitv data addition (ug/mL) Sample Prep OBSERVATIONS/NOTES Date/Tim e / Step 4-1 T o ta l v o lu m e s o lv e n t a d d e d (m L )... 10 A p pro xim ate S o lubility (u g /m L )... 1,000 Flask v o rte x-m ixe d ? Y e s /N o R o o m Te m p Flask so n ica te d ? Y e s/N o T im e Flask a llo w e d to s e ttle ? Y e s/N o T im e ___ !S m in m in Is there solute still present? Yes/N o Date/Tim e / Step 4-2 T o ta l vo lu m e so lv e n t a d d e d (m L )... 50 A p p ro xim a te S o lu b ility (u g /m L )... 200 Flask vo rte x-m ixe d ? Y e s /N o R o o m T em p Flask so n ica te d ? Y e s/N o Tim e Flask a llo w e d to settle? Y e s/N o T im e ____! m in m in Is there solute still present? Yes/N o Date/Tim e / Step 4-3 T o ta l v o lu m e so lve n t a dd ed (m L )... 100 A p p ro xim a te S o lu b ility (u g /m L )... 100 Flask vo rte x-m ixe d ? Y e s/N o R o om T e m p Flask so n ica te d ? Y e s/N o T im e Flask a llo w e d to settle? Y e s/N o Tim e ____ !C m in ___ mm Is there solute still present? Y es/N o 5 Weigh approximately 10 mg 0 .5 mg of test substance into a 1 L graduated stoppered cylinder/volumetric flask/or equivalent. Weight of test substance: mo Balance ID: . Date/lnitials: Date/Tim e / Step 5-1 T o ta l v o lu m e solvent added (m L )... 1000 A p p ro xim a te S o lu b ility (u g /m L )... 10 Flask vo rte x-m ixe d ? Y e s/N o R o o m T e m p Flask so n ica te d ? Y e s/N o T im e Flask a llo w e d to se ttle ? Y e s/N o Tim e ____ ! m in ___ m in Is there solute still present? Y e s/N o Conclusions: Did the substance dissolve in 1000 mL or less of solvent? Yes -ADoroxImate concentration at which the test substance is soluble in solvent: ua/ml The solubility of the test substance is to be determined via the shake flask method. or No -The solubility of the test substance is to be determined via the column elution method. Notes/ additional comments: FACT -TCR002 (LIMS #E00-1716), Page 27 of 109 ETS-8-170.1 Solubility Determination: Screen Test Method Page 9 o f9 BACK TO MAIN 3M Environmental Laboratory_______________ Shake Flask M ethod: Solubility Determination of a T est Substance in Various Solvents Method Number: ETS-8-172.1 Adoption Date: 09/08/00 Effective Date: 03/27/01 Authors: Kristin L. Terrell, Mark L. Anderson, and Mark E. Ellefson Approved By: William K. Reagen, Labor^a_t_o_r__y__M____a_n__a__g__e_r__________ :__________________________________________________ Date MarkE. Ellefson, ProjectLeadZ ' ____________ ________gJty)/apte7 A / 1.0 Scope and Application_____________________________________________________ 1.1 PasonuldrupbOoirlsigetay.ndiAzeatcetciroomrndinfinoagrtitothonetohEfecsoUunbnosimttaeindccSeCtsaottohepsaetErhanatvivoiernosnaonmlduebDnitleaitvlieePslrooipntmeacetginoitvn(eOAnEgteCesnDtcm)yga(utUriid.xSe.l(ieEn.gPe.sA,) mwmReaeefttteehhrroo/taddoc(ieEsOtoTaEnSpCe-r/D8eml-i1Gem7tuhi0nia.d0aneroflyloi)nsreoctrhf1eeg0er5pne,raoeatlfneitmrdhteiOhnatPaenrPsytT1s0cSoo0lGmupbupgiio/ldmiuetnyLlidnsmceforu8erse3tin0tbs.te7ea8spa4tnp0par)orl.yoxzciTmeehddaeutvrepiearsseo.trhleueqbusihilsiatiykteeletfovlaetslh.kis . Solubility TEesTt:SS-8h-a1k7e2F.1lask Method FACT -TCR002 (LIMS #E00-1716), Page 28 of 109 Page 1of 11 BACK TO MAIN 1.2 Compatible Analytes. Test substance and degradation products for solubility testing. 1.3 Acceptable Matrices. Water, Acetone, and Methanol, or other solvents of interest. 2.0 Sum m ary of M ethod____________ ;___________________________________________________ 2.1 Uhhrhvohsssaocsaaaaocuauloopcnoeoipnfsigormbicsnupaurpqtiedthsmiecnslrcrrruhezpeyteessosoge(oenoall.tz,srTppntesntnseettastwerrstHhAhcietmderioindvaaeaeasaeiaPlatelvttptttvrcalheleqFi,isaeiyeyehnonsaeuwpOriinaet-tcdncnonaaiposLrteeScosltnttaird(niiuegeaCuae)nometgi)rrtlarlraail.dx/rhnnaetgunpMtcrwdiaiivaa.aftahmlvobi(eiulleiinnlSa1nuemllduo,gagssldeb:c/ttttt1edafseeobwiueaamstdego0u,ttuhelnnbowrimyanpdotiitddaoalairchslveir2tinana2rdildaoe-lecuurr0ds4avqhldrdndastltste/uieyisah.ehttisgaoe(daCnul.thoasfehisn,nigsocnq-ua.,ttesCtttg2orarkurariraref.6tsbmiaeeonaitapws,vsplshr1ntdtaelautpeei-eHiCasahmtvydciceahelrtte)e,faaycidantbpe1iimtptsfbnnfatdleeHiocitoipevltla,seaurueoyrm:,elesst2bma3vrtdataladianvHae0ytipctenihuodasdevi,la,ptam,tebue2ehwlLCocmrlssttHayoeeouvsaCiesinaotosxlnsiieapi/ltatntonilictlMlerionvml2asbelmaitstp/igexidrehla.Sna(nranatceCstbi.taipfhhtteSoneorelwu,cyrldfoatrAgaldeyaloosvdnimmiltehpltnltreoersk2ulhosaodepnatL)4ttbeiakp.lph,ltewmCsueneiehrpetteensbAaieo/reorqprotMgpflsloihauuyduelrrpatruxrerfisdSlelotsesscolloiaiayilueim.dsotrcrbtipnar.hdbhmionhreniatalTesenasocu,paatSitthntegectanhnlawpaeaiyelntenpodenadrdymasitocpnred,ttnirideoh4/elpxsaqrsecuqpeo.8)ltsiuemaftesim,ulospDeooinanihsuilalrradnctualidueoilenraibketaprpibbudedro1reafthteeriraleu:nfelasyoa1ntigtstatent0ndoeatee2ymdiisndd4ocnbtdo,rgeaut7n2t 33..10 3.2 3.3 3.4 3.5 DrMptpeciSttIscSSshnohenanoraaroaheaaoseomemrtmttmlaftgitrcehctvrreiekeiheepierueeeepnnsnsneoldmdssnlteissctnaudiaeatstFaitorteommnerlhemibrmlbnaeogtSaerspplsgtmlpo.tpanpsaatllraaliukeeaonmlesneeknTnignuae_kcksseSdpthh_sandoor:an:alaue_nedreuutarAa_meArtea(emrrrhnie_pastsccddnp_mmras)gar:eeeeo_ealldeta(oynReee_upcm(hnIdnn_nettfagSaeoTiitea_.pttriccrhpg)dd_lncrralpaaa:yl.ie_iotttibllinerpeti_hAtcnnoeooldpmedr_laeat-ceinsrf_tatkfntcaaeohtsse_,hmarnnnkastac_eevntr,ssontam_reieoeiaea.sneawl_edssualymspmada_rysugmun:t.t_tldetirpmieahs_ceTeoleeatle_a-dtrseencamh_drfvilsn.olerxr_itolpoentetona_(o,lersu(et_tutoaewmtaaa_ndmemtn.clni_getolponee_des.ieosnscis_dotdnsamustaf_oervigm.n_mpoaunefem_arrmtttpTstc_eoelihhopslyo_cnhsceaeerr_a(tmtteesnelieo_ltscsca)o._pprmasmgaone_lttono..l,aaan_eaarudkpm_wkltttTntynmah_reiesnaoheodmt_ontneeetnt_aicdehsnisr_fnsfean.rira_rtbddbnm,o,aaon_lauldtosmaem_oaiirrrlxn_oundlsea/_tknoaaks.sawrr_e,nclna_riividaedcsdanes_etttns_eociriunrau_ndoeraentsn_/lp)nrpeettac_arir,hr)daci_alneeyeen_aertgstsord_tntdoeseiio_dcfaennwt_nsreahdmt_toeaevalhar_pmntpoattbi_shiaaiclluv_oevurrelht_gohayelehau_htuatateoe_tioevglic_ltlfofyhiha_otntle_hhr)_ee_ Solubility TEesTt:SS-8h-a1k7e2F.1lask Method FACT -TCR002 (LIMS #EOO-1716), Page 29 of 109 Page 2 of 11 BACK TO MAIN 3.6 CpaulricbhraasteiodnstSatnadnadrdartdo:aAchdieivluetisotannodfavrdarsiooluustiaomnsouinntas coofnacestnotcrakt,ioinnterramngeedioafteinotrerest. 4.0 Warnings and Cautions_____________________________________________________ 4.1 4444....H1111....e1324althNpppFWHarraooaoocenrnctkamdpedericonldSotettghuuaieoraeftnmeehnltpl.tiapyarastotioleWpplarhevielaaatlertzlrntisnlainta,mirsgbndaeigsninasssd.to:taaif3rlhlMeeooawfocoEhderndcfav.ohlilrreopmanalilrmctpsaealnoruttfsastlehodLef,satrehbeeopferrdaoretctsooecrdrymiu'bsraeetCdes.rhsieaaWmlmseipacalfareelgtpHylroeadvpzaeaatsarrdaastnhRiodeenevetyise,ew. 4.2 44C..2a2.u.12tionmAtGosll:elatthshteesawsinrtoauvrlseeatsogisneerel.wsdhu(eicc.egh.tshcteeannptdoraisfrsudigbseialitrtueybpoersfe)paacarcreeiddteoanbrteaeltsocuobfnfeitcatirmeipninltelaytriironinns.seeddwwitihthascoeltvoennetapnrdior 5.0 Interferences_______________________________________________________________ 5.1 5.2 thbIsCemoaeoslrtpuundusbstwauerimilabdtiritsieetytnoasmasndmnccaerteasyemyesiconnhsanioiusngsuosgtnlreldiavpfiteribneconetacttehsnekr,aftdnlertuyoertrewaheangef.ncefreeenac.tnistsd,Ttnhgdhoeloeacsisrnouostwlmueutrabeifrnnieeletrieetaaydnnncdopaerfloiyutothshnrieedstreotoerssfsatttlhmaaserbuptociblneorsgantpatdtornhoircteycieoep.mnsrsTseeiltnhoihmgefotpidohnurebararliaayntnynaakloylsyfssmitsihsue. st 6.0 Equipment___________________________________________;______________________ 66666.....12345 AICVDnenoiclnaruuttltberyexaitrfit-,ucomHgareliwaxbmceiaartilh.platanhobcenleaeMtsioneifcnghrs/ocoitolliadvobielnintgog5100c5.a01mpSamLebgricil.eietsni,etsor.irfueqgeuitvuableens to.r equivalent. 7.0 Supplies and Materials_____________________________________________________ 777777......123546 5DDTGC-hriil2ssiaem5ppsr0smoopssbmoaacembbaLapllkeeepetaeoggrursllltyaa,ocsspvavssrapioaprgapilarbosyasl-udetl1eseu.oun5asrefitmzerpceedieLsapnp.d,etiitcrpntiaeefgpsuttsgaea,tesnc,ldtreu1iamrbsumetpbsLe1b,r5eot,orrabCne1ud-q0l4ubdm0isev.LcaC.ale.pnpte.r. 77..87 HPiapmetitlet-omnaGnamstaignhutal psiypreinttgoer.s (precision 1% of the total volume), 5 p.L to 1000 p,L. Solubility TEesTt:SS-8h-a1k7e2F.1lask Method FACT -TCR002 (LIMS #E00-1716), Page 30 of 109 Page 3 of 11 BACK TO MAIN 8.0 Supplies and Materials 888...132 AWMceaetttheoran,neAo, lHS(TPMMLeCOT/HSyPp),eEHC1P./GLCC/SgrPaEdCe /fGroCmgEraMdeSfcrioemncEeMor Seqciueinvcaele,notr. equivalent. 888...456 wTC0d.iee0alusi1lgtctihiMsnuiugnmbCgtsoCat1aCt.hh4nUlecogemrsCioodalafrueCkktDLinwoionihintw,yhnadEMrwxpaiaueltlmeirig,-ipQthAylebTM.p:opawrAtoaax0tnie.m0dr.1atrtMeanlysCf9ea9rCr%iln2ogsrttoobcekattse1orL,lufvtriooomlnumiSsiepgtrrmeicap.aflraesdkbaynd 9.0 Sample Handling 9.1 9.2 pRdaOurienletuccopotevaerridtdaahltstesiiaomsumnanepmstslihelpoesltfeehmtsienohaitrtiyaimlvaboleegepbbokreoefeeopapnkantr.adialnityliucsoiotnsel.,dds,setthto-euryapg,meaan(yed.bgs.eamaapnppalreloyaxzlieimqduavotietailnyLgC1/a-/5nMaSlCy.)siiAsnlotcenrrinamasptai-vmceaplpylpe,etdhe 10.0 Quality Control__________________________________________________ 10.1 10.2 mpSSoaheimaankstpu)elrieeFnRlomaefsuptkhlltieSicpaaplmetreerpsce.ilpseiPloiTcrnerapitopeanslriecs(2aaamtnoedprsl.maenopSarrleeeyt)pzuateopraapeltliraooscnavh.midtepesltaesvme(sfersaoesmluirneeatorcifhptlhtieecsapttreveetcosisspeiolronfvooirdneeaacanhaltyimsise. 10.3 Q110u0..a33l..i12tyMbcvpSfcdCooolreeoaoresnotnlnecstvpntthcaekaeeottmldmonrssiaudsostiiwnrinnlcBbebyaaBia.ltlltterihaailinroaonncitsnenneokktdrksn.a.outttcSfmSahAsctmeuarrhenotubmneiuuensatptgpdsaalaoihllnqntealthcvucstsfhor.ee.oooen,ntuuTtotsoar(ghnatsmfhhme)ltyoihtunseueensoastseolttdtavidhviomteleeednunspsutsttosilraoebesrimnnlulpbagbwpranseslcotkietphtklahvaiepgnsorerrcasuneuoeatpttsuimoieat(nseindrpd.saaelpttted.ioirnsdompoutdenercebodereptsfpchdtertuahaaourrmnnrecraonecoeteusecislno)gseattn.shods.aoipTmtnruhreyhoteecepctatthlesomhyeussresrsaee,etinenhbaaatotlnileenrdydseyztteod 11.0 Calibration and Standarization -_______________ __ 1111..12 AcTahllleibecrqoautmiepdpmopuernniotdrsutsooefdui,snestue(crdehasiatlysm,tuhwseeteabnkealylsy,tateintccda.al)rbdaasizlasepndecacecifacinoeddrdaiinuntgiotstmosatltaaenbddoadrarildtuootreypre,srpsahetoicniufglidcpabrtoieocnesd.ure. ETS-8-172.1 Solubility Test: Shake Flask Method Page 4 of 11 FACT -TCR002 (LIMS #E00-1716), Page 31 of 109 BACK TO MAIN 11.3 tAesltl ssuambsptalenscea,naanlydzaedfiwxeildl abme oruunntaogafiinnstteransatlasntdaanrddarcdu.rve containing varying amounts of 12.0 Procedures__________________________________________________________ 12.1 12.2 pP11111E1111111r2222222r22222qe.....e.......111p11u1122222p.....a...i....123456a17l2345rirabatVAPrwcbtWPasttoPbR(istPSATacTstA2pTsrihoheneacheadtenulrorporple6raehidhhpeehsiaftrtemnfeaeeeedseabnpanoepoettidteeneaeppmcputainpitcleicssertneprrgstsaeCkoewapaaaao3ttahtrtsdhtsimitnoiulohtausuhrefro"cnhrpla;trxneoioaaleulebtneba(tadcbsteetn1ameruiyioalhfbs/rrenpgstcovttoemmvyetl2amtattekanuiateotTiscephrhdneiexevscofel.oacomsidotteaa(uu1sliseartoinesesnnoshwtlenafexaptrnpomtem.(struatpusnasDee.2ec.irersEstied,elgsef2btblddsbdelfshmntiesuaoe)lueaeityioas.Tiwp4oeeetstVsegtzthgtlrstytlgrea{aepwlit)ueslvhmhSses.eth3(eiaheoanvs.etsnalbcchlttuAdi3eee-y0dstnatoaonseihetdsrpeisD.e8bn,stoistficrstinvtuphaDtohe2"ebtie-sbameettn-.wetaccterpCraar1hnDa:trR4eetlvlasesyatsntkc.lyo7dwetedsvuylesoaopeasnshlhoseoee0rtetoosa,ectpyRnacascohueomnawnR.setsfv1lllleo2ls0r(ehlenucsuupeese,tee1aldsttvetl)eterrekrcmldbreoa,hvis-.),qteapensimsRenfsioRCrmniseibeteu-sno,eritn4l.ateeteorrRanoveieaeeiotndfApndt;dlsstarlnwstwdesyape.oyp1eiutey.eseInDpabs)sapuh2)iuttlrfnbsvisbdhlMo1tu,hirlf"nAa.atartocrllsmmeea12,oeaannteste,tyrvrrttsbhotunid.,rbe-ur1osaiied"a2eiei5xsReneebretrdcaiolanb2sDtiddesb.,/beedqaoseetdRtonsnessc.dldiseaw)l1stmuadilhltitpdervToteeiteedlgouafea.fyienedaaerefp1llpdvihoenorolmtt2-fasevolsnkgnisiva-eR4aoer,cfrstr,p2ort(esg1(deReveponlss;erai2hv10eenanaaseb2dneoiterdttoeat0plcn2uoe.dbmnhtamoe.rhgslep1nbaots,.pdbrdnotevausoC10hne3.iesS.daa2sndasttduetzck4.0.re-ttcmue-itrt3erc"esdvortoeR.liD2ale0atrosreeainnio,Aeeinnoanv6ecpzowe(nacnmsari"nsRtssrecaaenlpteltli2aytDseeweiives.etettldprCmeitdgeli4Cinih3locaesss3h)net,loyail.eieFvt,.tetetn,t;osohsyRnisaiierihtt,isuvt1,ocmnvnDdouuaohnsdrl.fIste5tneen,eobtcoetstuedfthRapaeaohessntutdplnnlrmtrnehnyisupu4sn1epnehtt:ceeslmoarhpeaebd2srriLtekcapoi2ttsatplteenee.ue.sefhehtnhpsyp33r,ltpurtlseftrpnrobed.eeoioaatseit"-teda)germhofhotnitsRnrer,.ordcoe,uteelttedetclogedaecahaxiioexyRerdao.ncscletbfncdepimsatpwttnyhfulneomahhoeiodaiameuarencsbrrtnplie1naepyonsnareayitoec"s,tpdoup(dtshpccdtdwan"tuDharoaae-ldumeseraytdimesrRtbteomlveforninnnhaelbuyoterbamiexoleaiisedtciyeergpucnntpreofnasplitlee,1otlailolmhbhurigarmntew,netn.rtheR2rahtwmomisiaisialtdasapeenuo,somndlieeteetpleuteeldfnuaeestuthypeinfultnhnunltgreherii4tlaym)tetcebddgha,atoi.t"ihlbeesht2)eo.-seed0.nflt Solubility TEesTt:SS-h8-a1k7e2F.1lask Method Page 5 of 11 FACT -TCR002 (LIMS #E00-1716), Page 32 of 109 BACK TO MAIN 12.3 S1111111112222a22222....m....33.2233333....p....12.6735647leAtAplgAOe"1111ttULUmTtssceoSapqDhhhlu2222uuoqlbyttpaaoassueeeeril....binuassbe33ma2qlaii2tteitlennsseyacaaharpalep...u.hapt252ipd3rggblep3pnlappacyoboeva.).l-nlptpn,anrr1tr2ee.r(ttfap1epeRorthabesiotfolhrarlocrshmtr2laysiiaoqoodeePxdSxettThaeealnatpoeo.ebthtwl,uhlppspnii)ip2retasiaiihefoldmlmesefo.iicidreatro2tuamo.-liuotoeleowtilii5alrcsctlni"ttueeaaactaaalcnUpsrleybob.elpeeaeu,sdutts)ttrntosabtttlrteesplrfeme.stt"htobaiutoaenars,aodite"olelcooDttslediaolyynvttuecmerDisaialayieofantcoilztbeeiitscooalslhllduth4a7tnolatuaaae)incieefuiyuylnueselq/o8qt2acvnkulylrrtstsi3raiotstyauuilraduiiotntie(aif)ha2stybh,haloaatintoslo.apo.oRuntvlteoie,eoztelosaniofyucnrcRtatsris.ennudoeedusuioseidsfarasann1n.adp,eibra,aairrlntmimmnnitsmog:ssepc3ltsnnit.1lrav.tuDe,atufeiaapf"ldaaoao0nasandit"tkb1ratl,tnyulaeahtndofeehr,ieenioe2tapgwemrqeeco,rihfLbea"lynr.oiencieutie2ntacDeietppnCoaf,duthocothdo.hdi(eewlhtl3rttuaonsir/eeetoms"dstetagMada-yobabo.thitDtoq1gkseuhmth(cl2aittafefhtisouSfn2.oateeoaekh.t,softopoelRii.itpsrayhnnaoeeeu2rnoe.rllvattaop3euedteehseu.tregnicmssaeb5ipsisdnsp,taieordaeooadpRqilsd.y.trlta2poufriamnnt.eiiiouasilnseiombp"lnutssrn,soauxioeipsps,ieuav.attoltribieltlato4tlt"momtbmtaiupanhe,dtrnNaitv"Dvlmemnittoyeitpeata)niiiioolihsdnaaodotnytluaeacgpotatfieeeyal.nnalrteytposrntfls,bsrig2tnh:esyi,noddhbaoetebs(i,deielthcnRnmeeysimea3wcfaaercmee.sgttkeeopgtrqcpeednnuhendcppoii.nuoautsnlrteslengnhoer3iatdslfnittc1cnpa/agcl:lermiws"tmces.ueeioitores5hubs,ufiescdypxrimentnoueeLabnrsvntabmittscealnasgp(nrergestsse/olteatcrereLdeotntaaotecoaynocaraafidtrdmbdnteptttf"ntnnpfti3iteeieraeoeanDooidocpavocma0dlnnsstgosneecnleitl0a.tptegitiyduorts'eyr0odsottoiveseptihsnorups2enoa"esnefnttnrdeycsesed,tDtlgsotsaRbge,isievrctlns,tnslaptliyudnea/yreeeaeetndkmmgyiisutpysnlpsbegteinrstltorean3stpLaa4xaeneieobbfmmt,(nl"dnpcoowefRetilt)tdeye.ireeadatfhiepneaihlnastyto.nleteproteniortdnblod"ge, 13.0 Data Analysis and Calculations____________________________________________ 13.1 13.2 13.3 ebAMSSsaqytacameumctnaahepndpteslisalesoenrwnsdwuiwwmitdllolelihblbvbcileceiaebrahlcetocqiaiuofusallncaniabnsunatadelltwsayiifevstziietdlieealddddnoubbdnaaveyaglitcraaheadaiendalndctdsiciuentitainvldealagiiistabvs.etttrihdiadaoentuunidaois.nalinndrTedcginhvutceeiriduitvbtiurehevua.seeilrl.(TtenMnih)nteibictfeairueiomnnsscogoatufinlotnednEstsdoxcitcfovhetniaeldtnsaitni3ngso0sur:tbthMhseetiarcfnerocsoluesloloitwfnatnitnthgesum InZx2 -(Lx)2 - y (-!) Solubility TEesTt:SS-8h-a1k7e2F.1lask Method FACT -TCR002 (LIMS #E00-1716), Page 33 of 109 Page 6 of 11 BACK TO MAIN 13.4 cSSawaalmmchuepplrllaeee.t:wepRdhrPeeuDAcBrsiei==s:wniogBAasi|ntlvA=atl=ehnwbr-eccdaeBiooalgflncnore|adbcclA/lole(eeocd(/nnfuwABrettselvrri+aapaaniXmtBatotgeiitroodp)ite1/onnle2uqe0nd)ossuo0=ioaaffn=tsfsSfgiieoa%SarcvtnsmahoRet:menprrSaedplfDegpolreellReild(cop%PoawlsrDiRtacei%mSnatgDCpelVeeqs)u. aStiaomn:ple precision will be 13.5 Evwqauxirtecihsalutb9isol0ieno%a"nbQcoloeofnbdafsnaiedtroaevunpetcodleii.e"n(rtsdIemfaeatQtayaopbebolrseirent1rtovbmetehdaleoy>whbQiegftohparbeoQrurflotalaortbemwdue,leadtnthebdedynovuftahttliheuleiezdsdian)at.gatapDsoeiixtn.otnCm'saalQycu-bTleaetreset.jtehcTetheed where: RGQToaaabnpbsge=lreevt=eh1de=tCodgtraiaifltpfees/rrpraierannegacfeoderboRefttewhjeeecedtnaiottahn.eoqfuOesuttiolinearbVleapluoeisn:t and the nearest value. oNbsuemrvbaetrioonfs Qtabulated, 9R0a%ngCeonfidence 3 0.886 4 0.679 5 0.557 14.0 Data Analysis and Calculations 14.1 P(ootahobnurerdvetlrciqieioeiunlsuraceisotvlsiutnaovidloueuoenteplfarieeedebrrsxalcsueite.slandtt.ssTta,tohdSaseifaafptmmfQhoeeipp-rnTellsteene.tcasdaettDvai)msetotaoricaacmfuyga<melubsaee1atnn5nahat%dplatyp.phvslreeiNiesenacdowoipnstnieio-t-ocrhccneooextmihmncselptpurlrfelideii-analecnanaaqttltliucdvrdeuaeeasstltaaustaittlomaetosnndn.uadsabdatnlraebddteadrdeaseeputvvaomairpaltmutoeiaiodantrnewtyds(.i%sfthhoIReorfeuSattDns,) 14.1.1 14.1.2 ddcrmSTaafeiovnaaahnpenttedmeataaorf,ltaipr%pihdartgsloeepeeteR>pihnpndrSo1aecletaynrD5esptdtd,,%aetlahibaedRtcdeapxeRaodP.tpctQweSaeDllsuytD-ea%tdnef.et,eohonsReTretttvSshttmhDhaoheDelaeeiuos'kxresaarueeotetmmstentmlfhhipl'ateoaseahlirsueineQcnkldirfdistn-airnhTtgotbsgeruehmeersmstioehwta<u.f.a,v1uolktadI5Irheltfvf%uheaattfengehhl.lsaurreeteseIhdfokeqfsoeasu.utrwthdtaefalIeisoaictnfettrhiaaanrooitvlonhvcsnueeueaatdr1tlllabatiu5amiegltt%meeareiaoiv.edpyosnpaaofsIrnlotifuetanoaihjetntntephe.stdcboissctsTeiecahnacodamunatrlslicqwipbltesueulebdiedlreteaiheisitatsnxrtue9ciiicsoptsa0thlenhlru%nidedaecdoebatetodltdee ETS-8-172.1 Solubility Test: Shake Flask Method FACT -TCR002 (LIMS #E00-1716), Page 34 of 109 Page 7 of 11 BACK TO MAIN vtiimaethpeoiQnt-.TeInstc,luthdeenjuthsteifnicoant-icoonmfpolriadnrotpsphiankgetfhlaesskhdakateafilsasnkot(eto.g.beq-utessetdrefosur ltthse). 