Document 15V1vDoBdQad2bMaw6b2y4w3o

AR226-1030A026 BACK Study Title Characterization Study of PFOS, Primary Standard - Test Control Reference # T C R -0 0 0 17-046 ` Ph ase: Solubility of PFOS in Natural S eawater and an A queous Solution o f 3.5% Sodium Chloride 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 138 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 Natural Seawater and an Aqueous Solution of 3.5% Sodium Chloride. 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 138 BACK TO MAIN Q uality Assurance Statement Study Title: Characterization Study of PFOS, Primary Standard - Test Control Reference # TCR-00017-046, PHASE: Solubility of PFOS in Natural Seawater and an Aqueous Solution of 3.5% Sodium Chloride. 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 4/23/01 -4/26/01 4/26/01 -4/27/01 ---- 1---------- !----------------------------------- Phase Date Reported to I Management Study Director Data 4/27/01 4/27/01 Draft Phase Report 4/27/01 4/27/01 QAU Representative ^ [fate 'ltc rO l ' FACT-TCR002 (UMS #E00-1716), Page 3 of 138 BACK TO MAIN Table of Contents GLP Compliance Statement............................................................................................................... 2 Quality Assurance Statement............................................................................................................. 3 Study Information............................................................................................................................... 6 Summary............................................................................................................................................ 7 Purpose.............................................................................................................................................. 7 Test Substance................................................................................................................................... 8 Test System........................................................................................................................................ 8 Method Summaries.............................................................................................................................9 Preparatory Methods..........................................................................................................................9 Sample Collection and Analysis......................................................................................................... 10 Analytical Method................................................................................................................................11 Analytical Results................................................................................................................................12 Data Summary....................................................................................................................................13 Statistical Methods........................... ................................................................................................. 16 Statement of Conclusion.................................................................................................................... 16 References......................................................................................................................................... 17 List of Attachments............................................................................................................................. 17 Signature Page................................................................................................................................... 18 Attachment A: Extraction and Analytical Methods............................................................................ 19 Attachment B: Data Summary Tables............................................................................................... 40 Attachment C: Sample Chromatograms........................................................................................... 63 A ttachm ent D: D eviations from the P roto co l....................................................................................................133 Attachment E: Sample Calculations.................................................................................................. 138 FACT-TCR002 (LIMS #E00-1716), Page 4 of 138 BACK TO MAIN List of Tables Table 1a. Summary Table of Solubility of PFOS TCR-00017-046 in Natural Seawater.................... 7 Table 1b. Summary Table of Solubility of PFOS TCR-00017-046 in an Aqueous solution of 3.5% Sodium Chloride................................................................................................................... 7 Table 2. Characterization of the Test Substance.............................................................................. 8 Table 3. Characterization of the Analytical Reference Substances.................................................. 8 Table 4. Test System........................................................................................................................ 8 Table 5a. Shake Flask Method Preparation for Natural Seawater.................................................... 9 Table 5b. Shake Flask Method Preparation for an Aqueous Solution of 3.5% Sodium Chloride..... 9 Table 6a. Sample Collection and Preparation for Study FACT-TCR002 in Natural Seawater.*......10 Table 6b. Sample Collection and Preparation for Study FACT-TCR002 in Aqueous 3.5% Sodium Chloride.*......................................................................................................... ....................10 Table 7a. Calibration Standard Reprocessing Summary for PFOS in Natural Seawater.................. 12 Table 7b. Calibration Standard Reprocessing Summary for PFOS in an Aqueous Solution of 3.5% Sodium Chloride...................................................................................................................13 Table 8a. PFOS TCR-00017-046 Solubility in Natural Seawater Data Summary........................... 14 Table 8b. PFOS TCR-00017-046 Solubility in an Aqueous Solution of 3.5% Sodium Chloride Data Summary..................................................................................................................... 15 Table 9a. Summary Table of Solubility of PFOS TCR-00017-046 in Natural Seawater....................16 Table 9b. Summary Table of Solubility of PFOS TCR-00017-046 in an Aqueous solution of 3.5% Sodium Chloride.................................................................................................................. 16 FACT-TCR002 (LIMS #E00-1716), Page 5 of 138 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 Dr. William K. Reagen (Sponsor Representative) 3M Environmental Technology and Safety Services (ET&SS) 3M Environmental Laboratory 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Experimental Dates Experimental Start Date: 22 January 2001 Experimental Termination Date: 07 February 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 138 BACK TO MAIN Summary The solubility of PFOS in natural seawater and an aqueous solution of 3.5% sodium chloride was determined quantitatively via the Shake Flask Method. Results are presented in Tables 1a and 1b: Table 1a. Summary Table of Solubility of PFOS TCR-00017-046 in Natural Seawater. Sampling Event P FOS SdujBiLiTY in Natural Seawater (Corrected for Purity) Standard Deviation Day 1 12.2 ng/mL 0.47 Day 2 11.9(xg/mL 0.07 Day 3 13.2ng/mL 1.30 Average Value 12.4 ng/m L 0.71 %CV 3.9% 0.6% 9.8% 5.7% The solubility of PFOS TCR-00017-046 in natural seawater was determined to be 12.4 |xg/mL at 22-23 C. Table 1b. Summary Table of Solubility of PFOS TCR-00017-046 in an Aqueous solution of 3.5% Sodium Chloride. Sampling Event Day 1 PFO S!Solubility in an AQUEOUSSOLUTIONOF 3.5% Sodium Chloride (Corrected for Purity) Excluded Standard Deviation Excluded % CV Excluded Day 2 20.0 |ig/mL 2.20 11.0% Day 3 19.9 ng/mL 1.31 6.6% Average Value 20.0 ng/mL 0.07 0.4% The solubility of PFO S T C R -0 00 17 -0 46 in an aqueous solution of 3.5% sodium chloride was determined to be 20.0 ng/mL at 22-24 C. Day 1 data was excluded because the %CV was greater than 15% as per the quality controls defined in ETS-8-172.0. Purpose The purpose of this phase of the study was to determine the solubility of PFOS in natural seawater and an aqueous solution of 3.5% sodium chloride as part of the characterization of this test, control, and reference substance. FACT-TCR002 (LIMS #E00-1716), Page 7 of 138 BACK TO MAIN Test Substance PFO S, T est Control Reference #T C R -00 01 7-046 Table 2. Characterization of the Test Substance ---------- 1--------------------- T est 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 8/31/01 Frozen TCR-00017-046 White Powder 97.9% Reference Substance Table 3. Characterization of the Analytical Reference Substances Reference S ubstance Source Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity PFOS ... i Re-crystallized by George Moore, 3M Specialty Materials, Bldg. 236-1 B-10 8/31/01 Frozen TCR-00017-046 White Powder 97.9% THPFOS SynQuest Labs Not Available Frozen TCR-00017-047 Lot #Q75-30 White Powder NA PFBS 3M, Cottage Grove 12/04/01 Frozen TCR-99030-023 Lot #101 White Powder 96.7 Test System Table 4. Test System T est System ----------------- !------ Natural S eawater Source Expiration Date Storage Conditions 3M Laboratory Identification Number Purity/Grade Ocean Scientific International 2005 Ambient TN-A: 4193 Salinity = 3.5% S odium chlo ride EM Science 2010 Ambient TN-A: 2458 99% FACT-TCR002 (LIMS #E00-1716), Page 8 of 138 BACK TO MAIN Method Summaries The solubility determination of PFOS TCR-00017-046 in natural seawater and aqueous 3.5% NaCI was performed according to 3M Environmental Laboratory method 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. ETS-8172.0 was subsequently revised to include additional information/clarification. The new revision, ETS-8-172.1, is procedurally the same as its predecessor and is included in Attachment A of this report. All analyses were performed according to the 3M Environmental Laboratory method ETS8-155.0 "Analysis of Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry". The approximately solubility oF PFOS in natural seawater and in an aqueous solution of 3.5% NaCI was estimated using the previously determined solubility of PFOS in water. The Shake Flask Method was used for the quantitative determination of PFOS solubility. A detailed description of the Shake Flask method used in this study is located in Attachment A. Preparatory Methods ETS-8-172.1 "Shake Flask Method: Solubility Determination of a Test Substance in Various Solvents." Greater than 6.5 mg PFOS was weighed into a tared 15 mL plastic centrifuge tube. Approximately 5 g of natural seawater or 3 g of of 3.5% sodium chloride solution was added gravimetrically to each 15 mL centrifuge tube. Nine centrifuge tubes were prepared, along with three method blanks (tubes with natural seawater or 3.5% sodium chloride solution only) for each test system. The centrifuge tubes were placed in a temperature-controlled orbital shaker set at approximately 30C. See the following tables documenting the shake flask method preparation: Table 5a. Shake Flask Method Preparation for Natural Seawater. Step Centrifuge Tube Preparation Replicates 1 >6.5 mg PFOS weighed into tared 15 mL centrifuge tube 9 2 Natural seawater added to centrifuge tube such that total weight of 9 PFOS and solvent was approximately between 5.0 - 5.2 g. 3 Method Blank Preparation- Approximately 5 g natural seawater 3 added to a tared centrifuge tube gravimetrically. 4 Samples sealed with tape, vortex-mixed, and placed in a 12 temperature-controlled orbital shaker set at approximately 30.0C, rotation speed set at approximately 150 rpm. Date(s) Performed 01-22-01 01-22-01 01-22-01 01-22-01 Table 5b. Shake Flask Method Preparation for an Aqueous Solution of 3.5% Sodium Chloride. FACT-TCR002 (LIMS #E00-1716), Page 9 of 138 BACK TO MAIN Step Centrifuge Tube Preparation Replicates 1 >9.5 g PFOS weighed into fared 15 mL centrifuge tube 9 2 3.5% Sodium Chloride solution added to centrifuge tube such that 9 total weight of PFOS and solvent was approximately between 3.0 3.1 g. 3 Method Blank Preparation- Approximately 3 g of aqueous solution 3 3.5% sodium chloride added to a fared centrifuge tube gravimetrically. 4 Samples sealed with tape, vortex-mixed, and placed in a 12 temperature-controlled orbital shaker set at approximately 30.0C, rotation speed set at approximately 150 rpm Date(s) Performed 01-29-01 01-29-01 01-29-01 01-29-01 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 from the incubator/shaker and allowed to equilibrate at 22-24 C for approximately 24 hours. After this, they were centrifuged and then had aliquots of supernatant collected. The aliquots were diluted using 100X dilutions (990 pL methanol: 10 pL sample). The diluted samples were spiked with internal standard (17pL of 15 pg THPFOS/mL and 15 pg 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 tables describe the sample collection and preparation regimen: Table 6a. Sample Collection and Preparation for Study FACT-TCR002 in Natural Seawater.* --------------------!----------------------------------------------- Step Procedure Replicates Date(s) Performed 1 At 24,48, and 72 hours of shaking, 3 PFOS+ 4 centri Day1 01-23-01 solvent, and 1 solvent (method blank) centrifuge fuge tubes tubes are removed from the incubator and per day Day2 01-24-01 equilibrated at 24-25 C for approximately 24 Day3 01-25-01 hours. 2 Aliquots of the supernatant (solvent containing 4 per Day1 01-24-01 dissolved PFOS or solvent only from the method blanks) were collected and dispensed into autovials. centrifuge tube Day2 Day3 01-25-01 01-26-01 3 The aliquots were diluted 100X with methanol (using a dual syringe diluter). Day 1 Day 2 01-24-01 01-25-01 Day 3 01-26-01 4 Internal Standard was added to the 100X sample dilutions (17pL of 15 pg THPFOS/mL and 15 pg PFBS/mL in methanol). Day 1 Day 2 Day 3 01-24-01 01-26-01 01-26-01 5 Samples were analyzed via HPLC/ES/MS on HP 1100 LC/MSD Day 1 Day 2 01-25-01 01-27-01 -01-28-01 Day 3 01-30-01 Table 6b. Sample Collection and Preparation for Study FACT-TCR002 in Aqueous 3.5% Sodium Chloride.* FACT-TCR002 (LIMS #E00-1716), Page 10 of 138 BACK TO MAIN S tep 1 2 3 4 5 -----------------------------------------------^------------- !------------------------------ Procedure i At 24,48, and 72 hours of shaking, 3 PFOS+ solvent, and 1 solvent (method blank) centrifuge tubes are removed from Ihe incubator and equilibrated at 24-25 C for approximately 24 hours. Aliquots of the supernatant (solvent containing dissolved PFOS or solvent only from the method blanks) were collected and dispensed into autovials. R ep lic a tes 4 centri fuge tubes per day Day1 Day2 Day3 4 per centrifuge tube Day1 Day2 Day3 The aliquots were diluted 100X with methanol (using a dual syringe diluter). Day 1 Day 2 Day 3 Internal Standard was added to the 100X sample dilutions (17pL of 15 pg THPFOS/mL and 15 pg PFBS/mL in methanol). 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 01-30-01 01-31-01 02-01-01 01-31-01 02-01-01 02-02-01 01-31-01 02-01-01 02-02-01 01-31-01 02-02-01 02-02-01 01-31-01-02-01-01 02-05-01 -02-06-01 02-06-01 -02-07-01 ` information pertains to sample preparation and dates of final reported data only. A nalytical 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 Liquid Chromatograph: Hewlett-Packard Series 1100 Liquid Chromatograph system Analytical column: Keystone BetasilTM C182x50mm, 5pm particle size Column temperature: Ambien t Cycle Time: 9.75 minutes Flow rate: 300pL/min Injection volume: 10pL Mobile phase components: Solvent A: 2.0 mM ammonium acetate in water Solvent C: Methanol FACT-TCR002 (LIMS #E00-1716), Page 11 of 138 BACK TO MAIN Solvent Gradient: Time 0.00 0.50 0.80 3.50 6.50 7.00 9.75 %C 15% 15% 60 % 100% 100% 15% 15% Mass Spectrometer: Hewlett-Packard Series 1100 API/Mass Spectrometer Detector Software: HP ChemStationTM 6.0 Fragmentar Voltage: m/z 427=100 V; m/z 499= 140 V; m/z 299 = 100 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) A nalytical 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 0.990 or greater (R2 values ranged from 0.9992 - 0.9999). Calibration Standards. Eleven standards ranging in concentration from approximately 2.5 to 1000 ng PFOS/mL methanol were used for the calibration curves. Calibration curves were run before and after every analytical sequence. Sample Replicates. Samples 012201-swPFOS-2.3.1, 012201-swPFOS-2.3.2, 012201swPFOS-2.3.3, 012201-swPFOS-2.3.4 and naclPFOS.2.2.1 were excluded from the reported data using Dixon's Q-Test. Continuing Calibration Verification. For quantitative determinations, a mid-level matrix calibration check was analyzed every eight samples to monitor instrumental drift, with a limit of 15% deviation of the target concentrations. Limit of Quantitation (LOQ). The LOQ is equal to the lowest standard in the calibration curve (either 2.5, 5.0 or 10.0 ng/mL). Table 7a. Calibration Standaird Reprocessing Summary for PFOS in Natural Seawater. --i------------------------ D a ta S ub B a t c h , A n alysis D ate C alib r a tio n S ta n d a r d s no t u s e d , r ea so n fo r ex c lu s io n S tandards Day 1 data: 01-25-01 2.5 -- 1002 ng/mL All curve pointswere used* Day 2 data: 01-27-01 - 01-28-01 2.5 -1 0 0 2 ng/mL All curve pointswere used* Day 3 data: 01-30-01 2.5 -1 0 0 2 ng/mL All curve pointswere used.* FACT-TCR002 (LIMS #E00-1716), Page 12 of 138 BACK TO MAIN Table 7b. Calibration Standard Reprocessing Summary for PFOS in an Aqueous Solution of 3.5% Sodium Chloride. D a t a S ub B a t c h , A n a lysis D UE Day 1 data: 01-31-01-02-01-01 Day 2 data: 02-05-01 - 02-06-01 Day 3 data: 02-06-01 - 02-07-01 C a lib r a tio n Standards 5 -- 501 ng/mL 10 -1 0 0 2 ng/mL 5 -- 501 ng/mL S ta n d a r d s no t u s e d , r e a s o n fo r e x c lu s io n Sntd 2 (2.5 ng/mL), and Stnd 13 (1002 ng/mL) were excluded to better fit the data at the low end of the curve* Stnd 2 (2.5 ng/mL) and Stnd 3 (5.0 ng/mL) was excluded to better fit the data at the low end of the curve.* Stnd 2 (2.5 ng/mL), and Stnd 13 (1002 ng/mL) were excluded to better fit the data at the low end of the curve.* *The first standard, Stnd 1 (0 ng/mL), is not used since there is no response measurable. Blanks. Method blanks (natural seawater or the aqueous solution of 3.5% sodium chloride 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 S ummary Tables 8a and 8b summarize individual sample data. Representative chromatograms are presented in Attachment C. The tables display PFOS concentrations for individual injections. Also included for each centrifuge tube replicate are the averages, standard deviation, and % coefficient of variation. FACT-TCR002 (UNIS #E00-1716), Page 13 of 138 BACK TO MAIN Table 8a. PFOS TCR-00017-046 Solubility in Natural Seawater Data Summary S a m p l e ID TCR-00017-046 P F O S ug/m L C orrected for P urity A verage ug/m L Std D ev "/ C o e f f ic ie n t o f v a r ia t io n Day 1 Centrifuge Tube #1 Rep 1: 012201-swPFOS-l .1.1 Rep 2: 012201-swPFOS-1.1.2 Rep 3: 012201-sviPFOS-1.1.3 Rep 4: 012201-swPFOS-1.1.4 12.3 12.7 12.6 12.9 12.6 0.25 2.0% Day 1 Centrifuge Tube #2 Rep 1:012201-swPFOS -1.2.1 Rep 2 :012201-swPFOS -1.2.2 Rep 3 :012201-swPFOS -1.2.3 Rep 4 :012201-swPFOS -1.2.4 11.6 12.0 11.7 11.6 11.7 0.19 1.6% Day 1 Centrifuge Tube #3 Rep 1:012201-swPFOS -1.3.1 Rep 2 :012201-swPFOS -1.3.2 Rep 3 :012201-swPFOS -1.3.3 Rep 4 :012201-swPFOS -1.3.4 12.2 12.5 12.4 12.3 12.4 0.13 1.0% Day 2 Centrifuge Tube#1 Rep 1:012201-swPFOS -2.1.1 Rep 2 :012201-swPFOS -2.1.2 Rep 3 :012201-swPFOS -2.1.3 Rep 4 :012201-swPFOS -2.1.4 11.9 11.7 11.7 11.8 11.8 0.10 0.8% Day 2 Centrifuge Tube #2 Rep 1:012201-swPFOS -2.2.1 Rep 2 :012201-swPFOS -2.2.2 Rep 3 :012201-swPFOS -2.2.3 Rep 4 :012201-swPFOS -2.2.4 12.0 12.1 11.8 11.7 11.9 0.18 1.5% Day 2 Centrifuge Tube #3 Day 3 Centrifuge Tube#1 Rep 1:012201-swPFOS -23.1 Rep 2 :012201-swPFOS -23.2 Rep 3 :012201-swPFOS -23.3 Rep 4 :012201-swPFOS -2 3 4 R e p 1: 01 2 2 0 1 -s w P F O S -3/1.1 Rep 2 :012201-swPFOS -3.1.2 Rep 3 :012201-swPFOS -3.1.3 Rep 4: 012201-swPFOS -3.1.4 15.2 15.3 15.8 16.0 14.5 14.3 14.5 14.5 15.6* 0.39 2.5% *Excluded via Dixon's Q-Test 14.5 0.10 0.7% Day 3 Centrifuge Tube #2 Rep 1:012201-swPFOS -3.2.1 Rep 2 :012201-swPFOS -3.2.2 Rep 3: 012201-swPFOS -3.2.3 Rep 4 :012201-swPFOS -3.2.4 13.4 13.1 13.3 13.5 13.3 0.17 1.3% Day 3 Centrifuge Tube #3 Rep 1:012201-swPFOS-3.3.1 Rep 2 :012201-swPFOS -3.3.2 Rep 3: 012201-swPFOS -3.3.3 Rep 4 :012201-swPFOS -3.3.4 11.7 12.1 11.7 12.1 11.9 0.23 1.9% FACT-TCR002 (LIMS #E00-1716), Page 14 of 138 BACK TO MAIN Table 8b. PFOS TCR-00017-046 Solubility in an Aqueous Solution of 3.5% Sodium Chloride Data Summary S a m ple ID I TCR-00017-046 PFOS A verage ug/m L ug/m L C orrected for S td D ev _ _ _ _ _ _ i_ _ _ _ _ P urity % C o e ffic ie n t o f v a r ia tio n Rep 1:012901-naclPFOS -1.1.1 22.2 22.3** Day 1 Centrifuge Tubetti Rep 2 :012901-nadPFOS -1.1.2 Rep 3 :012901-nadPFOS -1.1.3 22.3 21.7 0.45 2.0% Rep 4 :012901-nadPFOS-1.1.4 22.8 Day 1 Centrifuge Tube #2 Rep 1:012901-nadPFOS -1.21 Rep Z 012901-nadPFOS -1.Z2 Rep 3 :012901-nadPFOS -1.23 Rep 4 :012901-nadPFOS-1.24 19.8 19.9 19.7 20.1 19.9" 0.17 0.9% Day 1 Centrifuge Tube M3 Rep 1:012901-nadPFOS -1.3.1 Rep 2 :012901-nadPFOS -1.3.2 Rep 3 :012901-naclPFOS -1.3.3 Rep 4 :012901-nadPFOS -1.3.4 15.5 16.1 15.7 15.9 15.8" 0.26 1.6% Day 2 Centrifuge Tube#l Rep 1 :012901-naclPFOS -2.1.1 Rep 2:012901 -nadPFOS -2.1.2 Rep 3 :012901-naclPFOS -2.1.3 Rep 4 :012901-nadPFOS -2.1.4 21.0 21.4 22.1 24.4 22.2 1.52 6.8% Day 2 Centrifuge Tube #2 Rep 1:012901-nadPFOS -2.21 Rep 2 :012901-nadPFOS -2.2.2 Rep 3: 012901-nadPFOS -2.2.3 Rep 4: 012901-nadPFOS -2.2.4 28. r 20.3 19.9 19.9 20.0 0.23 1.2% *Rep 1 excluded via Dixon's Q-Test Day 2 Centrifuge Tube #3 Rep 1:012901-nadPFOS -2.3.1 Rep 2 :012901-nadPFOS -2.3.2 Rep 3 :012901-nadPFOS -2.3.3 Rep4: 012901-nacJPFOS-2.3.4 18.1 17.9 17.8 17.5 17.8 0.25 1.4% Day 3 Centrifuge Tube#1 Rep 1:012901-nadPFOS -3.1.1 Rep 2 :012901-nadPFOS -3.1.2 Rep 3 :012901-nadPFOS -3.1.3 Rep 4 :012901-nadPFOS -3.1.4 21.2 20.9 21.1 21.1 21.1 0.13 0.6% Day 3 Centrifuge Tube #2 Rep 1:012901-nadPFOS -3.2.1 Rep 2 :012901-nadPFOS -3.2.2 Rep 3 :012901-nadPFOS -3.2.3 Rep 4 :012901-nadPFOS -3.2.4 20.4 20.3 20.1 19.4 20.1 0.45 2.2% Day 3 Centrifuge Tube #3 Rep 1 :012901-nadPFOS -3.3.1 Rep 2 :012901-nadPFOS -3.3.2 Rep 3 :012901-nadPFOS -3.3.3 Rep 4 :012901-nadPFOS -3.3.4 18.6 18.5 18.1 18.6 18.5 0.24 1.3% ** Triplicates not excluded via the Q-Test. Howev er, when the triplicates for Day 1 were averaged, the %CV was outside of the acceptable range. The Day 1 solubility was therefore excluded. FACT-TCR002 (LIMS #E00-1716), Page 15 of 138 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 9a. Summary Table of Solubility of PFOS TCR-00017-046 in Natural Seawater. Sampling Event P FOS SdujBiLiTY in Natural Seawater (Corrected for Purity) Standard Deviation Day 1 12.2 pg/mL 0.47 Day 2 11.9 pg/mL 0.07 Day 3 13.2 pg/mL 1.30 Average Value 12.4 pg/mL 0.71 %CV 3.9% 0.6% 9.8% 5.7% The solubility of PFOS TCR-00017-046 in natural seawater was determined to be 12.4 pg/mL at 22-23 C. Table 9b. Summary Table of Solubility of PFOS TCR-00017-046 in an Aqueous solution of 3.5% Sodium Chloride. S a m plin g Eve n t P F O S 1S o l u b il it y in a n IQUEOUS SOLUTION OF 3.5% SodiuM C h l o r id e (C o r r e c te d fo r P u r it y ) S ta n d a rd D e v ia tio n %CV Day 1 Excluded Excluded Excluded Day 2 Day 3 20.0 pg/mL 19.9 pg/mL 2.20 11.0% 1.31 6.6% Average Value 20.0 pg/mL 0.07 0.4% The solubility of PFOS TCR-00017-046 in an aqueous solution of 3.5% sodium chloride was determined to be 20.0 pg/mL at 22-24 C. Day 1 data was excluded because the %CV was greater than 15%, as per the quality controls defined in ETS-8-172.0. Attachm ent B contains data sum m ary tables. Statistical Methods Statistical methods were limited to calculating means, standard deviations, and %CVs using Dixon's Q-Test to exclude data points. 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 natural seawater and an aqueous solution of 3.5% sodium chloride is 12.4 pg/mL at 22-23 C and 20.0 pg/mL at 22-24 C respectively. FACT-TCR002 (LIMS #E00-1716), Page 16 of 138 BACK TO MAIN 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. 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 FACT-TCR002 (LIMS #E00-1716), Page 17 of 138 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: nark E. Ellefson Principal Analytical Investigator 0 * 5 ^ /o f Date William K. Reagen Laboratory Manager Date FACT-TCR002 (LIMS #E00-1716), Page 18 of 138 BACK TO MAIN Attachment A: Extraction and A nalytical Methods ETS-8-172.0, the method approved during the study, has been replaced with a new version ETS-8-172.1. The new version is procedurally the same as the original version, but since it gives more details on the actual procedures, this new version is presented instead. FACT-TCR002 (LIMS #E00-1716), Page 19 of 138 BACK TO MAIN 3M Environmental Laboratory Shake Fla sk M etho d: Solubility D eterm ination of a Test 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, Laboratory Manager Date Date 1.0 Scope and Application_______________ - '_________________________________ 1.1 Purpose. According to the United States Environmental Protection Agency (U.S. EPA) and Organization for the Economic Cooperation and Development (OECD) guidelines, solubility determination of substances that have solubilities in a given test matrix (e.g. water/acetone/methanol) of greater than 100 pg/mL must be analyzed via the shake flask method (OECD Guideline 105, and OPPTS Guideline 830.7840). The prerequisite to this . method is a preliminairy screen of the test compound for its approximate solubility level. Refer to ETS-8-170.0 for the preliminary solubility screen test procedures. Exact Copy Of Original ETS-8-172.1 Solubili -1716), Page 20 of 138 Page 1 of 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 Summary of M ethod___________ ;______________________________________________ 2.1 Using the qualitative/semi-quantitative data obtained from the preliminary solubility screen test, weigh out more than five times the estimated soluble concentration of test substance into each of twelve screw-capped vessels (three time points with four test vessels each-sample, duplicate, triplicate, and matrix blank). Add the appropriate amount of test solvent gravimetrically. Cap the tubes, seal the caps with tape, and place horizontally on an incubator/shaker set to 30 C 2 C, shaking for approximately 24 hours. At approximately 24 hours, the first time point will be pulled and equilibrated at room temperature (about 20 C-26 C) for approximately 24 hours. The equilibrated samples are centrifuged and aliquoted into autovials. Samples are then diluted 1:10 or higher with a suitable solvent for analysis via LC/MS. At approximately 48 hours and 72 hours, the second and third sets, respectively, will be pulled, equilibrated, centrifuged, aliquoted and diluted ivith a suitable analytical solvent for LC/MS analysis. Depending on the analytical range, dilutions may be made using a diluter or syringe to make successive serial diluti ons using a suitable analytical solvent to reach the desired concentration (e.g. 1:10 or higher sample:methanol/acetone serial dilutions), and an appropriate internal standard (e.g. 1H,1H,2H,2H tetrahydroperfluorooctane sulphonic acid (THPFOS)) will be added to the final dilution prior to analysis. Samples are to be analyzed via LC/MS against a standard curve containing the test substance and an appropriate internal standard. 3.0 D e f i n i t i o n s ______________________________________________________________ 3.1 Method blank: An analyte-free matrix (e.g. methanol, water, or acetone) to which all reagents agree are added in the same volumes or proportions as used in title sample processing. The method blank is used to document contamination resulting from the entire sample treatment and analytical process. The method blank is earned through the complete sample preparation, treatment, mid analytical procedure. 3.2 Solvent blank: A sample of analyte-free medium (e.g. methanol/water/acetone solution) that is not taken through the sample treatment process. This blank is used to evaluate instrument and reagent cont amination. 3.3 Shake Flask Sample Triplicates: Three test vessels taken from and representative of the same sample source carried through all steps of the treatment, extraction, and analytical procedures in an identical manner. 3.4 Sample replicates: Replicate samples (two or more) taken from and representative of the same sample source (e.g. test vessel containing test analyte and solvent) and separately carried through analytical procedures in an identical manner. 3.5 Internal Standard (IS): A known amount of a compound similar in analytical behavior to the compound(s) of interest, added to all samples and standards, and carried through the entire measurement process. ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 21 of 138 Page 2 of 11 BACK TO MAIN 3.6 Calibration Standard: A dilution of various amounts of a stock, intermediate or purchased standard to achieve standard solutions in a concentration range of interest. 4.0 W arnings and Cautions_______________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Wear the proper lab attire for all parts of these procedures. Wear gloves and eye protection at all times. 4.1.2 Handle all solvents in a hood for all parts of the described sample preparation procedure. 4.1.3 For potential hazards of each chemical used, refer to material safety data sheets, packing materials, and 3M Environmental Laboratory's Chemical Hazard Review. 4.1.4 No mouth pipetting is allowed. 4.2 Cautions: 4.2.1 Glassware in which standards are prepared are to be triple rinsed with acetone and methanol to reduce the possibility of accidental contamination. 4.2.2 All test vessels (e.g. centrifuge tubes) are to be sufficiently rinsed with solvent prior to their usage. 5.0 Interferences______________ ________;_____________________________________ 5.1 Impurities may significantly affect the solubility of the test substance. The purity of the test substance should tie known and documented prior to starting the preliminary solubility screening procedure. 5.2 Contaminants in solvents, reagents, glassware and other sample processing or analysis hardware may cause interference. The routine analysis of laboratory method blanks must be used to demonstrate: that there is no interference under the conditions of the analysis. 6.0 Equipment____________________________________________ ^________________________ 6.1 Analytical balance sensitive to 0.1 mg. 6.2 Centrifuge capable o f holding 15 mL centrifuge tubes or equivalent. 6.3 Incubator with heating/cooling capabilities. 6.4 Diluter, Hamilton Microlab 500 Series, or equivalent. 6.5 Vortex-mixer. 7.0 Supplies and Materials_________________________________________________ 7.1 Thermometer capable of reading at least 15 C-40 C. 7.2 5-250 mL polypropylene centrifuge tubes, or equivalent. 7.3 Disposable glass graduated pipettes, 1 mL to 10 mL. 7.4 Disposable glass pasteur pipettes and rubber bulbs. 7.5 Glass beakers, various sizes. 7.6 Crimp cap autovials-1.5 mL, caps, crimper, and decapper. 7.7 Hamilton Gastight syringes (precision 1% of the total volume), 5 pL to 1000 pL. 7.8 Pipette-man manual pipettor. E T S -8 -172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 22 of 138 Page 3 of 11 BACK TO MAIN 8.0 Supplies and Materials 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 W ater, ASTM Type 1. 8.4 Test substance of known purity. 8.5 Calcium Chloride Dihydrate, Approximately 99% or better, from Sigma. 8.6 0.01 M CaCh solution, Example: A 0.01 M CaCL stock solution is prepared by weighing 1.4 g CaCL in a weigh boat and transferring to a 1 L volumetric flask and diluting to the mark with Milli-QTM water. 9.0 Sample H andling 9.1 Record times of initial preparation, set-up, and sample aliquoting/analysis on a sample preparation sheet or logbook. 9.2 Once the samples have been diluted, they may be analyzed via LC/MS. Alternatively, the diluted samples may be kept in cold storage (e.g. approximately 1-5 C) in crimp-capped autovials until the time of analysis. 10.0 Quality Control_____________________ ;______________________ ;__________ 10.1 Shake Flask Sample Triplicates. Set up each test vessel in triplicate to provide a measure of the precision on sample preparation. 10.2 Sample Replicates. Prepare and analyze all samples (from each test vessel for each time point) in multiple replicates (2 or more) to provide a measure of the precision on analysis. 10.3 Quality Control Blank Samples. 10.3.1 Method blank. Set up a fourth test vessel without test substance to measure any contamination accrued throughout the sample preparation process. The method blank is carried through the same sample preparation procedures as the three test vessels with test substance, only no test substance is added throughout the entire procedure. 