14.1.3 .bdfefAilreanarntsoanadklre.fsfcmoioenrelsaupstlhbaoloyrislyd,siti.ttybho.lIeerfIe%otfphuRteihtsalSritceeDrterhistbc.eeeoreTtinwanhsteeiriserceeeunnttoaitevhtgseemtr,etteeoihmtarr,bereileetpe-moddtiaiianmlyyutssetbesdie/hnrooenten-uersolcvhdetaosbalossgeatrar<seryae1emt5wroep%irqlteehu-sfiieonrtveroad1tlc5huth%eoaets,rceehiktpathkfomoeerartythe 14.2 hLstiiagmnhdeitasrtodQfuQusaeuldaitnyintCifthiocenatctriaoollnibB.rlFaatoniorkn.thcisursvtuedcyo,ntthaeinLinOgQmwoirlel tbheaenqtuwailcteoththeealroewaecsotucnatlsiborfatthioen 14.3 bLQ((ctploOeaurnsonQattvkala.iiisntdnIypafeslrdbCiyigaottocnehrnkiatOftogtircrRtothoahlneuienBrtnetcbdleaaaarllnnrceiebkkavlrgnsea:rsoltostiMaoouonntnefhddtsaeahtnrrlaoedaindvnldayednaatliesracndlaodeytxcftoSeuiars)orsntvlsativehhnleyaaanttltrheltee)eb.Bicetilhlnealeieantrsinkast,hlttsemhhaaesmenatdmhpa5oltp0eadl%sem.bsloTaaoyfnhrtkebhthseel,eebaavicruneectlsaetsorpucuftobemausdneenaqntlsutyeotenftthe 15.0 Pollution prevention and Waste Management 15.1 bDrioskpeonsegolafsssacmopnlteaiwnearsstetobydipsplaocsiengofinglhaisgshpoipreltotews.BTU containers as appropriate. Use 16.0 Records 1166..12 FSiilglnoauntdaldlaatpeparlolporbiasteervsaatmiopnlse apnredpcaarlactuiolantiwonosrk. sheets. 17.0 Attachments 17.1 Attachment A-Example Sample Preparation Worksheet. 18.0 References 18.1 18.2 UoO(GfnrgeCitnahenederimzaSatiottcairaotelCnss.ofElouWnrmvEaintcreooMrnnSmeootmehlnuoictbdai)Cll.iPotPyorrope-tOveerecEanttCitioioDonnnAG,aPngudeeidnsDtecilyeciv.indeeOelosP1p0Pam5nT:dSepnTp8to..3xO01i.-cE77C8S, 6uDA0bdsGWotaupanitetdcedeerlsi1S:n9oFe9lau5ftober,ilTiteysting 18.3 UTCronalinutesmdpnoSrEttalatuentsdioETnnrMvaniresotfhnoomrmde;anSttiaholanPkTeroeFtseltacGstikounMidAeeltgihneoendsc..yPE.rPOeAvPeP7nT1tiS2o-n8C,3-P09e.67s-t80i4c4i02d:Wespapatn.edr1--ST1oo7lxu,ib1ci9li9t6y: ETS-8-172.1 Solubility Test: Shake Flask Method FACT -TCR002 (LIMS #E00-1716), Page 35 of 109 Page 8 of 11 BACK TO MAIN 18.4 18.5 18.6 NpEBHSCS1puu9Tuoaa.b6btrmrSrre3ss1e-itpta;8s-laaua,1lP-nnan1D2acoc,y7g,eeaMf1:0senSi9:.sna0iNt9eFra,1Vley6an7SwCtda-Geo3ra.,lYii,ruobTdSaobubrstnrisaoalkdHnitnS,tissyaTsop1.tn-ilS9oT2vcd8crs7ebht2r.n.oee;atoeQsnTpnk.dru7eT9aT0a1en-rt;s7mtaitUn1t:ea.s.AntfSiotpv.roepGmfrCooaOxvhtiuieeomtmrnlniaiemTctreaese.slnStAtoEGnPlxuaurpbilienydirlsteiiiitnlmsyi.gneDenO4sett.hfatfeEleircSdPme.tA:;aintWi7Was1tt.iHia2ocs-.snhC,Fio-nrN9feg6eaat-omt0Tino4ae,n1nsDa:tal.Cnd., 19.0 Affected Documents _________ ,_______ ______ 19.1 ESuTbSs-t8a-n1c7e0i.n0,V"aSroioluubsiSliotylvSecnrtese."n Test: Approximate Solubility Determination of a Test 20.0 Revisions RNeuvmi1sbioenr FSSSaSnieeeexdccccettttsiiiidooooonnnntlhv3e111e..24ni62..nt,,32cbrr,.o5elema,rfmnreaoekronrcesvetn.oenccpdleutesi"moaitrnnboltayeReslrrepdihnnaeeiagscgfloiihnofsn-ietfcsadFpsntoeeetdhcresatedtRirosdaecuncvebbscnilsseat1tirpnao3itkfn.na5u"cngetcfhasretrowiocomurenigrtdeeshetrrefi1eoipn4mnwi.3tofi.avooserndams.deedctethidoo.nd. R03eD-v2ai7st-eio01n ETS-8-172.1 Solubility Test: Shake Flask Method FACT -TCR002 (LIMS #E00-1716), Page 36 of 109 Page 9 of 11 BACK TO MAIN ATTACHMENTA: Example Sample Preparation Sheet (page 1 of2). 3 M Environmental Laboratory Solubility Test: Shake Flask Method S tu d y #. Temperature o f Study: __ !C Sample preparation worksheet A n a lv s tfs ): Test Substance: ID#: Source: Date: Test Solvent: ID#: Test Vessel: 15ml centrifuge tube/Other<specify): solvent density:___________ fl/m l Source: Was the solubilityscreen test performed prior to start? Y/N If so, what Is theapproximate concentration? uQ/mt B a lann ID- T h e rm o m e te r ID: Room Terrm: SFM vials ID#: "samplelD" = Sample Description Total mass weight test substance (solute + solvent) added: added: 'internal Standard addition _______ uU_____mis soln IS added to dilution factor: samplelD-1.1.1 thru -1.1.4 Day1,Smp1 1 samplelD-1.2.1 thru -1.2.4 Day1, Smp2 1 samplelD-1.3.1 thru -1.3.4 Day1, Smp3 1 samplelD-1.4.1 thru -1.4.4 Day1, Smp4 blank none added 1 samplelD-2.1.1 thru -2.1.4 Day2, Smp1 1 samplelD-2.2.1 thru -2.2.4 Day2, Smp2 1 samplelD-2.3.1 thru -2.3.4 Day2, Smp3 1 samplelD-2.4.1 thru -2.4.4 Day2, Smp4 blank none added 1 samplelD-3.1.1 thru -3.1.4 Day3, Smp1 1 samplelD-3.2.1 thru -3.2.4 Day3, Smp2 1 samplelD-3.3.1 thru -3.3.4 Day3, Smp3 1 samplelD-3.4.1 thru -3.4.4 Day3, Smp4 blank none added 1 Date/Time: . Initials: Test Vessels sealed w/tape? Y/N Test Vessels shaken/vortex-mixed? Y/N 'internal Standard: Int. Std. Cone.: Test vessels placed on orbital Incubator? Y/N Incubator ID: Speed: ram Initial Temperature: ID#: -ita/m l C Date/TIme/lnltlals: Observations/Comments: . Day 1: Four "Day 1* samples are pulled and allowed to be placed In a temperature controlled environment for approx. 24 hours with no agitation. Location of samples:______ Temperature of environment:___ C Thermometer ID: Visual observations: D a ie /T im e/irntia ls : ____________ FACT -T C R 0 0 2 (LIMS #E00-1716), Page 37 of 109 ETS-8-172.1 Solubility Test: Shake Flask Method Page 10 of 11 BACK TO MAIN ATTACHMENTA CONTINUED (page 2 of2). Day 2: Four "Day 2" samples are pulled and allowed to be placed In a temperature controlled environment for approx. 24 hours with no agitation. Location of samples:______ ' _________ Visual observations: Temperature of environment: ____ ! Thermometer ID: Date/nme/initiais: .___________ Day 1" Test Vessels Centrifuged: Cent. ID: Visual observations: RPM or RCF readout: duration:, .............. jnia,_________________ oate/rime/initiats: -Four aliquots from each of the four samples are to be made into glass/plastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution 1:______with methanol. Methanol TN-A:_____________________ Date/Time/lnitiais: Additional dilutions: Dilution factor (test solution:methanol): 1:___________ X's how many dilutions:_____________=final dilution factor: 1:______________ . s, Diluter ID used:______________________ Amounts used:________________ uL methanol._________________________ul samples -Store samples and extracts in a cooler at until time of analysis._____ Cooler ID: _ Cooler Temp:_ C__________________ Date/Time/lnitiais: Day 3: Four "Day 3" samples are pulled and allowed to be placed In a temperature controlled environment for approx. 24 hours with no agitation. 1nnatinn nf samntes- Temoerature of environment: C Thermometer ID: Visual observations: Date/Time/lnitiais:------------- :---------------------------------. "Day 2" Test Vessels Centrifuged: Cent. IDVisual observations: RPM or RCF readout: duration: min. Date/Time/lnitiais: -Four aliquots from each of the four replicates are to be made into glass/plastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution 1:______with methanol. Methanol TN-A'____________________. Date/rime/initiais: Additional dilutions: Dilution factor (test solution:methanol): 1:___________ X's how many dilutions:_____________=final dilution factor 1:______________ . t Diluter ID used:______________________ Amounts used:________________ uL methanol,_________________________ul samples -Store samples and extracts in a cooler at until time of analysis. Cooler ID :_______________Cooler Temp:_____________ 2C D a te /T im e /ln it ia is : Day 4: At approx. 24 hours of equilibration, the "Day 3" samples are to be allquoted/extracted. Test Vessels Centrifuged: Cent. ID: RPM or RCF readout: Visual observations: . Environment Temp.:_____________ ! duration: Therm. ID:_______________ . milL___________________ Date/rime/initiais: . -Four aliquots from each of the four samples are to be made into glass/plastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution 1:_____ with methanol. Methanol TN-A____________________ ,, D a te /T im e /ln it ia is : Additional dilutions: Dilution factor (test solution:methanol): 1:___________ X's how many dilutions:____________ =fmal dilution factor: 1:______________ . Diluter ID used:______________________ Amounts used:________________ uL methanol,_________________________ul samples -Store samples and extracts in a cooler at until time of analysis._____ Cooler ID: Cooler Temp: .......... fC __________________________ Daie/tim e/initiais: FACT -T C R 0 0 2 (LIM S #E00-1716), Page 38 of 109 ETS-8-172.1 Solubility Test: Shake Flask Method Page 11 of 11 BACK TO MAIN 3M Environmental Laboratory Method Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in W aste Stream or W ater Extracts Using HPLC-Electrospray/Mass Spectrometry Method Number: ETS-8-155.0 Author: Mark L. Anderson, Mark E. EUefson Approved By: Adoption Date: ((f(foo Revision Date: WAnoarldys9i7s of Potassium Perfluorooctanesulfonate or OEtThSe-r8F-l1u5o5r.o0chemicals in Waste Stream or Water ExtraPcatsge 1of 9 Using HPLC-Electrospray/Mass Spectrometry FACT -TCR002 (LIMS #E00-1716), Page 39 of 109 BACK TO MAIN 1.0 Scope and Application____________________________;___________________ 1.1 eSlceocptreo:spTrahyis/mmaestshsopdedctersocmriebtersy.the analysis ofwaste stream or water extracts using HPLC1.2 Applicable Compounds: Fluorochemicals or other electrospray ionizable compounds. 1.3 Matrices: Tap water, ground water, wastewater and other aqueous solutions. 2.0 Summary of Method_________________________________________________ 2.1 TEcppoeaShmrri/ftsMilpcumoSuouel)ra.nothrdoTocscdhoteamedxnetaporsnoaacautcreltniyebd(sdeP,issFfsrtiuOhoscemAphea)aw,rnfsmaoalttryh/emzseri,e=spudeo4srbfi1fnylf3uglt.uohoHreorPomoLccahCtsaes-nmeesliseeculcaeltlcfrsootionsopranrtoeaotyhf(PeamrFsaOeisnlsSegc)slteparoneiosciopntrnroca,mhymaiero/tazrncyi=tze(aH4rbi9Psl9etLicoCro-fa 3.0 De f in it io n s_______________________________________________________ 3.1 usilToiynmhnsAdetiieerzttmemmradtaoioaotsvsonnppa:drchbaEuoyeylutre,uhmicectetit)rrlcP.oi.czrsoiepTnmsrghasmeyuaeriIveorocannIirioiaizzelnaaltyiyttziioaooavnntfiasoi(ionElnauStbr(hIclAe)ee,sPsLeA,ICp)pt:mrr/MooTobchSseepesssh,sMyeeassrniticeodcrmcoPicnsmruteaerasslrsslfsoauawtcrPeealasftcom.thfroeoTvrmshmapeirhcisLoeaeulrCiisIcnZomcpnslreuiiezntdhsagesotliuebdorusnqetuo((aaAifr.deePr.uc,nIpno)oo,tlte 3.2 pTrheesEsseulerdecr,torwpolhsepetsrreaabyryeIipoornnoisdziuanctiesodonlbu(ytEiotShn,eaEarSepIpt)rl:iacnAastfimeornerteohdoftdaoosttfhroieongngaizsealpteihcoatnrsiecpaevlrifafoietrilmnd.yedchaatragtemdodsprohpelreitcs. 3.3 EseSle/MMctiSavsesslyySstdpeimesccsrtiramoremineeaqtteeudrip(bpMyedSm)wa:siTsthhtoaecPshilnaagtrfgloeerqmrautaLidoCruZ(mpao/nzle)damontahdsessruscbeoslemecqmtuiveeenrctdliyaeltdleyecttmeocrat.neudIof.ancstuarreed 3.4 upcdsospotyainifrsnsllfaityseeCzeyiremwnaoescgpnnsioeta,tvthm,rhee"ttrtuspZnhcoiroetm.-ue)isn..omgpielnhrnaOeIaanrttaysthlhs"totvayheodnscserr.sotdteccuZnomocoof-fmonoussonvrpsm(mpveirpe.eneaaearnrtt.yatic,ithotoiipiZowannorln-a.nlasoaly,ypblTcmcriecoahlnoeanyeiamnntfchsonutoppeerifnmmorracagnfcoapya,tetuoucniaenonrentmes:netdedniTaritmttErtsheeeiSaledsaeni/rcMnMafoetrittrmeoiScoccnmoderoasmoedymntm.hspcdpteaeaTeiartsmpihatesbirrcobsloePteullmbeltygawheawhtaefiyittoisthsthhtrhaohmeasmreovotchneLemco.oeoCnsegniafHZmooeingontosiahuwlaytpaerlhseearrtetvrteofZirtemeou,-rtanrsbh,tepuueZi,rsrt-aeaysft.er 3.5 Lv(MeCrasZMisosMnaLssay.ssnsLAxsylNplneTvxcetUrrSsoosimoefnrtew'stseaaGrrr.eeu:CisdSiuemyrrosieltraenrMmt.lyisFcoMrofortamwmssaaoLsrresyenPddxeleashttiafgaoinslrsemWdseiLfenoCdtrhoZtewhUemsss9aepn5re'ucsaainGflidscupWioedpceiine)f.rdiacotwitoosntNhoTefiM4n.s0itcrruommeansts AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes2 of9 FACT -TCR002 (LIMS #E00-1716), Page 40 of 109 BACK TO MAIN 4.0 Warnings and Cautions_______________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Uemseplcoayustiaonvowltiathgethoefavpopltraogxeimcaabtleelsyf5o0r0t0heVporlotsb.e. When engaged, the probe 4.1.2 Wanhdeenyehwanedarli.ng samples or solvents wear appropriate protective clothing, gloves, 4.2 Cautions: 4.2.1 bOapcekrparteesssoulrveeenxtcpeuemdsp4s0b0elboawr,athbeacHkPp1re1s0s0urweilolfi4n0it0iabtearau(5to8m00atpicsi)s.huItfdtohwen. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences________________________ ;______________________________ 5.1 Tstoormagineiomriazneyinptaerrfteorefnincsetsruwmheenntaantiaolnyztihnagt csaommpelseisn, Tceofnltoanctshwoiuthldthneotsabme upsleedorfoerxstraamctp.le 66..10 EqmEuqoiudpiimpfimecanetntiot_nl_is_sti_en_dt_hb_ee_lr_oa_ww_m_d_aa_yta_b_ae_s_mm_o_edt_hi_foi_ed_dd_ie_nv_io_ar_tdi_oe_nr_st.o__o_p_ti_m__iz_e_t_h_e_s_y_s_te_m__._D__o_c_u_m_e_n_t any 6.1.1 iMonicizroamtioansssoPularctfeo.rm LCZ Mass Spectrometer equipped with an electrospray 6.1.2 HanPd1a1u0t0osloamwppluerls.e solvent pumping system, solvent degasser, column compartment, 7.0 Supplies and Materials_______________________________________________ 7.1 Supplies 7.1.1 Hsyisgthempu.)r.ity grade nitrogen gas regulated to approximately 100 psi (or house air 7.1.2 HsizPeL)Coraneqaluyitviaclaelncto. lumn, such as a Betasil Cl8 column (50x2mm, 5 pm particle 7.1.3 Capped autovials or capped 15 mL centrifuge tubes. AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfoetnrayte or OETthSe-r8F-l1u5o5r.o0chemicals in Waste Stream or Water ExPtraagcets3 of9 FACT -TCR002 (LIMS #E00-1716), Page 41 of 109 BACK TO MAIN 8.0 Reagents and Standards___________ ;__________________________________ 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent. 8.1.2 wvMeainltldeiro-Qro.TMr eqwuaivtearle(nAtS, TanMd tmypaeyIb)e, palrlowviadteedr ubsyeadMinitlhlii-sQmTeOthCodPlsuhsousyldstbeemMorilloit-hQeTMr 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 2aaSmp.t0opmrrmeooMpanrtiiuaraomtmeommvacooeltnuetaimmutempe.eoraPfacoMteuutraireltlie.in-stQoolwauta2iot0en0r:,0WmLiexvigouhlnutamiplepatrrlolicxsoifmllaidasskte,alayred0dd.3its0hs0eolgved. 8.2 Calibration Standards 8.2.1 Tstyapnidcaarldlystawreopmreepthaoreddbdlaunrkinsg(Mthiellsi-aQmpwlaeteerx)t,ratwctoiomnaptrroixcebdluarnek.s, and solvent 9.0 Sample Handling_______________________________ ;___________________ 9.1 tSutbaensduarndtislaanndalysasmis.ple extracts are stored in capped autovials or capped 15 mL centrifuge 9.2 Iafpapnroalxyismisatweliyll4beCdeulanytielda,nsatalynsdeasrdcasnanbde psaermfoprlme eexd.tracts may be refrigerated at 10.0 Quality Control____________________________________________________ 10.1 Solvent Blanks, Method Blanks and Matrix Blanks 10.1.1 eSaoclvhesnatmblpalneksse,tmtoetdheotedrbmlainneksc,oanntadmminaatrtiixonbloarnkcasraryreovperre.pared and analyzed with 10.1.2 Analyze a method blank and a matrix blankprior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Meffaetcritxonsptihkeesreacroevperreypaefrfeidcifeonrcyea.ch sample set and analyzed to determine the matrix 10.2.2 Massaotrciixatsepdikweitdhutphliecaatneaslyasries.prepared periodically to measure the precision 10.2.3 tAhneaolyrizgeinthalesmamatprliex.spike and matrix spike duplicate (ifprepared) in the same run as 10.2.4 Mofathtreixinsiptiikalecaanldibmraatitorinxcsuprivkee odrupshliocuatledcboenpcreenptraarteidonasf s1h.5o-u5ldtifmalelsinthteheenmdiodg-ernanogues UAsnianlgysHisPoLfCP-oEtalescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-l1u5o5r.o0chemicals in Waste S.tream or Water ExPtraagcets4 of9 FACT -TCR002 (UNIS #E00-1716), Page 42 of 109 BACK TO MAIN cthoencineinttiraaltcioanliborfatthioenacnuarlyvtee.if eSxptirkeemceolnycleonwtrlaetvioenlssasrheoeuxldpefcatleldi.n the low-range of 10.3 Continuing Calibration Verifications 10.3.1 Cacocnutriancuyinogfcthaelibcraaltiibornatvioenrifciucravtieo.ns (CCV) are analyzed to verifythe continued 10.3.2 Aofnoanlyezpeearmsaimd-pralengseet.calibration standard after every tenth sample, with a minimum 10.4 Internal Standard/Surrogate Standard 10.4.1 Aacwthonrienlelclieanfexattntielrotlrarnnwacsattiihiltoohisnpnitnaobpnterfhdottweahcreeemdseasin(dnIaS-atnrhl)aydemntebrgaaeeoytfifooobirfeneotthufaeesnraeeancsdlaatyl.ltsyioibtTseqr.haurteeaiosnIpnStiofcsnyuhsrtoevhueetlo.dtaITbSrgehreesetpsIaiSpknoesanhdlsyoeatuetalsadnbndbyaeaemaskdtonaduobenwlditsntahhfitanetgr 10.4.2 Atqahnuedsauncartanirltoiaabgltyriavastteieislo.ysnteTacvnhuaderlavusreaud.tremrothageyatbeenestuhirsoeeudalndfaoblryetqsiucpaaikllieptdyrotccooenfdaturlorlelw.iinTtchhliunedtsihunergrlosoagwmattpeoliemspuirdse-eprdaanrtaogteioonf 11.0 Calibration and Standardization____________________________________ 11.1 Afssithtnao(nauyldyl=adzrendaxotch2tueb+rvesbetfaxsonmr+dcaeacrdy)dubthcesuriponrvlugoegtMshtepadzrseisborLyory.ltnionxeaaonrrdrofetoghlreleorswssuiionitngabe(ylaec=hsomsfetxwt +oarfbee.)xwtTreahicegtshc.taelTdibhr1ea/xtai,ovonerrcaqugurevadeosrfattwico 11.2 pIfrethpearceaalibnreawtiosntacnudravreddcouersveno(itfmneeceetsascacreyp)taanndcerecarnitaelryizaep.erform routine maintenance or 11.3 uFacphtospoitgenebrhsmtpthiouscpetorti1pilnnon0ocgwg0se0oentesoftpnrtopaqhdtfbueio)aoa.scfnntctatThsuinttheraadaitncascedarywdlaaiwpsribdlprlfhsarrer.ootenimxodiqnum5ucceaaputnpirentvbliyaetactro1tcai0unt1hrgp0aep0clrboyptwhopaatbfltnearrivnabteahtulhlestyeetfordeuf,tlthlagoanrealnaninlnetygherteaaee.tr,efiruEtealxgmlcarraamealysnipsbgbilroeeea:ntoniowwefnctehheiceesgunshcratuvriryenvgteoo(5f 12.0 Procedures_________________________________________________________ 12.1 Acquisition Set up . 