10.3.2 Solvent Blank. An aliquot of the dilution solvent (i.e. methanol) directly analyzed for possible contaminants. The solvent blank is used to document any possible contamination of the solvent(s) used during the sample preparation process, and to detect any instrumental contamination or background interferences. 11.0 Calibration and Standarization 11.1 The compounds of interest must be standardized according to laboratory specifications. 11.2 All equipment used, such as the analytical balance and automated diluter, should be calibrated prior to use (daily, weekly, etc.) as specified in its standard operating procedure. ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 23 of 138 Page 4 of 11 BACK TO MAIN 11.3 All samples analyzed will be run against a standard curve containing varying amounts of test substance, and a fixed amount of internal standard. 12.0 Calibration and Standarization______________________________ 12.1 Preparation of Test Vessel. Record all data and observations on the example sample preparation worksheet (Attachment A) or equivalent. 12.1.1 Prepare a solution at least five times more concentrated than the concentration at which the substance was known to be dissolved at in the preliminary solubility screen test (ETS-8-170.0). 12.1.2 Weigh out test substance into a tared test vessel (e.g. 15 mL polypropylene centrifuge tube). . 12.1.3 Add the test solvent to the test vessel gravimetrically until the desired volume has been obtained {note: solvents have differing densities, therefore the weight needed to achieve a specific volume will be dependent on the density.). Record all weights on a standardized preparation sheet or logbook. 12.1.4 Visually confirm that there are undissolved particles. If no particles are present, repeat 12.1.2 wilh more test substance or add more test substance and record the additional weight. 12.1.5 Prepare the solution described in 12.1.1-12.1.4 nine times and label (at minimum) the test vessels as Day 1, -Rep 1, -Rep 2, and -Rep 3; Day 2, -Rep 1, -Rep 2, and - Rep 3; and Day 3, -Rep 1, -Rep 2, and -Rep 3. Also include the day of initial sample prep, the person(s) responsible for the sample, the test compound, nature of the study (e.g. water solubility), the solvent utilized, and the study number. 12.1.6 Prepare three test vessels as described in 12.1.3 without the test substance and label (at minimum) as Dayl ,Rep4; Day2,Rep4; and Day3,Rep4 along with the information described under 12.1.5. These three test vessels are the "method blank" samples. 12.1.7 Seal the cap to the test vessel. Mix/shake test vessel to ensure contact between the test substance and the solvent. And wrap the cap with tape. 12.2 Equilibration o f samples. 12.2.1 Place all of the test vessels on their side (horizontal) in an orbital incubator set to approximately 30 C 2 C and rotating at a considerable speed to ensure sufficient contact/mixing between the test substance and solvent. 12.2.2 At approximately 24 hours, four test vessels are removed: three containing test substance labeled "Day l,R epl", "Dayl,Rep2", "Dayl,Rep3", and "Dayl,Rep4". 12.2.3 The samples are shaken to ensure no test substance is stuck to the side of the tube. 12.2.4 The tubes are then placed in a stable temperature environment of approximately 20 26 C (record the actual temperature) for about a 24 hour period. 12.2.5 After about 24 hours of equilibration at 20 C-26 C, centrifuge the samples until the solution is visibly clear. If micelle formation is suspected, an additional high speed centrifugation step may be added (20,000 RCF for approximately 1 hour). The test vessels are now ready for dilution. See section 12.3 for further sample preparation. ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 24 of 138 Page 5 of 11 BACK TO MAIN 12.2.6 At approximately 48 hours of incubation time, the second set of test vessels may be pulled (labeled "Day2,Repl", "Day2,Rep2", "Day2,Rep3", and "Day2,Rep4") and equilibrated as described in 12.2.3-12.2.5. 12.2.7 At approximately 72 hours, the final set of samples is pulled (labeled "Day3,Repl", "Day3,Rep2", "Day3,Rep3", and "Day3,Rep4") and equilibrated as described in 12.2.3-12.2.5. 12.3 Sample preparation for analysis. 12.3.1 Observe the test solution. Due to the possibility of emulsions/or a concentrated layer of solute at the surface of the solution, it may be necessary to pipette off the top layer of solution (or an aliquot of sample may be centrifuged as stated in 12.2.5). The use of a pasteur pipette or equivalent is recommended. 12.3.2 Aliquot the test solution into each of four autovials (e.g. 1.5 mL polypropylene or glass crimp-cap vials). 12.3.2.1 Sample aliquots may be taken by submerging the pipette or syringe tip below the surface of the test solution. Note: when selecting the type o f pipette to be used, take into consideration the test substance's tendency to adsorb to certain materials (i.e. adsorption o f test substance to glass or plastic). 12.3.2.2 Prior to aliquoting sample to the autovial, the pipette tip must be equilibrated/saturated with the test solution by drawing and gently expelling the test solution in and out of the pipette tip, taking care not to disturb the solid particulate. 12.3.3 Label the four autovials and record the sample id. 12.3.4 Using a diluter, make a 1:10 or higher dilution of sample:extraction solvent (i.e. methanol, acetone) into a labeled autovial. 12.3.5 Using the solubility information obtained in the preliminary screen test, estimate the appropriate dilutions, if any, required to bring the concentration of sample into the appropriate analytical range (e.g. approximately 3 ng/mL to 3000 ng/mL test substance). Utilize the diluter to make serial dilutions of the sample using a suitable analytical solvent. 12.3.6 To the final andytical sample, add internal standard at a concentration suitable to the analytical method . 12.3.7 Samples will be analyzed via LC/MS against a standard curve of varied, known concentrations of test: substance with a constant concentration of internal standard equal to the concentration in the samples. 13.0 Data A nalysis and Calculations_____________________________________________ 13.1 Samples will be analyzed via a calibration curve. The amount of test substance in the sample will be quantified against a standard curve. 13.2 Means will be calculated by adding the individual entities and dividing the resultant sum by the number of individual entities. 13.3 Standard deviations will be calculated using either Microsoft Excel or Microsoft Access to calculate standard deviation. The built in function contains the following equation which is bailed on the individual entities (n) being less than 30: ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 25 of 138 Page 6 of 11 BACK TO MAIN 13.4 Sample precision will be reported as %RSD (or %CV). Sample precision will be calculated using the following equation: A/B X 100 = Sample %RSD where: A= standard deviation of averaged samples B= average of samples Sample RPD will be calculated using the following equation: | A-B | /((A+B)/2)= Sample RPD where: A= concentration of first replicate B= concentration of second replicate 13.5 Exclusion of an outlier data point may be performed by utilizing Dixon's Q-Test. The questionable data point may err to the high or low end of the data set. Calculate the variable "Qobserved." If Qobserved > Qtabulated, then the data point may be rejected with 90% confidence (see table 1 below for Qtabulated values). Qobserved gap/range where: Gap= the difference between the questionable point and the nearest value. Range=: total spread of the data. Table 11Criteria for Rejection of Outlier Values: Number of observations Qtabulated 90% Confidence Range 3 0.886 4 0.679 5 0.557 14.0 Data A nalysis and Calculations_____________________________________________ 14.1 Precision of data. Sample data must have a percent relative standard deviation (%RSD) (or relative percent difference) of < 15%. Non-compliant data must be evaluated for obvious outliers. The Q-Test may be applied to exclude questionable data points. If an outlier value exists, sample average and precision is re-calculated and reported without the questionable data point. Document die non-compliant data on data summary sheets, and include results of the statistical analysis with the final results. 14.1.1 Sample replicate %RSD's should be <15%. If the average of the sample triplicate data is >15% RSD, evaluate the three values for an outlier value. To questionable data points, apply the Dixon's Q-Test. If the outlier value is rejected with 90% confidence, exclude the sample from further data calculations and calculate the average and RPD for the remaining two values. If no data points can be excluded and the data does not meet the criteria, then the data set may not be used in the final reported data. The remaining shake flasks for the timepoint shall be used to report the data. 14.1.2 The %RSD between shake flasks should agree within 15%. If this criteria is not met, apply the Q-test to outlier datum. If the questionable data point is discarded ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 26 of 138 Page 7 o f 11 BACK TO MAIN via the Q-Test, then the non-compliant shake flask data is not to be used for the timepoint. Include justification for dropping the shake flask (e.g. q-test results). 14.1.3 And finally, the %RSD between the three days should be <15 % for the shake flask method. If this criteria is not met, it may be necessary to re-evaluate the data for possibl e outliers. Three agreeable time intervals are required to report the final solubility. If three consecutive timepoints do not agree within 15%, it may be necessary to repeat the entire test, or re-dilute/re-shoot samples to check for error. 14.2 Limit of Quantification. For this study, the LOQ will be equal to the lowest calibration standard used in the calibration curve containing more than twice the area counts of the highest Quality Control Blank. 14.3 Quality Control Blanks: Method and Solvent Blank samples. The level of analyte (test analyte OR internal standard analyte) shall be less than 50% of the area counts of the LOQ. If background levels of analyte exist in the initial method blanks, but subsequent blanks prior to the calibration standard curve are clean, the data may be accepted (provided that there are no oilier indicators that either the samples or the instrument contain significant background levels of analyte). 15.0 Pollution prevention and W aste Management 15.1 Dispose of sample waste by placing in high or low BTU containers as appropriate. Use broken glass containers to dispose of glass pipettes. 16.0 Records '___________________________________ 16.1 Sign and date all observations and calculations. 16.2 Fill out all appropriate sample preparation worksheets. 17.0 Attachments _____________. 17.1 Attachment A-Example Sample Preparation Worksheet. 18.0 References 18.1 Organization for Economic Cooperation and Development. OECD Guideline for Testing of Chemicals. Water Solubility -OECD Guideline 105: pp. 1-7, Adopted 1995 18.2 United States Environmental Protection Agency. OPPTS 830.7860 Water Solubility (Generator Column Method). Prevention, Pesticides and Toxic Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-C-96-042: pp. 1-17,1996 18.3 United States Environmental Protection Agency. OPPTS 830.7840 Water Solubility: Column Elution Method; Shake Flask Method. Prevention, Pesticides and Toxic ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 27 of 138 Page 8 of 11 BACK TO MAIN Substances: Fate, Transport and Transformation Test Guidelines. EPA 712-C-96-041: pp. 1-12,1996 18.4 ETS-8-170.0, Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents. 18.5 Harris, Daniel C. Statistics. Quantitative Chemical Analysis. 4thed.; W.H. Freeman and Company: New York, 1982; p 70-71. 18.6 Natrella, Mary Gibbons. The Treatment of Outliers. Experimental Statistics, National Bureau of Standards Flandbook 91; U.S. Government Printing Office: Washington, D.C., 1963; Pages 17-3, and T-27. 19.0 A ffected Documents 19.1 ETS-8-170.0, "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents." 20.0 Revisions Revision Number 1 Reason For Revision Section 1.2, references to specific test substances were removed. Section 3.6, removed "internal standard blank" from definition section. Section 12.2.5, an optional high-speed centrifugation step was added. Fixed the incorrect numbering of sections 13.5 through 14.3. Section 14.3, more clearly defined the acceptance criterion for method and solvent blanks. Revision Date 03-27-01 ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCR002 (LIMS #E00-1716), Page 28 of 138 Page 9 of 11 BACK TO MAIN ATTACHMENTA: Example Sample Preparation Sheet (page 1 o f 2). Temperature of Study:_____ !C 3M Environmental Laboratory Solubility Test: Shake Flask Method Sample preparation worksheet Study #____ Analyst(s):. Test Substance:_____________________________ID*__________________ Source; Date:___________________________ ___________ Test Solvent:____________________________ id:_____________________ Test Vessel:____________________ 15ml cenlrifuoa tube/Other(spedfy): solvent density:_____________aiml Source:_________________ Was the solubility screen test performed prior to start? Y/N If so, what Is the approximate concentration? . . . . . . . . . ...us/ml Thermometer ID: . Room Temp: SFM vials ID#: "samplelD" Sample Description Total mass weight test substance (solute + solvent) added: added: 'internal Standard addition ________ uJU______m is m in IS added to dilution factor: samplelD-1.1.1 thru-1.1.4 Day1, Smp1 1: samplelD-1.2.1 thru -1.2.4 samplelD-1.3.1 thru -1.3.4 samplelD-1.4.1 thru -1.4.4 samplelD-2.1.1 thru -2.1.4 samplelD-2.2.1 thru -2.2.4 samplelD-2.3.1 thru -2.3.4 samplelD-2.4.1 thru -2.4.4 Day1,Smp2 Day1,Smp3 Day1, Smp4 blank Day2, Smp1 Day2, Smp2 Day2, Smp3 Day2, Smp4 blank none added none added 1: 1: 1: 1: 1: 1: 1: samplelD-3.1.1 thru -3.1.4 samplelD-3.2.1 thru -3.2.4 Day3, Smp1 Day3, Smp2 1: 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-mlxed? Y/N Test vessels placed on orbital incubator? Y/N Incubator ID: Speed: 11nternal Standard: Int. Std. Cone.: rom Initial Temperature: . . . ID * ua/ml _ _C C Date/TIme/Inltials: Observatlons/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: Date/Time/lniuais: __ ,,_____________ FACT-TCR002 (LIMS #E00-1716), Page 29 of 138 ETS-8-172.1 Solubility Test: Shake Flask Method Page 10 of 11 BACK TO MAIN ATTACHMENTA CONTINUED (page 2 o f 2). 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: C Thermometer ID: Date/Time/lnitials: ..______________ "Day 1" Test Vessels Centrifuged: Cent. ID:_ Visual observations: . RPM or RCF read out. duration:. mm. Date/Time/initlals:. -Four aliquots from each of the four samples are to be made Into glass/plastic autovials (also, check autovlals for correct labeling). Yes/No -Immediately dilute the solution 1:______ with methanol. Methanol TN-A:_____________________ ,, Date/Time/lnitials:. Additional dilutions: Dilution factor (test solution:methanol): 1:. X's how many dilutions:. =final dilution factor: 1: Diluter ID used: Amounts used: _ul metnanoi, . _ui adlibica -Store samples and extracts in a cooler at until time of analysis. Cooler ID :. . Cooler Temp:. Dale/TIme/lnitlals:. 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. Date/Time/lnitials:-------------- ------------------------------------- i nratinn nf samniBs- TemDerature of environment C Thermometer ID:__ _______ Visual observations: "Day 2" Test Vessels Centrifuged: Cent. ID' Visual observations: RPM or RCF readout: duration: min. Date/Tlme/lnltlals:--------------------------------------------------- -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 solutior1 1: with methanol. Methanol TN-A . Additional dilutions: Dilution factor ftest solutiommethanol): 1: X's how manv dilutions: =final dilution factor. 1: Y Diluter ID used: -Store samples and extracts lr a cooler at until time of analysis. Amounts used: Cooler ID: uL methanol. Cooler Temp: "C Date/Time/lnitials:--------------------------------------------------. ul samples Date/Time/iniuais:--------------------------------------------------- Day 4: At approx. 24 hours of equilibration, the "Day 3* samples are to be allquoted/extracted. Environment Temp.: Test Vessels Centrifuged: Cent. ID:_____________________RPM or RCF readout________` duration:. Visual observations: ! C Therm. ID:. min. Date/Time/lnitials:. -Four aliquots from each of the four samples are to be made Into glass/plastic autovlals (also, check autovials for correct labeling). with methanol. Methanol TN*Ar Additional dilutions: Dilution factor (test solution:methanol): 1:_______ X's how many dilutions:. Diluter ID used:________________________ Amounts used: _uL methanol,. -Store samples and extracts In a cooler at until time of analysis. Cooler ID :. Cooler Temp:. Yes/No =final dilution factor 1: Date/Time/lnitials:. jjIsamples Date/Time/lnitials: _ FACT-TCR002 (LIMS #E00-1716), Page 30 of 138 ETS-8-172.1 Solubility Test: Shake Flask Method Page 11 of 11 BACK TO MAIN 3M Environmental Laboratory M ethod A nalysis of P otassium Perfluorooctanesulfonate or Other Fluorochemicals in W aste Stream or W ater Extracts U sing HPLC -El e c tr o spr a y /M a ss Spec tr o m etr y Method Number: ETS-8-155.0 Author: Mark L. Anderson, Mark E. Ellefson Approved By: Adoption Date: l(f (ofGO Revision Date: Laboratory Manager Date Exact Copcrfr9mal Word 97 ETS-8-155.0 Page 1 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Soectrometry " FACT-TCR002 (LIMS #E00-1716), Page 31 of 138 BACK TO MAIN 1.0 Scope and Application_________________________________________________ 1.1 Scope: This method describes the analysis of waste stream or water extracts using HPLCelectrospray/mass spectrometry. 1.2 Applicable Compounds: Fluorochemicals or other electrospray ionizable compounds. 1.3 Matrices: Tap water, ground water, wastewater and other aqueous solutions. 2.0 Summary of Method___________________________________________________ 2.1 This method describes the analysis of fluorochemicals or other electrospray ionizable compounds extracted from water, using HPLC-electrospray mass spectrometry (HPLCES/MS). The analysis is performed by the mass selection of a single ion characteristic of a particular compound, such as the perfluorooctanesulfonate (PFOS) anion, m/z = 499 or perfluorooctanoate (PFOA), m/z = 413. 3.0 De f i n i t i o n s _______ ;_________________________________________________ 3.1 Atmospheric Pressure Ionization (API): The Micromass Platform LCZ single quadrupole system and other commercially available LC/MS systems allow for various methods of ionization by utilizing a variety of sources, probes, and interfaces. These include but are not limited to: Electrospray Ionization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ionization in these processes occurs at atmospheric pressure (i.e., not under a vacuum). 3.2 Electrospray Ionization (ES, ESI): A method of ionization performed at atmospheric pressure, whereby ions in solution are transferred to the gas phase via tiny charged droplets. These droplets are produced by the application of a strong electrical field. 3.3 Mass Spectrometer (MS): The Platform LCZ and other commercially manufactured ES/MS systems are equipped with a single quadrupole mass selective detector. Ions are selectively discriminated by mass to charge ratio (m/z) and subsequently detected. 3.4 Conventional vs. Z-spray probe interface: The Micromass Platform LCZ system utilizes a "Z-spray" conformation. The spray emitted from the probe is orthogonal to the cone aperture. In the conventional conformation it is aimed directly at the cone aperture, after passing through a tortuous pathway in the counter electrode. Though the configuration is different, the methods of operation, cleaning, and maintenance are the same. However, Zspray components and conventional components are not compatible with one another, but only with similar systems (i.e., 2'-spray components are compatible with some other Z-spray systems, etc.). Other commercially manufactured ES/MS systems may have similar features. 3.5 Mass Lynx Software: System software designed for the specific operation of Micromass LCZ Mass spectrometer. Currently MassLynx has Windows 95 and WindowsNT 4.0 versions. All versions are: similar. For more details see the manual specific to the instrument (MassLynx NT User's Guide or Micromass Platform LCZ User's Guide). ETS-8-155.0 Page 2 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 32 of 138 BACK TO MAIN 4.0 Warnings and Cautions________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Use caution with the voltage cables for the probe. When engaged, the probe employs a voltage of approximately 5000 Volts. 4.1.2 When handling samples or solvents wear appropriate protective clothing, gloves, and eyewear. 4.2 Cautions: 4.2.1 Operate solvent pumps below a backpressure of400 bar (5800 psi). If the backpressure exceeds 400 bar, the HP1100 will initiate automatic shutdown. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences_______________________ :______________________________ 5.1 To minimize interferences when analyzing samples, Teflon should not be used for sample storage or any part of instrumentation that comes in contact with the sample or extract. 6.0 Equipment_____________ :_________________________________________ ;____ 6.1 Equipment listed below may be modified in order to optimize the system. Document any modifications in the raw data as method deviations. 6.1.1 Micromass Platform LCZ Mass Spectrometer equipped with an electrospray ionization source. 6.1.2 HP1100 low pulse solvent pumping system, solvent degasser, column compartment, and autosampler. 7.0 Supplies and Materials____________________________________________ 7.1 Supplies 7.1.1 High purity grade nitrogen gas regulated to approximately 100 psi (or house air system.). 7.1.2 HPLC analytical column, such as a Betasil C18 column (50x2mm, 5 pm particle size) or equivalent. 7.1.3 Capped autovials or capped 15 mL centrifuge tubes. ETS-8-155.0 Page 3 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 33 of 138 BACK TO MAIN 8.0 Reagents and Standards___________ ;___________________________________ 8.1 Reagents 8.1.1 Methanol, HPLC grade or equivalent. 8.1.2 Milli-QTM water (ASTM type I), all water used in this method should be Milli-QTM water or equivalent, and may be provided by a Milli-Q TOC Plus system or other vendor. 8.1.3 Ammonium acetate, reagent grade or equivalent. 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.1.3.2 2.0 mM ammonium acetate solution: Weigh approximately 0.300 g ammonium acetate. Pour into a 2000 L volumetric flask, add the appropriate volume of Milli-Q water, mix until all solids are dissolved. Store at room temperature. 8.2 Calibration Standards 8.2.1 Typically two method blanks (Milli-Q water), two matrix blanks, and solvent standards are prepared during the sample extraction procedure. 9.0 Sample Handling____________________________________________ .____ 9.1 Standards and sample extracts are stored in capped autovials or capped 15 mL centrifuge tubes until analysis. 9.2 If analysis will be delayed, standards and sample extracts may be refrigerated a.t approximately 4 C until analyses can be performed. 10.0 Quality Control____________________________________________________ 10.1 Solvent Blanks, Method Blanks and Matrix Blanks 10.1.1 Solvent blanks, method blanks, and matrix blanks are prepared and analyzed with each sample set to determine contamination or carryover. 10.1.2 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Matrix spikes are prepared for each sample set and analyzed to determine the matrix effect on the recovery efficiency. 10.2.2 Matrix spike duplicates are prepared periodically to measure the precision associated with the analysis. 10.2.3 Analyze the maitrix spike and matrix spike duplicate (ifprepared) in the same run as the original sample. . 10.2.4 Matrix spike and matrix spike duplicate concentrations should fall in the mid-range of the initial calibration curve or should be prepared at 1.5-5 times the endogenous . ETS-8-155.0 Page 4 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 34 of 138 BACK TO MAIN concentration of the analyte. Spike concentrations should fall in the low-range of the initial calibration curve if extremely low levels are expected. 10.3 Continuing Calibration Verifications 10.3.1 Continuing calibration verifications (CCV) are analyzed to verify the continued accuracy of the calibration curve. 10.3.2 Analyze a mid-range calibration standard after every tenth sample, with a minimum of one per sample set. 10.4 Internal Standard/Suirrogate Standard 10.4.1 An internal standard (IS) may be used to quantify the target analytes by establishing a relationship between the ratio of analyte response to IS response and a known concentration of the analyte of interest. The IS should be spiked at an amount that will fall within die mid-range ofthe calibration curve. The IS should be added after the extraction process and before analysis. 10.4.2 A surrogate standard may be used for quality control. The surrogate is used to quantitatively evaluate the entire analytical procedure including sample preparation and analysis. The surrogate should be spiked to fall within the low to mid-range of the calibration curve. 11.0 Calibration and St a n d a r d iz a t io n ________________________________ 11.1 Analyze the standard curves prior to and following each set of extracts. The average of two standard curves may be plotted by linear regression (y = mx + b) weighted 1/x, or quadratic fit (y = ax2+ bx + c) using MassLynx or other suitable software. The calibration curves should not be forced through zero. 11.2 If the calibration curve does not meet acceptance criteria perform routine maintenance or prepare a new standard curve (ifnecessary) and reanalyze. 11.3 For purposes of accuracy when quantitating low levels of analyte, it may be necessary to use file low end of the calibration curve rather than the full range. Example: when attempting to quantitate approximately 10 ppb of analyte, generate a calibration curve consisting of the standards from 5 ppb to 100 ppb rather than the full range of the curve (5 ppb to 1000 ppb). This will reduce inaccuracy attributed to linear regression weighting of high concentration standards. 12.0 PROCEDURES_______________________ ,_______________________________________ 12.1 Acquisition Set up . 12.1.1 Set up the sample list. 12.1.1.1 Assign a sample list filename using the first letter of the name ofthe instrument (T for Tucker), the year (00 for 2000), the month (04 for April), and the day (TOO1012 for October 12,2000). If more than one list is made on the same day, use increasing letters of the alphabet starting with A at the end of the list. ETS-8-155.0 Page 5 of 9 Analysis of Potassium Perfluorooctanesulfbnate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 35 of 138 BACK TO MAIN 12.1.1.2 Assign, a method (MS) file. 12.1.1.3 Assign, an HPLC program (Inlet file). , 12.1.1.4 Type in sample descriptions and vial position numbers. 12.1.2 To create a method, click on method in the Acquisition control panel then mass spectrometer headings and select SIR. Set ionization mode as appropriate and mass to 499 or other appropriate masses. A full scan is usually collected in addition to the SIRs. Save acquisition method. See the Micromass MassLynx GUIDE TO DATA ACQUISITION for additional information. 12.1.3 Typically the analytical batch run sequence begins and ends with a set of solvent standards. 12.1.4 Samples are analyzed 'with a continuing calibration verification (CCV) injected after every tenth sample. Solvent blanks should be analyzed periodically to monitor for possible analyte carryover. 12.2 Using the Autosampler/Colnmn Heater 12.2.1 Place sample vials into the sample tray according to the sample list prepared in Section 12.1.1, 12.2.2 Attach the proper analytical column in the column heater compartment. If using the switching valve, make sure that the tubing is run to the appropriate ports. 12.3 Using the Inlet Editor 12.1.1 Set-up the HP1100 using the following conditions or at conditions the analyst considers appropriate for optimal response. Record actual conditions in the instrument logbook: 12.1.1.1 Sample size ==10 pL injection 12.1.1.2 Flow rate = 300 pL/min. 12.1.1.3 Cycle time = 10.0 minutes 12.1.1.4 Mobile phase components: Solvent A: 2.0 mM Ammonium Acetate Solvent B: Methanol (MeOH) Solvent Gradient: Time tain.) 0.00 1.00 4.50 8.00 8.50 10.0 %B 5.00 % 5.00 % 95.0 % 95.0% 5.00 % Stop ETS-8-155.0 Page i Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (UNIS #E00-1716), Page 36 of 138 BACK TO MAIN 12.4 Instrument Set-up 12.4.1 Refer to the Platform LCZ User's Guide, the MassLynx NT User's Guide or ETS9-36, "Operation and Maintenance ofthe Micromass Platform LCZ Electrospray/Mass Spectrometer". 12.4.2 Check the solvent level in reservoirs and refill if necessary. 12.4.3 Check the tip of the stainless steel capillary at the end of the probe with an eyepiece. The tip should be flat with no jagged edges. If the tip is found to be unsatisfactory, disassemble the probe and replace the stainless steel capillary. 12.4.4 Turn on the nebulizing gas. 12.4.5 Open the tune page. Click on `Operate' to initiate the desolvation heaters. 12.4.6 Open the Inlet Editor. 12.4.5.1 Set HPLC pump to "On". 12.4.5.2 Set the solvent flow to the desired flow rate. 12.4.5.3 Observe droplets coming out of the tip of the probe. A fine mist should be expelled with no nebulizing gas leaking around the tip ofthe probe. Readjust the tip of the probe if no mist is observed. 12.4.5.4 Allow to equilibrate for at least 10 minutes. 12.4.6 The instrument uses these parameters at the following settings. These settings may change in order to optimize the response: 12.4.6.1 Drying gas 250-425 liters/hour 12.4.6.2 ESI nebulizing gas 10-15 liters/hour 12.4.6.3 HPLC constant flow mode, flow rate 10 - 500 |xL/min 12.4.6.4 Pressure <400 bar (This parameter is not set, it is a guide to ensure the HPLC is operating correctly.) 12.4.6.5 Source Block temperature 150. 12.4.6.6 Desolvation temperature 250. 12.4.7 Print the tune page with its parameters, the Inlet page, sample list, mass spec information, and all other applicable information and store it in the study binder with copies taped into the instrument run logbook. 12.4.7.1 All copies must be initialed and dated. 12.4.8 Click on start button on the MassLynx toolbar. Ensure start and end sample numbers include all samples to be analyzed. 13.0 Data Analysis and Calculations______________________________________ 13.1 Calculations: 13.1.1 Calculate matrix spike percent recoveries using the following equation: ETS-8-155.0 Page 7 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 37 of 138 BACK TO MAIN % Recovery = Observed Result - Background Result x 100 Expected Result 13.1.2 Calculate percent difference using the following equation: % Difference = Expected Cone. - Calculated Cone, x 100 Expected Cone. 13.1.3 Calculate actual concentration of analyte in matrix Qlg/mL): On-Column Concentration (|ig/mL) x Dilution Factors = Calculated Concentration 14.0 Method Performance _____________________________________ ______ 14.1 The Limit of Quantitation (LOQ) is method, analyte, and matrix specific. For many analytes, the LOQ concentration is selected as the lowest acceptable non-zero standard in the calibration curve. 14.2 Solvent and method blank values must be < Vi that ofthe lowest standard used in the calibration curve. 14.3 The coefficient of determination (r2) value for the calibration curve must be greater than or equal to 0.980. 14.4 Continuing Calibration Verification (CCV) percent recoveries must be 30% of the standard concentration. 14.5 Internal Standard recoveries should be within 50% of the spiked concentration. 14.6 If criteria listed in this method performance section are not met, maintenance may be performed on the system and samples reanalyzed or other actions as determined by the analyst. Document all actions in the raw data. 14.7 If data is to be reported when performance criteria have not been met, the data must be footnoted on tables and. discussed in the text of the report. 15.0 Pollution Prevention and Waste Management________________________ 15.1 Sample extract waste and flammable solvent is disposed in high BTU containers, and glass pipette waste is disposed in broken glass containers located in the laboratory. 16.0 Records______________________________________________________________ 16.1 Each page generated for a study must have the following information included either in the header or hand written on the page: study or project number, acquisition method, integration method, sample mime, extraction date, dilution factor (if applicable), and analyst. 16.2 Print the tune page, sample list, and acquisition method from MassLynx and other applicable information to include in the appropriate study folder. Copy these pages and tape into the instrument runlog. 