12.1.1 Set up the sample list. 12.1.1.1 iaoeAnnnnssddttsrhiotughefmnetsheaadenmastylaei(ms(TdtT.paf0yloe0,r1ulTi0ssue1tc2fiiknlfeecornrr)ea,aOmtshcienetougybseleienartgrt1e(2tr0hs,0e2of0ffoi0rtrhs0t2e).0lea0tlI0tpfe)hmr,aotobhfereetthmstehtaonarnnattimhnogen(e0ow4lfiittsfhhoteriAsAmaptratidhl)ee, AUsnianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes5 of9 FACT -TCR002 (LIMS #E00-1716). Page 43 of 109 BACK TO MAIN 111222...111...111...324 ATAysspssiieggnninaasnammHeptPhlLeoCdde(psMrcorSgi)pratfimiolen.(sInalnedt vfiilael).position numbers. 12.1.2 tDtTshopoAee4ccT9Str9rAIeoRaomtsAre.eCoatSetQhmarUevhereItehSaaapoIdcTpdqinrI,uOogcipsslNiirctaiiakfnootdneornsmmaedmaledestecihsttteoihosSdo.n.IdRaAliS.niefnSetufhelotlethrsmieAocMaanctnqiiziouciansirtso.iuiomtsinouanamslslcoyModnceatoraslosslelLacpyptaenpndxreoiGlnptUrhaiaedIDtndeiEmtainoTadnsOstmoass 12.1.3 Tstyapnidcaarldlys.the analytical batch run sequence begins and ends with a set ofsolvent 12.1.4 peSvoaesmsryibptlleeensathnaraselayamtnepaclleay.rzreySdoovwleviret.hntabclaonnktisnushinogulcdabliebraantiaolynzveedripfeicraiotidoinca(lClyCtVo)minojneicttoerdfaofrter 12.2 Using the Autosampler/Column Heater 12.2.1 SPelcatcieonsa1m2p.1l.e1v. ials into the sample tray according to the sample list prepared in 12.2.2 sAwtittacchhintghevaplrvoep,emr aaknealsyutirceatlhcaotltuhmentuibninthgeicsorluunmtnohtheeataeprpcroomprpiaarttempeonrtt.s.Ifusing the 12.3 Using the Inlet Editor 12.1.1 ciSnosenttsr-uiudmperetshneatplHopgProb1op1or0ik0a:tuesfionrgotphteimfoalllorewsipnogncseo.ndRiteioconrsdoarcatut acloncodnitdioitniosnthseinanthaelyst 12.1.1.1 Sample size = 10 pL injection 12.1.1.2 Flow rate = 300 pL/min. 12.1.1.3 Cycle time = 10.0 minutes 12.1.1.4 MSSSoooolllvbvveieelnnnetttpAGBh::raas2dMe.0iecenmothtm:MapnooAnlme(T04818nM1m.....it005005mse.o0:00000OneiHfum)minA.icetate %55995S.5..5t000o.B.0000p0%%%%% AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfoetnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes6 of 9 FACT -TCR002 (LIMS #E0O-1716), Page 44 of 109 BACK TO MAIN 12.4 Instrument Set-up 12.4.1 RE9-le3efc6et,rr"otoOsptphreaeryaP/tMlioaatnfsosarnmSdpLMecCatrZionmUteensteaernr'c"se.Goufidthee, tMheicMroamssaLssyPnxlaNtfoTrmUsLeCr'Zs Guide or ETS- 12.4.2 Check the solvent level in reservoirs and refill ifnecessary. 12.4.3 TdCihhseaesctskiepmthsbehloteiuptlhdoebfpetrhofelbasettawainnitdlhersnesopsljtaaecgeelgtechdaepeisdltlagaiernsyl.eastIsfthsthteeeeeltnicpdapoisiflfltaohrueynp.drotobebewuitnhsaatnisefyaecptoieryce,. 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. 111222...444...555...132 12.4.5.4 AeROSSxeeelbptltasoetHdewhlrjlPuevetLsedostCodwtelhrqvipoetueuhpnitmllinetipbtopfsrlooantcfotweoetbhm"tfuOeooilnirpntzghr"aioen.tobgldueetegaisosafitsfrnet1lohed0aemfmkltioiiisnpnwtguoitrsafearosttohe.bu.esnepdrrvotehbdee..tipAoffintheempirsotbseh. ould be 12.4.6 cThhaenignestirnumorednetrutoseosptthiemsiezpeatrhaemreesteprosnaste:the following settings. These settings may 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, flowrate 10- 500 (iL/min 12.4.6.4 HPrPeLssCuries <o4p0e0rabtianrg(cTohrirsecptalyra.)meter is not set, it is a guide to ensure the 12.4.6.5 Source Block temperature 150. 12.4.6.6 Desolvation temperature 250. 12.4.7 Picnorfiponirtemsthateatipotuendn,eiannptdaogatehllweoiittnhhsetirrtusampppaelrniactmarbiemlteerilnso,fgotbhromeoaIknt.iloent paangde,stsoarme pitleinlitshte, mstausdsysbpiencder with 12.4.7.1 All copies must be initialed and dated. 12.4.8 nCulimckbeorns isntacrlut dbeutatollnsaomnpthleesMtoabsseLaynnaxlytzoeodl.bar. Ensure start and end sample 13.0 Data Analysis and Calculations_____________________________________ 13.1 Calculations: 13.1.1 Calculate matrix spike percent recoveries using the following equation: AUnsianlgysHisPoLfCP-oEtalescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfoetnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes7 of9 FACT -TCR002 (UNIS #E00-1716), Page 45 of 109 BACK TO MAIN % Recovery = Observed REexsupletc-teBdaRckegsuroltund Result x 100 13.1.2 Calculate percent difference using the following equation: % Difference = Expected CoEnxep.e-ctCeadlcCuolnatee.d Cone, x 100 13.1.3 Calculate actual concentration ofanalyte in matrix (jlg/mL): On-Column Concentration (|j.g/mL) x Dilution Factors = Calculated Concentration 14.0 Method Performance _________________________________ ;_________ 14.1 TathnheaelcyLatleiimsb,ritathtoieofLnQOcuuaQrnvtceiot.antcioennt(rLatOioQn)iisssmeleetchtoedd,aasntahleytleo,waensdtmacacterpixtasbpleecnifoicn.-zFeoror mstaanndyard in 14.2 cSaollivbernattioanndcumrveteh.od blank values must be < %that ofthe lowest standard used in the 14.3 Teqhueacloteoff0i.c9i8e0nt. ofdetermination (r2) value for the calibration curve must be greater than or 14.4 sCtoanndtianrudincgonCcaelnibtrraattiioonn. Verification (CCV) percent recoveries must be + 30% ofthe 14.5 Internal Standard recoveries should be within + 50% ofthe spiked concentration. 14.6 pIafnecrafrloyitrsemtr.ieaDdliooscnteudtmhieennsttyhasiltslemmacetatinhodnosdsaipnmertphfloeersmrarawenacndeaaltsyae.zcetdioonraorethneortamcteiot,nms aasindteetnearnmcienmedabyybtehe 14.7 Ifofodtantoatiesdtoonbetarbelpeosratenddwdihsecnuspseerdfoinrmthaencteexctroitfetrhiaehraevpoernt.ot been met, the data must be 15.0 Pollution Prevention and Waste Management_______________________ 15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 16.0 Records____________________________________________________________ 16.1 Ehianneataaceldhgyersprata.toigorenhgamennedethrwaortdei,tdtsefanomropanlesthtnueadmpyaemg,eue:sxstttrhuaadcvyteiootnrhepdrafotoejle,lcodtwilniuuntgmioibnneffroa,cramtocarqtu(ioiisfniatiiponpncllimucadebetldheo)e,dita,hnedr in the 16.2 tPaaprpipneltiicntahtboelettuhinenefionprsamtgruaetm,ioseannmttopruliennlcloilsgut.,deanind athcequaipspitrioopnrmiateethsotuddfyrofmoldMera.ssCLoypnyxtahnesdeopthageres and 16.3 Plot the calibration curve then print these graphs and store in the study folder. AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes8 of9 FACT -TCR002 (LIMS #E00-1716), Page 46 of 109 BACK TO MAIN 16.4 Panridntstdoarteaiinnttehgerasttuiodnysfuomldemr.ary, integration method, and chromatograms, from MassLynx, 16.5 Summarize data using suitable software and store in the study folder. 16.6 Banadckloucpateiolenctorofnbaicckduaptaetloecatpropnroicprdiaattae.medium. Record in study notebook the file name 17.0 Attachments________________________________________________________ 17.1 None 18.0 References ________________________________________________________ 18.1 P5RlaZtf;oormr FLloCaZtsURsoeard's, WGuyitdhee,nMshiacwroemMas2s3U9KLZL;imUinteitde,dTKuidnogrdRomoa.d, Altrincham, WA14 18.2 M5RaZss;LoyrnFxloNatTs URoseard',sWGyuitdhee,nMshiacwroemMas2s3U9KLZL;iUmnitietded, TKuidnogrdoRmoa.d, Altrincham, WA14 18.3 AMltarsisnLcyhnamx N, WTAG1u4id5eRTZo; DoraFtaloAactsquRiosaitdio,nW, yMthicernosmhaawsseUMK23Li9mLiZte;dU, nTiuteddorKRinogaddo,m. 18.4 EETleSct-r9o-s3p6r.a0y,/"MOapsesraStpiorencatrnodmMetaeirn"t.enance ofthe Micromass Platform LCZ 19.0 Affected Documents_______________________________________;________ 19.1 None 20.0 Revisions_________________________________________________ ;_________ NReuvmisbieorn. Reason For Revision ReDvaistieon AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes9 of9 FACT -TCR002 (LIMS #E00-1716), Page 47 of 109 BACK TO MAIN Attachment B: Data Summary Tables FACT -TCR002 (LIMS #E00-1716), Page 48 of 109 BACK TO MAIN Exact of Dritti J M ____ rntia Date PFOS in Octanol Day 1 Hillary, H010126 `if.'Ml'ii.'l*. >* hii-U r ' '* I* ' , ' | zn* V it ' oPFOS-1.1.1 TCR-002, 012201-oPFOS-1.1.1,100X Dll. SFM 01-24-01 MEE(MLA) oPFOS-1.1.2 TCR-002, 012201-OPFOS-1.1.2,100X Dll. SFM 01-24-01 MEE(MLA) TCR-002, 012201-OPFOS-1.1.3,100X Dii. oPFOS-1.1.3 SFM 01-24-01 MEE(MLA) TCR-002, 012201-OPFOS-1.1.4,100X Dii. oPFOS-1.1.4 SFM 01-24-01 MEE(MLA) oPFOS-1.2.1 TCR-002, 012201-OPFOS-1.2.1, 100X Dii. SFM 01-24-01 MEE(MLA) oPFOS-1.2.2 TCR-002, 012201-oPFOS-1.2.2,100X Dll. SFM 01-24-01 MEE(MLA) TCR-002. 012201-OPFOS-1.2.3, 100X Dii. oPFOS-1.2.3 SFM 01-24-01 MEE(MLA) oPFOS-1.2.4 TCR-002, 012201-oPFOS-1.2.4,100X Dii. SFM 01-24-01 MEE(MLA) TCR-002, 012201-OPFOS-.3.1, 100XDII. oPFOS-1.3.1 SFM 01-24-01 MEE(MLA) oPFOS-1.3.2 TCR-002, 012201-OPFOS-1.3.2,100X Dii. SFM 01-24-01 MEE(MLA) oPFOS-1.3.3 TCR-002, 012201-OPFOS-1.3.3,100X Dii. SFM 01-24-01 MEE(MLA) . TCR-002, 012201-oPFOS-1.3.4,100X Dll. oPFOS-1.3.4 SFM 01-24-01 MEE(MLA) 45 H010126A.M HILL0045.D 46 H010126A.M HILL0046.D 47 H010126A.M HILL0047.D 48 H010126A.M HILL0048.D 52 H010126A.M HILL0052.D 53 H010126A.M HILL0053.D 54 H010126A.M HILL0054.D 55 H010126A.M HILL0055.D 57 H010126A.M HILL0057.D 58 H010126A.M HILL0058.D 59 H010126A.M HILL0059.D 60 H010126A.M HILL0060.D 18 19 20 21 22 23 24 25 26 27 28 29 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 .X-Kii .. ( 15147632 14930350 14776497 14962900 14992721 15098625 14869642 14727877 14778751 14632795 14831350 14666605 M 603.6 -- .'.'.hii'., . 59.1 57.8 586.0 57.4 0.88 588.4 57.6 1.5% 583.7 57.1 603.3 59.1 56.9 569.0 55.7 1.87 589.4 57.7 3.3% 561.3 55.0 568.5 55.7 56.0 568.9 55.7 0.65 581.5 56.9 1.2% 567.3 Day 1 average: std dev: % C .V .: 55.5 56.9 ng/mL 0.9 1.6% FACT -T C R 0 0 2 (LIM S #E00-1716), Page 49 of 109 3M Environ m enial Laboratory Solubility. S h a k i Fta lk M athod 4/18/01 Paga 1 o f 3 BACK TO MAIN FACT -TCR002 (LIMS #E00-1716), Page 50 of 109 PFOS in Octanol Day 2 Hillary, H010126 r ~ -lln j.!' >1 1, ....... ` ' 9, . oPFOS-2.1.1 TCR-002, 012201-oPFOS-2.1.1,100X Dii. SFM 01-25-01 MEE(MLA) 25 H010126B.M HILL0103.D 34 TCR-002, 012201-OPFOS-2.1.2 ,100X Dii. oPFOS-2.1.2 SFM 01-25-01 MEE(MLA) 26 H010126B.M HILL0104.D 35 TCR-002, 012201-oPFOS-2.1.3,100X Dii. oPFOS-2.1.3 SFM 01-25-01 MEE(MLA) 27 H010126B.M HILL0105.D 36 TCR-002, 012201-oPFOS-2.1.4 ,100X Dii. oPFOS-2.1.4 SFM 01-25-01 MEE(MLA) 28 H010126B.M HILL0106.D 37 cv TCR-002, 012201-oPFOS-2.2.1, 100X Dii. oPFOS-2.2.1 SFM 01-25-01 MEE(MLA) 32 H010126B.M HILL0110.D 38 Q TCR-002, 012201-oPFOS-2.2.2,100X Dii. oPFOS-2.2.2 SFM 01-25-01 MEE(MLA) 33 H010126B.M HILL0111.D 39 2 (0 Q TCR-002. 012201-OPFOS-2.2.3,100X Dii. oPFOS-2.2.3 SFM 01-25-01 MEE(MLA) 34 H010126B.M HILL0112.D 40 1 10 c0 oPFOS-2.2.4 TCR-002. 012201-oPFOS-2.2.4,100X Dii. SFM 01-25-01 MEE(MLA) 35 H010126B.M HILL0113.D 41 TCR-002, 012201-OPFOS-2.3.1,100X Dii. oPFOS-2.3.1 SFM 01-25-01 MEE(MLA) 37 H010126B.M HILL0115.D 42 TCR-002, 012201-oPFOS-2.3.2,100X Dii. oPFOS-2.3.2 SFM 01-25-01 MEE(MLA) 38 H010126B.M HILL0116.D 43 TCR-002, 012201-oPFOS-2.3.3,100X Dii. oPFOS-2.3.3 SFM 01-25-01 MEE(MLA) 39 H010126B.M HILL0117.D 44 TCR-002, 012201-oPFOS-2.3.4,100X Dii. oPFOS-2.3.4 SFM 01-25-01 MEE(MLA) 40 H010126B.M HILL0118.D 45 *n v 5.14 14,706,785.0 564.2 5.14 14,920,516.0 577.2 5.14 14,680,691.0 557.4 5.14 14,975,314.0 579.8 5.14 14,469,565.0 560.9 5.14 14,290,466.0 549.1 5.14 14,221,117.0 553.7 5.14 14,265,295.0 552.5 5.14 14,756,722.0 585.6 5.14 14,880,485.0 582.6 5.14 14,413,925.0 567.0 5.14 14,903,941.0 595.9 Day 2 average: std dev: %C.V.: 3M Environ mental Laboratory Sohjbllity, Shake Flask M ethod 4/1B/01 t -."- ->;... 'X'vrr-m Vit* iniU}' :JV f . . 1 - 55.2 55.8 56.5 1.04 54.6 1.9% 56.8 54.9 54.2 53.8 0.48 54.2 0.9% 54.1 57.3 57.1 57.0 1.17 55.5 2.1% 58.3 55.7ng/mL 1.4 2.5% Page 2 of 3 BACK TO MAIN FA C T -T C R 0 0 2 (LIM S # E 00-1716), Page 51 of 109 PFOS in Octanol Day 3 Hillary, H010129 IfiilfS i l$fnTj\ 1 TCR-002, 012201-OPFOS-3.1.1,100X Dii. oPFOS-3.1.1 SFM 01-26-01 MEE(MLA) TCR-002, 012201-oPFOS-3.1.2,100X Dii. oPFOS-3.1.2 SFM 01-26-01 MEE(MLA) TCR-002, 012201-oPFOS-3.1.3 ,100X Dii. oPFOS-3.1.3 SFM 01-26-01 MEE(MLA) TCR-002, 012201-oPFOS-3.1.4 ,100X Dii. oPFOS-3.1.4 SFM 01-26-01 MEE(MLA) co TCR-002, 012201-oPFOS-3.2.1,100X Dii. oPFOS-3.2.1 SFM 01-26-01 MEE(MLA) Q TCR-002, 012201-oPFOS-3.2.2,100X Dii. oPFOS-3.2.2 SFM 01-26-01 MEE(MLA) a co Q TCR-002, 012201-oPFOS-3.2.3,100X Dii. a oPFOS-3.2.3 SFM 01-26-01 MEE(MLA) 1 co (0 TCR-002, 012201-OPFOS-3.2.4,100X Dii. oPFOS-3.2.4 SFM 01-26-01 MEE(MLA) TCR-002, 012201-OPFOS-3.3.1,100X Dii. oPFOS-3.3.1 SFM 01-26-01 MEE(MLA) TCRr002' 012201-oPFOS-3.3.2,100X Dii. oPFOS-3.3.2 SFM 01-26-01 MEE(MLA) TCR-002, 012201-oPFOS-3.3.3,100X Dii. oPFOS-3.3.3 SFM 01-26-01 MEE(MLA) TCR-002, 012201-oPFOS-3.3.4,100X Dii. oPFOS-3.3.4 SFM 01-26-01 MEE(MLA) 45 H010129A.M HILL0045.D 46 H010129A.M HILL0046.D 47 H010129A.M HILL0047.D 48 H010129A.M HILL0048.D 52 H010129A.M HILL0052.D 53 H010129A.M HILL0053.D 54 H010129A.M HILL0054.D 55 H010129A.M HILL0055.D 57 H010129A.M HILL0057.D 58 H010129A.M HILL0058.D 59 H010129A.M HILL0059.D 60 H010129A.M HILL0060.D 31 32 33 34 35 36 37 38 39 40 41 42 , C' ! Militi ' t i * * * ? 5.14 12,608,096.0 559.0 S te a 54.7 55.4 5.14 12,676,281.0 565.6 55.4 1.23 5.14 12,836,214.0 582.9 57.1 2.2% 5.14 12,513,073.0 554.1 54.2 5.14 12,316,146.0 545.9 53.4 53.0 5.14 12,252,723.0 540.8 52.9 0.34 5.14 12,205,875.0 538.7 52.7 0.6% 5.14 12,170,612.0 538.4 52.7 5.14 12,979,064.0 605.8 59.3 58.0 5.14 12,939,967.0 584.4 57.2 0.91 5.14 12,913,836.0 589.6 57.7 1.6% 5.14 12,899,195.0 589.7 Day 3 average: std dev: %C.V.: 57.7 55.4 ng/mL 2.5 4.5% 3M EnvirofimenUI labocetory S o lu b ity , Shake Flask M ethod 4/18/01 Page 3 of 3 PFO Ostami M FACT-TCR0C2 Exact Copy of Original ^ initial O W fl ! a v& Date Study # FACT-TCR002 Compound: PROS Study: Octinol Solubility DAY 1 Analytical Instrum ent Hillary on 01-25-01 Reprocessing Workstation: Dioana 01/30/01 batch H0125a2.b Hap M id 0100347-13 010Q3417-13 CM003-07-01 310007-02 0100307-03 01003-07-04 01003-07-09 01003-07-00 31003-07-07 01003-07-00 01003-07-00 01003-07-10 0100307-11 0100347-12 01003-07-13 1002.0m * PFOB Syttam SdtabUyfEqdftratton O p * PFOO Qym m QiO*U 4Eqidtafaltan 9p* ppo o 10p*PFO O f " --------- ------ " 40m * PFOS O ptantSuMBpCquBbraOwi O O .fp* PFOO tp tam iw 4W)rT i|uebratten 7 5 .1 *6 PFOO Qptawi 0i4taf >4C4*9taaHM> 1 0 0 .2 *6 PFOO Qpmw Q* tata>p * iiiH i)ii 290,5m * PFOO OyttamOUMOpE^UOmtan 4 0 0 6 *6 PFOO Qptaiw Qy--OMpTCuu--iiH ijii 501.C *6 PFOO Qytasm 0yO *eyrC*0 6 r*M i 3 H010126A.M 4 H01012SA.M 0 H010120A.M 9 H010120A.M 10 H010120A.M t i H01012SA.M 12 H01012SA.M 13 H010120A.M 14 H010120AM 19 H010120AM 10 H01012SAM 17 H010120A.M 10 H010120A.M 11 H01012SAU 20 H01012SAM H1U0003.D HILL0004.D HILLOOOO.O H4U0OOO.O H1U0010.0 HU.14011.0 HU10012.0 HU10013.0 M U0Q14.D HILL0019.0 M U0010.0 H IU 0017.0 HILLOOIO.O HIUOOIO.O H1UJ20.O 0100347-01 01003-07-02 0100347-03 0100347-04 3100347-00 010034740 010034747 0100347-00 010034740 0100347-10 0100347-11 0100347-12 0100347-13 010034740 010034740 Ota33 * 1* 6 PFOO, u re a t ip t o p , 3n a p * n ipptproa nmroo,3H,o*> loppt eroe Tw*oo,340p*PFf OM 9, 29.09* p ro s , 29 4.4*0 2 9 *0 PTO4 THPFOO.254.CM* PFBS OU0 .4 0 .0 9 t* PFOO, 25 4.4*0 40p*P FO O THPFOO.2S40p* PFBS OU7 .80.101* PFOS.294.4M * 9 0 .1 *6 PFOO THPFOO,294.0*6 PFBS SUO. 7& 19*6 PFOS, 2 5 4 .* * 7 5 .1 *6 PFOO THPFOO.254.0*6 PFBS 0 U 0 ,100.20*6 PFOO. 234.4*6 1 0 0 4 *6 PFOS tHFFOO,2940*6 PFB8 SU 10.290.81*6 PFOO, 29 4.4*6 2 9 0 .9 *6 PFOO THFFOO. 2940*6 P F H SU 1 1 .4 0 0 ,8 *6 PFOO, 294.4*6 4 0 0 .0 *6 PFO0 THPFOO,254.0*6 PFBS SU 12.00101*6 PFOO, 294.4*6 9 0 1 4 *6 PFOO THPFOO,2940*6 PFBS OU 13. 10021*6 PFOO.29 4.4p * 1002 .0 *6 PTOO THPFOO,2 5 4 .** PFBS SU 0,10 04 0*6 PFOO. 2 9 4 .* * 1 0 0 4 *6 PFOO. CCV THFFOO.294.0*6 PFBS OU0 ,100.2C*b PFOO. 254.4m * 1 0 0 4 *6 PFOO. CCV THFFOO.294.0*6 PFBS 24 H01012SA.M H1U0024.0 29 H01012SA.M KH U 829.0 20 H01012SA.M M U0020.D, 27 H01012SA.M H IU M 27.0 20 HO1O120A.M MUMBO.O 20 H010120A-M MLUXBO.O 30 H010120A.M HRX0030.D 31 H010120A.M HNX0031XI 32 H01012SA HIU0032.D 33 H01012AAJN WLL0033.D 34 H010120A.M HIU0C34.D 39 H010120AJ4 HUU039.0 30 H01012AAJ4 MUOCOO.O 40 H010120A.M H IU0040.0 01 HOI0120A.M H IU0001.0 010034741 09 K010120A.M H IU 0009.0 010034742 3 .0 *6 PFOO THPFOO, 204,8*6- OS H010126A.M HILLOOOO.O 010034743 010034744 010034749 910034740 010034747 010034740 010034749 0100347-10 Ipp6 PFOO THPFOO, 204,8*6 PFOO OU 4, 10.03*6 POOS, 294 4 *6 io*> pros THPFOO,aoiiBpptanoto OU9 .2S.0Bp* PFOS. 2 5 4 .* * 2 9 *6 PFOS THPFOO. 294.0*6 PFBS BUS. 40.00*6 PFOS. 25 4.4p * 4 0 *6 PFOO THPFOO,254.0*6 PFBS OU7, 90.10*6 PFOS, 29 4.4*6 S O .Ip * PFOO THPFOS,294.0*6 PFBS SU 0 .79.19*6 PFOS. 2S 4.4p* 79.Ip * PFOO THPFOO, 2S4.0p* PFBS SUO. 10 04 (6* PFOS. 29 4.4p * 1004p*P P O S THPFOO. 294.0p* PFBS 8 U 10.290.90*6 PFOS. 2S 4.4p* 2 9 0.5*6 PFOO THPFOO. 2S4.0p* PFBS 07 H010126A.U HUX0007.0 SO H01012BAM HILLOOOO.O H01012BA.M HILLOOOO.O 70 H0UM 39A.il HIUOOTO.O 71 H010129AU HILL0071.D 72 K010120AJI HHJL0072.D 73 H010120A.M HIU0073.D 74 H010120A.M HILL0074.0 0100347-11 0100347-12 0100347-13 400.8p*PPO S THPFOO. 234.0p* PFB8 OU 12.90150*6 PFOS.2S 4.4p* 9 0 1.0p * PFOS THPFOO.254.0p* PFBS 8 U 13, 1002.0*6 PFOS. 29 4.4p * 1002.0p* PFOO THPFOO,2$4.0p* PFOO 73 H010120A.M HILL007S.D 70 H010120A.M HU10070.D 77 H010126AJ4 HIU0077.0 FACT -T C R 0 0 2 (LIMS #E00-1716), Page 52 of 109 eXPOOT 0* 1 OaU PFOO Oe*wl a * * 0U 601<OObjOi BACK TO MAIN |FBOntrfmL 13 234.0 13 234.0 2t 254.0 234.0 3 234.0 4 234.0 3 254.0 234.0 7 234.0 234.0 0 234.0 IO 234.0 11 234.0 12 254.0 13 234.0 1 234.0 2 234.0 3 234.0 4 254.0 P 234.0 234.0 7 254.0 234.0 0 254.0 10 254.0 11 234.0 12 234.0 13 234.0 234.0 234.0 1 234.0 2 254.0 3 234.0 4 234.0 3 234.0 e 234.0 7 254.0 254.0 9 254.0 10 254.0 11 254.0 12 254.0 13 234.0 PFBSKT 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.t1 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 CEKUoi 2.278,003.5 2.208,970.3 2.234,820.3 2.247,057.3 2,202,106.5 2,223,519.3 2.223.333.5 2.220,632.9 2X10X92.0 2.198.272.3 2.232.307.3 2.217,083.3 2X46.434.3 2X30.829.6 2X30X20.8 2X96,990.9 2.238,528.0 2X07,812.3 X183380.0 2.248,184.8 2XM.180.6 2X42,1203 2,1*4,9030 2,234,002.3 2X04,718.3 2X71,192.0 2X48.770.3 2X43,8054 2X93.730.0 2X48.4284 2X24.4944 2.254,833.6 2X87.0864 2X48.1804 2X54.077.3 2X48X90.0 2X38.474.0 2X34X06.0 2X53,184.0 2X23,327.0 2.2084334 2X93.4084 2X724864 THPTPSnofwL 254.4 234.4 234.4 254.4 234.4 234.4 254.4 234.4 254.4 234.4 254.4 234.4 254.4 234.4 234.4 254 4 254.4 254.4 234.4 234.4 234.4 234.4 294.4 234.4 234.4 234.4 254.4 234.4 254.4 234.4 254 4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 234.4 234.4 TyyfOS RT 4.66 4.06 4.86 4M 4M 4M 4M 4.M 4.M 4M 4M 4M 4.M 4M 4.66 4M 4.M 4.M 4M 4M 4M 4M 4M 4M 4M 4M 4M 4M 4.88 4M 4M 4M 4M 4M 4M 4M 4M 4M 4M 4M 4M 4M 4M TWPfPSarw 1.061.303.8 1,046,830.0 1.084,672.8 1,081,741. 1,005,120.0 1.0M.30J.4 1,090,125.0 1.108.340.1 1,111.054.1 1,111,112.6 1,126.504.0 1,000.946. 1.003.849.1 1.007.350.4 1,001,033.0 1,157,070X 1.160,401.3 1,162X07.4 1.181,1603 1.134X60.4 1,162,826.6 1.142,174.1 1,144X506 1.130X79.1 1.127,420.8 1,141X90.4 1,129X10.3 1,000,469.1 1.171.457,8 1.184,541.1 1,173.286.4 1,180,849.3 1,181,686.0 1,174,018.4 1,177,197.3 1,180.158.4 1,164.408.3 1.180.544.0 1.174,082.5 1,144,983.8 1.167.0903 1.145.707,0 1,100.402.0 PFOS OcMnd S d FACT-TCR002 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility DAY 1 Analytical instrum ent Hillary on 01-25-01 Raprocessing Workstation; Dioana 01/30/01 batch H0125a2.b PF06-1.1.1 eP FO S-I.U pP F O S -U J- TCR-002,012201-oPFO S-1.il. 100X DUO 2 ,SFM 01-24-01 MEE(MLA) TCR-002.012201-ePFOS>1.1 10QX DS.Q SFM 01-244)1 MEEfMLA) TCR-002.012201-ePFOS-1.t.3,10QX D4.D SFM 01-344)1 M(ULA) TCR-002.012201-PFOS-1.1.4.10QX 0S.Q SFM 01-24-01 MEE(MLA) 4S H010128AM HILL0045.0 4 H01012SAM MLL004S.D 47 H01012SAM HILL0047.0 44 H010126AJI HILL0044.0 P F O S -IJJ opfos- u j oPFOS-1.2.4 oP FO S -IJ.1 oPFOS-1J-2 TCR-002.012201-P F O S -IZ I. 100X01.0 SFM 01-244)1 MCE(MLA) TCR-002.012201-oPFOS-12J2.10QX OI.D SFM 01-2401 MEE(MIA) TCR-002.012201-oPFOS-1X 3.100X DS.D SFM 01-2401 MEE(MLA) TCR-002.012201-*PFOS-1.2.4,100X DUD SFM 014401 MEEIMLA) TCR-002.012201-ePFOS-IS.1.100X 04.D TCR-002, O ISStnS-FoMPf0c1a4-4IA0Z1 M10E0XEjOMLlAO) SFM 014401 M EEfMlA) TCR-002,012201-ePFOS-M J.IO M DS.D SFM 014401 MEEfMLA) TCR-002.012201-oPFOS-1.3.4.100X 01.0 SFM 01444)1 M U 0 K A ) a H010126AJ4 HICLOOa.O a H010126AM m a o o a o 54 H01012SAJ4 HILLOOS4.O SS H01012SAM HILL005S.01 a H01012SAU HILL0057.D M H01012SAJI HULOOMJ) S H01012SAJ4 HU1005S.D SO H010120AJI HILLOOSO.D TCR-002,0122O1-oPFOS-1.4.1,100X DUO Mdhod M , SFM 14401 MEEfMLA) TCR-002.01220t-PFOS-1 .4 4 , 100X M .Q Mathed BNnk, SFM 01-24-01 MEE(MLA) TCR-002.012201-*PPOS*1.4,S. 100X 01.0 MaOied B M f*. SFM 01-24-01 M tE (M lA ) TCR-002.012201-OPFOS-1.4.4. 10QXDUO Mdhod S tar*. SFM 01-2441 UEE(MLA) 40 H01012SAM HILL004Q.D 41 H01012SAM HILL0041.0 H01012SAM HUUXM2.D 42 H01012SAM HUL0043.D tWrbOOHH8S MU*aOOMH 88 llaO H 8 MIP*OOHH8 M eONtt MMaOOHHSaI MaOHB MaOHB UaOH 8 TM-A-4740, 04 0m 00 TN-A-4740, 04 Dm 00 TNA-4740, 04OMO0 TM-A-4740, 04 Dm 00 TN-A-4740. 04 0M O0 TN-Ap4740, 04 0m 00 TM-A-4740. 04 Dm 00 TM-A-4740, 040m 00 TN-A-4740, 040m 00 TM-A-4740. 040m 00 TM-A-4740, 04 Dm 00 TN-A-4740, 04 Dm 00 TM-A-4740, 04 Dm 00 TN-A-4740. 04 Dm 00 TN-A-4740. 04 Dm 00 TM-A-4740, 04 Dm 00 TM-A-4740, 04 Dm 00 TN-A-4740. 04 Dm 00 TN-A474Q, 04 Dm 00 TNA-4740. 04 Dm 00 1 H01012SAM 2 H01012SAM S H01012SAM S H010126A.M 7 H01012SA.M 21 H01012SAM 22 H01012SAM 22 H010120A.M 37 HO10126AM M N01012SAM 35 H01012SAM 44 HOI0128AM M H01012SAM 51 H01012SA.M M H01012SAM a H010126AM H0I012SAM S4 H 0t012flAM 74 H010t26A.M 78 H010128A.M HILL0001.0 HILL0002.D HILLOOOS.D H IU 0008.0 H IU 0007.0 HILL0021.0 HILL0022.0 HIU0G22.O HHIIUlL0O0t3O7i..DD HIUOOM.D HILL0044.D HILLOOSO.D HILL00S1.D HILLOOSO.D HILLOOS2.D HILLOOS3.0 HILL00S4.D HILL0074.D KILL0079.0 FACT -TCR002 (LIMS #E00-1716), Page 53 of 109 EXPORT CMy 1 4Ma PFOS OcMnd M h M ty hOIOM uM BACK TO MAIN 1 254.0 1 254.0 20 254.0 21 254.0 22 254.0 254.0 24 254.0 25 254.0 2* 254.0 27 2545 29 254.0 2 254.0 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 14 2540 ts 254.0 1 254.0 17 254.0 4.11 4.11 4.11 4.11 dOm * C.V.: 4.11 0.0010 0.025% * * * * * I8 8 8 B B 8 S 8 S 2 000...000000 00..0000 00..0000 00..0000 0.00 0.00 0.00 0.00 00.0000 0.00 0.00 0.00 0o..0o0o 2,iw.ie.a 2.218.200.8 2.1M.018.0 2,195,7085 2,1*8,583.3 2,23*,*144) 2,178,0284) 2,137,0*80 2,188,01841 2,173.1325 2.1*55195 2,105.4*3.0 2,1*8,8*8. 2,180,183.3 2.180.1M0 2,200,340.0 2524.480.1 38,8*7.8 1.96% 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 4.8* 4.8* ili 4.88 4.88 4.88 4.68 4.88 4M 4M 4M 4.M 4M 4M 468 4M 4.68 0.0010 0.021% 000...000000 00..0000 00..0000 0000....00000000 0.00 000...000000 00..0000 00.0000 0.00 1,000,250.1 1,103570.1 1.0U.040.S 1,100,8*4.0 1,079,6015 1,145571.1 1.003517J 1,131,074.0 1,122.133.0 1,1105105 1,103.617.4 1,115,824.0 1,136,4125 1,182,181.1 1.144,7325 1,1535805 1,142,0065 28.9605 254% I < O o*<m ||:sS5s5|i8s|s " S s 3 S S E | ^ 5 i i l i S 3 2 s1 a sT *^ llHliSilliiiii =1i i i i i 1i 1 * *5 a ri n i i *! n g v N km n tri nS m Study: OcUnol Solubility DAY 1 ~ m i Q Q O B a o o o Q a o o o Q a a o a a o o o o o o o o a H g S * j o - : r r V ,ri<0 K : B i6 jr y j is jb ei r) n W qqqa qqa qqaq qao iiiiiilllillllii i i i f i i f i i i l i i l l i i i l i i l l " "^ssssstsaR S R R s s s s s a a s n j i t s a s t s s E i eg Q o o o o o o o o o o o o o o a o o S o o a o o o o S o o S o S a o S S S o s s iiiiiiiis is s i i i i s s i i l i s S s i i i i l s i s i i i ) 1111!! 1H i em m m u. * * i aU H I U I I H 8 S9 i 4 igStagEssg^taiSjatglstggatgglstilst 12i1B2i5i1IS|n!-itIii1f5i52i5i1 H| i6H*I %Ui> I$HI I Analytical Instrument: Hillary on 01-25-01 Reprocessing Workstation: Dioana 01/30/01 batch H0125a2.b Study #FACT-TCR002 Compound: PFOS FACT -TCR002 (LIMS #E00-1716), Page 54 of 109 PFOS O ctm i M FACT-TCR0Q2 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility DAY 1 Analytical Inttrumenfc Hillary on 01-25-01 Raprocataing Workstation: Dioana 01/30/01 batch H0125a2.b oPFOS-1.1.1 PFOS-1.1.2 PFOS-1.1.3 o P fo e -i.M o p fo a -u .i e p fo a -u a m am oPFOO-UA PFO S -1J.1 PFO S-t.3.2 P FO S -t.3.3 PFOS-1.3.4 TCR-002.012201-OPFOS-1.1.1,1Q0X H .0 SFM 01-2+01 MEE<MLA) TCR-002,012201-oPFOS-l.l.2. 100X D8.0 8FM 01-24-01 MEE{MLA) TCR-002.012201-4PFOS-1.14 .10QX 08.0 8FM 01-2401 MEC(MA) TCR-002.012201-PFOS-1.1.4. 10QX OLQ a m 01-2+01 8CE(MLA) TCR-002.012201-ePFOS-1.2.1.100X 08.0 a m 01-34-C1 ME<MLV TCR-002.012201-oPfOS-1.2J,100X DLQ a m 01-2+01 mcE(m u ) TCR-002.012201-PFOS-1.2 .3 ,100X ORO a m 01-2+01 m e e q jia ) TCR-002,012201*PF05-1-2.4, TOOK08.0 a m 01-2+01 MEC(MLA) TCR-002.012201 uP f06 -1-3.1 ,100X 08.0 a m 01-2+01 ME(MLA) TCR-002.012201-oPFOS-l4 .2 .100X D8.Q a m 01-2+01 MEE(MIA) TCR-002.012201-PFOS-1.3.3.100X 08.0 a m 01-2+01 MEE(MIA) TCR-002. 012201-ePFC*-1-3.4. 10CW08.0 a m 01-2+01 MEE(MIA) BuoC 45 45 47 41 a 53 54 55 57 58 58 80 IU p 88M Q fe flt H010126A.M H1U0045.D M010130A.U HIU0048.0 H010128A.M HIU0047.0 H010126A.M MUMMS.O H M O StA . MH100S2.0 M010128A.M M U0053.D H010126A.M HILL0084.O H010128A.M HIU00S5.O H010128A.M 110057.0 M 10128A.U HILU0S8.0 H01012SA.M U 0050.0 K010128A.M HIU0080.D U K PFOEIT 18 It 20 21 J .I4 33 23 24 * * 25 544 28 544 27 544 28 544 28 FACT -TCR002 (LIMS #E00-1716), Page 55 of 109 expoar or i pfoo O dM t ahMir M ioiau* BACK TO MAIN 15,147,632.0 144304504 14,778.407.0 14482,900.0 1440,721.0 15406.625.0 14,609,842.0 14,727,6774 14,776.7314 14,832.7954 14,631,350.0 14.686.805.0 n a w .m a 803.6 5684 568.4 583.7 6033 5894 S80.4 N I3 5884 5884 561.5 5674 Dy 1 gvt *ard*9rr .: C.V.: 'utsJmL Anna* S%tdCD.Vav. 80.4 384 88.6 040 36.8 14 38.4 804 56.1 564 1.91 384 34 38.1 984 574 364 0.87 36.1 1.2 38.7 66.1 termi 6.9 < * P*0 4 o#5 p ro CMMMl M FACT-TCM02 FACT -TCR002 (LIMS #E00-1716), Page 56 of 109 Study FACT-TCRQ02 Compound: PFOS Study. Octanol Solubility DAY 1 Analytical Instrument: Hillary on 01-25-01 Raprocotng W tukilallon: Dioana 01/30101 batch H0125a2.b /_ ------------ ----- ------- Buna Rh H U Dari. Ma VI aPFOS-1.4.1 PFOS-1.42 ma 1A1 P F 0 6-1.4.4 TCR-002. W2201-OPFOB-1.4.1,100X 04.0 TC ft-002.0l2201-aPfO 8-1-4.2. 10QXM .Q M atted Hank. BFM 01*24*1 MCE04LA) TCM-C02.OJ2201-cPf0 0 -1 .0 ,100X 04.D IM te d Hank. 07*4 0 1 -2 0 1 MCI(MLA) TCK-002,012201-aPFO B-M .4,1 0 00.0 MaBNd H w *. BFM 01-2401IC KM LA ) 40 41 HOI0120AM* WLL0040.D H01012BAM HIU0041.D MQ10120A.M KIU0042.0 H010120A.M WLL0043.0 MaOH O te * MaOH B M l MaOH I M M iO H B M M aO H Bte* MaOH Blank MaOH I M MaOH H w * M aO H BIw * MaOH Blank MaOH Blank MaOH Blank MaOH Blank MaOH Blank MaOH Blank TN-A-4740, 04 Dae00 H010120AM HtLLOOOl.D TH-A-4740. 04 Dec00 TN-A-4740. 04 Oae00 HH001100112286AA.MU HIU0002.D HXOCOS.O TN-A-4740, 04 Oae 00 H01012SA.M HttiOOOa.D TM-A-4740, 04 Oae 00 HQ1012BAM HNA0007.D TN-A-4740, 04 Dae 00 HO1O120AJ4 HIUXCB1.0 TM-A-4740, 04 Dae 00 H010126AJ4 HILL0022.D TM-A-4740. 04 Dae00 H01012BA.M HILUXS23.D TM-A-4740. 04 Dae 00 HOI0120AM HILU037.D TM-A-4740, 04 Dae 00 H010120AM HIUX03S.0 TN A4740. 04 Dae 00 H01012SAJ4 HHL0090.D 50TN-A-4740, 04 Dae 00 TN-A-4740, 04 Dae 00 H010120AM HILL0044.D H010120A.M HILL00S0.D TM-A-4740, 04 Dae 00 51 H01012BAM HIUX0S1.D TN-A-4740, 04 Dae 00 2TN-A-4740. 04 Dae 00 nTN-A-4740. 04 Dae 00 H010128AM MU0050.D H010120A.M MU0082.D H010120A.M HILL0063-D TN-A-4740. 04 Oae 00 TN-A-4740. 04 Dec 00 HOI0120AM HIUQ004.D to H010120AM MU007S.O TN-A-4740. 04 Dae00 70 H010120A.M HILLQ07S.O W PS NT 0.00 14 15 0.00 1 0.00 0X0 0011 I ai 0n2 000...000000 0000...X0000000 00..0000 00 00..0000 OS M 000..X00000 04 0.00 0.00 0.00 04 0.00 as 0.00 os 0.00 EXPORT Day 1 M a MFCS OctanafaeOryaJICOBaj* BACK TO MAIN Pf03H I nateJ-PfOS 04) 04) 0.0 0.0 0.0 0.0 00..00 00..00 00..00 004.0) 004.0) 00..00 00..00 00..00 04) 0.0 0.0 0.0 0.0 0.0 0.0 0.0 00..00 00..00 0.0 0.0 0.0 0.0 000...000 000...000 Pa0*s<rs 5 o O o7J o 2(/) m o o (Q (V o<0 PFOS SokiM ty FACT-TCR002 Exact Copy of Original M _____ ^ I f D l Bnitlal _ Date ^ Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument: .SasetUB Hillary on 01-2641 Reprocessing Workstation: ftaunn,Dr*t"fDPMWcfrftsWOon Dioana 01/30/01 batch H010126b.b Rm HW O rta-- 8141, Oppb P F 0 3 X * n IPTOS, 381.0ppb 01003-07-01 OppbPFOS P W - H010126B.M HILLOO01.O 0100307-02 0100307-03 2Sppb PFOS 284,Oppb PFBS W ), I.Q1ppbPF0ti * 44 SppbPFOS 314,Oppb PFBS H010126B.M HH10062D HO1O120B.M HHX083.0 0100307-04 0100307-03 0100307-08 0100307-07 0100307-08 S 0100307-00 0100307-10 0100307-11 0100307-12 0100307-13 5p 0100307-00 0100307-00 0100307-01 IS 0100307-02 0100307-03 0100307-04 0100307-09 0100307-09 D100307-07 0100307-09 0100307-09 0100307-10 0100307-11 0100307-12 0100307-13 10ppbPFOS 28<,0ppbPFBS SU S, 2S.09ppb PF08,254.4ppb THPFOS, 2Sppb PFOS 2S4.0ppb PFBS LOQ SU 9 ,40.06ppb PFOS. 254.4ppb THPFOS. 40ppb PFOS 2ft4.0ppb PFBS SU 7. SO.IOppb PFOS,294.4ppb THPFOS. 80.1ppb PFOS 2S4.0ppb PFBS SU 8 .75.1Sppb PF08,2S4.4ppb THPFOS. 7S.1pp6 PFOS 2S4.0ppb PFBS 8U 9 .10O20ppb PF0S. 2S4.4ppb THPFOS, 100.2ppb PFOS 2S4.0ppb PFBS SU 10,2S0.50ppb PFOS.2S4.4ppb THPFOS. 2S0.Sppb PFOS 2S4.0ppbPFBS SU 11,40ae0ppb PFOS,294.4ppb THPFOS. OO.Bppb PFOS 2S4.0ppb PFBS SU 12. SOl.OOppbPFOS. 294.4ppb THPFOS. SOl.Oppb PFOS 2S4.0ppb PFBS SU 13. 1002OppbPFOS.254.4ppb THPFOS. 10Q20ppbPFOS 254.Oppb PFBS SU 9 .10020ppb PFOS.2S4.4ppb THPFOS. 100 2ppb PFOS, CCV 254.OppbPFBS SU 9 .100.20ppb PFOS. 254.4ppb THPFOS. aw100.2pp6 PFOS. CCV 254.0ppb PFBS 8U 91, Bpph PFOSi <ppb THPFOS, 384,Qp OppbPFOS PFBS- suaaaiippbP iM 4 b THPFOS, a i, P2 SppbPFOS 384,OppbP F S t U liO Ippb an.ippbTvnros, S & b P fO S at l . p b P F B t SU34| 100199 38,aS4,4pphTHPFOS, 10ppb PFOS 984,Oppb PFBS 6U 29 ,29.09ppb PFOS.294 4ppb THPFOS. 29ppb PFOS 2S4.0ppb PFBS LOQ 8U 26 .40.08ppb PFOS.2S4.4ppb THPFOS. 40ppbPfO 8 254.0ppb PFBS SU 27. SO.IOppbPfOS. 294.4ppb THPFOS. 50.1ppb PFOS 254.0ppb PFBS SU 26 .7S.19ppb PFOS,2S4.4ppb THPFOS. 7S.1ppbPFOS 254.OppbPFBS 8U 29. 10020ppb PFOS, 2S4.4ppb THPFOS. 10Q.2ppbPFOS 254.Oppb PFBS SW30. 290.9OppbPFOS. 254.4ppb THPFOS. 2S0.5ppb PFOS 254,0ppb PFBS SU 31. 400.80ppb PFOS. 2S4.4ppb THPFOS. 400.8ppb PFOS 254.Oppb PFBS SU 32 SOl.OOppbPFOS. 2S4.4ppb THPFOS. SOI.Oppb PFOS 254.0ppb PFBS SU 33,1002.Oppb PFOS. 2S4.4ppb THPFOS, 10Q20ppb PFOS 254.0ppbPFBS 41 45 46 47 H010128B.M HKX084.D H010126B.M H2L00S5.D H010126B.M HNX0088.0 H0101266.M H2LQ067.D H0101268.M H21068.D H01012S8.M H0101268.M HOI01268.M HfLLOOOl.D H01012SB.M HXL0092D H010126B.M HILIQOe&D HOI01288.M, WLL107.0 H0101268.M HN20119.D H010128B.M HILL0123.D HOI01268.M HUJL0124.D HOI01268.M H1U125.D HOI01268.M HILL0128.D H0101268.M HIUD127.D HOI01268.M H2L0128.D H0101268.M HHL0129.O H010126B.M HIU0130.D H010126B.M H1LL0131.D H010126B.M HILLQ132D H010126B.M HILL0133.D H010126B.M H1LL0134.0 H0101268.M KIU013S.O oPFOS-21.1 nPFOS-2.1.2 oPFOS-2.1.3 O PF0321.4 bPFOS-2.2.1 oPFOS-222 oPFOS-223 uPFOS-224 OPF0323.1 ePFOS-23.2 sPFOS-2.33 oPFOS-23.4 TCR-002 012201-oPFOS-2.1.1 ,100X 01.0 SFM 01-25-01 MEE(MLA) TCR-002 012201-OPFOS-21.2 100X 08.0 SFM 01-25-01 MEE(MLA) TCR-002 012201-OPFOS-21.3,100XOI.D SFM 01-25-01 MEE(MLA) TCR-002 012201-oPFOS-214,100X D ID SFM 01-2301 MEE(MLA) TCR-002, 012201-OPFOS-221.100X 01. SFM 01-2301 MEE(MLA) TCR-002 012201-ePFOS-222 100X DIG SFM 01-25-01 MEE(MLA) TCR-002 0122O1-OPFO8-223.10QX DIO SFM 01-2301 MEE(MLA) TCR-002 012201-OPFOS-224.100X D ID SFM 01-2S4J1 MEE(MCA) TCR-002 012201-OPFOS-221. 10OXWLQ SFM 01-2301 MEE(MLA) TCR-002 012201-PF0323.2 100X D ID 8FM 01-2301 MEE(MIA) TCR-002 012201-OPF03Z3 3 .100X D ID SFM 01-2301 MEE(MLA) TCR-002 012201-OPF0323.4.100X D ID SFM 01-2301 MEE(MLA) 2825 H010126B.M HIU0103.D HOI01266.M HJLL0104.D 2827 H01012S8.M HILL010S.D H0101268M HIU0106.D 32 H0101286.M HJUD110.D 33 H0101268.M HILL0111.0 34 H0101268.M HILL01120 39 H0101268.M HJU0113.D 3037 H0101268M HILL011S.O H0101288.M WLL0119D 39 HO10126B.M M 10117.D H0101268.M H0L01160 SMCanfkMnUi BACK TO MAIN PFB8 no/VnL PFB8 RT PFB9rw 1 254.0 4.11 2.291,287.0 2 254.0 4.11 271.901.$ 3 254.0 4 .tf 249,933.0 4 254.0 4.11 269.913.3 5 254.0 4.11 269,5129 9 254.0 4.1( 291,470.0 7 254.0 4.11 251.117.3 B 254.0 4.11 259,454.3 9 254.0 4.11 2,255.950.3 10 254.0 4.11 249,693.0 11 2540 4.11 299,309.5 12 254.0 4,11 299,165.3 13 254.0 4.11 279.750.3 9 254.0 4.11 252,279.9 9 254.0 4.11 207.970.9 1 254.0 4.11 174.920.9 2 254.0 4.11 165.245.8 3 254.0 4.11 173,091.3 4 254.0 4.11 190,006.3 5 254.0 4.11 159,3629 6 254.0 4.11 139.737.5 7 254.0 4.11 156,561.5 9 254.0 4.11 121,3020 9 254.0 4.11 2119.639.5 10 254.0 4.11 2104.847.5 11 254.0 4.11 141.753.0 12 254.0 4.11 139.963.3 13 2540 4.11 140.710.0 34 254.0 35 254.0 36 254.0 37 254.0 39 254.0 39 254.0 40 254.0 41 254.0 42 254.0 43 254.0 44 254.0 45 254.0 4.11 153.706.3 4.11 190.550.5 4.11 236,268.0 4.11 177.803 8 4.11 187,2690 4.11 190.380.3 4.11 174,788.8 4.11 168,575.8 4.11 150,440.8 4.11 179.948.3 4.11 154.809.3 4.11 118.548.8 mereretai THPf08 RT IHPf<?gyw 254.4 489 1.195.010.6 2544 4.66 1,187,274.1 254.4 4.88 1,191,710.3 254.4 4.88 1.2120620 254.4 4.88 1,187,586.0 254.4 4.69 1,191,1820 254.4 488 1,178.983.0 254.4 498 1.179,2191 254.4 4.88 1,188,973.8 254.4 468 1.179,8530 254.4 468 1,181,679.1 254.4 4.86 1,1622208 254.4 4.88 1,124,507.8 254.4 4.88 1,219,023.5 254.4 4.88 1,193,548.0 254.4 4.68 1,200,885.4 254.4 488 1202591.4 254 4 4.88 1,214,081.1 254.4 4.88 1201,2226 254.4 4.88 1,194,229.0 254.4 4.88 1,198,086.9 254.4 4.88 1,182276.1 254.4 4.88 1,176,191.4 254.4 4.88 1,192396.8 254 4 4.68 1.178,220.3 254 4 4.88 1,165,390.6 254.4 4.88 1.152.965.6 254.4 4.80 1.117.016.8 254.4 2544 254.4 254 4 2544 254.4 254.4 254.4 254.4 254 4 254 4 254 4 4.88 1.158.5658 488 1,151,004.5 4.88 1,169.309.6 4 88 1.150,598.4 4.68 1.146.024.4 488 1,154.088.0 4.88 1,139.746.3 4.88 1,145.566.9 4.88 1,123,474.5 4.86 1,138,2008 4.88 1,130,344.4 4.88 1,118,728.5 PAGE 1 o(5 PFOS SoluMty FACT-TCR002 Study #FACT-TCR002 Compound: PFOS Study: Octanot Solubility Analytical Instrument Hiflary on 01-26-01 Reprocessing Workstation: Dioana 01/30/01 batch H010126b.b TCR-002.012201-OPFOS-2.4.1.1C0XDIO oPFCS-2.4.1 MethodBtank,SFM01-2*01 MEE(MIA) 20 H01012BB.M, HtUOOOB.D TCR-002,012201-OPFOS-2.4.2. 