16.3 Plot the calibration curve then print these graphs and store in the study folder. ETS-8-155.0 Page 8 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 38 of 138 BACK TO MAIN 16.4 Print data integration summary* integration method, and chromatograms, from MassLynx, and store in the study folder. 16.5 Summarize data using suitable software and store in the study folder. 16.6 Back up electronic data to appropriate medium. Record in study notebook the file name and location of backup electronic data. 17.0 Attachments_________ ;________________________________________________ 17.1 None 18.0 Re f e r e n c e s__________ ;__________________________________;_____________ 18.1 Platform LCZ User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.2 MassLynx NT User's Guide, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.3 MassLynx NT Guide To Data Acquisition, Micromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.4 ETS-9-36.0, "Operation and Maintenance ofthe Micromass Platform LCZ Electrospray/Mass Sprectrometer". 19.0 Affected Document;!;________________________________________ '________ 19.1 None 20.0 Revisions Revision Number. Reason For Revision Revision Date ETS-8-155.0 Page 9 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 39 of 138 Attachment B: Data S ummary Tables BACK TO MAIN FACT-TCR002 (LIMS #E00-1716), Page 40 of 138 FACT-TCR-002 TCR-002,012201-swPFOS-1.4.4,100X Dil. swPFOS-1.4.4 Method Blank, SFM 01-24-01 MEE(MLA) MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012201-SWPFOS-1.1.1,100X Dil. swPFOS-1.1.1 SFM 01-24-01 MEE(MLA) TCR-002, 012201-SWPFOS-1.1.2, 100X Dil. swPFOS-1.1.2 SFM 01-24-01 MEE(MLA) TCR-002,012201-SWPFOS-1.1.3, 100X Dil. swPFOS-1.1.3 SFM 01-24-01 MEE(MLA) TCR-002,012201-SWPFOS-1.1.4,100X Dil. swPFOS-1.1.4 SFM 01-24-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012201-SWPFOS-1.2.1,100X Dil. swPFOS-1.2.1 SFM 01-24-01 MEE(MLA) TCR-002, 012201-SWPFOS-1.2.2, 100X Dil. swPFOS-1.2.2 SFM 01-24-01 MEE(MLA) TCR-002,012201-swPFOS-1.2.3, 100X Dil. swPFOS-1.2.3 SFM 01-24-01 MEE(MLA) TCR-002, 012201-swPFS-i .2.4, 0GX D. swPFOS-1.2.4 SFM 01-24-01 MEE(MLA) MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012201-SWPFOS-1.3.1,100X Dil. swPFOS-1.3.1 SFM 01-24-01 MEE(MLA) TCR-002, 012201-SWPFOS-1.3.2,100X Dil. swPFOS-1.3.2 SFM 01-24-01 MEE(MLA) TCR-002, 012201-SWPFOS-1.3.3, 100X DH. swPFOS-1.3.3 SFM 01-24-01 MEE(MLA) TCR-002, 012201-SWPFOS-1.3.4,100X Dil. swPFOS-1.3.4 SFM 01-24-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 0100307-07 50.1 ppb PFOS 01003-07-08 75.1ppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 0100307-11 400.8ppb PFOS 0100307-12 501 .Oppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 43 H0125A1.M HILL0043.D 44 H0125A1.M HILL0O44.D 45 H0125A1.M HILL0045.D 46 H0125A1.M HILL0046.D 47 H0125A1.M H1LL0047.D 48 H0125A1.M HIU0048.D 49 H0125A1.M HILL0049.D 50 H0125A1.M HIU0050.D 51 H0125A1.M HILL0051.D 52 H0125A1.M HILL0052.D 53 H0125A1.M u1MnUUiAWnwCw'a.wn 54 H0125A1.M HILL0054.D 55 H0125A1.M HJLL0055.D 56 H0125A1.M HILL0056.D 57 H0125A1.M HILL0057.D 58 H 0125A 1.M HILL0058.D 59 H0125A1.M HILL0059.D 60 H0125A1.M HILL0060.D 61 H0125A1.M HILL0061 .D 62 H0125A1.M HILL0062.D 63 H0125A1.M HILL0063.D 64 H0125A1.M HILL0064.D 65 H0125A1.M HILL0065.D 66 H0125A1.M HILL0066.D 67 H0125A1.M HILL0067.D 68 H0125A1.M HILL0068.D 69 H0125A1.M HILL0069.D 70 H0125A1.M HILL0070.D 71 H012SA1.M H.0071.D 72 H0125A1.M HILL0072.D 73 H0125A1.M HILL0073.D 74 H0125A1.M HILL0074.D 75 H0125A1.M HILL0075.D 76 H 0125A 1.M HILL0076.D 77 H0125A1.M HILL0077.D 78 H0125A1.M HILL0078.D 79 H0125A1.M HILL0079.D 24 93 31 32 33 34 9 93 93 35 36 37 38 94 39 40 41 42 9 94 94 94 1 2 3 4 5 6 7 8 9 10 11 12 13 94 95 FACT-TCR002 (LIMS #E00-1716), Page 42 of 138 3M Environmental Laboratory BACK TO MAIN 4.11 0.00 2,194,236.0 0.0 254.0 0.0 4.11 2,102,494.3 254.0 4.11 2,158,897.3 254.0 4.11 2,209,667.8 254.0 4.11 4.11 0.00 0.00 2,201,234.8 2,265,761.0 0.0 0.0 254.0 254.0 0.0 0.0 4.11 2,127,831.0 254.0 411 2,140.157.8 254.0 4.11 2,234,175.8 254.0 4.11 2,133,177.8 0.00 0.0 254.0 0.0 4.11 2,171,835.0 254.0 4.11 2,169,104.3 254.0 4.11 2,169,278.8 254.0 4.11 4.11 0.00 0.00 0.00 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 0.00 0.00 2,124,585.3 2,256,450.0 0.0 0.0 0.0 2,223,529.8 2,218,475.3 2,246,805.0 2,228,379.8 2,213,923.0 2,240,633.3 2,212,715.5 2,188,168.8 2,235,874.0 2,186,509.0 2,224,174.0 2,213,476.0 2,203,661.3 0.0 0.0 254.0 254.0 0.0 0.0 0.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 4.94 0.00 4.92 4.93 4.94 4.94 4.86 0.00 0.00 4.92 4.94 4.94 4.94 0.00 4.94 4.94 4.94 4.92 4.86 0.00 0.00 0.00 4.86 4.86 4.86 4.86 4.86 4.86 4.86 4.86 4.86 4.86 4 S 4.86 4.86 0.00 0.00 1,141,147.0 0.0 1,112,681.4 1,116,756.6 1,119,839.4 1,126,401.0 1,118,630.0 0.0 0.0 1,118,494.1 1,113,286.9 1,141,315.6 1,121,531.1 0.0 1,127,920.3 1,115,169.9 1,100,957.0 1,098,603.0 1,132,609.1 0.0 0.0 0.0 1,103,581.8 1,145,372.3 1,132,338.8 1,155,401.0 1,134,933.8 1,146,786.6 1,137,843.9 1,132,896.5 1,130,818.8 1,132,445.8 1,115,520.0 1,120,492.8 1,072,897.5 0.0 0.0 254.4 0.0 254.4 254.4 254.4 254.4 254.4 0.0 0.0 254.4 254.4 254.4 254.4 0.0 254.4 254.4 254.4 254.4 254.4 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 0.0 0.0 0.00 0.0 0.0 0.00 0.0 0.0 5.14 3,780,994.0 125.7 5.14 3,919,050.5 129.9 5.14 3,895,319.3 128.8 5.14 4,009,264.5 131.9 5.14 3,109,402.5 102.2 2.0% 0.00 0.0 0.0 0.00 0.0 0.0 5.14 3,576,569.5 118.0 5.14 3,702,940.0 122.9 5.14 3,689,192.8 119.4 5.14 3,597,278.5 118.4 0.00 0.0 0.0 5.14 3,797,896.8 124.5 5.14 3,862,721.8 128.2 5.14 3,785,649.3 127.2 5.14 5.14 0.00 0.00 0.00 0.00 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.15 5.14 0.00 0.00 3,743,934.3 3,095,466.3 0.0 0.0 0.0 0.0 89,005.9 157,410.9 294,185.4 762,781.4 1,228,505.9 1,540,320.4 2,309,656.3 3,059,424.8 7,190,109.5 11,059,693.0 13,505,453.0 23,746,392.0 0.0 0.0 126.1 100.4 0.0 0.0 0.0 0.0 2.0 4.2 8.5 23.7 38.4 48.8 74.3 99.4 241.2 389.1 482.9 1,000.9 0.0 0.0 0.2% 19.6% 15.2% 15.6% 5.4% 4.2% 2.6% 1.1% 0.8% 3.7% 2.9% 3.6% 0.1% Solubility. Shake Flask M ethod 5/17/2001 Page 2 of 11 FACT-TCR-O 02 RAW DATA Agilent 1100 HPLC/MSD "Hillary" Acquistion Run: H010126 FACT-TCR002 (LIMS #E00-1716), Page 43 of 138 MeOH Blank MeOH Blank 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 MeOH Blank MeOH Blank MeOH Blank MeOH Blank swPFOS-2.4.1 swPFOS-2.4.2 swPFOS-2.4.3 swPFOS-2.4.4 MeOH Blank swPFOS-2.1.1 swPFOS-2.1.2 swPFOS-2.1.3 swPFOS-2.1.4 01003-07-09 MeOH Blank MeOH Blank swPFOS.2'2.1 swPFOS-2.2.2 swPFOS-2.2.3 swPFOS-2.2.4 MeOH Blank TN-A-4740, 04 Dec 00 TN-A-4740, 04 Dec 00 Oppb PFOS 2.5ppb PFOS 5ppb PFOS 10ppb PFOS 25ppb PFOS 40ppu PFOS 50.1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.Oppb PFOS 1002.0ppb PFOS TN-A-4740, 04 Dec 00 TN-A-4740, 04 Dec 00 TN-A-4740, 04 Dec 00 TN-A-4740, 04 Dec 00 TCR-002,012201-swPFOS-2.4.1, 100X DU. Method Blank, SFM 01-25-01 MEE(M(-A) TCR-002,012201-swPFOS-2.4.2,100X Oil. Method Blank, SFM 01-25-01 MEE(MLA) TCR-002,012201-swPFOS-1.4.3,100X Oil. Method Blank, SFM 01-25-01 ME(MLA) TCR-002,012201-swPFOS-2.4.4,100X Dll. Method Blank, SFM 01-25-01 MEE(MLA) TN-A-4740, 04 Dec 00 TCR-002,012201-SWPFOS-2.1.1, 100X Dll. SFM 01-25-01 MEE(MLA) TCR-002,012201 -swPFOS-2.1.2,100X Dll. SFM 01-25-01 MEE(MLA) TCR-002,012201-sw PFOS-2.1.3,100X Dll. SFM 01-25-01 MEE(MLA) TCR-002, 012201-swPFOS-2.1.4,100X Dll. SFM 01-25-01 MEE(MLA) 100.2ppb PFOS, CCv TN-A-4740, 04 Dec 00 TN-A-4740, 04 Dec 00 TCR-002,012201-swPFOS-2.2.1.100X Dll. SFM 01-25-01 MEE(MLA) TCR-002,012201-swPFOS-2.2.2,100X Oil. SFM 01-25-01 MEE(MLA) TCR-002,012201-swPFOS-2.2.3,100X Dil. SFM 01-25-01 MEE(MLA) TCR-002,012201-SWPFOS-2.2.4,100X Dll. SFM 01-25-01 MEE(MLA) TN-A-4740, 04 Dec 00 1 H010126C.M HILL0137.D 2 H010126C.M HILL0138.D 3 H010126C.M HILL0139.D 4 H010126C.M HILL0140.D 5 H010126C.M HILL0141.D 6 H010126C.M HILL0142.D 7 H010126C.M HILL0143.D 8 H010126C.M HILL0144.D 9 H010126C.M HILL0145.D 10 H010126C.M HILL0146.D 11 H010126C.M HILL0147.D 12 H010126C.M HILL0148.D 13 H010126C.M HILL0149.D 14 H010126C.M HILL0150.D 15 H010126C.M HILL0151.D 16 H010126C.M HILL0152.D 17 H010126C.M HILL0153.D 18 H010126C.M HILL0154.D 19 H010126C.M HILL0155.D 20 H 010126C .M HILL0156.D 21 H010126C.M HILL0157.D 22 H010126C.M HILL0158.D 23 H010126C.M HILL0159.D 24 H010126C.M HILL0160.D 25 H010126C.M HILL0161.D 26 H010126C.M HILL0162.D 27 H010126C.M HILL0163.D 28 H010126C.M HILL0164.D 29 H010126C.M HILL0165.D 30 H010126C.M HILL0166.D 31 H010126C.M HILL0167.D 32 H010126C.M HILL0168.D 33 H010126C.M HILL0169.D 34 H010126C.M HILL0170.D 35 H010126C.M HILL0171.D 36 H010126C.M HILL0172.D 98 98 46 47 48 49 50 51 52 53 54 55 56 57 58 98 98 99 99 59 60 61 62 99 63 64 65 66 54 99 100 67 68 69 70 100 3M Environm ents Laboratory BACK TO MAIN PFOS in Natural Seawater Shake Flask Method Day 2 Raw Data 0.00 0.00 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 0.00 0.00 0.00 0.00 0.0 0.0 2096939.6 2130418.5 2141519.8 2104440.5 2090966.6 2091922.9 2075323.6 2114582.0 2099818.0 2100878.0 2H5191.3 2092776.1 2112700.5 0.0 0.0 0.0 0.0 4.11 2043336.4 4.11 2117351.0 4.11 2050763.3 4.11 2056015.4 0.00 0.0 4.11 2073482.0 4.11 2018667.1 4.11 2037984.0 4.11 2037142.3 4.11 2060367.5 0.00 0.0 0.00 0.0 4.11 1998534.4 4.11 2011509.9 4.11 2076255.3 4.11 2085483.0 0.00 0.0 Sok&lity, S h aki Ftaak M#tbod 6/17/2001 0.0 0.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 0.0 0.0 254.0 254.0 254.0 254.0 0.0 254.0 254.0 254.0 254.0 254.0 0.Q 0.0 254.0 254.0 254.0 254.0 0.0 0.00 0.00 4.92 4.92 4.93 4.92 4.92 4.93 4.93 4.93 4.93 4.93 4.93 4.92 4.93 0.00 0.00 0.00 0.00 4.93 4.92 4.92 4.93 0.00 4.92 4.92 4.92 4.93 4.92 0.00 0.00 4.92 4.92 4.92 4.92 0.00 0.0 0.0 1174597.3 1173146.4 1194294.9 1183290.1 1189051.0 1167906.5 1188761.4 1169896.0 1166198.0 1160032.3 1144943.4 1149592.4 1110896.4 0.0 0.0 0.0 0.0 1126808.1 1132002.3 1126241.6 1129527.3 0.0 1116196.9 1111696.8 1107790.4 1106296.8 1155895.6 0.0 0.0 1107285.0 1102966.4 1119362.8 1109671.5 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 0.0 0.0 0.0 0.0 254.4 254.4 254.4 254.4 0.0 254.4 254.4 254.4 254.4 254.4 0.0 0.0 254.4 254.4 254.4 254.4 0.0 "- * 0.00 0.00 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 0.00 0.00 0.00 0.0 0.0 0.0 81704.0 159329.1 284697.0 760289.3 1195676.5 1513715.1 2240501 2934306.3 7028210.5 10446112.0 1272862S. 22114552.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 2.2 4.7 8.9 24.8 40.2 50.2 7fi ft 100.9 251.9 392.0 466.4 993.7 0.0 0.0 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 0.0 0.0 5.14 3379581.8 122.1 5.14 3307267.8 119.9 5.14 3271451.3 119.0 5.15 3334039.3 5.14 2889710.8 0.00 0.0 0.00 0.0 121.5 100.2 0.0 nA 5.14 3367552.8 122.6 5.14 3381544.5 123.7 5.14 3372612.8 121.5 5.14 3277744.3 0.00 0.0 119.0 0.0 13.1% 6.1% 10.7% 1.0% 0.2% 0.2% 1.9% 0.7% 0.6% 2.2% 2.9% 0.8% 0.0% FA C T-TC R -002 swPFOS-2.3.1 swPFOS-2.3.2 swPFOS-2.3.3 swPFOS-2.3.4 01003-07-09 MeOH Blank MeOH Blank MeOH Blank 01003-07-01 01003-07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-06 13-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-13 MeOH Blank MeOH Blenk TCR-002, 012201-SWPFOS-2.3.1,100X Dil. SFM 01-25-01 MEE(MLA) TCR-002.012201-SWPFOS-2.3.2,100X Dil. SFM 01-25-01 MEE(MLA) TCR-002, 012201-SWPFOS-2.3.3,100X Dil. SFM 01-2501 MEE(MLA) TCR-002, 012201-swPFOS-2.3.4,100X Dil. SFM 01-2501 MEE(MLA) 100.2ppb PFOS, CCV TN-A-4740, 04 Dec 00 TN-A-4740, 04 Oec 00 TN-A-4740, 04 Dec 00 Oppb PFOS 2.5ppb PFOS 5ppb PFOS 10ppb PFOS 25ppb PFOS 40ppb PFOS 50.1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.Oppb PFOS 1002.0ppb PFOS TN-A-4740, 04 Dec 00 TN-A-4740, 04 D ec 00 37 H010126C.M HILL0173.D 38 H010126C.M HILL0174.D 39 H010126C.M HILL0175.D 40 H010126C.M HILL0176.D 41 H010126C.M HILL0177.D 42 H010126C.M HIU-0178.D 43 H010126C.M HILL0179.D 44 H010126C.M HILL0180.D 45 H010126C.M HILL0181.D 46 H010126C.M HILL0182.D 47 H010126C.M HILL0183.D 48 H010126C.M HILL0184.D 49 H010126C.M HILL0185.D 50 H010126C.M HILL0186.D 51 H010126C.M HILL0187.D 52 H010126C.M HILL0188.D 53 H010126C.M HILL0189.D 54 H010126C.M HILL0190.D 55 H010126CM HILL0191 .D 56 H010126C.M HILL0192.D 57 H010126C.M HILL0193.D 56 H010126C.M HILL0194.D 59 H010126C.M HILL0195.D 71 72 73 74 54 100 100 90 46 47 48 49 50 51 52 53 54 55 56 57 58 90 90 FACT-TCR002 (LIMS #E00-1716), Page 44 of 138 3M Erwironm antol Laboratory BACK TO MAIN 4.11 2060058.4 4.11 2075784.8 4.11 1989603.4 4.11 4.11 0.00 0.00 0.00 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 0.00 0.00 2027539.0 2098973.5 0.0 0.0 0.0 2101071.5 2121610.3 2147140.8 2105029.8 2099930.5 2102480.8 2091009.0 '^Ur\rO-\rUy-T(OVTA.vO 2089134.9 2049022.3 2091091.1 2071210.9 2082979.1 0.0 0.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 0.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.Q 254.0 254.0 254.0 254.0 254.0 0.0 0.0 4.93 1103978.5 4.93 1111200.3 4.93 1098706.6 4.92 1114992.9 4.92 1158588.0 0.00 0.0 0.00 0.0 0.00 0.0 4.92 1160805.3 4.93 1176425.8 4.93 1180347.3 4.92 1157096.3 4.93 1170934.4 4.92 1157893.0 4.92 1159863.6 4 93 1153628.9 4.93 1146130.8 4.93 1134578.9 4.92 1112228.0 4.93 11OSSI7.9 4.92 1082716.6 0.00 0.0 0.00 0.0 254.4 254.4 254.4 254.4 254.4 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 0.0 0.0 5.14 4200268.0 5.14 4268221.0 5.14 4350863.0 5.14 4451651.5 5.14 2959959.5 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 5.14 83007.1 5.14 152217.0 5.14 277895.2 5.14 735110.4 5.14 1160993.9 5.14 1481490.6 5.14 2222684.0 5.14 2895124.5 5.14 6880929.5 5.14 10583437.0 5 14 12823226.0 5.14 21835648.0 0.00 0.0 0.00 0.0 154.6 156.2 161.2 162.6 102.5 0.0 0.0 0.0 0.0 2.2 4.5 8.9 24.3 39.3 50.4 76.7 101.3 252.2 410.6 510.6 1011.5 0.0 0.0 2.3% 11.6% 9.7% 10.9% 2.9% 1.9% 0.6% 2.1% 1.1% 0.7% 2.4% 1.9% 1.0% So)utility, Shak* F tetk M*thod 5/ 17/2001 P*0* 4 of 11 FACT-TCR-002 RAW DATA Agilent 1100 HPLC/MSD "Hillary" Acquistion Run: H010129 FACT-TCR002 (LIMS #E00-1716), Page 45 of 138 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppK ppQS 01003-07-06 40ppb PFOS 01003-07-07 50.1ppb PFOS 01003-07-08 75.1 ppb PFOS 01003-07-09 100.2ppb PFOS 0100307-10 250.5ppb PFOS 01003-07-11 400.8ppb PFOS 0100307-12 501 .Oppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012201-SWPFOS-3.4.1, 100X Dll. SWPF033.4.1 Method Blank, SFM 01-2301 MEE(MLA) TCR-002, 012201-swPFOS-3.4.2, 100X DU. swPFOS-3.4.2 Method Blank, SFM 01-2301 MEE(MUA) TCR-002, 012201-SWPFOS-3.4.3,100X Dll. SWPF033.4.3 Method Blank. SFM 01-2301 MEE(MLA) TCR-002, O12201-SWPFOS-3.4.4,100X Dll. SWPF033.4.4 Method Blank, SFM 01-26-01 MEE(MLA) MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, O12201-SWPFOS-3.1.1,100X Dll. SWPF033.1.1 SFM 01-26-01 MEE(MLA) TCR-002, 012201-SWPFOS-3.1.2, 100X Oil. swPFOS-3.1.2 SFM 01-2301 MEE(MLA) TCR-002, 012201-SWPFOS-3.1.3,100XDil. swPFOS-3.1t3 SFM 01-2301 MEE(MLA) TCR-002, O12201-SWPFOS-3.1.4, 100X DU. SWPF033.1.4 SFM 01-26-01 MEE(MLA) 0100307-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012201-SWPFOS-3.2.1.100XDII. swPFOS.3.2.1 SFM 01-2301 MEE(MLA) TCR-002, 012201-swPFOS-3.2.2, 100X Dil. swPFOS-3.2.2 SFM 01-2301 MEE(MLA) 1 " H010129B.M HILL0080.D 2 H010129B.M HILL0081.D 3 H010129B.M HILL0082.D 4 H010129B.M HILL0083.D 5 H010129B.M HILL0084.D 6 H010129B.M HILL0085.D 7 H010129B.M HILL0086.D 8 H010129B.M HILL0087.D 9 H010129B.M HILL0088.D 10 H010129B.M HILL0089.D 44 11 HCIO^SB.M HILL0090 H 12 H010129B.M HILL0091.D 13 H010129B.M HILL0092.D 14 H010129B.M HILL0093.D 15 H010129B.M HILL0094.D 16 H010129B.M H1LL0095.D 17 H010129B.M HILL0096.D 18 H010129B.M HILL0097.D 19 H010129B.M HILL0098.D 95 95 1 2 3 4 5 6 7 8 9 10 11 12 13 96 96 96 96 20 H010129B.M HILL0099.D 51 21 H010129B.M HILL0100.D 52 22 H010129B.M HILL0101.D 53 23 H010129B.M HILL0102.D 54 24 H010129B.M H1LL0103.D 97 25 H010129B.M HILL0104.D 61 26 H010129B.M HILL0105.D 62 27 H010129B.M HILL0106.D 63 28 H010129B.M HILL0107.D 64 29 H010129B.M HILL0108.D 9 30 H010129B.M HILL0109.D 97 31 H010129B.M HILL0110.D 97 32 H010129B.M HILL0111.D 65 33 H010129B.M HILL0112.D 66 3M Envirwimantul Laboratory BACK TO MAIN PFOS in Natural Seawater Shake Flask Method Day 3 Raw Data 0.00 0.00 4.11 4.11 4.11 4.11 4.11 4. 4.11 4.11 4.11 4.11 4.11 4.11 4.11 0.00 0.00 0.00 0.00 4.11 4.11 4.11 4.11 0.00 4.11 4.11 4.11 4.11 4.11 0.00 0.00 4.11 4.11 0.0 0.0 1,842,994.6 1.857,425.3 1,866,181.9 1,845,838.8 1,855,556.4 a1,nU<Ji-J1 MO AT 1,867,504.0 1,849,679.9 1,842,005.6 1.844,809.3 1,856,680.0 1,868,779.4 1,857,213.8 0.0 0.0 0.0 0.0 1,755,606.0 1,742,145.9 1,812,297.9 1,745,632.9 0.0 1,793,595.8 1,750,895.1 1,840,319.5 1,828,943.3 1,833,049.3 0.0 0.0 1,827,610.6 1,813,043.8 0.0 0.0 254.0 254.0 254.0 254.0 254.0 oca n 254.0 254.