100XDID oPFOS-2.4.2 MethodBtank,SFM01-25-01ME(MLAJ TCR-002,012201-PFOS-2.4.3,10QXOLD 21 H010126S.M MLL009B.D oPFOS-2.4.3 MethodBtank,SFM01-2*01 MEE(MLA) 22 H010126B.M HJLL0100.D a ,oPFOSZ.4.4 TCR-002.012201-ePFOS-2.4.4,100XDl.Q MattedBtank.SFM01-2*01 MEE(MLA) 23 HQ1012B8.M HRU0101.0 3 t? MaOH6M 5 MaOHBtank H5 MaOHBtank MaOHBtank TN-A-4740, 04Dae00 TN-A-4740, 04Dac00 TN-A-4740, 04Dac00 TN-A-4740. 04Dac00 C MaOHStank 5 MaOHBtank MaOHBtank TN-A-4740, 04Deo00 TNA-4740. 04Dae00 TN-A-4740. 04Doc00 o V) MaOHBtank MaOHBtank TN-A-4740, 04Dac00 TN-A-4740, 04Dae00 MaOHBtank TN-A-4740, 04Dae00 MaOHBtank TN-A-4740, 04Dae00 MaOHBtank TN-A-4740. 04Dae00 2 MaOHBtank TN-A-4740, 04Dae00 CO MaOHBtank MaOHBtank TN-A-4740. 04Dac00 TNA-4740, 04Dae00 m o 9 1 H0101266.M HK100T9.D 2 H010126B.M HILL00B0.D 16 H0101268.M HILL00B4.D 17 H0101268.M HILL0095.0 ie H010126B.M H1U00B6.D 19 HOI01266.M HILL0097.0 24 HOI01266.M H1110102.0 30 H010126B.M HHL0106.D 31 36 HOI01266.M H0101268.M HHIHLLL00110U9..DD 42 H0101268.M HIUL0120.D 43 H0101268.M HILL0121.D 44 H010126BM HILL0122.D 58 H010126B.M HIU0136.D 59 H010126B.M HILL0137.D "0)0 <71<Q (D 00 O CO 311 ConfldanlM BACK TO MAIN 30 254.0 4.11 2,236,216.3 31 254.0 4.11 2,204,048.0 32 254.0 4.11 2 ^2 1.5 83 .8 33 254.0 4.11 2,232,058.5 8S3SS88S8888888 A vragK IW D rr. % C .V .: 0.0 a.o o.o 0.0 0.0 0.0 ao o.o o.o 0.0 0.0 o.o a.o o.o o.o 4.11 0.0011 0 .0 2 7 * 000 o.oo o.oo 0.00 0.00 0.00 ara o.oo ora 0.00 0.00 ora o.oo ora ora 2.199,293.8 83.635.1 2 -4 5 * 0.0 o.o o.o ao 0.0 00 ao o.o co 0.0 0.0 ao ao Q-o o.o 254.4 254.4 254.4 254.4 o.o ao o.o ao o.o o.o o.o o.o o.o o.o 0.0 0.0 0.0 0.0 o.o 4.68 4.68 ' 4.86 4.86 4.86 0.0012 0 .0 2 5 * ora ora ora ara ora ara ora ora ora oro 0.00 0.00 0.00 0.00 ora 1,202,328 0 1,186,0826 1.189,771.3 1,194,130.1 1.174.135 6 27,404.5 2 .3 3 * oo o.o o.o ao o.o o.o o.o o.o oo o.o 0.0 0.0 0.0 Q.O o.o PAGE 2 <45 PFOS SduM ty FACT-TCR002 2c%o om o (Tf<c<QiD>DnJ o<o Standards/CCVs/CalbratlonData Study #FACT-TCR002 Compound: PFOS Study: Octand Sohirtity Analytical Instalment Hillary on 01-26-01 Reprocessing Workstation: Dioana 01/3CV01 batch H010126b.b ft * O f 11 0 1O &C 7-01 01003-07-02 01003-07-03 01 003^7-04 01003-07-08 0 1 0 0 3 0 7 -0 8 0 1 0 0 3 0 7 -0 7 0 1 0 0 3 0 7 -0 8 01003-07-08 0 1 0 0 3 0 7 -1 0 0100307-11 0 1 0 0 3 0 7 -1 2 0 1 0 0 3 0 7 -1 3 010030700 010030700 0100307-01 010030702 010030703 010030704 010030705 010030708 010030707 010030706 010030708 0 1 0 0 3 0 7 -1 0 0100307-11 0 1 0 0 3 0 7 -1 2 0 1 0 0 3 0 7 -1 3 4 * PFOS K B S - ZSpptoPFOS 2H .0pF> P T lt SppbPFOS 2 lt.0 p p b PFBS 10ppbPFO 8 a4,0ppPC TS _________ Std 6 .2 5 .0 6 * PFOS.2 5 4 .4 * THPFOS. 25ppb PFOS 2S4.0ppb PFBS LOQ Std 6 . 4 0 0 8 * PFOS. 2 5 4 .4 * THPFOS, 4 0 * PFOS 254.0ppb PFBS Std 7 . SO.IOppb PFOS. 2S4.4ppb THPFOS, SO .Ippb PFOS 254.0ppb PFBS Std 6 .7 5 .1 5 * PFOS, 254.4ppb THPFOS. 7 5 .1 * PFOS 2 5 4 .c n * PFBS Std 9 .1 0 0 2 C fe * PFOS. 2 5 4 .4 * THPFOS. 100.2ppbP F 08 2 5 4 .0 * PFBS Std 1 0 .2S0.50ppb PFOS. 254 4 * THPFOS. 2S0.5ppb PFOS 254.O p t* PFBS Std 1 1 .400.80ppb PFOS, 2 5 4 .4 * THPFOS. 4 0 0 .8 * PFOS 2S4.0ppb PFSS S tf1 2 .5 0 1.00 pfb PFOS. 2 5 4 .4 * THPFOS. SOI.Oppfa PFOS 254.Oppb PFBS S td 1 3 .10020ppb PFOS, 254.4ppb THPFOS, 1002.Oppb PFOS 2S4.0ppb PFSS Std 9 .100.20ppb PFOS. 254.4ppb THPFOS. 100.2ppb PFOS, CCV 254.0ppb PFBS Std 9 .100.2Qppb PFOS, 254.4ppb THPFOS. 1 0 0 -2 * PFOS. C C V 254.0PP* PFSS Oppb PFOS P F B S - ZSppbPFO S 2 6 1,Oppb PFBS tO ppb PFOS 2S4.0ppb PFBS Std 25. 2S.05ppb PFOS. 254 4 * THPFOS, 2Sppb PFOS 2S4.0ppb PFBS LOQ Std 28. 4008ppb PFOS. 2S4.4ppb THPFOS. 40ppbPFO S 2S4.0ppb PFBS Std 2 7 .50.10ppb PFOS, 2 5 4 .4 * THPFOS. 50.1ppbPFO S 254.0ppb PFBS Std 28, 7 S .1 5 p f* PFOS, 254.4ppb THPFOS, 75.1ppb PFOS 254,Oppb PFBS Std 2 9 .10020ppb PFOS. 2 5 4 .4 * THPFOS, 100.2ppb PFOS 254.0ppb PFB8 Std 3 0 .250.50ppb PFOS. 2S4.4ppb THPFOS, 250.5ppb PFOS 2 5 4 .0 * PFBS Std 3 1 .400.80ppb PFOS. 2 5 4 .4 * THPFOS, 400.8ppb PFOS 2 5 4 .0 * PFBS S%13 2 ,5 0 1 .0 0 * PFOS, 2 5 4 .4 * THPFOS, SOI.Oppb PFOS 254.0ppb PFBS Std 3 3 ,10Q2.Oppb PFOS. 254.4ppb THPFOS. 1 0 0 2 .0 * PFOS 254.0ppb PFBS 3 4 5 S 7 8 9 10 11 12 13 14 15 29 41 45 4S 47 48 49 80 51 52 53 54 55 58 57 H010126B.M HILL0061.D H0101268.M H IU 00 62 .0 H010126B.U HILL0063.D H01012BB.U HILL00S4D H0101268.M H H X0086.0 H0101268.M H ILL0086.0 HOI01268.M H IU 00 87 .0 H 0101266.U H1LL0068.D H0101268.M HtLL0090.D H 0101268.U HILL0091.D H010126B.M HJLL0092.D H0101268.M H 1U 0093.0 H010126B.M KIU01O 7.D H 01012S8M HILLD119.D H0101268.14 H R X0123.0 HOI01268.14 HHL0124.D H010126B.M HILL0125.D H010126B.M HILL0128.D H010126B.M HILL0127.D H010126B.M HILL0128.D HOI01260.14 H fU .0129.0 HOt01268.14 H IU 0130.D H010126B.M H IU 0131.D H01012S6.U H ILL0132.D HOI01288.M HILL0133.D H0101268.M HU10134.D H0101268.M H ILL0135.0 SM C onM m lW BACK TO MAIN curve eecuraey Y W P f06 RT P fQ 6 f P f08 no/mL %Dev i 0.00 0.0 0.0 MA 2 5.15 87,712.5 0.0 Exdudcd 3 5.14 153.688.9 0.1 Exdudwl 4 5.14 302,871.8 52 Exdudcd 5 5.14 757,518.8 21.5 14.2% e 5.14 1,240,298.9 38.5 4.0% 7 5.14 1.530,777.4 49.4 1.3% 8 5.14 2,345.388.3 758 4.8% 9 514 3,071,783.3 104.3 4.1% 10 5.14 7,337,688.0 2632 51% 11 5.14 11,118,735.0 408.4 1.9% 12 514 13.388,041.0 488.3 0.5% 13 8.14 24,221,508.0 1,022.3 20% e 5.14 3.097.818.0 102.3 21% 9 5.14 3042,428.3 102.8 24% 1 0.00 0.0 0.0 MA 2 5.14 87,171.0 0.0 Exdudcd 3 5.14 154,013.5 0.1 Exdudcd 4 514 290,544.1 4.9 Exrtxtod 5 5.14 765,2794 216 13.7% 8 514 1,217,724.1 37.5 7 5.14 1,487,584.3 48.0 6.4% 4.2% 8 5.14 2,263,834.5 75.9 1.0% 9 5.14 3,014,363.8 101.7 1.5% 10 5.14 7.022.418.0 251.7 0.5% 11 5.14 10,839,108.0 395.5 1.3% 12 5.14 12.822,872.0 4858 24% 13 5.14 23,298,2020 984.5 1.7% PAGE 3 75 PFOS SoJuMty FACT-TCR002 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument H illa ry o n 0 1 -2 6 4 1 Reprocessing Workstation: Dioana 01/3CV01 batch H010126b.b S am ple IP oPFO S-21.1 oP FO S-21.2 oP FO S-21.3 oP FO S-21.4 oP F O S -221 oP F O S -222 oP F O S -22 3 0 P F 0 S -2 2 4 oP FO S -211 oP FO S -23.2 oP FO S -23.3 oP FO S-23.4 S w iM ltP K flD M o a TC R -002 012201-oPFO S -2 1.1 ,1 00 X 01 .0 SFM 01-2501 M EE(M LA) TCR-002, Q1Z201-OPFO&-Z1J2,10Q X M O SFM 01-2501 M EE(M LA) T C R -002,012201-oP FO S -21.3, tOQX OLD SFM 01-2501 M EE(M LA) T C R -002,012201-oP F O S -21.4,100X DLO SFM 01-25-01 M EE(M LA) T C R -002,012201-oP FO S -221.100X M .O SFM 01-25-01 M EE(M LA) TC R -002 012201-O PFO S -22210Q X 0 1 .0 8FM 01-2501 M EE(M IA) TC R -002 012201-oP FO S -223,10Q X D IO SFM 01-25-01 M EE(M LA) TC R -002 012201-oPFO S-224,10Q X D IO SFM 01-2501 M EE(M LA) TC R -002 012201-oP F O S -23.1,100X D i.0 SFM 01-2501 M EE(M LA) TC R -002 012201-P F O S -23.2100X D ID SFM 01-2501 MEE(MLA) TC R -002 012201-O P F05-23.3,100X M .O SFM 01-2501 M EE(M IA) TC R -002 012201-oPFO S*23.4,10Q X O I.D SFM 01-2501 M EE(M LA) Run 25 26 27 26 32 33 34 35 37 36 38 40 R-- MM D ata AM H010126B.M H IU 0103.D HO1O1260.M HILL0104.D H010126B.M HILL0105.D H0101268.M H1LL0106.D H0101268.M KILL0110.D HOI01268.M HILL0111.D H010126B.M H ILL0112D H0101288.M HILL0113.D H 0101288.M H1LL011S.0 H010126B.M HILL0116.D H010126B.M HILL0117.D H0101268.M H ILL0118.0 FACT -T C R 0 0 2 (LIM S #E00-1716), Page 60 of 109 BACK TO MAIN dltoflon Factor Avarwt co t f ctton gftt D*v PfgSRT irei ua/roLww P ro noftnLPFQ % c,y. 34 6.14 14,706,785.0 564.2 56.4 57.0 36 6.14 14,020.516.0 577.2 57.7 1.06 36 6.14 14,660,601.0 657.4 55.7 1 37 5.14 14,075,314.0 570.8 58.0 36 5.14 14,468,565.0 580.9 56.1 55.4 38 5.14 14,280,4660 540.1 64.0 0.49 40 5.14 14,221,117.0 553.7 55.4 0.0 41 5.14 14,2,295.0 5525 55.2 42 5.14 14,756,722.0 585 6 58.6 56.3 43 8.14 14,860,485.0 582.6 56.3 1.20 44 8.14 14,413.025.0 567.0 56.7 21% 46 5.14 14,903,941.0 595.9 59.6 Day 2 v a ra ti : H .l m j/m t s td d m tA % C .V.: 25% PAGE 4 ai 5 pros S oU flty FACT-TCR002 CO 9m o (0nOT>)J o CO Solvent/MethodBlinkDota Study #FACT-TCR002 Compound PFOS Study; Octanol Solubility Analytica! Instalment Hillary on 01-26-01 Reprocessing Workstation: Oioana 01/30/01 batch H010126b.b S M tw to lP TCR-0Q 2,0122D1-oPFO S-Z4.1,10Q X D ID B ut R ae M id D a ta ria oP F O S -2.4.1 o p fO S -2.4.2 M a te d B lank, SFM 01-254)1 M EE(M LA) TC R -002,012201-O P F0S -24Z, 100X OSO M alhod B lank, SFM 01-2501 M EE(M LA) T C R -002.012201-oPFO S-2.4.3,10G X DSC 20 21 H010126B.M HILL00S6.O H 0101268.M HELL0066.D oPFO S-2.4.3 O P FO S2.4.4 M atted B lank. SFM 01 -25-01 M EE(M IA) TC R-002, 012201-O PFO S -Z4.4,100X 0 .0 M atted B lank. SFM 01-254)1 M EE(M LA) 22 23 H01012B8.M HLL0100.D H010126B.M H IU 0101.D MaOH Blank MaOH Blank MaOH Blank M aO H B tar* MaOH Blank M aOH Blank MaOH Blank M aOH Blank MaOH B M c MaOH Blank MaOH Stank MaOH Blank MaOH Blank MaOH Blank MaOH Blank TN-A-4740, 04 Dae 00 TN -A-4740, 04 Dae 00 TN-A-4740, 04 Dae 00 TN -A -4740 04 Dec 00 TN-A-4740, 04 Dae 00 TN -A-4740, 04 Dae 00 TN-A-4740, 04 Dae 00 TN -A-4740, 04 Dae 00 TN -A-4740, 04 0 e c 0 0 TN-A-4740. 04 Dae 00 TN-A-4740, 04 Oac 00 T N A r4740. 04 Oac 00 TN-A-4740, 04 Oac 00 TN-A-4740, 04 Dae 00 TN-A-4740. 04 Dae 00 1 2 16 17 16 16 24 30 31 36 42 43 44 $6 58 H 0101268.M H 010126B .M H 010126B .M H 010126B .M H010126B.M H O I0 1 2 6 8 .M H010126B.M H O I0 1 2 6 8 .M H 0101268.M H010126B.M H010126S.M H010126B.M H0101268.M H010126B.M H0101268.M H H L0078.D H ILL0060.D H LL0004.D H1LL0095.D HHX0096.D H ILL0097.0 H IU 0102.0 H IU 0106.0 H ILL0106.0 H ILL0114.0 H ILL0120.D H IU 0121.0 H IU .0122.D H IU 0136.D H ILL0137.D SSSSSSSSSSfcSSSS 32 33 SM C onftfcntW BACK TO MAIN PFOSftT natoti P fo a 0.00 0.0 0.0 0.00 0.0 0.0 0.00 0.0 0.0 0.00 0.0 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 o.o 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 PFOS O ctanol Solub, FACT-TCR002 Exact Copy of Original iftr _ Initial M jf ^ Dat_ FACT -TCR002 (LIMS #E00-1716), Page 62 of 109 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument Hillary on 01-29-01 Reprocessing Workstation: Dioana 01/31/01 batch H010129a.b B anw telP 8 im a h D--crintton Run* RaaMtd D a tafile Via* 01003-07-13 1002.0ppb PFOS System SuttabMy/EquBbrstion 3 H010129A.M HILL0003.D 13 01003-07-13 1002.0ppb PFOS SyatomSuRabBty/EquAratJon 4 H010129AJ4 HILL0004.D 13 01003-07-01 Oppb PFOS S yM nnS ullaM iyE quam ion 8 H010129A.M HILL0008.D 1 01003-07-02 2.5ppto PFOS System S dtsbilyE quB usllon 9 H010129A.M HJLL0009.D 2 01003-07-03 Sppb PFOS System 8dteM tyEquAraton 10 H010129A.M HILL0010.O 3 01003-07-04 10ppb PFOS System SuRabBty/EquAralion 11 H010129AJ4 H ia0011.D 4 01003-07-0$ 2Sppb PFOS System SuRabMy/EquAration 12 H010129A.M HILL0012.D 5 01003-07-06 40ppb PFOS System SuRabHy/EquAration 13 H010129A.M HILL0013.O 6 01003-07-07 50.1ppb PFOS System S(Otsblty1Eqi0brstion 14 H010129A.M H1LL0014.D 7 01003-07-06 75.1ppb PFOS System SoRabBty/EquAratfon 15 H010129A.M H0X0015O 6 01003-07-09 100_2ppb PFOS System StetaHty/EqUBsstlon 16 H010129A.M HKJ.0016.0 9 01003-07-10 250.5ppb PFOS System StetebUy/EquAraten 17 H010129A.M HILL0017.D 10 01003-07-11 400.8ppb PFOS System 8uRabMyquArson 18 H010129AJ* HILL0018.0 11 01003-07-12 501.Oppb PFOS System SuftabSty/EquAration 19 H010129A.M HILL.0019.D 12 01003-07-13 1002.0ppb PFOS System SultaMRy/EquAration 20 H010129A.M HILL0020.D 13 01003-07-01 01003-07-02 01003-07-03 01003-07-04 01003-07-09 01003-07-06 01003-07-07 01003-07-06 01003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-13 01003-07-09 01003-07-09 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 01003-07-13 Oppb PFOS THPFO8t a64.0ppbPFB8 Std 2, a.i1ppb PFOS, 264.4ppb Std 3 ,1.OIppb PFOS, 2S4.4ppb 5ppb PFOS THPFOS, 364 .OppbPFBS Std 4 ,10,0appb PFOS, 254.4ppb Std S, 25.0Sppb PFOS. 254.4ppb 25ppbPFOS THPFOS.2S4.0ppb PFBS LOQ Std 6 .40.0Sppb PFOS. 254.4ppb 40ppb PFOS THPFOS, 2S4.0ppb PFBS Std 7 .50.10ppb PFOS, 254.4ppb SO.Ippb PF08 THPFOS, 254.0ppb PFBS Std 8 .79.15ppb PFOS, 254.4ppb 75.1ppb PFOS THPFOS, 254,0ppb PFBS Std 9, lOO^OppbPFOS, 254.4ppb 100J2ppbPFOS THPFOS,254.0ppb PFBS Std 1 0 ,250.50ppb PFOS, 254.4ppb 2$0.Sppb PFOS THPFOS, 294.0ppb PFBS Std 11,400.80ppb PFOS, 254.4ppb 400.8ppb PFOS THPFOS, 294.0ppb PFBS Std 12.501 .OOppbPFOS, 254.4ppb 501.0ppb PFOS THPFOS, 254.0ppb PFBS Std 1 3 ,1002.0ppb PFOS, 254.4ppb 1002.0ppb PFOS THPFOS, 254.0ppb PFBS Std 9 ,100_20ppbPFOS. 254.4ppb 100.2ppb PFOS, CCV THPFOS, 254.0ppb PFBS Std 9,100.20ppt.PFOS, 254.4ppb 100.2ppb PFOS, CCV THPFOS, 2S4.0ppb PFBS Std 31TOppb-PFOS,-264.4ppbOppb PFOS THPFOS, 264.Oppb PFBS Std 22,3.51 ppb PFOS, 254.4ppb 2.5ppb PFOS THPFOSr264yQppb PF8S Std 23, 6.01ppb PFOSi 264.4ppb 5ppb PFOS THPFOS,3640ppb PFBS Std 2 4 ,10.0appbPF08, 264.4ppb 10ppb PFOS THPFOS, 264Jppb PFBS Std 2 5 ,2S.05ppb PFOS, 254.4ppb 25ppb PFOS THPFOS, 254.0ppb PFBS tO Q Std 2 6 .40.08ppb PFOS, 254.4ppb 40ppb PFOS THPFOS,2S4.0ppb PFBS Std 27,50.1 Oppb PFOS, 254.4ppb 50.1ppbPFOS THPFOS, 254.0ppb PFBS Std 28,75.15ppb PFOS, 254.4ppb 7S.1ppb PFOS THPF08,254.0ppb PFBS Std 29, lOO^Oppb PFOS, 254.4ppb 100.2ppb PFOS THPFOS. 254.0ppb PFBS Std 3 0 .250.50ppb PFOS, 254.4ppb 250.5ppb PFOS THPFOS, 254.0ppb PFBS Std 3 1 .400.60ppb PFOS, 254.4ppb 400.8ppb PFOS THPFOS, 264.0ppb PFBS Std 32, 901.OOppbPFOS, 254.4ppb 501.0ppb PFOS THPFOS, 254.0ppb PFBS Std 33,1002.Oppb PFOS, 254.4ppb 1002.0ppb PFOS THPFOS, 254.0ppb PFBS 24 H010129AJ4 HtLL0024.0 1 25 H010129AJA H1LL0025.D 2 28 H010129A.M HILL0026.D 3 27 H010129AJA HILL0027.D < 26 . H010129A.M H1LL0026.D 4 5 29 H010129A.M HILL0029.D 6 30 H010129A.M HILL0030.D 7 31 HQ10129A.M HILL0031.D 6 32 H010129A.M WLL0032.D 9 33 H010129A.M HILL0033.0 10 34 H010129A.M HILL0034.D 11 35 H010129A.M HILL0035.D 12 36 H010129A.M HILL0036D 13 49 H010129A.M HILL0049.O 9 61 H010129A.M HILL0061.0 9 65 H010129A.M HILL0065.D 1 66 H010129A.M HILL0066.D 2 67 H010129A.M HILL0067.D 3 66 H010129A.M HILL0068.D 4 69 H010129A.M H1LL0069.D 5 70 H010129A.M HJLL0070.0 6 71 H010129A.M HILL00710 7 72 H010129A.M HILL0072.D 8 73 H010129A.M HILL0073.D 9 74 H010129A.M HILL0074.D 10 75 H010129A.M HIU.0075.D 11 76 H010129A.M HILL0076.D 12 77 H010129A-M H1LL0077D 13 BACK TO MAIN PFB3 ng/mL 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 PFBSRT 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 PFB3 rei 2.185.510.6 2.174.915.0 2,082,220.9 2.118.167.8 2.122.751.3 2.093.721.4 2.109.799.8 2.096.566.4 2.060.409.6 2.073.192.3 2.063.078.4 2.024.400.1 2.063.849.5 2.055.936.8 2.040.294.1 1,981,596.8 2,014,626.0 2,024,508.6 2,005,504.4 1,995,039.6 2,010,020.5 1,983,160.1 1,981,870J 2,004,324.4 1,980,388.6 1,991,979.6 1,964,675.6 1,960,113.1 1,916,286.5 1,840,462.3 1,842,181.5 1,858,774.6 1,853,154.5 1,861,994.1 1,636,225.1 1,642,147.3 1,642,968.9 1,860,163.4 1,856,262.6 1,848,609.3 1,856,547.8 1,851,927.5 1,849,576.3 IHP.EQS natali. 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 THPFOS RT 4.93 4.92 4.92 4.92 4.93 4.92 4.93 ' 4.92 4.92 4.93 4.92 4.92 4.93 4.93 4.92 4.92 4JS2 4.93 4.93 4.92 4.93 4.92 4.92 4.92 4.93 4.92 4.93 4.92 4.93 4.92 4.92 4.92 4.92 4.93 4.92 4.92 4.92 4.93 4.93 4.93 4.93 4.92 4.93 IHPFQg.WM 1.068.177.5 1.064.676.6 1.063.930.8 1,080,905.1 1.102.538.4 1.097.531.3 1.088.912.5 1.077.263.8 1.086.394.4 1.081.277.8 1.073.770.8 1.067.952.5 1.047.256.6 1,039,712.0 1,011,818.3 1,080,712.1 1,083,416.9 1,094,411.0 1,087,423.1 1,095,695.8 1,079,264.4 1,086,759.6 1,079,623.0 1,079,205.6 1,073,789.1 1,053,604.4 1.042.784.3 998,226.0 1,046,334.4 1,042.889.3 1.032.203.5 1,036,027.6 1,043,668.0 1,043,395.3 1,035,159.4 1,032,746.5 1,030,456.4 1,034.624.0 1,036,166.8 1,014,587.7 1,006,745.6 1,010,418.6 962,453.6 Page 1 of5 PFOS OctanoJ S olub, FACT-TCR002 FACT -TCR002 (LIMS #E00-1716), Page 63 of 109 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument Hillary on 01-29-01 Reprocessing Workstation: Dioana 01/31/01 batch H010129a.b OPFOS-3.1.1 oPFOS-3.1.2 oPFOS-3.1.3 oPFOS-3.1.4 oPFOS-3.2.1 oPF03-3.2-2 oPFOS-3.2.3 oPFOS-3.2.4 oPFOS-3.3.1 oPFOS-3.3.2 oPFOS-3.3.3 oPFOS-3.3.4 oPFOS-3.4.1 oPFOS-3.4.2 oPFOS-3.4.3 oPFOS-3.4.4 TCR-002, 012201-oPFOS-3.1.1,100X Dl.D SFM 01-26-01 ME(MLA) Day 3, Sample 1. Rapi TCR-002,012201-OPFOS-3.12,100X 01.0 SFM 01*26-01 MEE(MtA) Day 3, Sample 1,Rep2 TCR-002.012201-ePFOS-3.U, 100X D I.0 8FM 01-26-01 MEE(MLA) Day 3, Sanate 1.Rap3 TCR-002,012201-OPFOS-3.1.4,100X Dl.D SFM 01-26-01 MEE(MLA) Day 3 .8ampie 1,Rep4 TCR-002,012201-OPFOS-3.2.1,100XDI.O SFM 01-26-01 MEE(MLA) Day 3. Sample 2, Rapt TCR-002.012201-OPFOS-3-22,100X 01.0 SFM 01-26-01 MEE(MLA) Day 3, Serrale 2, Rep2 TCR-002,012201-OPFOS-3.2.3,10QX 0 L 0 SFM 01-26-01 MEE(MLA) Day 3, Sample 2, RapS TCR-002,012201-OPFOS-32.4,100X D l.D SFM 01-26-01 MEE(MLA) Day 3, Sample 2, Rep4 TCR-002,012201-oPFOS-3.3.1,100X OLD SFM 01-26-01 MEE(MLA) Day 3. Sample 3.Rapi TCR-002,012201-OPFOS-3.32,100X Dl.D SFM 01-26-01 MEE(MLA) Day 3, Sample 3,Rep2 TCR-002, 012201-ef*FOS-3.3.3,100XDI.D SFM 01-26-01 MEE(MLA) Day 3, Sample 3, Rep3 TCR-002,012201-oPFOS-3.3.4,100X DEO SFM 01-26411 MEE(MLA) Day 3, Sanato 3, Rep4 TCR-002.012201-ePFOS-3.4.1,100X D l.D Day 3, Sample 4,Rapi Method Blank, SFM 01-26-01 MEE(MLA) METHOD BLANK TCR-002,012201-OPFOS-3.4.2,100X OLD Day 3, Sanale 4, Rep2 MMhed Blank, SFM 01-26411 MEE(MLA) METHOD BLANK TCR-002,012201-oPFOS-3.43,100X OLD Day 3, Sanale 4, Rep3 Method Blank, SFM 01-264)1 MEE(MLA) METHOD BLANK TCR-002,012201-oPFOS-3.4.4,100X OLD Day 3, Sample 4,Rep4 M ated Blank, SFM 01-26-01 MEE(MLA) METHOD BLANK 45 H010129A.M HJLL0045.D 31 46 H010129A.M HILL0046.D 32 47 H010129A.M HILL0047.D 33 46 H010129A.M HILL0048.D 34 52 H010129A.M HILL00S2.D 35 53 H010129A.M H I00053.0 36 54 H010129A.M HILL0054.D 37 55 H010129A.M HILL0055.D 35 57 H010129A.M HILL0057.D 39 56 H010129A.M HILL0056.D 40 59 H010129AJ4 HILL0059.D 41 60 H010129A.M HILL0060.D 42 40 H010129A.M HILL0040.D 21 41 H010129A.M HILL0041.D 22 42 H010129A.M HILL0042.D 23 43 H010129A.M HJLL0043.D 24 MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dae 00 SOLVENT BLANK TN-A4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK 1 H010129A.M HILL0001.D 91 2 H010129A.M HILL0002.D 91 5 H010129A.M hillooos.o 91 6 HQ10129A.M HILL0006.D 91 7 H010129A.M HILL0007.D 91 21 H010129A.M HILL0021.D 92 22 H010129AM HILL0022.D 92 23 H010129A.M HILL0023.D 92 37 HQ10129A.M HILL0037.D 92 35 H010129A.M HILL0038.D 92 39 H010129A.M H1LL0039.D 93 44 H010129A.M HILL0044.D 93 50 H010129A.M HILL0050.D 93 51 H010129A.M HIIL0051.D 93 56 H010129A.M HILL0056.0 94 62 H010129A.M HILL0062.D 94 63 H010129A.M HHX0063.D 94 64 H010129A.M HHL0064.D 94 75 H010129A.M HILL0078.D 95 79 H010129A.M HILL0079.D 95 80 H010129A.M HILL0080.D 95 BACK TO MAIN 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 4.11 4.11 4.11 4.11 4.11 4.11 254.0 254.0 254.0 254.0 Avaraga: Std Dav: % C.V.: 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 4.11 4.11 4.11 0.0012 0.030% 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1,884,887.0 1,872,279.8 1,859,351.0 1,803.739.0 1,834,715.0 1,850,544.0 1,790,803.3 1,827,500.5 1,798,130.1 1,783,884.0 1,812,003.9 1,024,825.8 1,875,281.5 1,898,774.0 1.803,103.3 1,053,592.9 1,890,788.5 70,882.5 3.75% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 . 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 4.93 4.92 4.92 4.92 4.93 4.93 4.92 4.93 4.92 4.93 4.92 4.92 4.92 4.92 4.93 4.92 4.92 0.0011 0.022% 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 986,381.6 981,228.1 960,612.5 986,834.1 984,672.3 988,068.8 987,671.7 985,5092 943,755.3 972,262,3 962,445.7 961252.4 1,039.401.3 1.047255.1 1,032,528.0 1,031,346.7 1,027277.8 42,009.1 4.09% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Pag 2 of 5 PFOS O ctanol SoU>, FACT-TCR002 FACT -TCR002 (LIMS #E00-1716), Page 64 of 109 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument: Hillary on 01-29-01 Reprocessing Workstation: Dioana 01/31/01 batch H010129a.b Saniate ID 01003-07-13 01003-07-13 01003-07-01 01003-07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-06 010034)7-07 01003-07-08 01003-07-09 010034)7-10 010034)7-11 010034)7-12 01003-07-13 01003-07-01 01003-07-02 01003-074)3 01003-074)4 010034)7-05 01003-07-06 010034)7-07 010034)7-06 01003-074)9 01003-07-10 01003-07-11 010034)7-12 010034)7-13 010034)74)9 010034)74)9 010034)7-01 01003-07-02 01003-074)3 010034)7-04 010034)74 01003-07-06 01003417-07 01003-074)8 010034)7-09 01003-07-10 01003-07-11 01003-07-12 010034)7-13 8m pk D re rlp fo n 1002.0ppb PFOS System SUtabfity/Equibratfon 1002.0ppb PFOS System SuftabHty/EquNfcration Oppb PFOS System SuiUbity/EquSbratjon 2.5ppb PFOS System SuKabSty/Equttvatton 5ppb PFOS System SuNabtty/EquBbration 10ppb PFOS System Suttabttty/EquCbratfon 25ppb PFOS System SutUMHy/EquMxatfon 4Oppb PFOS System SuKabty/EqLbratton 50.1ppb PFOS System SufcabifyfEquB>rition 75.1ppb PFOS System SuMabMyquBmitlon 100.2ppb PFOS System Suttebflty/Equttwation 2S0.Sppb PFOS System SdtaW fty/Eqdfccitton 400.8ppb PFOS System Suttabity/Equflixstfon 501 .Oppb PFOS System SutebMy/EqiAbratton 1002.Oppb PFOS System Stetebyqutt)ra8on Std 1t 0ppb PFOS. 354.4ppb Oppb PFOS THPFOS, 354.0ppb PFBS std a, a .sip p t PFOS. a ii.ip p b SW 3) 5.0lppfe PFOS, 354,4ppb 5ppbPFOS THPFOS1354,Oppb PFBS Std 4 ,IQ.QSppb PFOS, 354.4ppb < lOppb PFOS TMPFOS, 354.0ppb PFBS Std 5 ,2$.05ppb PFOS. 254.4ppb 25ppb PFOS THPFOS, 254.0ppb PFBS LOQ Std 6 .40.08ppb PFOS, 254.4ppb' 40ppb PFOS THPFOS, 2S40ppb PFBS Std 7 ,50.10ppb PFOS, 2S4.4ppb SO.Ippb PFOS THPFOS, 254.0ppb PFBS Std 8 .7S.15ppb PFOS, 254.4ppb 75.1ppb PFOS THPFOS. 254.0ppb PFBS Std 9, t0020ppb PFOS, 254.4ppb 1002ppb PFOS THPFOS. 2S4.0ppb PFBS Std 10,25O.50ppb PFOS, 254.4ppb 250.5ppb PFOS THPFOS. 2S4.0ppb PFBS Std 11,400.80ppb PFOS, 254.4ppb 400.8ppb PFOS THPFOS, 254.0ppb PFBS Std 12,501 .OOppbPFOS, 254.4ppb 501.Oppb PFOS THPFOS. 254.0ppb PFBS Std 13,1002.0ppb PFOS, 254.4ppb 1002.Oppb PFOS THPFOS, 2S4.0ppb PFBS Std 9, lOO^Oppb PFOS. 254.4ppb 100.2ppb PFOS. CCV THPFOS. 254.0ppb PFBS Std 9 .10020ppb PFOS, 254.4ppb 100.2ppb PFOS, CCV THPFOS, 254.0ppb PFBS Std 31. Oppb PFOS, 354,4ppb S td33r3r61ppb PFOSi 3S4,4ppb Std 31, B.OIppb PFOS, 364.4ppb Sppb PFOS THPFOS, 354,Oppb PFBS Std 3 4,10,02ppb PFOS, 2S4,4ppb 10ppb PFOS THPFOS, 354,Oppb PFBS Std 25,25.05ppb PFOS, 254.4ppb 2Sppb PFOS THPFOS, 254.0ppb PFBS LOQ Std 26,40.08ppb PFOS, 254.4ppb 40ppb PFOS THPFOS, 254.0ppb PFBS Std 27,5O.10ppb PFOS, 2S4.4ppb 50.1ppb PFOS THPFOS. 254.0ppb PFBS Std 26,75.15ppb PFOS, 254.4ppb 75.1ppb PFOS THPFOS. 254.0ppb PFBS Std 2 9 ,10020ppb PFOS, 254.4ppb lOO^ppb PFOS THPFOS, 254.0ppb PFBS Std 30,25O.50ppb PFOS. 2S4.4ppb 250.5ppb PFOS THPFOS, 254.0ppb PFBS Std 31,400.80ppb PFOS, 254.4ppb 400.8ppb PFOS THPFOS. 254.0ppb PFBS Std 32,501 .OOppbPFOS, 254.4ppb 501 .Oppb PFOS THPFOS, 254.0ppb.PFBS Std 33.1OO2.0ppb PFOS, 254.4ppb 1002.Oppb PFOS THPFOS, 254.0ppb PFBS Buoi 3 4 8 9 10 11 12 13 14 15 19 17 19 19 20 Rap Mid Data fite H010129A.M HIU.0003.D H010129A.M HIU.0004.D H010129A.M HILL0006.D H010129A.M HKX0009.D H010129A.M HILL0010.0 H010129A.M HILL0011.D H010129A.M HILL0012.D H010129A.M HILL0013.D H010129A.M HILL0014.0 H010129AJ4 HIU.0015.D H010129A.M HILL0016.0 H010129A.M HILL0017.D H010129A.M HILL0018X) H010129A.M HILL0019.D H010129A.M HILL0020.D V te tf 13 13 1 2 3 4 5 6 7 8 9 10 11 12 13 24 H010129A.M H1LL0024.0 1 25 H010129A.M HILL0025.D 2 20 H010129A.M HILL0026.D 3 27 H010129A.M HILL0027D 4 28 H010129AJ4 HILL028.O 5 29 HQ10129A.M HILL0029.0 30 H010129A.M HILL0030.D 7 31 H010129M HILL0031.0 8 32 H010129A.M HILL0032.D 9 33 H010129AJ4 H1LL0033.D 10 34 H010129A.M HILL0034.D 11 35 H010129A.M H1LL0035.0 12 36 H010129A.M HILL0036.D 13 49 H010129A.M HILL0049.D 9 61 H010129A.M HILL0061.D 9 65 H010129A.M HILL0065.D 1 66 H010129A.M HILL0066.D 2 67 H010129A.M HIU.0067.D 3 68 H010129A.M HILL0068.D 4 69 H010129A.M HILL0069.D 5 70 H010129A.M H1LL0070.D 6 71 H010129A.M H1U0071.D 7 72 H010129A.M HILL0072.D 6 73 H010129A.M HIU.0073.D 9 74 H010129A.M HILL0074.D 10 75 H010129M HHL0075.D 11 76 H010129AJ4 HILL0076.D 12 77 H010129A.M HIU0077.D 13 BACK TO MAIN PFOS RT 5.14 5.14 0.00 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 0.00 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 0.00 5.14 5.14 5.14 5.14 5.15 5.14 5.14 5.14 5.14 5.15 5.14 5.14 P.FQ3 i r u 23,386,894.0 22,420,586.0 0.0 83,275.0 155,562.0 283,831.5 741,962.1 1,180,222.5 1,470,558.1 2,211,967.5 2,854,793.0 6,799,126.0 10,210,912.0 12,352,513.0 22,059,942.0 PFOS ng/mL 1,030.0 983.5 0.0 0.0 2.3 7.1 24.4 41.4 52.1 60.8 106.4 265.3 417.0 516.1 1,024.9 0.0 0.0 80,837.8 0.0 145,969.6 2.0 263,658.3 6.4 702,802.3 22.8 1,112,506.3 38.8 1,397,411.9 49.3 2,101,189.8 76.6 2,785,570.5 103.1 6,607,229.0 256.0 9,909,537.0 4012 12,095,500.0 502.9 21,541272.0 1,012.4 2,665,064.8 101.7 2,647,865.8 101.4 0.0 0.0 73,876.5 0.0 135,444.5 1.8 254,129.7 6.5 657,037.1 22.5 1,050,459.5 382 1,316268.3 48.9 1,991,026.9 75.7 2,637,624.3 101,7 6243,744.5 256.0 9,534,313.0 4042 11,346,758.0 485.5 20,449,734.0 994.0 NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA NA Excluded Excluded Excluded 9.1% 3.3% 1.8% 2.0% 2.9% 2.2% 0.1% 0.4% 1.0% 1.5% 12% NA Excluded Excluded Excluded 10.2% 4.7% 2.3% 0.8% 1.5% 22% 0.8% 3.1% 0.8% Page 3 of 5 PFOS O ct.n o ! Solub. FACT-TCR002 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument: Hillary on 01-29-01 Reprocessing Workstation: Dioana 01/31/01 batch H0 1 0 1 2 9a.b S am plaP oPFOS-3.1.1 oPFOS-3.1.2 oPFOS-3.1.3 oPFOS-3.1.4 oPFOS-3.2.1 oPFOS-3.2.2 oPFOS-3.2.3 PFOS-3.2.4 oPFOS-3.3.1 oPFOS-3.3.2 oPFOS-3.3.3 oPFOS-3.3.4 Snmptf Piwriiitlpn TCR-002,012201-PFOS-3.1.1,100XD10 SFM 01-26-01 MEE(MLA) Day 3, Sample 1. Rapi TCR-002,012201hjPFOS-3.12 , 100X 01.0 SFM 01-26-01 MEE(MLA) Day 3, S a n ** 1, Rep2 TCR-002,012201-oPFOS-3.1.3,100X DI.D SFM 01-26-01 MEE(MIA) Day 3, S a n ** 1, Rp3 TCR-002,012201-oPFOS-3.1.4,100X D5.0 SFM 01-264)1 MEE(MLA) Day 3, S a n ** 1, Rp4 TCR-002,012201-QPFOS-32.1,100X Dl.O SFM 01-26-01 MEE(MLA)Day3,Samp(e2.Rp1 TCR-002,01220l-oPFOS-322,100X 0LQ SFM 01-26-01 MEE(MLA) Day 3, S a n ** 2, Rep2 TCR-002,012201-CPFOS-3.2.3. 100X DI.D SFM 01-264)1 MEE(MLA) Day 3, Sample 2, Rep3 TCR-002,012201-oPFOS-3.2.4,100X OLD SFM 01-26-01 MEEfMLA) Day 3, S a n ** 2, Rep4 TCR-002,012201-OPFOS-3.3.1,100X Dl.O SFM 01-264)1 MEE(MLA) Day 3. S a n ** 3. R api TCR-002,01220l-oPFOS-3.3^, 100X Dl.O SFM 01-264)1 MEE(MLA) Day 3. Sample 3. Rep2 TCR-002.012201-OPFOS-3.3.3.100X Dl.O SFM 01-26-01 MEE(MLA) Day 3, Sample 3, Rep3 TCR-002, 012201-OPFOS-3.3.4,100X Dl.O SFM 01-264)1 MEE(MLA) Day 3, Sample 3, Rep4 Sinf RapM td Data Ala VMM 45 H010129A.M HIU.0045.D 31 46 H010129A.M HU10046.D 32 47 H010129A.M HILL0047.D 33 46 H010129A.M HILL0046.D 34 52 H01Q129A.M H010052.D 35 53 H010129A.M HTU0053.D 36 54 H010129A.M HILL0094.D 37 55 H010129A.M HILL0055.D 38 57 H010129A.M HILL00S7.D 39 58 H010129A.M HILL0058.D 40 59 H010129A.M H11L0059.D 41 60 H010129A.M HILL0060.D 42 FACT -TCR002 (LIMS #E00-1716), Page 65 of 109 BACK TO MAIN PFQ8 RT 5,14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 . PFOSataa nq/mL PFOS dilution factor correction uq/mL Avaraoa 8td Dav %C.V. 12,805,086.0 559.0 55.9 565 12.676,261.0 12,838,214.0 565.6 582.9 56.6 58.3 1.2 22% 12,513.073.0 554.1 55.4 12,316,146.0 545.9 54.6 54.1 12,252,723.0 540.8 54.1 0.35 12,205,875.0 538.7 53.9 0.6% 12,170,612.0 538.4 53.8 12,979,064.0 605.8 60.6 59.2 12,939,967.0 584.4 58.4 0.93 12.913,836.0 589.6 59.0 1.6% 12,899,195.0 589.7 Day 3 avaraga: aid d*v: %C.V.: 59.0 66.6 nfl/mL 2.6 4.5% Page 4 of 5 PFOS O dano) SoU>, FACT-TCR002 FACT -TCR002 (LIMS #E00-1716), Page 66 of 109 Study # FACT-TCR002 Compound: PFOS Study: Octanol Solubility Analytical Instrument Hillary on 01-29-01 Reprocessing Workstation: Dioana 01/31/01 batch H010129a.b S d ito te lo Run# Ran Mtd Paia file V ial# oPFOS-3.4.1 TCR-002.012201-oPFOS-3.4.1,100XDI.O Day 3,Sam pk4, Rep1 Method Blank, SFM 01-26-01 MEE(MLA) METHOD BLANK TCR-002,0122C1-oPFOS-3.4.2.100X DI.D Day 3, Sample 4, Rep2 40 H010129A.M HILL0040.D 21 oPFOS-3.4.2 Method Blank, 8FM 01-2641 MEE(MLA) METHOD BLANK TCR-002,012201-oPFOS-3.4.3,100X D I.0 Day 3 ,8ample4, Rep3 41 H010129A.M HILL0041.D 22 PFOS-3.4.3 oPFOS-3.4.4 MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank MeOH Blank Method Blank, SFM 01-2641 MEEfMLA) METHOD BLANK TCR-002,012201-oPFOS-3.4.4 100X D I.0 Day 3 ,3ampH4, Rep4 Method Blank, SFM 01-2641 MEE(MLA) METHOD BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dae 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740. 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740. 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740. 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dec 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BLANK TN-A-4740, 04 Dee 00 SOLVENT BUNK TN-A-4740. 04 Dee 00 SOLVENT BLANK 42 H010129A.M HILL0042.D 23 43 H010129A.M HILL0043.D 24 1 H010129A.M HHL0001.D 91 2 H010129A.M HILL0002.D 91 5 H010129A.M HILL0005.D 91 6 H010129A.M HILL0006.D 91 7 H010129A.M HILL0007D 91 21 H010129A.M HILL0021.D 92 22 H010129A.M HILL0022.D 92 23 H010129A.M HILL0023.D 92 37 H010129AJ4 HILL0037.0 92 38 H010129A.M HILL0038.D 92 39 H010129A.M HILL0039.D 93 44 H010129A.M HILL0044.D 93 50 H010129A.M HILL0050.D 93 51 H010129AM HILL0051.D 93 56 H010129A.M HILL0056.D 94 62 HQ10129A.M HILL0062.D 94 63 H010129A.M HILL0063.D 94 64 H010129A.M HILL0064.D 94 76 H010129A.M HILL0078.D 95 79 H010129A.M HILL0079.D 95 60 H010129A.M HIU0060.D 95 BACK TO MAIN PfOS RT 0.00 0.00 0.00 00..0000 0.00 0.00 0.00 0.00 5.14 0.00 000...000000 0.00 0.00 0.00 0.00 0.00 0.00 00..0000 0.00 0.00 0.00 PfOS i r -- 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 41.422.1 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 ntfmLPFQg 0.0 0.0 0.0 0.0 0.0 0.0 0.0 00..00 0.0 0.0 0.0 00..00 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Pag 5 of 5 Attachment C: Sample Chromatograms BACK TO MAIN FACT -TCR002 (LIMS #E00-1716), Page 67 of 109 Batch Run # 37 of 79 Data File C:\HPCHEM\l\DATA\H010126\HILL0037.D TN-A-4740, 04 Dec 00 Injection Date : 1/26/01 8:44:34 PM Seq. Line : 37 Sample Name : MeOH Blank Vial : 92 Acq. Operator : MLA Acq. Instrument : Hillary Inj Inj Volume :1 : 10 pi Acq. Method : C:\HPCHEM\1\METHODS\H010125.M Last changed : 1/25/01 9:13:04 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010126A.M Last changed ': 1/30/01 8:17:48 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT Samp BACK TO MAIN Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : D ilu tio n : Sample ISTD Information: ISTD ISTD Amount Name Signal 1/30/01 8:17:46 AM 1.0000 1.0000 lExact Copy of Original Initial P D a te Instrument 1 1/30/01 8:21:09 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 68 of 109 Page 1 of 3 Batch Run # 37 of 79 Data File C:\HPCHEM\1\DATA\H010126\HILL0037.D # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type . Area Amt/Area Amount Grp Name --[--m-i-n-]__|---------| --------------- | ----r--a-t--i-o----- | ---[-n--g-/-m--L-]---- | - | ----------- 4.108 - - - PFBS Totals without ISTD(s) : ' 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name ---[-m-i--n-]-- | ----------| ---------------- | -----r-a--t-i--o----- | ---[--n-g--/-m--L-]---- | - | ----------- 4.878 - - - THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]---I-- -- | --------------- | ----r--a-t-io-- I---[-n--g-/-m--L-]---- | - | ---------- 5.144 - - - PFOS Totals without ISTD(s) : 0.00000 1 Warnings or Errors : . Warning : ISTD compound(s) not found Area Percent Report Sorted By Calib. Data Modified Multiplier Dilution : : : : Signal 1/30/01 8:17:46AM 1.0000 1.0000 Signal 1: MSD1 299, EIC=298.7:299.7 Peak RetTime Type Width Area Area Name - --# I--[--m-i-n-]---I--------- I---[-m--i-n-]---I--------------- I-------%----- I------- 1 4.108 I 0.0000 0.00000 0.0000 PFBS Totals : 0.00000 BACK TO MAIN Sampj. vtcxiiuz ; n c u n o x c l l l A Instrument 1 1/30/01 8:21:09 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 69 of 109 Page 2 of 3 Batch Run # 37 of 79 Data File C:\HPCHEM\l\DATA\H010126\HILL0037.D Signal 2: MSD1 427, EIC=426.7:427.7. Peak RetTime Type # [min] ___ II_______ iI_ 1 4.878 -I Width [min] O.OOQO Area Area Name % _______ I 0.00000 0.0000 THPFOS Totals : 0.00000 Signal 3: MSD1 499, EIC=498.7 :499.7 Peak RetTime Type Width # [min] [min] 11 I1___ 11 ____ i1_ ____ _______ 0.00001 5.144 Totals : Area ! Area % Name 0.00000 0.0000 PFOS 0.00000 1 Warnings or Errors : Warning : ISTD compound(s) not found *** End of Report *** BACK TO MAIN Samp Instrument 1 1/30/01 8:21:09 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 70 of 109 Page 3 of 3 Batch Run # 36 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0114.D TN-A-4740, 04 Dec 00 Injection Date : 1/27/01 11:01:20 AM Sample Name : MeOH Blank Acq. Operator : MLA Acq. Instrument : Hillary Seq. Line : 114 Vial : 96 Inj : 1 Inj Volume : 10 Last changed : 1/25/01 9:13:04 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010126B.M Last changed ': 1/30/01 9:16:52 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample 4 'iU .V U J_>J . 0 .1 1 A . Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name Signal 111/..00300000/0001 9:16:50 AM Exact Copy of Original fit M # ;' Date Instrument 1 1/30/01 9:20:18 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 71 of 109 Page 1 of 3 Batch Run # 36 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0114.D # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSD1 299, EIC=298.7 :299.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]-- | ---------| --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- | - | ----------- 4.111 - - - PFBS Totals without ISTD(s) : 0.00000 signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]-- | --------- | --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- | - | ---------- 4.881 - - - THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area . Amt/Area Amount Grp Name --[--m-i-n-]---| ---------| --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- | - | ----------- 5.144 - Totals without ISTD(s) - - PFOS 0.00000 1 Warnings or Errors : Warning : ISTD compound(s) not found Area Percent Report Sorted By Calib. Data Modified Multiplier Dilution Signal 111/..00300000/0001 9:16:50 AM Signal 1: MSD1 299, EIC=298.7:299.7 Peak RetTime Type Width Area --#" I--[--m-i-n-]---I---------I--[-m-i-n--]--- I--------------- 1 4.111 I 0.0000 0.00000 Totals : 0.00000 Area % Name 0.0000 PFBS BACK TO MAIN S a m p j.