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 0.0 0.0 254.0 254.0 254.0 254.0 0.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 254,0 254.0 0.00 0.00 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 0.00 0.00 0.00 0.00 0.0 0.0 1,031,596.8 1,036,276.1 1,060.254.5 1,039,973.3 1,037,191.3 1,041.723.2 1,040,650.0 1,035,925.8 1,041,005.9 1,018,040.1 1,012,298.0 1,006,363.1 963,085.4 0.0 o.o 0.0 0.0 4.92 1,010,853.3 4.91 1,006,413.9 4.91 1,004,414.6 4.91 1,006,855.0 0.00 0.0 4.91 . 989,057.5 4.91 997,469.1 4.91 991,852.5 4.91 4.91 0.00 0.00 998,891.9 1,041,913.1 0.0 0.0 4.91 996,184.2 4.91 994,797.9 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 0.0 0.0 0.0 0.0 254.4 254.4 254.4 254.4 0.0 254.4 254.4 254.4 254.4 254.4 0.0 0.0 254.4 254.4 0.00 0.00 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 0.00 0.00 0.00 0.0 0.0 0.0 72,946.1 135,320.8 243,659.0 653,528.8 1,070,409.0 1,313,965.6 1,998,355.9 2,624,728.3 5,254,823.5 9.555,368.0 11,624,301.0 20,656,982.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 2.1 4.4 8.6 24.5 40.4 49.9 76.9 101.1 254.7 399.1 496.5 1,009.0 0.0 0.0 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 0.0 0.0 5.14 3,606,191.8 147.6 5.14 3,599,729.5 146.1 5.14 3,632,102.3 148.3 5.14 5.14 0.00 0.00 3,656,226.8 2,644,160.3 0.0 0.0 148.2 101.8 0.0 0.0 5.14 3,371,343.3 136.7 5.14 3,298,727.8 133.9 15.6% 12.2% 13.7% 2.4% 0.8% 0.4% 2.3% 0.9% 1.7% 0.4% 0.9% 0.7% 1.6% Solubility, Shake Flask Method 5/17/2001 FACT-TCR-002 TCR-002,012201-SWPFOS-3.2.3,100X Dil. swPFOS-3.2.3 SFM 01-26-01 MEE(MLA) TCR-002, 012201-SWPFOS-3.2.4,100X Dil. swPFOS-3.2.4 SFM 01-26-01 MEE(MLA) MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012201-swPFOS-3.3.1, 100XDII. swPFOS-3.3.1 SFM 01-26-01 MEE(MLA) TCR-002,012201-SWPFOS-3.3.2,100X Dil. swPFOS-3.3.2 SFM 01-26-01 MEE(MLA) TC R -002, 012201-SW PFOS-3.3.3, 100X Dil. swPFOS-3.3.3 SFM 01-26-01 MEE(MU) TCR-002, 012201-SWPFOS-3.3.4, 100X Dil. swPFOS-3.3.4 SFM 01-2601 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Oec 0 0 01003-07-01 01003-07-02 01003-07-03 1003-07-04 01003-07-05 01003-07-06 Oppb PFOS 2.5ppb PFOS 5ppb PFOS iCppb PFOS 25ppb PFOS 40ppb PFOS 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-13 MeOH Blank MeOH Blank 50,1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501 .Oppb PFOS 1002.0ppb PFOS TN-A-4740. 04 Dec 00 TN-A-4740. 04 Dec 00 34 H010129B.M HILL0113.D 67 35 H010129B.M HILL0114.D 68 36 H010129B.M HILL0115.D 97 37 H010129B.M HILL0116.D 69 38 H010129B.M HILL0117.D 70 39 H010129B.M HILL0118.D 71 40 H010129B.M HILL0119.D 72 41 H010129B.M HILL0120.D 9 42 H010129B.M HILL0121.D 97 43 H010129B.M HILL0122.D 97 44 H010129B.M HILL0123.D 97 HaUe Put Hll 10124.D 1 46 H010129B.M HILL0125.D 2 47 H010129B.M HILL0126.D 3 48 H010129B.M HILL0127.D 4 49 H010129B.M HILL0128.D 5 50 H010129B.M HILL0129.D 6 51 H010129B.M HILL0130.D 7 52 H010129B.M HILL0131.0 8 53 H010129B.M HILL0132.D 9 54 H010129B.M HILL0133.D 10 55 H010129B.M HILL0134.D 11 56 H010129B.M HILL0135.D 12 57 H010129B.M HILL0136.D 13 58 H010129B.M HILL0137.D 98 59 H010129B.M HILL0138.D 98 FACT-TCR002 (LIMS #E00-1716), Page 46 of 138 3M Environmental Laboratory BACK TO MAIN 4.11 4.11 0.00 4.11 4.11 4.11 4.11 4.11 0.00 0.00 0.00 4.11 4.11 4.11 4.11 4. il 4.11 4.11 4.11 4.11 4.11 4.11 4.11 4.11 0.00 0.00 1,821,905.5 1,804,143.4 0.0 1,763,726.3 1,824,344.0 1,806,923.3 1,817,528.4 1,823,161.8 0.0 0.0 0.0 1,797,068.0 1,807,103.9 1,806,916.9 1,808,355.9 i 732 502.9 1,790,624.0 1,809,404.6 1,801,089.3 1,773,768.8 1,809,450.4 1,756,825.4 1,816,221.0 1,840,075.4 0.0 0.0 254.0 254.0 0.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 0.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 0.0 0.0 4.91 4.91 0.00 4.91 4.91 4.91 4.91 4.91 0.00 0.00 0.00 4.91 4.9i 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 4.91 0.00 0.00 1,001,176.3 983,479.1 0.0 987,376.1 990,274.6 995,121.1 992,111.4 1,039,414.1 0.0 0.0 0.0 1,041,6229 ,046,4^j .vi 1,054,742.1 1,046,836.9 1,048,370.6 1,042,150.7 1,041,860.6 1,028,674.6 1,036,261.8 1,025,689.3 1,009,207.4 1,003,265.8 977,330.4 0.0 0.0 254.4 254.4 0.0 254.4 254.4 254.4 254.4 254.4 0.0 0.0 0.0 254.4 'iC.sSAT.-AT 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 5.14 3,367,698.0 5.14 3,367,747.0 0.00 0.0 5.14 2,909,405.8 5.14 3,057,538.8 5.14 2,972,588.3 5.14 3,043,574.5 5.14 2,664,370.3 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 5.14 73,997 4 5.14 134,066.8 5.14 248,733.9 5.14 653,704.9 5.14 1,053,882.6 5.14 1,323,609.8 5.14 1,972,099.5 5.14 2,618,876.0 5.14 6,271,318.5 5.14 9,627,486.0 5.14 11,622,508.0 5.14 20,749,418.0 0.00 0.0 0.00 0.0 135.9 138.4 0.0 118.6 124.4 120.3 123.6 102.8 0.0 0.0 0.0 0.0 2.1 4.4 8.8 24.2 35.6 50.2 76.4 101.4 252.2 403.7 498.1 996.5 0.0 0.0 2.6% 15.1% 12.7% 12.4% 3.4% Un.O00fl/ 0.2% 1.7% 1.2% 0.7% 0.7% 0.6% 0.6% Solubility, Shake Rack Mettiod 5/17/2001 Paga 6 of 11 BACK TO MAIN FACT-TCR002 PFOS in Seawater Day 1 Hillary, H010125 I I B S i RHH iH TCR-002, 012201-SWPFOS-1.1.1,100X Dll. swPFOS-1.1.1 SFM 01-24-01 MEE(MLA) 45 H0125A1.M HILL0045.D 31 5.14 TCR-002, 012201 -swPFOS-1.1 .2 ,100X Dii. swPFOS-1.1.2 SFM 01-24-01 MEE(MLA) 46 H0125A1.M HILL0046.D 32 5.14 TCR-002, 012201-swPFOS-1.1.3,100X Di!. swPFOS-1.1.3 s>t-M 01-24-01 mEE(MLA) 47 H0125A1.M HILL0047.D 33 5.14 TCR-002, 012201-SWPFOS-1.1.4, 100X Dii. swPFOS-1.1.4 SFM 01-24-01 MFH(MLA) 48 Y- TCR-002, 012201-SWPFOS-1.2.1, 100X Dll. V swPFOS-1.2.1 SFM 01-24-01 MEE(MLA) 52 3 Q a TCR-002, 012201 -swPFOS-1.2 .2 ,100X Dii. swPFOS-1.2.2 SFM 01-24-01 MEE(MLA) 53 <0 Q TCR-002, 012201 -swPFOS-1.2 .3 ,100X Dll. swPFOS-1.2.3 54 <Qs. SFM 01-24-01 MEE(MLA) s ns swPFOS-1.2.4 TCR-002, 012201-swPFOS-1.2.4, 100X Dii. 55 w SFM 01-24-01 MEE(MLA) H0125A1.M HILL0048.D H0125A1.M HILL0052.D H0125A1.M HILL0053.D H0125A1.M HILL0054.D H0125A1.M HILL0055.D 34 35 36 37 38 5.14 5.14 5.14 5.14 5.14 TCR-002, 012201 -swPFOS-1.3 .1 ,100X Dii. swPFOS-1.3.1 SFM 01-24-01 MEE(MLA) 57 H0125A1.M HILL0057.D 39 5.14 TCR-002, 012201-swPFOS-1.3.2, 100X Dll. SWPFOS-1.3.2 SFM 01-24-01 MEE(MLA) 58 H0125A1.M HILL0058.D 40 5.14 TCR-002, 012201-swPFOS-1.3.3, 100X Dii. SwPFOS-1.3.3 SFM 01-24-01 MEE(MLA) 59 H0125A1.M HILL0059.D 41 5.14 TCR-002, 012201-swPFOS-1.3.4, 100X Dii. swPFOS-1.3.4 SFM 01-24-01 MEfc(MLA) 60 H0125A1.M HILL0060.D 42 5.14 SSI*Yel'owed/greyed areas indicatepointsthat are notused m m udon factory purttvifactoiMi H -- 3,780,994 125.7 12.6 12.3 12.6 3,919,051 129.9 13.0 12.7 0.25 3,895,319 128.8 12.9 12.6 2.0% 4,009,265 131.9 13.2 12.9 3,576,570 118.0 11.8 11.6 11.7 3,702,940 122.9 12.3 12.0 0.19 3,689,193 119.4 11.9 11.7 1.6% 3,597,279 118.4 11.8 11.6 3,797,897 124.5 12.5 12.2 12.4 3,862,722 128.2 12.8 12.5 0.13 3,785,649 127.2 12.7 12.4 1.0% 3,743,934 126.1 Day 1 average: std dev: %C.V.: 12.6 12.3 12.2 pg/mL 0.47 3.9% FACT-TCR002 (LIMS #E00-1716), Page 47 of 138 3M Environmental Laboratory Solubility-Shake Flask Method 5/17/2001 Page 7 o f 11 BACK TO MAIN FACT-TCR002 PFOS in Seawater Day 2 Hillary, H 010126 ih h h h h h h h h h h h ih h b h h h h ^s TCR-002, 012201-SWPFOS-2.1.1,100X Dii. swPFOS-2.1.1 SFM 01-25-01 MEE(MLA) 25 H010126C.M HILL0161.D 63 5.14 3379582 122.1 12.2 11.9 11.8 TCR-002, 012201-swPFOS-2.1.2,100X Dii. swPFOS-2.1.2 SFM 01-25-01 MEE(MLA) 26 H010126C.M HILL0162.D TCR-002, 012201 -swPFOS-2.1.3, 100X Dii. swPFOS-2.1.3 SFM 01-25-01 MEE(MLA) 27 H010126C.M HILL0163.D 64 65 5.14 5.14 3307268 3271451 119.9 119.0 12.0 11.9 11.7 0.10 11.7 0.8% TCR-002, 012201 -swPFOS-2.1 .4 ,100X Dii. swPFOS-2.1.4 SFM 01-25-01 MEE(MLA) 28 H010126C.M HILL0164.D 66 5.15 3334039 121.5 12.1 11.8 TCR-002, 012201-swPFOS-2.2.1,100X Dii. swPFOS.2.2.1 SFM 01-25-01 MEE(MLA) 32 H01O126C.M HILL0168.D Q TCR-002, 012201-SWPFOS-2.2.2, 100X Dii. swPFOS-2.2.2 SFM 01-25-01 MEE(MLA) 33 H010126C.M HILL0169.D s (0 Q TCR-002, 012201-swPFOS-2.2.3,100X Dii. swPFOS-2.2.3 SFM 01-25-01 MEE(MLA) 34 H010126C.M HILL0170.D 67 68 69 5.14 5.14 5.14 3367553 3381545 3372613 122.6 123.7 121.5 12.3 12.4 12.1 12.0 11.9 12.1 0.18 11.8 1.5% E <0 to TCR-002, 012201-swPFOS-2.2.4,100X Dii. swPFOS-2.2.4 SFM 01-25-01 MEE(MLA) 35 H010126C.M HILL0171.D 70 5.14 3277744 119.0 11.9 11.7 TCR-002, 012201-SWPFOS-2.3.1,100X Dii. SwPFOS-2.3.1 SFM 01-25-01 MEE(MLA) 37 H01O126C.M HILL0173.D 71 5.14 4200268 154.6 15.5 15.2 15.6 TCR-002, 012201 -swPFOS-2.3.2,100X Dii. swPFOS-2.3.2 SFM 01 -25-01 MEE(MLA) - 38 . H010126C.M HILL0174.D 72 5.14 4268221 156.2 '05 .6: 15.3 0.39 TCR-002.012201-SWPFOS-2 3 3 , 100X Dll swPFOS-2.3.3 SFM 01-25-01 MEE(MLA) 39 H010126C.M HILL0175.D 73 5.14 4350863 161.2 16.1 15.8 2.5% 74 ' 5.14 : 4451652 ; 162.6;. . Sfcl* 160 i , Day 2 average: std dev: %C.V.: 11.9 ng/mL 0.07 0.6% FACT-TCR002 (LIMS #E00-1716), Page 48 of 138 3M Environmental Laboratory Solu bity-S hake Flask Method 5/17/2001 Page 8 of 11 BACK TO MAIN PFOS in Seawater Day 3 Hillary, H 010129 TCR-002, 012201-swPFOS-3.1.1, 100X Dii. swPFOS-3.1.1 25 HC10129B.M HILL0104.D SFM 01-26-01 MEE(MLA) TCR-002, 012201-swPFOS-3.1 .2 ,100X Dii. swPFOS-3.1.2 SFM 01-26-01 MEE(MLA) 26 H010129B.M HILL0105.D TCR-002, 012201 -swPFOS-3.1 ,3 ,100X Dii. SWPFOS-3.1.3 SFM 01-26-01 MEE(MLA) 27 H01O129B.M HILL0106.D TCR-002, 012201 -swPFOS-3.1.4, 100X Dii. SwPFOS-3.1.4 SFM 01-25-Q1 MEE(MLA) 28 H010129B.M HILL0107.D <*) TCR-002, 012201-8WPFOS-3.2.1,100X Dii. >- swPFOS.3,2.1 SFM 01-26-01 MEE(MLA) 32 H01O129B.M HILL0111.D Q TCR-002, 012201 -swPFOS-3.2.2,100X Dii. swPFOS-3.2.2 SFM 01-26-01 MEE(MLA) 33 H01O129B.M HILL0112.D Qa<0 TCR-002, 012201 -swPFOS-3.2.3,100X Dii. swPFOS-3.2.3 34 H01O129B.M HILL0113.D SFM 01-26-01 MEE(MLA) a S TCR-002, 012201-SWPFOS-3.2.4,100X Oil. (0 swPFOS-3.2.4 SFM 01-26-01 MEE(MLA) 35 H010129B.M HILL0114.D TCR-002, 012201-swPFOS-3.3.1, 100X Dii. swPFOS-3.3.1 SFM 01-26-01 MEE(MLA) 37 H01O129B.M HILL0116.D TCR-002, 012201-swPFOS-3.3.2, 100X Dii. swPFOS-3.3.2 SFM 01-26-01 MEE(MLA) 38 H010129B.M HILL0117.D TCR-002, 012201-SwPFOS-3.3.3, 100X Dll. swPFOS-3.3.3 SFM 01-26-01 MEE(MLA) 39 H 010129B.M H ILL0118.D TCR-002, 012201-SWPFOS-3.3.4, 100X Dii. SwPFuS-3.3.4 40 H010129B.M HILL0119.D SFM 01-26-01 MEE(MLA) 61 62 63 64 65 66 67 68 69 70 71 72 5.14 3,606,192 5.14 3,599,730 5.14 3,632,102 5.14 3,656,227 5.14 3,371,343 5.14 3,298,728 5.14 3,367,698 5.14 3,367,747 5.14 2,909,406 5.14 3,057,539 5.14 2,972,588 5.14 3,043,575 147.6 146.1 148.3 148.2 136.7 133.9 135.9 138.4 118.6 124.4 120.3 123.6 average: std dev: %C.V.: 14.8 14.5 14.6 14.3 14.8 14.5 14.8 14.5 13.7 13.4 13.4 13.1 13.6 13.3 13.8 13.5 11.9 11.7 12.4 12.1 12.0 11.7 12.4 12.1 13.2 ng/mL 1.30 9.8% 14.5 0.10 0.7% 13.3 0.17 1.3% 11.9 0.23 1.9% FACT-TCR002 (LIMS #E00-1716), Page 49 of 138 3M Environmental Laboratory Solubility-Shake Flask Method 5/17/2001 Page 9 of 11 FACT-TCR002 (LIMS #E00-1716), Page 50 of 138 FACT-TCR002 FACT-TCR002 PFOS Solubility of TCR-00017-46 in Seawater Day 1 data source acquisition instrument/sequence: Agilent 1100 HPLC/MSD "Hillary"/H010125.s Day 2 data source acquisition instrument/sequence: Agilent 1100 HPLC/MSD "Hillary"/H01012i.s Day 3 data source acquisition instrument/sequence: Agilent 1100 HPLC/MSD "HiIlary'7H010129.s DATA SUMMARY FOR INDIVIDUAL SAMPLES BACK TO MAIN swPFOS-1.1.1 12.6 swPFOS-1.1.2 13.0 sw P F O S -1 .1.3 12.9 sw PFOS-1.1.4 13.2 swPFOS-1.2.1 11.8 sw P F O S -1 .2.2 12.3 sw P F O S -1 .2.3 11.9 sw P F O S -1 .2.4 11.0 s w P F O S -1 .3.1 12.5 s w P F O S -1 .3.2 12.8 SwPFOS-1.3.3 12.7 s w P F O S -1 .3.4 12.6 swPFOS-2.1.1 12.2 SwPFOS-2.1.2 swPFOS-2.1.3 SwPFOS-2.1.4 12.0 11.9 12.1 SvvPFOS-2.2.1 SwPFOS-2.2.2 SwPFOS-2.2.3 12.3 12.4 12.1 swPFOS-2.2.4 swPFOS-2.3.1 , swPFOS-2.3.2;, ,, 11.9 15 5 - 15 5 S : . ,& $ & * $ & & & % ; 161 1 evkPFnS-? * M 6:3. swPFOS-3.1.1 swPFOS-3.1.2 swPFOS-3.1.3 swPFOS-3.1.4 S w P F O S .3.2.1 swPFOS-3.2.2 SwPFOS-3.2.3 swPFOS-3.2.4 swPFOS-3.3.1 swPFOS-3.3.2 swPFOS-3.3.3 swPFOS-3.3.4 14.8 14.6 14.8 14.8 13.7 13.4 13.6 13.8 11.9 12.4 12.0 12.4 3M Environm ental Laboratory ' 12.3 12.7 12.6 12.9 11.6 12.0 11.7 n .6 12.2 12.5 12.4 12.3 11.9 11.7 11.7 11.8 12.0 12.1 11.8 11.7 15 2 53-N | ] 14.5 14.3 14.5 14.5 13.4 13.1 13.3 13.5 11.7 12.1 11.7 12.1 12.6 0.25 2.0% 11.7 0.19 1.6% 12.4 0.13 1.0% 11.8 0.10 0.8% 11.9 0.18 1.5% 156 ` ?25% 14.5 0.10 0.7% 13.3 0.17 1.3% 11.9 0.23 1.9% FACT-TCR002 PFOS Solubility of TCR-00017-46 in Seawater. ___________ DAILY AND TOTAL DATA SUMMARIES Day 1 data summary Average: 12,2 ppm Sul Dev: 0.47 %CV: 3.9% Day 2 data summary Average: 11.9 ppm Std Dev: 0,07 %CV: 0.6% (Sample 3 excluded via Q-Test) Day 3 data summary Average: 13.2 ppm Std Dev: 1.30 %CV: 9.8% TOTAL data summary Average: 12.4 ppm Std Dev: 0.71 %CV: 5.7% !*' Greyed /yellowedareas hvebeenSinittd&ni theciicutations. Solubility-Shake Flask Method 6/17/2001 Page 10 of 11 FACT-TCR-002 PFOS in Seawater Shake Flask Method BACK TO MAIN Q-TEST Data Calculations: Sample ID: swPFOS-2.1 swPFOS-2.2 swPFOS-2.3 Sample Cone., Rep1 Sample Cone., Rep2 Sample Cone., Rep3 . 11.8 11.9 ` 15.5 Range: 3.70 Gap: 3.60 Qobs: 0.97 No. observations: 3 Retain? no Exclude sample set swPFOS-2.3 Qobserved = gap/range where "gap" is the difference between the questionable data point and the closest value of the data set, and "range" is the difference between the highest and lowest value of the data set. If Qobserved is > Q-tabulated, then the data point may be excluded with 90% confidence. Q-tabulated for 3 observations (or data points) is 0.88. The samples highlighted in yellow in the above table have Q-observed > 0.88, and were therefore excluded from the reported data.__________________ 3M Environmental Laboratory Solubility, Shake Flask Method, 5/17/2001 FACT-TCR002 (LIMS #E00-1716), Page 51 of 138 Page 11 of 11 FACT-TCR-002 RAW DATA Agilent 1100 HPLC/MSD "Hillary" Acquistion Run: H010131 PFOS in 3.5% NaCI Solution Shake Flask Method Day 1 Raw Data FACT-TCR002 (LIMS #E00-1716), Page 52 of 138 .jjb asw u ir* A MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 01003-07-13 1002.0ppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank lIVlI.CnWul awQliomniiUh TN-A-4740, 04 Dec 00 TM.A-4740 04 Dec 00 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 01003-07-07 50.1ppb PFOS 01003-07-08 75.1ppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 01003-07-11 400.8ppb PFOS 01003-07-12 501 .Oppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 01003-07-07 50.1ppb PFOS 01003-07-08 75.1ppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 01003-07-11 400.8ppb PFOS UiOOO-U/- 14. 501 .Oppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012901-nadPFOS-1.4.1, 100X Oil. Method Blank, SFM 01-31- naclPFOS-1.4.1 01 MEE(MLA) TCR-002, 012901-nadPFOS-1.4.2, 100X Dil. Method Blank, SFM 01-31- nadPFOS-1.4.2 01 MEE(MLA) ' 1 H010131A.M HILL0001.D 91 2 H010131A.M HIU0002.D 91 3 H010131A.M HILL0003.D 13 4 H010131A.M HILL0004.D 13 5 H010131AM hiliooos.d 91 6 H010131A.M HILL0006.D 91 7 H010131A.M HILL0007.D 91 8 H010131AM HILIOUUB.D 1 9 H010131A.M HILL0009.D 2 10 H010131AM HILL0010.D 3 11 H010131.A.M H.i.linnn D 4 12 H010131A.M HIU.0012.D 5 13 H010131AM HILL0013.D 6 14 H010131AM HILL0014.D 7 15 H010131A.M HILL0015.D 8 16 H010131A.M HILL0016.D 9 17 H010131A.M HILL0017.D 10 18 H010131A.M HILL0018.D 11 19 H010131AM HILL0019.D 12 20 H010131A.M HILL0020.D 13 21 H010131A.M HILL0021.D 92 22 H010131A.M HILL0022.D 92 23 H010131AM HILL0023.D 92 24 H010131A.M HILL0024.D 1 25 H010131AM HILL0025.D 2 26 H010131A.M HILL0026.D 3 27 H010131AM HILL0027.D 4 28 H010131A.M HILL0028.D 5 29 H010131A.M HILL0029.D 6 30 H010131AM HILL0030.D 7 31 H010131A.M HILL0031.D 8 32 H010131AM HILL0032.D 9 33 H010131AM HILL0033.D 10 34 H010131AM HILL0034.D 11 35 H010131AM HILL0035.D 12 36 H010131AM HILL0036.D 13 37 H010131AM HILL0037.D 92 38 H010131AM HILL0038.D 92 39 H010131AM HILL0039.D 93 '< V -: 4.124 0.000 4.121 4.121 4.119 4.117 4.118 4.121 4.122 4.118 4.119 4.118 4.121 4.118 4.115 4.122 4.119 4.118 4.119 4.121 4.119 4.121 4.122 4.119 4.119 4.121 4.119 4.121 4.122 4.117 4.118 4.118 4.118 4.118 4.121 4.121 4.118 4.119 0.000 21409.6 0.0 2143601.3 2124774.3 11608.7 12030.3 11730.2 4rtUrtTAUOWOVQUft.W1 2093037.3 2110525.8 2097033.9 2087465.6 2089456.8 2089359.4 2087226.1 2097466.5 2091827.3 2081840.1 2127462.5 2128281.3 11259.9 11279.0 11475.7 2095800.8 2092956.8 2136092.8 2134188.0 2101620.5 2118756.3 2094413.3 2107698.3 2107941.5 2085320.1 2104751.3 2089080.4 2132100.5 11790.3 8487.4 0.0 40 H010131AM HILL0040.D 21 4.117 202277a1.3 Exact Copy of Or: 41 H010131AM HILL0041.D 22 4.119 2012977.0 3M Environm ental Laboratory lia U ia l SoluWj m * ^&k Method ______ 5/2/2001 BACK TO MAIN ' 0.0 0.0 301.1 305.6 0.0 0.0 0.0 269.5 270.5 269.8 268.2 266.3 268.0 268.0 264.3 264.9 264.0 262.9 270.6 277.4 0.0 0.0 0.0 254.9 253.9 255.4 254.6 251.3 254.2 250.6 253.3 253.2 251.0 260.1 254.8 270 5 0.0 0.0 0.0 `- . C 0.000 0.000 4.821 4.821 0.000 0.000 0.000 4.821 4.823 4.822 4.819 4.822 4.821 4.819 4.823 4.822 4.820 4.819 4.820 4.821 0.000 0.000 0.000 4.819 4.819 4.822 4.819 4.821 4.822 4.821 4.819 4.822 4.822 4.822 4.821 4.821 0.000 0.000 0.000 0.0 0.0 993466.1 970509.3 0.0 0.0 0.0 1060946.9 1080061.5 1091921.6 1091357.9 1094229.1 1088254.4 1087986.1 1102227.4 1105173.9 1105860.1 1105371.5 1097313.3 1070927.4 0.0 0.0 0.0 1147396.9 1150438.9 1187485.3 1169935.9 1167190.9 1163371.8 1166273.0 1161204.9 1161693.0 1159443.8 1129470.5 1144288.3 1099943.1 0.0 0.0 0.0 0.0 0.0 250.7 250.7 0.0 0.0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0.0 0.0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0.0 0.0 0.0 A 5.153 5.156 5.206 5.206 5.156 5.160 5.161 5.157 5.152 5.162 5.155 5.161 5.157 5.155 5.159 5.158 5.156 5.232 5.240 5.200 5.163 5.165 5.158 5.155 5.155 5.158 5.156 5.158 5.158 5.161 5.155 5.162 5.162 5.218 5.157 5.164 5.161 5.155 5.162 10335.3 7224.9 22127404.0 21844558.0 8180.2 3006.9 7961.4 12540.2 87037.7 155338.9 283237.4 7311S1 4 1153655.3 1443086.4 2167099.3 2856232.3 6777085.5 10322257.0 12413629.0 22093346.0 4968.3 6091.6 7088.3 8761.4 85318.9 158275.4 294889.3 731035.8 1194338.3 1473480.0 2231440.0 2926687.3 6886002.0 10541540.0 12617936.0 22841106.0 4108.8 7473.4 6551.3 V> 0"- 0.9 0.9 0.0 0.0 0.9 0.9 0.9 1.3 4.0 6.4 10.9 26.8 42.2 52.8 78.4 103.6 256.7 411.4 517.0 1319.8 0.9 0.9 0.9 1.2 3.7 6.1 10.6 25.2 40.9 50.3 76.6 101.0 248.1 411.2 501.1 1346.3 0.9 0.9 0.9 22.1 6.1 0.3 2.0 0.4 1.9 0.7 -1.0 2.6 0.0 250.5 4.821 1126861.6 250.7 5.161 4319.0 1.0 252.9 4.819 1111055.0 250.7 5.156 2599.3 1.0 Page 1 o# 11 FACT-TCR-002 TCR-002, 012901-nac!PFOS-1.4.3, 100X Dil. Method Blank, SFM 01-31naclPFOS-1.4.3 01 MEE(MLA) TCR-002, 012901-nadPFOS-1.4.4, 100X Dil. Method Blank, SFM 01-31naclPFOS-1.4.4 01 MEE(MLA) MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012901-nadPFOS-1.1.1, nadPFOS-1.1.1 100XDI. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.1.2, nadPFOS-1.1.2 100XDB. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.1.3, nadPFOS-1.1.3 100XDB. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.1.4, nadPFOS-1.1.4 100XD. SFM 01-31-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 TCR-002, 012901-nadPFOS-1.2.1, nadPFOS-1.2.1 100XDI. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.2.2, nadPFOS-1.2.2 100XDI. SFM O1-31-01 m E E (M LA ) TCR-002, 012901-nadPFOS-1.2.3, nadPFOS-1.2.3 100XDII. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.2.4, nadPFOS-1.2.4 100XD. SFM 01-31-01 MEE(MLA) MeOH Blank TN-A-4740. 04 Dec 00 TCR-002, 012901-nadPFOS-1.3.1, nadPFOS-1.3.1 100XDB. SFM 01-31-01 MEE(MLA) TCR-002, O12901-nadPFOS-1.3.2, nadPFOS-1.3.2 100X Dil. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.3.3, nadPFOS-1.3.3 100XDII. SFM 01-31-01 MEE(MLA) TCR-002, 012901-nadPFOS-1.3.4, nadPFOS-1.3.4 100XDH. SFM 01-31-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 01003-07-07 SO.Ippb PFOS 01003-07-08 75.1ppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 01003-07-11 400.8ppb PFOS 01003-07-12 501.Oppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4740, 04 Dec 00 MeOH Blank TN-A-4740, 04 Dec 00 42 H010131A.M HILL0042.D 23 43 H010131A.M HILL0043.D 24 44 H010131A.M HIU0044.D 93 45 H010131A.M HILL0045.D 31 46 H010131A.M HIU0046.D 32 47 H010131A.M HILL0047.D 33 48 H010131A.M HILL0048.D 34 49 H010131A.M HILL0049.D 9 50 H010131A.M HILL0050.D 93 51 H010131A.M HILLOOS1.D 93 52 H010131A.M HILL0052.D 35 53 HILL0053.D 36 54 H010131A.M HILL0054.D 37 55 H010131A.M HILL0055.D 38 56 H010131A.M HILL0056.D 94 57 H010131A.M HILL0057.D 39 58 H010131A.M HILL0058.D 40 59 H010131A.M HILL0059.D 41 60 H010131A.M HILL0060.D 42 61 H010131A.M HILL0061.D 9 62 H010131A.M HILL0062.D 94 63 H010131A.M HILL0063.D 94 64 H010131A.M HILL0064.D 94 65 H010131A.M HILL0065.D 1 66 H010131A.M HILL0066.D 2 67 H010131A.M HILL0067.D 3 68 H010131A.M HILL0068.D 4 69 H010131A.M HILL0069.D 5 70 H010131A.M HILL0070.D 6 ' 71 H010131A.M HILL0071.D 7 72 H 0 1 0 1 3 1 A .M H ILL0072.D 8 73 H010131A.M HILL0073.D 9 74 H010131A.M HILL0074.D 10 75 H010131A.M HILL0075.D 11 76 H010131A.M HILL0076.D 12 77 H010131A.M HILL0077.D 13 78 H010131A.M HILL0078.D 95 79 H010131A.M HILL0079.D 95 FACT-TCR002 (UNIS #E00-1716), Page 53 of 138 3M Environmental Laboratory BACK TO MAIN 4.119 2083439.9 259.2 4.819 1121788.5 250.7 5.155 8289.1 1.2 4.119 4.121 2038687.6 12652.4 257.2 0.0 4.820 0.000 1106088.3 0.0 250.7 0.0 4.119 2044713.0 263.8 4.820 1081767.8 250.7 4.118 2043153.5 267.1 4.822 1067474.3 250.7 4.119 2047704.3 263.1 4.820 1086182.9 250.7 4.118 4.121 4.118 4,118 2040932.9 2112425.0 11531.6 8666.6 266.2 251.0 0.0 0.0 4.822 4.822 0.000 0.000 1070219.3 1174724.8 0.0 0.0 250.7 250.7 0.0 0.0 4.118 1995595.9 261.8 4.819 1063811.5 250.7 4.119 2011646.8 265.8 4.819 1056323.1 250.7 4.118 1994192.1 261.7 4.822 1063676.3 250.7 4.118 4.120 1986943.1 9279.7 261.5 o.o 4.822 0.000 1060499.5 0.0 250.7 0.0 4.118 1922033.9 250.0 4.819 1073103.1 250.7 4.118 1988949.3 258.8 4.822 1072507.3 250.7 4.121 1991271.4 261.3 4.821 1063607.5 250.7 4.120 4.121 4.121 4.119 4.122 4.120 4.119 4.118 4.119 4.120 4.119 4.118 4.119 4.119 4.120 4.115 4.120 4.120 4.120 4.119 1982020.0 2055678.9 9943.1 11681.8 11540.1 2041874.0 2069020.8 2081127.1 2070209.8 2059409.9 2080276.8 2077642.6 2084619.8 2089444.1 2067633.0 2096577.1 2113937.3 2036590.3 8770.0 11212.9 262.7 249.3 0.0 0.0 0.0 245.9 245.7 244.2 244.3 243.5 245.4 244.2 246.0 245.3 247.4 255.5 255.7 253.5 0.0 0.0 4.821 1052995.8 4.821 1150774.1 0.000 0.0 0.000 0.0 0.000 0.0 4.820 1159008.5 4.819 1175189.9 4.822 1189579.9 4.819 1182606.9 4.821 1180256.6 4.820 1183280.5 . 4.819 1187313.3 4.819 1182561.1 4.819 1188650.3 4.821 1166542.9 4.822 1145464.9 4.820 1154010.9 4.821 . 1121090.4 0.000 0.0 0.000 0.0 250.7 250.7 0.0 0.0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 ocn ~1I 250.7 250.7 250.7 250.7 250.7 0.0 0.0 5.163 5.158 4842.2 5851.6 1.0 0.9 5.156 5915846.0 227.0 5.162 5851699.5 227.5 5.156 5827699.0 222.4 5.162 5.158 5.162 5.161 5990611.0 2899438.8 1726.1 6133.9 232.7 98.9 0.9 0.9 5.155 5222047.5 202.2 5.155 5201276.0 202.9 5.162 5192852.5 201.0 5.161 5.156 5269990.5 6002.4 204.9 0.9 5.155 4172225.8 158.1 5.161 4317565.0 164.0 5.157 4187921.5 160.2 5.157 5.157 0.000 5.156 0.000 5.156 5.155 5.162 5.156 5.157 5.156 5.155 5.155 5.155 5.157 5.159 5.219 5.164 5.157 5.155 4194090.0 2847996.0 0.0 6434.6 0.0 8746.7 80179.2 150817.4 286563.4 720880.0 1170613.4 1480991.4 2180932.8 2894335.8 6910958.0 10501242.0 12580502.0 23094802.0 7282.3 6371.0 162.2 99.1 0.0 0.9 0.0 1.2 3.5 5.8 10.2 24.6 39.4 49.6 73 5 97.5 247.4 402.7 494.2 1314.3 0.9 0.9 -1.3 -1.1 15.3 2.3 -2.1 -1.7 -0.9 -22 -2.7 -1.2 0.5 -1.4 Solubflity, Shake Flask Method 5/Z/200Y Page 2 oi 11 FACT-TCR002 (LIMS #E00-1716), Page 54 of 138 FACT-TCR-002 RAW DATA Agilent 1100 HPLC/MSD "Hillary" Acquistion Run: H010205 ft 'S T u n ^ lj. MeOH Blank MeOH Blank 01003-07-13 01003-07-13 MeOH Blank MeOH Blank MeOH Blank u iuuo-ur-y i 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 MeOH Blank MeOH Blank MeOH Blank 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 MeOH Blank MeOH Blank MeOH Blank nadPFOS-2.4.1 naclPFOS-2.4.2 TN-A-4755. 05 Feb 01. exp:2005. TN-A-4755. 05 Feb 01, exp:2005. 1002.0ppb PFOS 1002.0ppb PFOS TN-A-4755. 05 Feb 01. exp:2005. TN-A-4755. 05 Feb 01. exp:2005. TN-A-4755. 05 Feb 01, exp:200S. r\_l. frtPrAwtj 2.5ppb PFOS 5ppb PFOS 10DDb PFOS 25ppb PFOS 40ppb PFOS 50.1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb P F O S 400.8ppb PFOS 501.Oppb PFOS 1002.0ppb PFOS TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755. 05 Feb 01, exp:2005. Oppb PFOS 2.5ppb PFOS 5ppb PFOS 10ppb PFOS 25ppb PFOS 40ppb PFOS 50.1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.Oppb PFOS 1002.Oppb PFOS TN-A-4755, 05 Feb 01. exp:2005. TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01. exp:2005. TCR-002, 012901-nadPFOS-2.4.1,100X Oil. Method Blank, SFM 02-01-01 MEE(MLA) TCR-002. 012901-nadPFOS-2.4.2,100X Oil. Method Blank. SFM 02-01-01 MEE(MLA) 3M Environmental Laboratory PFOS in 3.5% NaCI Solution Shake Flask Method Day 2 Raw Data T=TC ; 1 H010205A.M HILL0001.D 91 4.123 41176.2 2 H010205A.M HILL0002.D 91 4.119 9599.3 3 H010205A.M HILL0003.D 13 4.121 1774643.6 4 H010205A.M HILL0004.D 13 4.118 1808354.9 5 H010205A.M HILL0005.D 91 4.121 9271.7 6 H010205A.M HILL0006.D 91 4.118 12252.3 7 H010205A.M HILL0007.D 91 A i-inir9n5A m Mil I nnna D 1 4.121 4.120 13494.0 1837110.1 9 H010205A.M HILL0009.D 2 4.119 1829781.3 10 H010205A.M HILL0010.D 3 4.122 1874887.3 11 H010205A.M HILL0011.D 4 4.119 1836290.8 12 H010205A.M HILL0012.D 5 4.118 1854312.5 13 H01020SA.M HILL0013.D 6 4.120 1834995.5 14 H010205A.M HILL0014.D 7 4.117 1865783.1 15 H010205A.M HILL0015.D 8 4.121 1861396.1 16 H010205A.M HILL0016.D 9 4.120 1811954.0 17 H010205A.M HILL0017.D 10 4.121 1848057.6 18 H010205A.M HILL0018.D 11 4.118 1811635.1 19 H010205A.M HILL0019.D 12 4.119 1874128.5 20 H010205A.M HILL0020.D 13 4.118 1919553.6 21 H010205A.M HILL0021.D 92 4.119 13717.4 22 H010205A.M HILL0022.D 92 4.121 12992.0 23 H010205A.M HILL0023.D 92 4.120 12346.2 24 H010205A.M HILL0024.D 1 4.119 1888101.0 25 H010205A.M HILL0025.D 2 4.122 1894234.6 26 H010205A.M HILL0026.D 3 4.121 1897593.9 27 H010205A.M HILL0027.D 4 4.117 1880741.9 28 H010205A.M HILL0028.D 5 4.121 1869055.4 29 H010205A.M HILL0029.D 6 4.119 1881326.5 30 H010205A.M HILL0030.D 7 . 4.120 1896198.5 31 H010205A.M HILL0031.D 8 4.121 1845975.0 32 H010205A.M HILL0032.D 9 4.119 1871880.4 33 H010205A.M HILL0033.D 10 4.121 1880987.0 34 H010205A.M HILL0034.D 11 4.118 1871845.4 35 H010205A.M HILL0035.D 36 HG102C5A.M HILLG03S.D 12 4ts0j 4.118 4 118 1881822.5 1895748.5 37 H010205A.M HILL0037.D 92 4.121 13125.2 38 H010205A.M HILL0038.D 92 4.118 13076.4 39 H010205A.M HILL0039.D 93 4.119 8488.4 40 H010205A.M HILL0040.D 21 4.119 1943546.6 41 H010205A.M HILL0041.D 22 4.119 1900756.8 Sotubffity, Shake Rack Method 5/2/2001 BACK TO MAIN 0.0 0.0 296.4 298.3 0.0 0.0 0.0 288.1 281.8 286.5 278.0 281.4 275.9 277.9 272.6 265.8 268.6 270.2 271.6 283.3 0.0 0.0 0.0 264.0 261.4 256.3 256.5 256.7 258.3 258.7 250.8 256.5 255.7 263.3 260.2 268.2 0.0 0.0 0.0 0.000 0.000 4.821 4.819 0.000 0.000 0.000 4.820 4.819 4.822 4.819 4.822 4.821 4.821 4.821 4.820 4.821 4.822 4.819 4.819 0.000 0.000 0.000 4.819 4.822 4.821 4.821 4.821 4.820 4.821 4.821 4.820 4.821 4.822 4.819 4.822 0.000 0.000 0.000 0.0 0.0 873165.5 884255.3 0.0 0.0 0.0 930048.6 947156.8 954459.8 963263.3 960941.4 969887.6 979183.1 995988.6 994257.7 1003504.8 977732.8 1006423.3 9B8284.3 0.0 0.0 0.0 1042922.9 1057020.1 1079665.3 1069173.0 1061883.6 1062443.1 1068797.5 1073550.4 1064144.0 1072810.0 1036707.3 1054772.8 im n im a 0.0 0.0 0.0 0.0 0.0 250.7 250.7 0.0 0.0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0.0 0.0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0.0 0.0 0.0 5.153 5.156 5.263 5.253 5.158 5.162 5.157 5.156 5.156 5.158 5.155 5.162 5.157 5.161 5.158 5.157 5.157 5.232 5.226 5.225 5.155 5.158 5.156 5.156 5.158 5.157 5.161 5.157 5.156 5.157 5.157 5.156 5.255 5.162 5.204 5.162 5.157 5.162 5.155 30162.1 3212.3 19985400.0 20450016.0 18446.0 4197.1 7831.2 11402.0 86371.4 142977.5 266736.0 69703.3 1123236.8 1391739.1 2083089.4 2734341.5 6425435.5 9833563.0 11816095.0 21038770.0 6349.7 13127.0 9888.0 12737.3 91752.4 161460.5 286824.4 718901.5 1151040.3 . 1455018.6 2161271.8 2786907.8 6624594.0 10062423.0 12373037.0 220237920 13229.0 7287.5 3465.8 0.0 0.0 1124.4 1140.0 0.0 0.0 0.0 0.0 1.7 4.1 9.1 26.9 44.2 54.8 81.9 108.8 263.2 427.5 507.1 1022.9 0.0 0.0 0.0 0.0 1.6 4.0 8.7 25.0 41.2 52.4 78.7 103.5 253 3 411.2 506.6 10276 0.0 0.0 0.0 -12.5 -0.4 2.8 4.6 4.7 3.3 1.1 2.6 i.i 26 271.9 4.819 1042521.5 250.7 5.155 8906.6 0.0 263.2 4.819 1053132.4 250.7 5.155 16638.0 0.0 Pg3of11 FACT-TCR-002 TCR-002, 012901-nadPFOS-2.4.3,100X Dil. Method Blank, SFM 02-01-01 naclPFOS-2.4.3 MEE(MLA) TCR-002, 012901-naclPFOS-2.4.4,100X Dil. Method Blank, SFM 02-01-01 nadPFOS-2.4.4 MEE(MLA) MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-2.1.1,100X nadPFOS-2.1.1 Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.1.2,100X nadPFOS-2.1.2 Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.1.3,100X nadPFOS-2.1.3 Dil. SFM 02-01-01 MEE(MIA) TCR-002, 012901-nadPFOS-2.1.4,100X nadPFOS-2.1.4 Dil. SFM 02-01-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. MeOH Blank TN^A-4755, 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-2.2.1,100X nadPFOS-2.2.1 Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.2.2,100X nadPFOS-2.2.2. Dii. SFM 02-ui-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.2.3,100X nadPFOS-2.2.3 Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.2.4, 100X nadPFOS-2.2.4 Dil. SFM 02-01-01 MEE(MLA) MeOH Blank TN-A-4755. 05 Feb 01, exp:200S. TCR-002, 012901-nadPFOS-2.3.1, 100X nadPFOS-2.3.1 Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.3.2, 100X nadPFOS-2.3.2 DU. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.3.3, 100X nadPFOS-2.3.3 Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.3.4, 100X nadPFOS-2.3.4 Dil. SFM 02-01-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4755. 05 Feb 01, exp:2005. MeOH Blank TN-A-4755. 05 Feb 01, exp:2005. MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 01003-07-07 50.1 ppb PFOS 01003-07-08 75.1ppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 01003-07-11 400.8ppb PFOS 01003-07-12 501.Oppb PFOS 01003-07-13 1002.0ppb PFOS MeOH Blank TN-A-4755, 05 Feb 01. exp:2005. MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. 42 H010205A.M HILL0042.D 43 H010205A.M HILL0043.D 44 H010205A.M HILL0044.D 45 H010205A.M HILL0045.D 46 H010205A.M HILL0046.D 47 H010205A.M HILL0047.D 48 H010205A.M HILL0048.D 49 H010205A.M HILL0049.D 50 H010205A.M HILL0050.D 51 H010205A.M HILL0051.D 52 H010205A.M HILL0052.D 53 hul G2G5A.fvi HIL.LCC53.0 54 H010205A.M HILL0054.D 55 H010205A.M HILL0055.D 56 H010205A.M HILL0056.D 57 H010205A.M HILL00S7.D 58 H010205A.M HILL0058.D 59 H010205A.M HILL0059.D 60 H010205A.M HILL0060.D 61 H010205A.M HILL0061.D 62 H010205A.M HILL0062.D 63 H010205A.M HILL0063.D 64 H010205A.M HILL0064.D 65 H010205A.M HILL0065.D 66 H010205A.M HILL0066.D 67 H010205A.M HILL0067.D 68 H010205A.M HILL0068.D 69 H010205A.M HILL0069.D 70 H010205A.M HILL0070.D 71 H010205A.M HILL0071.D 72 H010205A.M HILL0072.D 73 H010205A.M HILL0073.D 74 H010205A.M HILL0074.D 75 H010205A.M HILL0075.D '76 H010205A.M HILL0076.D 77 H010205A.M HILL0077.D 78 H010205A.M HILL0078.D 79 H010205A.M HILL0079.D FACT-TCR002 (LIMS #E00-1716), Page 55 of 138 3M Environmental Laboratory BACK TO MAIN 23 4.117 1933177.9 272.1 4.821 1036265.4 250.7 5.161 5505.6 0.0 24 4.120 1981495.4 276.1 4.820 1046513.6 250.7 5.156 5787.1 93 4.118 8589.0 0.0 0.000 0.0 0.0 5.162 1716.6 0.0 0.0 31 4.118 1954489.6 280.0 4.819 1018035.8 250.7 5.155 5360243.5 214.2 32 4.119 1995386.6 283.3 4.820 1027304.7 250.7 5.156 5515177.0 218.6 33 4.119 1973433.0 282.4 4.819 1019282.8 250.7 5.155 5645223.0 225.9 34 4.119 1916815.9 275.8 4.820 1013776.3 250.7 5.156 6158368.0 249.0 9 4.120 1907227.4 255.0 4.820 1090911.0 250.7 5.157 2803938.5 101.5 1.3 93 4.118 13009.6 0.0 .000 0.0 0.0 5.161 2060.1 0.0 93 4.118 13189.6 0.0 0.000 0.0 0.0 5.162 2302.3 0.0 35 4.119 1966392.4 280.2 4.820 1023456.4 250.7 5.156 7113649.5 287.2 XUa 4 IIS *eocene o 0703 4.S19 1023781.8 250.7 * it* * 999/1 n 9/17 9 37 4.117 1880691.9 267.8 4.821 1024368.3 250.7 5.160 5134239.0 203.4 38 4.118 1976344.5 280.9 4.819 1026108.8 250.7 5.155 5143755.5 203.4 93 4.121 12975.6 0.0 0.000 0.0 0.0 5.158 7253.0 0.0 39 4.119 1949027.0 276.7 4.819 1027143.3 250.7 5.155 4691219.0 184.5 40 4.121 1899727.9 270.5 4.822 1024350.2 250.7 5.158 4632432.0 182.6 41 4.118 1893792.4 267.5 4.822 1032577.4 250.7 5.162 4642529.5 181.5 42 4.119 1925417.8 272.4 4.819 1031034.4 250.7 5.155 4582600.5 179.4 9 4.120 1878686.8 250.2 4.821 1095013.0 250.7 5.157 2811571.0 101.4 1.2 93 4.120 9121.0 0.0 0.000 0.0 0.0 5.157 7782.5 0.0 94 4.122 12767.6 0.0 0.000 0.0 0.0 5.158 6500.7 0.0 94 4.119 8712.4 0.0 0.000 0.0 0.0 5.155 5702.5 0.0 1 4.121 1859950.3 243.4 4.821 1114555.1 250.7 5.158 8455.8 0.0 2 4.120 1851090.0 240.7 4.820 1121590.6 250.7 5.156 88443.7 1.3 3 4.117 1863924.8 238.1 4.821 1141707.3 250.7 5.161 158514.7 3.6 4 4.122 1858022.6 240.7 4.822 1125752.9 250.7 5.158 268391.2 7.6 -24.4 5 4.121 1826781.8 236.4 4.821 1126887.1 250.7 5.157 711128.3 23.2 -7.7 6 4.120 1873868.3 246.3 4.821 1109607.5 250.7 5.157 1137256.0 38.9 -3.0 7 4.123 1789390.1 230.6 4.820 1131681.9 250.7 5.152 1464379.4 49.7 -0.8 8 4.119 1851169.0 239.7 4.820 1126242.4 250.7 5.156 2179371.0 75.6 0.5 9 4.121 1895202.0 246.7 4.822 1120633.3 250.7 5.158 2826115.3 99.5 -0.7 10 4.122 1881744.3 242.8 4.822 1130160.4 250.7 5.158 6735983.0 244.0 -2.6 11 4.120 1806523.5 240.8 4.821 1093945.6 250.7 5.220 10220093.0 394.5 -1.6 12 4.118 1874440.5 248.7 4.822 1099099.3 250.7 5.211 12558129.0 492.0 -1.8 13 4.121 1874729.0 252.1 4.821 1084462.3 250.7 5.213 22272594.0 977.2 -2.5 94 4.119 13199.4 0.0 0.000 0.0 0.0 5.156 10110.2 0.0 94 4.121 12154.5 0.0 0.000 0.0 0.0 5.165 4001.3 0.0 Solubility, Shake Flask Method 5/2/2001 Page 4 of 11 FACT-TCR-002 RAW DATA Agilent 1100 HPLC/MSD "Hillary" Acquistion Run: H010206 PFOS in 3.5% NaCI Solution Shake Flask Method Day 3 Raw Data FACT-TCR002 (LIMS #E00-1716), Page 56 of 138 MeOH Blank MeOH Blank 01003-07-13 01003-07-13 MeOH Blank MeOH Blank MeOH Blank 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 MeOH Blank MeOH Blank MeOH Blank 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 n -i n m _ n 7 _ - l9 01003-07-13 MeOH Blank MeOH Blank MeOH Blank naclPFOS-3.4.1 nadPFOS-3.4.2 TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. 