^ n a m e ; n e u n Instrument 1 1/30/01 9:20:18 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 72 of 109 Page 2 of 3 Batch Run # 36 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0114.D Signal 2: MSD1 427, EIC=426.7:427.7 Peak RetTime Type Width Area Area Name --# I--[--m-i-n-]---1--------- 1--[--m-i-n-]----1--------------- 1-------%----- 1--------- 1 4.881 I 0.0000 0.00000 0.0000 THPFOS Totals : . 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 Peak RetTime Type Width Area Area Name - --# I--[--m-i-n-]---I--------- I--[-m--i-n-]----I--------------- I------%------I--------- 1 5.144 0.0000 0.00000 0.0000 PFOS Totals : 0.00000 1 Warnings or Errors : Warning : ISTD compound(s) not found *** End of Report *** BACK TO MAIN Sample n a m e : raeuii uianx Instrument 1 1/30/01 9:20:18 AM KLT/MLA' FACT -TCR002 (LIMS #E00-1716), Page 73 of 109 Page 3 of 3 Batch Run # 56 of 80 Data File C:\HPCHEM\1\DATA\H010129\HILL0056.D TN-A-4740, 04 Dec 00 Injection Date 1/29/01 11:55:52 PM Seq. Line Sample Name MeOH Blank Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010129.M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C :\HPCHEM\1\METHODS\H010129A.M Last changed 1/31/01 10:09:47 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT 56 ' 941 10 p i BACK TO MAIN Sample Name: MeOH Blank Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name Signal 111/..00300100/0001 10:09:45 AM Instrument 1 1/31/01 10:30:50 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 74 of 109 Page 1 of 3 Batch Run # 56 of 80 Data File C:\HPCHEM\1\DATA\H010129\HILL0056.D # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type [min] _______I I______ i .I 4.110 . Area - Amt/Area ratio 1----------------------------1 Amount [ng/mL] - Grp Name .1 1 . PFBS Totals without ISTD(s) : 0.00000 BACK TO MAIN Sample Name: MeOH Blank Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type [min] ____________ 1I __________I 1. 4.926 Area - Amt/Area ratio 1 ----------------1 Amount [ng/mL] - Grp Name .1I Il . THPFOS Totals without ISTD(s) : 0.00000 iiii iiii iiiiiiiiiiiiiitiiiiiii iiiiiiiiiiiiiiiiii iiii iiii Signal 3: MSD1 499, EIC=498.7 :499.7 RetTime Type [min] _____I 1 ____ i.I 5.143 Area - Amt/Area Amount ratio [ng/mL] i-- -- i - Grp Name lI II PFOS Totals without :ISTD(s) : 0.00000 1 Warnings or Errors : Warning : ISTD icompound(s) not found Area Percent Report iiiiiiiiiin ================= ii iiii iiiiiiiiii iiiiiiiiii iiii iiii iin iiiiiiil Sorted By Calib. Data Modified Multiplier Dilution Signal 111/..00300100/0001 10 09:45 AM Signal 1: MSD1 299, EIC=298.7 :299.7 Peak RetTime Type Width Area Area Name - --# I--[--m-i-n-]---I--------- I---[-m--i-n-]-- I--------------- I-------%----- I.......... 1 4.110 I 0.0000 0.00000 0.0000 PFBS Totals : 0.00000 Instrument 1 1/31/01 10:30:50 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 75 of 109 Page 2 of 3 Batch Run # 5S of 80 Data File C:\HPCHEM\l\DATA\H010129\HILL0056.D Signal 2: MSD1 427, EIC=426.7:427.7 Peak RetTime Type Width # [min] [min] Area 1 4.926 I 0.0000 0.00000 Totals : . 0.00000 Area % Name 0.0000 THPFOS Signal 3: MSD1 499, EIC=498.7:499.7 Peak RetTime Type Width # [min] [min] ___ I_______ I _____ I1 1 1 5.143 0.0000 Area Area % Name 1 0.00000 0.0000 PFOS Totals : 0.00000 1 Warnings or Errors : Warning : ISTD compound(s) not found .*** End of Report *** BACK TO MAIN Sample Name: MeOH Blank Instrument 1 1/31/01 10:30:50 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 76 of 109 Page 3 of 3 Batch Run # 40 of 79 . Data File C:\HPCHEM\1\DATA\H010126\HILL0040.D TCR-002, 012201-oPFOS-l.4.1, 100X Dii. Method Blank, SFM 01-24-01 MEE(MLA) Injection Date Sample Name Acq. Operator 1/26/01 9:18:01 PM OPF0S-1.4.1 MLA Seq. Line Vial Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C :\HPCHEM\l\METHODS\H01012 6A.M Last changed 1/30/01 8:17:48 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample Name: oPFOS-1.4.1 40 141 10 l ______________________ 2______________________ 4 MSD1 427, EIC=426.7:427.7 (H010126\H!LL0040.D) API-ES, I, SIM, Frag: Var 175000 j 150000 125000 100000 75000 50000 025000 _ . J J MSD1 499, EIC =498.7:499.7 (H 010126\H ILL 0040.D ) A PI-ES, Neg, SIM. Frag: Var 1600 1400 1200 1000 800 600 420000 n2-_-_----r- -i---------- r 4 Exact Copy f Original initial L- J \ L 1 mm Instrument 1 1/30/01 8:21:25 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 77 of 109 Page 1 of 2 Batch Run # 40 of 79 Data File C:\HPCHEM\1\DATA\H010126\HILL0040.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300000/0001 8:17:46 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Are a Amount Grp Name ---[-m-i--n-]-- | ----------| ---------------- , -----r-a--t-i--o----- | ---[--n-g--/-m--L-]---- | - | ----------- 4.108 VBA+ I 2.16967e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] | | | | | - |------------------ ----------------- ---------------------------- ---------------------------- ---------------------------- -------------------- 4.878 VBA+ I 1.13641e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name ---[-m-i--n-]-- | ----------| _ _ ------------- | -----r-a--t-i--o----- | ---[--n-g--/-m--L-]---- | - | -------------------- 5.1 44 - - - PFOS Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : Calibrated compound(s) not found *** End of Report *** BACK TO MAIN Sample N a m e : o f f u - 1 . 4 . l Instrument 1 1/30/01 8:21:25 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 78 of 109 Page 2 of 2 Batch Run # 20 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0098.D TCR-002, 012201-OPF0S-2.4.1, 100X Dil. Method Blank, SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 8:03:06 AM Seq. Line Sample Name OPFOS-2.4.1 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010125 .M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010126B.M Last changed 1/30/01 9:16:52 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2,mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample name: o p f o s - 2 . 4 . l 98 13 0 10 /il 300000 -i 250000 - 200000 4 110500000000--!j 50000 -j 225000 -j 200000 -i 175000 150000 125000-i 100000 75000 j 50000-i 25000 MSD1 4 9 9, E IC =498.7:499.7 (H 010126\H ILL0098.D ) API-ES, Neg, SIM, Frag: Var 2000 5 1750 1500 1250-3 1000 750 Vvvy^v'Jw/\/JvAs/vW. 500 H 250 Exact Copy of Original l initial Data 2 mu Instrument 1 1/30/01 9:18:47 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 79 of 109 Page 1 of 2 Batch Run # 20 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0098.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300000/0001 9:16:50 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name ----[--m---i--n--]----- |----------------- |--------------------------------------r---a---t--i---o---------- |-----[---n--g---/--m--L---]--------|__|-------------------- 4.110 VBA+ I 2.23622e6 1.00000 254.00000 PFBS Totals without ISTD(s) : . 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]---\--------- 1--------------- , ----r--a-t--i-o----- , ---[-n--g-/-m--L-]----1 --!---------- 4.880 VBA+ I 1.20233e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]---1---------!--------------- 1----r--a-t--i-o----- 1---[--n-g-/--m-L-]---- 1 - 1 ---------- 5.144 - - - PFOS Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : Calibrated compound(s) not found *** End of Report *** BACK TO MAIN Sample marne: o f f u s -^ .4 . 1 Instrument 1 1/30/01 9:18:47 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 80 of 109 Page 2 of 2 Batch Run # 40 of 80 Data File C:\HPCHEM\l\DATA\H010129\HILL0040.D TCR-002, 012201-OPFOS-3.4.1, lOOX Dii. Method Blank, SFM 01-26-01 MEE(MLA) Injection Date 1/29/01 8:57:37 PM Seq. Line Sample Name oPFOS-3.4.1 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\1\METH0DS\H010129.M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010129A.M Last changed 1/31/01 10:09:47 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT MSD1 299, EIC=298.7:299.7 (H010129\HILL0040.D) API-ES, Neg, SIM, Frag: Var BACK TO MAIN Sam ple name: o t 'f 'U ij- J . .I 40 211 10 nl 250000 200000 150000 100000 50000 0 ~r 2 & min! MSD1 499, EIC=498.7:499.7 (H010129\HILL0040.D) API-ES. Neg. SIM, Frag: Var 1800" 1600 1400 1200 j 1000 800 600 400 200 ' --t---------- r 1 Exact Copy o f Originai J i f M '< n f-H? Bnitial D a te mm Instrument 1 1/31/01 10:29:28 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 81 of 109 Page 1 of 2 Batch Run # 40 of 80 Data File C:\HPCHEM\l\DATA\H010129\HILL0040.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300100/0001 10:09:45 AM Signal 1: MSD1 299, EIC=298.7 :299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ------ |-- -- |---------- |---------- |---------- |-|------- 4.108 VBA+ I 1.87528e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name | | | | | - |----[--m---i--n--]----- ----------------- ---------------------------- -------r---a---t---i---o---------- -----[---n--g---/--m---L--]-------- ------------------- 4.924 VBA+ I 1.03940e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]---| --------- | --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- 1 - | ---------- 5.143 - - - PFOS Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : Calibrated compound(s) not found *** End of Report *** BACK TO MAIN Sample Name: oPFOS-3.4.1 Instrument 1 1/31/01 10:29:28 AM KLT/MLA FACT -TCR002 (UNIS #E00-1716), Page 82 of 109 Page 2 of 2 Batch Run # 48 of 79 Data File C:\HPCHEM\l\DATA\H010126\HILL0048.D TCR-002, 012201-oPFOS-l.1.4, 100X Dii. SFM 01-24-01 MEE(MLA) Injection Date 1/26/01 10:47:12 PM Seq. Line Sample Name oPFOS-1.1.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\l\METHODS\H01012 5.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C :\HPCHEM\l\METHODS\HO10126A.M Last changed 1/30/01.8:17:48 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample name: ot'rus-1 .1 .4 48 10211/il MSD1 499. EIC =498.7:499.7 (H 010126\H ILL 0048.D ) A PI-ES. Neg, SIM. Frag: V ar 2000000 1750000 1500000 1250000 1000000 750000 500000 0250000 ~I 4 mu Instrument 1 1/30/01 8:22:08 AM KLT/MLA Page 1 of 2 Batch Run # 48 of 79 . Data File C:\HPCHEM\1\DATA\H010126\HILL0048.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300000/0001 8:17:46 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ---------- |_-------- |---------------- |-------------- ,| --------------- | - | --------- 4.110 VBA+ I 2.19577e6 1.00000 254.00000 PFBS Totals without ISTD(s) : ' 0.00000 Signal 2: MSD1 427, EIC=426.7 :427.7 RetTime Type Area Amt/Area Amount Grp Name | | | | | ~ | ---------------[--m---i--n--]----- ----------------- ---------------------------- -------r---a---t---i--o---------- -----[---n--g---/--m--L---]-------- 4.880 VBA+ I 1.10970e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ---------- | ----------| ---------------- | ---------------- | ----------- -- | " | ------------ 5.143 W A + 1.49629e7 1.70149e-l 583.65908 PFOS Totals without ISTD(s) : 583.65908 *** End of Report *** BACK TO MAIN Sample Name: oPFOS-1.1.4 Instrument 1 1/30/01 8:22:08 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 84 of 109 Page 2 of 2 Batch Run # 55 of 79 Data File C:\HPCHEM\1\DATA\H010126\HILL0055.D TCR-002, 012201-oPFOS-l.2.4, 100X Dii. SFM 01-24-01 MEE(MLA) Injection Date 1/27/01 12:05:06 AM Seq. Line Sample Name oPFOS-1.2.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C :\HPCHEM\1\METHODS\H01012 6A .M Last changed 1/30/01 8:17:48 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" . KLT 55 25 1 10 BACK TO MAIN Sample wame: o p f o s - 1 . 2 . 4 200000 175000 150000 125000 100000 75000 50000 02 5 0 0 0 MSD1 499. E IC = 4 98.7:499.7 (H 0 1 0 1 26\H IL L 0055.D ) A P I-ES . Neg. SIM . Frag: Var 2000000 1500000 1000000 500000 .0 _T_ 6 Original j 2h i i J V ' mir Instrument 1 1/30/01 8:22:45 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 85 of 109 Page 1 of 2 Batch Run # 55 of 79 Data File C:\HPCHEM\1\DATA\H010126\HILL0055.D BACK TO MAIN Sample Name: oPFOS-1.2.4 II II II II II II II II II II II II II II II II II II II II Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] ___ II_____________|I______ 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/30/01 8:17:46 AM 1.0000 1.0000 Signal 1: MSD1 299, EIC=298.7 :299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ______ |1______|1_____ _____|1 ________ | 1 __ _______ 4.109 VBA+ I 2.13707e6 1.00000 254.00000 PFBS ___ Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7 :427.7 RetTime Type Area Amt/Area [min] ratio ______ 1I______ |I ___ _ |_ _____ 4.879 VBA+ I 1.13107e6 1.00000 Amount Grp Name [ng/mL] _ _i1_ __ __ 254.40000 THPFOS Totals without ISTD(s) : 0.00000 __ _____ Signal 3: MSD1 499, EIC=498.7 :499.7 RetTime Type Area [min] _____ |______ i _ _____ __ 11 5.142 W A t 1.47279e7 Amt/Area ratio 1.69454e-l Amount Grp Name [ng/mL] ________ 1________________ 561.33095 PFOS Totals without ISTD(s) : 561.33095 1 1 1 1 1 ! 1 1 1il *** End of Report *** Instrument 1 1/30/01 8:22:45 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 86 of 109 Page 2 of 2 Batch Run # 60 of 79 Data File C:\HPCHEM\l\DATA\H010126\HILL0060.D TCR-002, 012201-oPFOS-l.3.4, 100X Dii. SFM 01-24-01 MEE(MLA) Injection Date 1/27/01 1:00:45 AM Seq. Line Sample Name oPFOS-1.3.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010126A.M Last changed 1/30/01 8:17:48 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT . BACK TO MAIN Sample Name: oPFOS-1.3.4 60 291 10 /il M SD1 4 2 7 , E IC =426.7:427.7 (H 010126\H IL L 0060.D ) A PI-ES, Neg, SIM , Frag: V ar 200000 175000 150000 125000 100000 i9> 75000 50000 025 0 00 Instrument 1 1/30/01 8:23:11 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 87 of 109 Page 1 of 2 Batch Run # 60 of 79 Data File C:\HPCHEM\l\DATA\H010126\HILL0060.D BACK TO MAIN Sample Name: oPFOS-1.3.4 Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/30/01 8:17:46 AM 1.0000 1.0000 Signal 1: MSD1 299, EIC=298.7 :299.7 RetTime Type Area [min] _-_-_-_-_-_-_-|_-_-_-_-_-_- |j_-_-_- _-_-_-_- 4.108 VBA+ I 2.19549e6 Amt/Area Amount Grp Name ratio [ng/mL] _________ _________ 1.00000 254.00000 1 _______________ PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area, [min] ratio _____ 11_____ |1 _____ 11____ __ 4.878 VPA+ I 1.11582e6 1.00000 Amount Grp Name [ng/mL] _l1_________________ 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7 :499.7 RetTime Type Area Amt/Area [min] ratio __ ____11_____ 1|___ ______ 1 ---- 5.145 W A + 1.46666e7 X .6963 9e-1 Amount Grp Name [ng/mL] |!__|1__ ______ 567.25132 PFOS Totals without ISTD(s) : 567.25132 ___ __ 1 1 1 1 11111 i1111 1111 1111 *** End of Report *** Instrument 1 1/30/01 8:23:11 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 88 of 109 Page 2 of 2 Batch Run # 28 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0106.D TCR-002, 012201-OPFOS-2.1.4, lOOXDil. SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 9:32:10 AM Seq. Line Sample Name oPFOS-2.1.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010126B.M Last changed 1/30/01 9:16:52 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample name : .l .4 106 10371il Exsei Copy of OrigialT . / tti-ai-m v M 7' initial _____ D a te Instrument 1 1/30/01 9:19:35 AM KLT/MLA FACT -TCR002 (UNIS #E00-1716), Page 89 of 109 Page 1 of 2 Batch Run # 28 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0106.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/30/01 9:16:50 AM 11..00000000' Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ----------|--------- |--------------- |--------------- |--------------- | - | ----------- 4.108 VBA+ I 2.17780e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name [min] . ratio [ng/mL] ----------|--------- |--------------- |--------------- |--------------- | - | ----------- 4.878 VBA+ I 1.15060e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area [min] ratio ---------- | ----------| ---------------- |---------------- 5.144 PVA+ 1.49753e7 1.75101e-l Amount Grp Name -[-n--g-/-m--L-]----1 - 1 ---------- 579.77372 PFOS Totals without ISTD(s) : 579.77372 *** End of Report *** BACK TO MAIN Sample Name: oPFOS-2.1. Instrument 1 1/30/01 9:19:35 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 90 of 109 Page of 2 Batch Run # 34 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0112.D TCR-002, 012201-OPF0S-2.2.3, 100X Dii. SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 10:38:59 AM Seq. Line Sample Name oPFOS-2.2.3 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C :\HPCHEM\l\METHODS\H01012 6B.M Last changed 1/30/01 9:16:52 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample Name: o p f o s - 2 . 2 . 3 112 14 0 10 n 1 300000 250000 200000 150000r 100000 50000 M SD1 4 2 7 , E IC = 426.7:427.7 (H 0 10 1 2 6 \H IL L 0 1 12 .D ) A P I-E S , Neg, SIM , Frag: V ar 200000 175000 150000 125000 100000 75000 50000 02 5 0 0 0 $ min Exact Copy Qf Origina!! __ Dat Instrument 1 1/30/01 9:20:08 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 91 of 109 Page 1 of 2 II II H 11 II II II II II II II II II II II II II II II II II It II II II II II II II II II Batch Rim # 34 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0112.D ' BACK TO MAIN Sample Name: oPFOS-2.2.3 Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] ___ |I_____________ |I_ ____ 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/30/01 9:16:50 AM 1.0000 1.0000 signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ______ |1____ _|_1__________i1 _ ______ 4.108 VBA+ I 2.17477e6 1.00000 254.00000 1______________ PFBS _ Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ___ |1_____ _1_______ 1 1_________ __ I1_________ _______ 4.879 W A + I 1.13975e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area [min] _______i ___ 1 5.141 W A + ratio |__ _______| 11 1.42211e7 1.74433e-l Amount Grp Name [ng/mL] _ _ i _ ______ 553.69686 1PFO S Totals without ISTD(s) : 553.69686 ____ II II II II II II II II IitI II II II II II II II II II II h *** End of Report *** Instrument 1 1/30/01 9:20:08 AM KLT/MLA FACT -TCR002 (LIMS #EOO-1716), Page 92 of 109 Page 2 of 2 Batch Run # 35 of 59 Data File C:\HPCHEM\1\DATA\H01012S\HILL0113.D TCR-002, 012201-OPF0S-2.2.4, 100X Dii. SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 10:50:10 AM Seq. Line Sample Name oPFOS-2.2.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010126B.M Last changed 1/30/01 9:16:52 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" . KLT MSD1 299, EIC=298.7:299.7 (H010126\HILL0113.D) API-ES, Neg, SIM, Frag: Var <r BACK TO MAIN Sample Name: oPFOS-2.2.4 113 41 1 10 i l 200000 175000 150000 125000 100000 75000 50000 025000 2000000 1750000 1500000 1250000 1000000 750000 500000 0250000 Exact Copyef Original J L u'flt tH Instrument 1 1/30/01 9:20:13 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 93 of 109 Page 1 of 2 Batch Run # 35 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0113.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] . 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300000/0001 9:16:50 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]---| --------- | --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- | - h --------- 4.111 VBA+ I 2.16658e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area [min] ratio ---------- | ----------| ---------------- | ---------------- 4.878 VBA+ I 1.14557e6 1.00000 Totals without ISTD(s) : Amount Grp Name [ng/mL] 254.40000 0.00000 THPFOS Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]-- | --------- | --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- J - l ---------- 5.144 PVA+ 1.42653e7 1.74403e-l 552.49733 PFOS Totals without ISTD(s) : 552.49733 *** End of Report *** BACK TO MAIN Sample Name: oPFOS-2.2.4 Instrument 1 1/30/01 9:20:13 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 94 of 109 Page 2 of 2 Batch Run # 40 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0118.D TCR-002, 012201-OPFOS-2.3.4, lOOXDil. SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 11:45:54 AM Seq. Line Sample Name oPFOS-2.3.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010125.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010126B.M Last changed 1/30/01 9:16:52 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium' Acetate Reprocessed on "Dioana" KLT 118 45 1 10 BACK TO MAIN Sample iMeune : orrus-ii .J .4 MSD1 499, EIC =498.7:499.7 (H 010126\H ILL0118.D ) 2000000 1750000 1500000 1250000 1000000 750000 500000 0250000 &A P I-E S , N eg . S IM . Frag: V a r mir Instrument 1 1/30/01 9:20:38 AM KLT/MLA Grgnaa Oat& FACT -TCR002 (LIMS #E00-1716), Page 95 of 109 Page 1 of 2 Batch Run # 40 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0118.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300000/0001 9:16:50 AM Signal 1: MSD1 299, EIC= 298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ______ 11______ I1_______ _ 1--------- 1 _________ 11|__|1 ______ 4.109 VBA+ I 2.11655e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7' RetTime Type Area Amt/Area Amount Grp Name [min] ' ratio [ng/mL] '___ _|__ __ 11________ 1--------- 1 1I_I_1_ ____ 4.880 W A + I 1.11673e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ---------- |--------- |----------------|--------------- |--------------- ---------------- 5.142 W A + 1.49039e7 1.75514e-l 595.91123 PFOS Totals without ISTD(s) : 595.91123 *** End of Report *** BACK TO MAIN Sample jName: .j .4 Instrument 1 1/30/01 9:20:38 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 96 of 109 Page 2 of 2 Batch Run # 48 of 80 Data File C:\HPCHEM\l\DATA\H010129\HILL0048.D TCR-002, 012201-OPF0S-3.1.4, 1 0 0 X D . SFM 01-26-01 MEE(MLA) Injection Date 1/29/01 10:26:40 PM Seq. Line Sample Name oPFOS-3.1.4 Vial Acq. Operator MLA . In j Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010129.M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010129A.M Last changed 1/31/01 10:09:47 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample name: owua-j .i .4 48 10341[ll MSD1 4 2 7 , E IC = 426.7:427.7 (H 0 10 129\H IL L 0048.D ) A P I-ES , Neg, SIM , Frag: Var 175000 150000 125000 100000 75000 50000 025000 4* min V.a (*-04 f-ft f ' Date Instrument 1 1/31/01 10:30:09 AM KLT/MLA FACT TCR002 (LIMS#E00-1716), Page 97of109 page 1 of 2 Batch Run # 48 of 80 Data File C:\HPCHEM\1\DATA\H010129\HILL0048.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300100/0001 10:09:45 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name ...[..m.i..n..]...I---------I------------- I ----r-a--t-i--o-----I - [..n..g./..m..L..].- 1 - 1 ---------- 4.109 VBA+ I 1.86374e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7 :427.7 RetTime Type Area ' Amt/Area Amount Grp Name --[--m-i-n-]---| ---------| --------------- | ----r--a-t--i-o----- | ---[--n-g-/--m-L-]---- l - l ----------- 4.925 VBA+ I 9.86834e5 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ----------|--------- |--------------- |--------------- | --------------- |__|----------- 5.142 PBA+ 1.25131e7 1.71782e-l 554.13421 PFOS Totals without ISTD(s) : 554.13421 *** End of Report *** BACK TO MAIN Sample iMctiue: urrus-j .1 . 4 Instrument 1 1/31/01 10:30:09 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 98 of 109 Page 2 of 2 Batch Run # 55 of 80 Data File C:\HPCHEM\l\DATA\H010129\HILL0055.D TCR-002, 012201-oPFOS-3.2.4, 100X Dii. SFM 01-26-01 MEE(MLA) Injection Date 1/29/01 11:44:43 PM Seq. Line Sample Name oPFOS-3.2.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C:\HPCHEM\1\METHODS\H010129.M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010129A.M Last changed 1/31/01 10:09:47 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT . M SD1 299, E IC =298.7:299.7 (H 010129\H ILL 0055.D ) A PI-ES, Neg, SIM , Frag: Var - 250000 <r 200000- ' i* 150000-: 100000- 50000T .U ,----------- , A 1----------- J----------- *----------- '----------- 1------- i 24 l . , . i 6 MSD1 427, E IC =426.7:427.7 (H 010129\H ILL 0055.D ) A PI-ES, Neg, SIM , Frag: V ar 180000 160000 114200000000 100000 80000 60000 40000 200000 BACK TO MAIN Sarapl g iMc im e u r r u o - j 55 381 10 n1 1 i 8 min 1750000 1500000 1250000 1000000 750000 500000 025 0 00 0 gxaet Copy f Origina! Initial Date m ir Instrument 1 1/31/01 10:30:45 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 99 of 109 Page 1 of 2 Batch Run # 55 of 80 Data File C:\HPCHEM\1\DATA\H010129\HILL0055.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300100/0001 10:09:45 AM signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] --------- |---------|------------- | -------------- |---------------| - | ------- - 4.111 VBA+ I 1.82751e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ----------- | ---------- | ------------------| ------------------| ------------------l - l - -- -- 4.927 VBA+ I 9.85509e5 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ---- _|---- |-------- |-------- |___----- |-|----- 5.144 W A + 1.21706e7 1.71363e-l 538.37559 PFOS Totals without ISTD(s) : 538.37559 *** End of Report *** BACK TO MAIN Sample ; urrua -J .4 .* Instrument 1 1/31/01 10:30:45 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716), Page 100 of 109 Page 2 of 2 Batch Run # 60 of 80 Data File C:\HPCHEM\l\DATA\H010129\HILL0060.D TCR-002, OI2 2 OI-0 PFOS-3 .3.4, 100X Dii. SFM 01-26-01 MEE(MLA) Injection Date 1/30/01 12:40:27 AM Seq. Line Sample Name OPFOS-3.3.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\l\METHODS\H010129.M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010129A.M Last changed 1/31/01 10:09:47 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample Name: oPFOS-3.3.4 60 14 2 10 p i M SD1 4 9 9. EIC =498.7:499.7 (H 010129\H ILL0060.D ) API-ES. Neg. SIM. Frag: Var 1600000 1400000 1200000 1000000 800000 600000 400000 0200000 ~r 4 m ir initial Date Instrument 1 1/31/01 10:31:10 AM KLT/MLA FACT -TCR002 (LIMS #E00-1716). Page 101 of 109 Page 1 of 2 Batch Run # 60 of 80 Data File C:\HPCHEM\1\DATA\H010129\HILL0060.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 111/..00300100/0001 10:09:45 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ----------|--------- |-----------_ ,, | --------------- |--------------- | - | - ------- 4.108 VBA+ I 1.82483e6 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type Area Amt/Area Amount Grp Name --[--m-i-n-]---1--------- 1--------------- -----r--a-t--i-o----- 1---[--n-g-/--m-L-]---- 1 - | ---------- 4.924 VBA+ I 9.61252e5 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ----------|--------- , --------------- |--------------- |--------------- | - | ----------- 5.145 W A + 1.2 8992e7 1.72729e-l 589.66683 PFOS Totals without ISTD(s) : 589.66683 *** End of Report *** BACK TO MAIN Sampl J.Ma m t ; . w * - w g - j ,a Instrument 1 1/31/01 10:31:10 AM KLT/MLA FACT -TCR002 (UNIS #E00-1716), Page 102 of 109 Page 2 of 2 Attachment D: Deviations from the Method and Protocol FACT -TCR002 (LIMS #E00-1716), Page 103 of 109 BACK TO MAIN Record of Deviation Study / Project No. Deviation Type: (Check one) I. Identification PFO SPSrOoOPtocctoalnol SMoOeltuhthebor:idlity/EFquAipCmTe-nTt PCroRce0d0u2re Document Number: TS-8-155.0 Date(s) of occurrence: 26 Jan, 01 to 29 Jan, Of II. Description: RwecxaehlcqielbuunridarqietunidoagnnPstrctioatuacnrtedvidnaeugrrdralesot/hpfwreroorlmecthveastehsnls:etohcEaeflaTfinbuSarl-lal8ytr-itao1enn5,g5icet.u.0m"rv,aTesy.ehbceteimonneetch1e1os.ds3adrsyotaettsoesnuo"sFtedothirsepcuulorspwsofseuenrstdhoeofrfamtchceeuthroacdys of AltiTdc6sahttao1hrcaawlc0getninuubeardneamtsrarhgaflarnoeet/PdnimernosfrgectuoLneeeatlcdhstclooeseutridnafhanrhursevncytritegohgaeltoeln/ehosupwdiefrmnruoaraocesrrwneceednnp)esdttdsduthhoswaoreeo:ptfpeafopsrtratthseSaohhmereivaeasntipnctcodcoluateeeufhflrryttverabhvhazeceeee2enctsd.tguwce5aexuerftr,aairra5wssavcoc,fcyemutaicaessrtwundeah2arddnha.att5hgetc1tt0eneohwy0-e+o1qqaan0usuuf/tg-a0tpat/m1hhmnn2p5eeotteLini%rtrtsrgeaaearst/tsmaaaitmepanncppnetLggcphlcdue.erestaoriaocarvAhpmdocfeirnsgynitpadhdhcwlrtaeeeeeeaetsrnqcsatrtoiluuersrenriaaevntrvtnthceeohiegteoml.tiasenodtie.AnnoawndcftIlta1aals,tatu1osawanrd.,an3uaraennadlnsdeygnok_lttgetiuhn_en,eadeo_(.rlrte_wl5ahes_5tfenh_ot0,oer-a,re walelorewnfootricnocnlusdisetde.ncSyuibnstehqeuwenatybtahtcehdeasta(iw.e.asDraeypsro2caenssde3d)awnderreerpeoprrteodc.essed the same way to ARemcoertdheoddBdyev: iation was(wsurcithteans. ameInIId.mAencttiisosunesd.TSaOkPenr:evision, etc.) Date: O fe tro i The deviation improves the quaIVlit.y oImf tpheacdtatoanbeSctauudseyt/hePcroaljiebcrattion standard range used to quantify the data is more appropriate to the sample range, and is thus more accurate. Authorized By: (Study Director / Project Lead) Exact Copy of Original iflnfitial ... W-DZatUeo > 3M Environmental Laboratory. Deviation No. (assigned by Study Director or Project Lead at the end o f study or project) FACT -TCR002 (LIMS #E00-1716), Page 104 of 109 BACK TO MAIN Record o f Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Octanol Solubility/ FACT-TCR002 PSrOoPtocol & MOeththeor:d Equipment Procedure Document Number: ETS-8-170.0 Date(s) of occurrence: 22 Jan 01 to 26 Jan 01 II. Description: ptRahraeeerqtssiuctoiiulrlulelabdotibePlssirteoyarc.rv"eeeddou,brtsehe/erpvrceoodcl,eutsmhs:en seEhluaTktSieo-n8fl-am1s7ek0thm.0oe,dtshweocidtlilo(bEneT1uS2t-i.1l8i.-z81e7dst2a(.Et0e)TssS"h-aI8lf-l1thb7ee1.uu0sn)ed.disItsfoonldoveevtedirspmibailrnetiecles Actual Procedure/process: Results of the solubility screening test indicated that the column elution method shall be used, however the shake flask method was used due to issues with octanol. The column elution method requires the test solvent to be compatible with the ACOGm 8i) nTM O <O>a9*- r?6 a ttAtcsouhionnbenwcoiteneativhtgihineetsuneritsrtsafe.aonedTcdfn,thcooaeelcrnxotidtpasnoeonpcdscouruolebirnnllaeiesmtaaiotdnokirneaiohragncareictyss.uaevnmblooaeetllctaohtftrroioilfrcidotatyrhdl eaeoonvufaetntellhtxeoiettcpseismnpoodaenlvetneddetdindeatdem.iumnTorsahouitendniosettte,norsaafotnttefsdidomthwltveehoeaaeuntnxlttddpumepbirsaoiiynmnsgeonetonwaittno.sbauaefledsvteyon~alotlahettdr~ibleeea,taibnle oo oj UX3 .*csjs Abmienmtdheeotrhdt.oodddoecvuimateionnt twhaatst(whsuercisththeaanks.eaAfmlaensInoIkIdt.ewmAtaeosncftutiilisoesesndwuseaadssT,aaaSnlsOkoaePlnwter:rreinvtatiestiinvoenan,tdoetitcnh.)celucodleudminntehleutsiotundy Recorded By: Date: d m > i- 0 4 H -a o IV. Impact on Study / Project TqrTAeuhhupaietoslhirstdotoyereldivuozibbweaijdtleiiitcBothytnyicvd:doeeo(nstSef.etisrudmSndeinoyinnctcDaeeat.idirtovheneecrtoqosefurlPay/lFPiatOyfrfSoecjcoientnctttohrocLelteaqpanuadoas)llsievtydia,otsfhhteahkreeedsfualltatass.kamreevthaolidd manedt mallaydabtea Date: 3M Environmental Laboratory A Deviation No. (assigned by Study Director or Project Lead at the end o f study or project) FACT -TCR002 (LIMS #E00-1716), Page 105 of 109 BACK TO MAIN Record of Deviation I. Identification Study / Project No. Deviation Type: (Check one) PFOS Octanol Solubility/ FACT-TCR002 PSrOoPtocol ^M eOtthheord: Equipment Procedure Document Number: ETS-8-155.0 Date(s) of occurrence: 22 Jan 01 to 29 Jan 01 II. Description: RftShoeeercqetsuiaaoicmrnehed1sr0aPu.mr2no.p3calesesdttsuahetreeteso/ap,nrr"idgoaicnanenaaslalsyl:syzaezmEetdhTpeltSeom-."8da-et1trei5xr5m.s0piniskeeecthtaienodnmlta0ht.er2i.xm1easfttrfaietxcetss,op"inkMtehdeautrrpeixcliocsvapteiekrye(seifaffrpiercepipernaercpeyad?r)edin AancatluyazlePdr.ocedure/process: The matrix spikes were not prepared, therefore, they were not TDhisecEreTtiSo-n8-o1f5t5h.e0pmroejtehcotd(lsehuaacdhs. baeseanmreeInvIIdi.smeAdencstotiiosthsnuasetdmT, aaStkOriexPnsr:peivkiseisomn,aeytcb.)e prepared at the Recorded By Date: (H I?'?l IV. Impact on Study / Project TTpohhsiessimdbelaevtriiianxtitiohsniwsdseotluelsddyenfositnineacddevatehnredseaclnyhaaalryfaftceetceotriftzhienedtqe. ureTaslhtiteiyscoarelfratethaieodnydaoattfa.msaatutrriaxtisopnikceosnacreentnroattioacntsu.ally Authorized By: (Study Din ct Lead) t'* / T- DateW ^/o ) 3M Environmental Laboratory Deviation No. 4 (assigned by Study Director or Project Lead at the end o f study or project) FACT -TCR002 (LIMS #E00-1716), Page 106 of 109 BACK TO MAIN Record of Deviation I. Identification Study / Project No. PFOS Octanol Solubility/ FACT-TCR002 Deviation Type: (Check one) PSrOoPtocol 8 MOeththeor:d Equipment Procedure Document Number: ETS-8-155.0 Date(s) of occurrence: 22 Jan 01 to 26 Jan 01 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: The criteria used for reprocessing data was that all CCVs and ct1ha7el2ibr.1er)qa.tuiiornemsteanntdoarfdtshehasdhatkoehfalvaeskas%amapclceusrtaocybeoafccu1r5a%te. toThwisithwians1d5o%ne(atoccboerdcionngstiosteEnTtSw-i8t-h oOoI>aoof*) sl ^ oa i. <0 (such as ameInIId.mAencttiiossnusedT, aSOkePnr:evision, A method deviation was written. etc.) 8 A * Recorded By: Date: v i- M l IV. Impact on Study/Project Trehqeuidreevmiaetniot nofptrhoevicdaelsibbraettitoernqsutaanlidtyar,dasnpdrmovoirdeedcoanhtrioglhleedr ldeavteal. oTfhceomnfoirdeenstcreinfgoerntht perreecpiosirotend sample d a t a . _______________________________________________________________ 3M Environmental Laboratory (assigned by Study DirectorDorePvrioajetcitoLneaNd aot.the end of study or project) FACT -TCR002 (LIMS #E00-1716), Page 107 of 109 Attachment E: Sample Calculations BACK TO MAIN FACT -TCR002 (LIMS #E00-1716), Page 108 of 109 BACK TO MAIN Mean and standard deviation were calculated using functions provided in Microsoft Excel software. Standard deviation was used to measure the scatter about the mean of a data set; thus, it can be used to estimate the precision of a method. Relative standard deviation presents a measure of the magnitude of the standard deviation and is calculated by dividing the standard deviation by the mean. Means are calculated by adding individual entities and dividing the resultant sum by the number of individual entities. Standard deviation was calculated using the following equation: InSx -(Sx)2I------ ---------- -- -Where n is the number of observations, and x is sample concentration. \ /7(/7--1 ) Average/Standard Deviation /%RSD example calculations: Sample ID Rep1 Rep 2 Rep 3 Rep 4 Concentration pg/mL 59.1 57.4 57.6 57.1 Calculations Average (59.1+57.4+57.6+57.1)/4= 57.8 Std Dev (see above equation)= 0.88 %RSD (0.88/57.8)= 1.5% FACT -TCR002 (LIMS #E00-1716), Page 109 of 109