1002.0ppb PFOS 1002.0ppb PFOS TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. Oppb PFOS 2.5ppb PFOS 5ppb PFOS IOppb PFOS 25ppb PFOS 40ppb PFOS 50.1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501. Oppb PFOS 1002.Oppb PFOS TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755. 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. Oppb PFOS 2.5ppb PFOS 5ppb PFOS 10ppb PFOS 25ppb PFOS 40ppb PFOS 50.1ppb PFOS 75.1ppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501 Oppb PFOS 1002.0ppb PFOS TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. TCR-002, 012901-naciPFOS-3.4.1, 100X Dll. Method Blank, SFM 02-02-01 MEE(MLA) TCR-002, 012901-naclPFOS-3.4.2,100X Oil. Method Blank. SFM 02-02-01 MEE(MLA) 1 H010206A.M HILL0001.D 2 H010206A.M HILL0002.D 3 HO10206A.M HILL0003.D 4 H010206A.M HILL0004.D 5 H010206A.M HILL0005.D 6 H010206A.M HILL0006.D 7 H010206A.M HILL0007.D 8 H012A,m HLL0005.D 9 H010206A.M HILL0009.D 10 H010206A.M HILL0010.D 11 H010206A.M HILL0011.D 12 H010206A.M HILL0012.D 13 H010206A.M HILL0013.D 14 H010206A.M HILL0014.D 15 H010206A.M H1LL0015.D 16 H010206A.M HILL0016.D 17 H010206A.M HILL0017.D 18 H010206A.M H1L.L0018.D 19 H010206A.M HILL0019.D 20 H010206A.M HILL0020.D 21 H010206A.M HIU.0021.D 22 H010206A.M HILL0022.D 23 H010206A.M HILL0023.D 24 H010206A.M H IL L0024.D 25 H010206A.M HILL0025.D 26 H010206A.M HILL0026.D 27 H010206A.M HILL0027.D 28 H010206A.M HILL0028.D 29 H010206A.M HILL0029.D 30 H010206A.M HILL0030.D 31 H010206A.M HILL0031.D 32 H010206A.M HILL0032.D 33 H010206A.M HILL0033.D 34 H010206A.M HILL0034.D 35 H010206A.M HILL0035.D 36 H010206A.M HILL036.D 37 H010206A.M HILL0037.D 38 H010206A.M HILL0038.D 39 H010206A.M HILL0039.D 95 95 13 13 95 95 95 4 2 3 4 5 6 7 8 9 10 11 12 13 96 96 96 1 2 3 4 5 6 7 8 9 10 11 12 13 96 96 97 40 H010206AM HILL0040.D 51 41 H010206A.M HILL0041.D 52 4.102 4.104 4.108 4.108 4.105 4.105 4.105 4.104 4.106 4.106 4.106 4.108 4.105 4.104 4.106 4.106 4.106 4.104 4.104 4.102 4.107 4.105 4.104 4.107 4.105 4.105 4.108 4.104 4.105 4.106 4.106 4.105 4.106 4.106 4.104 4.104 4.107 4.104 4.107 47304.4 9621.8 1891799.6 1887421.0 13291.9 13218.0 12931.8 1870716.5 1907032.1 1843009.6 1847886.0 1841950.1 1852270.8 1849483.9 1833357.3 1780889.1 1870953.8 1863719.8 1820228.4 12848.0 12476.6 12057.4 1840212.0 1846254.5 1865722.9 1863265.3 1894610.1 1861333.8 1830163.8 1851626.5 1833460.3 1855395.4 1858516.4 1891111.4 r1o r n e |rWa.a4 12090.8 11984.1 11526.1 4.108 1926670.8 4.106 2009192.8 5M Environmental laboratory Solubility, Shake Flask Method 5/2/2001 BACK TO MAIN 0 .0 0 .0 299.3 288.1 0 .0 0 .0 0 .0 266.2 268.4 267.0 264.8 264.4 262.6 262.2 263.2 261.5 251.6 272.3 267.6 266.8 0 .0 0 .0 0 .0 257.8 256.1 253.7 257.9 262.2 258.4 252.4 256.3 253.8 256.2 262.0 265.7 070 O 0 .0 0 .0 0.0 0 .0 0 0 0 .0 0 0 4.822 4.823 0 .0 0 0 0 .0 0 0 0 .0 0 0 4.822 4.821 4.821 4.820 4.822 4.820 4.822 4.820 4.820 4.820 4.822 4.822 4.820 0 .0 0 0 0.000 0 .0 0 0 4.821 4.820 4.819 4.822 4.822 4,819 4.821 4.820 4.819 4.821 4.821 4.822 A R 77 0 .0 0 0 0 .0 0 0 0 .0 0 0 0 .0 0 .0 967438.5 1002759.7 0 .0 0.0 0 .0 1039861.1 1066850.1 1092983.6 1065255.5 1069764.6 1073389.1 1081077.6 1075265.0 1072851.6 1083292.4 1051607.1 1065822.9 1044313.8 0 .0 0 .0 0 .0 1092359.3 1103289.0 1125402.9 1105801.0 1105694.1 1102618.5 1109924.9 1105607.3 1105475.6 1108144.0 1085765.9 1089443.1 1045348.4 0 .0 0 .0 0 .0 0 .0 0 .0 250.7 250.7 0 .0 0 .0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0 .0 0 .0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0 .0 0 .0 0 .0 5.153 5.162 5.208 5.208 5.155 5.156 5.155 5.162 5.157 5.157 5.156 e 9 . CoO 5.156 5.162 5.156 5.156 5.240 5.183 5.211 5.180 5.158 5.155 5.162 5.157 5.156 5.155 5.158 5.162 5.155 5.157 5.156 5.155 5.157 5.241 5.197 5.169 5.165 5.161 0 .0 0 0 6427.4 1366.8 22423620.0 21458074.0 10494.2 3099.5 7381.7 12818.6 86415.2 158469.1 273021.3 17W71U04"4*s1/.0v 1155762.5 1429296.4 2158808.0 2797833.8 6612530.5 10170355.0 12424400.0 22065096.0 3335.9 6796.1 6750.2 12639.4 89759.2 159703.8 268012.8 713836.3 1132725.6 1441188.8 2124345.5 2806380.8 6668410.0 9982846.0 12576619.0 22259990.0 6525.8 6927.2 0 .0 0.1 0.1 1538.4 1251.5 0.1 0.1 0.1 0.6 3.3 5.7 100 25.S 42.1 51.8 792 103.5 252.6 420.9 523.9 1219.6 0.1 0.1 0.1 0.6 3.3 5.6 9.5 25.2 40.1 50.8 75.7 100.7 248.7 397.2 517.8 1238.9 0.1 0.1 0 .0 0 .0 0 .0 12.3 -5.0 0.3 0.1 1.5 0.7 0.5 -0.7 -0.9 3.4 0 .0 278.3 4.823 1059642.9 250.7 5.152 8463.6 0.5 290.4 4.820 1058807.8 250.7 5.156 3730.3 0.3 p *a# 5 of11 FACT-TCR-002 TCR-002, 012901-nadPFOS-3.4.3,100X Dil. Method Blank, SFM 02-02-01 nadPFOS-3.4.3 MEE(MLA) TCR-002, 012901-nadPFOS-3.4.4, 100X Dil. Method Blank, SFM 02-02-01 nadPFOS-3.4.4 MEE(MLA) MeOH Blank TN-A-4755, 05 Feb 01. exp:2005. TCR-002, 012901-nadPFOS-3.1.1, 100X nadPFOS-3.1.1 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3.1.2, 100X nadPFOS-3.1.2 Dil. SFM 02-02-01 MEE(MLA) TCR-002. 012901-nadPFOS-3.1.3 ,100X nadPFOS-3.1.3 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3.1.4 ,100X nadPFOS-3.1.4 Dil. SFM 02-02-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-3.2.1 , 100X nadPFOS-3.2.1 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3.2.2,100X nadFFOS-3.2.2 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3,2.3,100X nadPFOS-3.2.3 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3.2.4, 100X n acIP F O S -3 .2 .4 Dil. SFM 02-02-01 MEE(MLA) MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-3.3.1, 100X nadPFOS-3.3.1 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3.3.2,100X nadPFOS-3.3.2 Dil. SFM 02-02-01 MEE(MLA) TCR-002, 012901-nadPFOS-3.3.3, 100X nadPFOS-3.3.3 Dil. SFM 02-02-01 MEE(MLA) TCR-002. 012901-nadPFOS-3.3.4,100X nadPFOS-3.3.4 Dil. SFM 02-02-01 MEE(MLA) 01003-07-09 100.2ppb PFOS, CCV MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 01003-07-04 10ppb PFOS 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 01003-07-07 SO.Ippb PFOS 01003-07-08 75.1ppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 01003-07-11 400.8ppb PFOS 01003-07-12 501 .Oppb PFOS 01003-07-13 1002.Oppb PFOS MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. MeOH Blank TN-A-4755, 05 Feb 01, exp:2005. 42 H010206A.M HILL0042.D 53 43 H010206A.M HILL0043.D 44 H010206A.M HILL0044.D 54 97 45 H010206A.M HILL0045.D 61 46 H010206A.M HILL0046.D 62 47 H010206A.M HILL0047.D 63 48 H010206A.M HILL0048.D 64 49 H010206A.M HILL0049.D 9 50 H010206A.M HILL0050.D 97 51 H010206A.M HILL0051.D 97 52 H010206A.M HILL0052.D 65 53 HQ1Q206A M HILL0053.D 66 54 H010206A.M HILL0054.D 67 55 H010206A.M HILL0055.D 56 H010206A.M HILL0056.D 68 97 57 H010206A.M HILL0057.D 69 58 H010206A.M HILL0058.D 70 59 H010206A.M HILL0059.D 71 60 H010206A.M HILL0060.D 61 H010206A.M HILL0061.D 62 H010206A.M HILL0062.D 63 H010206A.M HILL0063.D 64 H010206A.M HILL0064.D 65 H010206A.M HILL0065.D 66 H010206A.M HILL0066.D 67 H010206A.M HILL0067.D 68 HQ10206A.M HILL0068.D 69 H010206A.M HILL0069.D 70 H010206A.M HILL0070.D 71 H010206A.M HILL0071.D 72 H010206A.M HILL0072.D 73 H010206A.M HILL0073.D 74 H010206A.M HILL0074.D 75 H010206A.M HILL0075.D 76 H010206A.M HILL0076.D 77 H010206A.M HILL0077.D 78 H010206A.M HILL0078.D 79 H010206A.M HILL0079.D 72 9 98 98 98 1 2 3 4 5 6 7 8 9 10 11 12 13 98 98 FACT-TCR002 (LIMS #E00-1716), Page 57 of 138 3M Environmental L aboratory BACK TO MAIN 4.106 2025762.9 292.3 4.821 1060565.4 250.7 5.157 7621.1 0.4 4.105 4.106 1979531.4 11598.8 288.6 0.0 4.104 1986989.8 298.8 4.104 1903896.9 281.9 4.105 1903997.0 283.7 4.107 4.107 0,000 0.000 2028305.4 1828271.5 0.0 0.0 305.1 250.2 0.0 0.0 4.104 1998596.6 297.3 4.105 2000593.5 298.4 4.107 2000672.9 299.4 4.105 0.000 1891713.3 0.0 280.7 0.0 4.106 1896904.9 285.8 4.104 1956381.6 295.0 4.106 1902701.1 283.0 4.105 4.106 0.000 4.104 0.000 4.105 4.105 4.104 4.104 4.106 4.105 4.106 4.106 4.104 4.108 4.104 4.105 4.107 0.000 4.106 1894214.3 1756132.8 0.0 11876.2 0.0 1780994.1 1755939.4 1814153.1 1790839.6 1788983.0 1770309.1 1832118.0 1799289.3 1739000.9 1788427.6 1755005.4 1787929.6 1830473.3 0.0 11785.3 284.8 242.7 0.0 0.0 0.0 245.2 236.5 241.7 239.8 243.8 240.0 248.1 243.7 235.3 246.5 248.1 244.5 263.4 0.0 0.0 4.819 1049618.8 250.7 0.000 0.0 0.0 4.822 1017566.9 250.7 4.822 1033535.4 250.7 4.820 1027231.4 250.7 4.821 4.821 0.000 0.000 1017373.9 1118280.6 0.0 0.0 250.7 250.7 0.0 0.0 4.819 1028671.3 250.7 4.819 1025976.1 250.7 4.821 1022749.9 250.7 4.819 1031479.1 250.7 0.000 0.0 0.0 4.821 1015830.9 250.7 4.822 1015064.3 250.7 4.820 1028884.6 250.7 4.820 4.820 0.000 0.000 0.000 4.819 4.819 4.822 4.821 4.821 4.820 4.821 4.820 4.819 4.822 4.822 4.819 4.822 0.000 0.000 1017989.3 1107496.5 0.0 0.0 0.0 1111747.3 1136281.3 1148491.8 1143103.6 1122996.1 1129011.3 1130353.5 1129984.5 1131132.6 1110432.5 1082374.3 1119100.9 1063516.4 0.0 0.0 250.7 250.7 0.0 0.0 0.0 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 250.7 0.0 0.0 5.156 5.157 3744.8 5353.4 0.3 0.1 5.162 5394307.0 217.1 5.161 5387695.5 213.3 5.156 5409418.0 215.6 5.158 5.157 5.155 5.162 5367317.5 2840861.5 7618.2 8197.7 216.0 100.7 0.1 0.1 5.155 5247156.5 208.4 5.155 5202058.5 207.1 5.157 5144285.5 205.3 5.155 5.155 5024824.0 6650.2 198.5 0.1 5.157 4756814.0 190.3 5.162 4726155.5 189.2 5.156 4696616.0 185.3 5.156 5.156 5.155 0.000 5.156 5.156 5.155 5.161 5.161 5.157 5.156 5.157 5.156 5.155 5.194 5.162 5.155 5.193 5.156 5.156 4754382.0 2809160.5 6589.1 0.0 5586.4 12076.9 88457.2 156107.9 274913.9 709161.8 1158373.6 1436545.9 2169807.0 2826039.5 6744845.5 10142755.0 12195626.0 22142466.0 2995.9 1708.9 189.8 100.6 0.1 0.0 0.1 0.6 3.1 5.4 9.4 24.6 40.1 49.8 75.6 99.0 251.3 406.0 483.6 1185.0 0.1 0.1 0.5 0.4 0.0 0.0 7.7 -5.7 -1.9 0.0 -0.7 0.6 -1.2 0.3 1.3 -3.5 0.0 SofubWty, Shake F lw k Method 5/2/2001 Page 6 of 11 BACK TO MAIN FACT*TCR-002 TCR-002. 012901-naclPFOS-1.1.1,100X , naclPFOS-1.1.1 D|| g p y 01-31-01 MEE(MLA) PFOS in 3.5% NaCI Solution Day 1 Hillary. H010131 s mmSMRisis 45 -'H010131A.M HILL0045.D ' 31 5.156 . 5915846.0 ' 227.0 . ' 22.7 22.2 22.3 TCR-002, 012901-naclPFOS-1.1.2,100X nadPFOS-1.1.2 D]| SFM 01-31-01 MEE(MLA) 46 H010131A.M HILL0046.D 32 5.162 ' ' 5851699.5 .-227.5 -, , 22.8 . 22.3 'v 0.45 ,, TCR-002, 012901-naclPFOS-1.1.3, 100X "duP FG 3-1.1.3 D|| s p y 01-31-01 MEE(MLA) 47 - H010131A.M HILL0047.D 33 5.156 5827699.0 222.4 22.2 21.7 2.0% TCR-002, 012901-naclPFOS-1.1 4 , 100X> naclPFOS-1.1.4 ! ' UH. orivi u r v4r v I uI*IcUc.H/ Hu IiUa\/ ...V'':: . > 48 ' H010131AM HILL0048 D T- TCR-002, 012901-naclPFOS-1.2.1,100X 52 .` H010131A.M HIL.L0052.D > nadPFOS-1.2.1 Dl| 3 F m 01-31-01 MEE(MLA) ' .' <t Q TCR-002, 012901-nadPFOS-1.2.2,100X nadPFOS-1.2.2 Dj) gFM 01-31-01 MEE(MLA) <0 +# nj Q TCR-002, 012901-nadPFOS-1.2.3, 100X nadPFOS-1.2.3 M SFM 01-31-01 MEE(MLA) a 2 E TCR-002, 012901-nadPFOS-1,2.4,100X <0 nadPFOS-1.2.4 D j| s f m 01-3T-01 MEE(MLA) w .. 53 H010131A.M HILL0053.D 54 H010131A.M HILL0054.D 55 H010131A.M HILL0055.D TCR-002, 012901-nadPFOS-1.3.1, 100X ' ' 57 , .,H010131A.M HILL0057.D nadPFOS-1.3.1 q j gFM 01-31-01 MEE(MLA) \' 34 35 36 37 38' 39 5.162 5990611.0 1 232.7 ' < 23 3 5 155 5222047.5 202.2 20.2 5.155 5201276.0 ; '-l-"' 2 6 2 .9 ; ' - ' ; - :';- :20. 3 ' 5 162 1 '5192852.5 2010 / 20(1 5 161 , ,5269990.5 l 204.9 , ' S ; i > ' :.;V20.5 5,155 " 4172225.8 .^7: :,v;:';i5 8 ;i'-/-. S'15.8 ' *-V . . . . v f ""*>), ' .>. 22.8 19.8 :r.:; ; y 19.9 . .. 19 9 0.17 19.7 09% 20.1 15.5 15.8 TCR-002. 012901-nadPFOS-1.3.2; 100X' 58 nadPFOS-1.3.2 D(| spM 01. 31. 01 MEE(MLA) " , ' '-'in-:;: ." h.';:.:-.' TCR-002, 012901-nadPFOS-1.3.3, 1 0 0 X , nadPFOS-1,3.3 Di| 3 F m 01-31-01 MEE(MLA) 59 - , - ------------ :------------------------------ -------------------- : ----------------------- TCR-002, 012901-nadPFO5-1 3 4 ,,1 0 0 X ,-,i nadPFOS-1 3 4 M SFM 01. 31:0 1 MEEJMLA) ---- H010131.A:M HILL0058.D . ; H010131A.M HILL0059 D 40 : j 5.161 : ^ j 4 3 1 7 5 6 5 fd ;'-i Y^r ',` V v,.i ,41 ' * V 5.157' y @ i 8 7 9 2 l 5 ; : 164 0 . 16 4 ,,1 "V , <4* - H 1 6 0 2 '-' 160 16.1 15.7 0.26 1.6% -15,9 , : % c 6' ' ' , ,, i . - FACT-TCR002 (LIMS #E00-1716), Page 58 of 138 3M Environmental Laboratory Solubility, Shake Raak Method 5/2/2001 Page 7 of 11 BACK TO MAIN FACT-TCR-002 PFOS in 3.5% NaCI Solution Day 2 Hillary. H010205 I-J , f j .> irt TCR-002, 012901-nadPFOS-2.1.1.100X nadPFOS-2.1.1 DO. SFM 02-01-01 MEE(MLA) 45 H010205A.M HILL004S.D 31 u '.t ,n* '* P / ,\ - 5.155 5360243.5 214.2 21.4 * ; a a : v .iS lh tl> ... , , 21.0 22.2 TCR-002, 012901-nadPFOS-2.1.2, 100X nadPFOS-2.1.2 Dii. SFM 02-01-01 MEE(MLA) 46 H010205A.M HILL0046.D 32 5.156 5515177.0 218.6 21.9 21.4 1.52 TCR-002, 012901-nadPFOS-2.1.3,100X nadPFOS-2.1.3 Dii. SFM 02-01-01 MEE(MLA) 47 H010205A.M HILL0047.D 33 5.155 5645223.0 225.9 22.6 22.1 6.8% TCR-002, 012901-nadPFOS-2.1.4, 100X nadPFOS-2.1.4 Dii. SFM 02-01-01 MEE(MLA) 48 H010205A.M HILL004S.D 34 5.156 6158368.0 . 249.0 24.9 24.4 N TCR 002 012901-nadPFOS-2 2 1 , 100X >. nadPFOS-2.2.1 Dii SFM 02-01-01 MEE(MLA) 1 * < 35 5 156 - 7113649 5 ^ - ' ^28,7^ ,-p i :'- .1 V' : : 20.0 Q TCR-002, 012901-nadPFOS-2.2.2,100X nadPFOS-2.2.2 Dii. SFM 02-01-01 MEE(MLA) 53 H010205A.M HILL0053.D 36 5.155 5223066.0 207.2 3 > <0 oO Q TCR-002, 012901-nadPFOS-2.2.3,100X d nadPFOS-2.2.3 Dii. SFM 02-01-01 MEE(MLA) 54 H010205A.M HILL0054.D 37 5.160 5134239.0 203.4 oo7fO1 s (8 co TCR-002, 012901-nadPFOS-2.2.4,100X nadPFOS-2.2.4 Dii. SFM 02-01-01 MEE(MLA) 55 H010205A.M HILL0055.D 38 5.155 5143755.5 203.4 20.7 20.3 20.3 20.3 19.9 19.9 0.23 1.2% co TCR-002, 012901-nadPFOS-2.3.1,100X nadPFOS-2.3.1 Dii. SFM 02-01-01 MEE(MLA) 57 H010205A.M HILL0057.D 39 5.155 4691219.0 184.5 18.5 18.1 17.8 m oo TCR-002, 012901-nadPFOS-2.3.2, 100X nadPFOS-2.3.2 Dii. SFM 02-01-01 MEE(MLA) 58 H010205A.M HILL0058.D 40 5.158 4632432.0 182.6 18.3 17.9 0.25 c0"oJ0 TCR-002, 012901-nadPFOS-2.3.3, 100X nadPFOS-2.3.3 Dii. SFM 02-01-01 MEE(MLA) 59 H010205A.M HILL0059.D 41 5.162 4642529.5 181.5 18.2 17.8 1.4% CD TCR-002, 012901-nadPFOS-2.3.4, 100X nadPFOS-2.3.4 Dii. SFM 02-01-01 MEE(MLA) 60 H010205A.M HILL0060.D 42 5.155 4582600.5 179.4 17.9 17.5 Day 2 C0O0 average: std dev: 20.S fg/mL 2.20 %C.V.: 11.0% 3M Enwonm ental Laboratory Sotubtity, Shake Flask Method 5/2/2001 Page 8 o f 11 FACT-TCR-002 PFOS in 3.5% NaCI Solution Day 3 Hillary, 010206 BACK TO MAIN TCR-002, 012901-nadPFOS-3.1.1,100X nadPFOS-3.1.1 Oil. SFM 02-02-01 MEE(MLA) 45 H010206A.M HILL0045.D 61 5.162 5394307.0 217.1 21.7 21.2 21.1 TCR-002, 012901-nadPFOS-3.1.2, 100X naclPFOS-3.1.2 46 H010206A.M HILL0046.D Dii. SFM 02-02-01 MEE(MIA) 62 5.161 5387695.5 213.3 21.3 20.9 0.13 TCK-002, i2 9 G -n a u rF G S -3 ..3 , 1CGX naclPFOS-3.1,3 Dii. SFM 02-02-01 MEE(MLA) 47 H010206A.M HILL04/. 63 9. crii 5400416.0 215.6 21.6 21.1 0.6% TCR-002 012901-oadPFOS-3.1.4, 100X nadPFOS-3.1.4 Dii. SFM 02-02-01 MEE(MLA) AO H01020SA..M HLL0048 D 64 5.158 5367317.5 216.0 21.6 21.1 Sample Data, DAY 3 TCR-002, 012901-oadPFOS-3.2.1,100X naclPFOS-3.2.1 Dii. SFM 02-02-01 MEE(MLA) 52 H010206A.M HILL0052.D 65 5.155 5247156.5 208.4 20.8 20.4 20.1 TCR-002, 012901-oadPFOS-3.2.2, 100X nadPFOS-3.2.2 D. SFM 02-02-01 MEE(MLA) 53 H010206A.M HILL0053.D 66 5.155 5202058.5 207.1 20.7 20.3 0.45 TCR-002, 012901-nadPFOS-3.2.3.100X nadPFOS-3.2.3 Dii. SFM 02-02-01 MEE(MIA) 54 H010206A.M HILL0054.D 67 5.157 5144265.5 205.3 20.5 20.1 2.2% TCR-002, 012901-oadPFOS-3.2.4,100X nadPFOS-3.2.4 Dii. SFM 02-02-01 MEE(MLA) 55 H010206A.M HILL0055.D 68 5.155 5024824.0 198.5 19.8 19.4 (fi 4* m o01 TCR-002, 012901-nadPFOS-3.3.1,100X nadPFOS-3.3.1 Dii. S F M 02-02-01 MEE(MLA) 57 H010206A.M HILL0057.D 69 5.157 4756814.0 190.3 19.0 18.6 18.5 j o> TCR-002, 012901-nadPFOS-3.3.2,100X nadPFOS-3.3.2 Dii. SFM 02-02-01 MEE(MLA) 58 H010206A.M HILL0058.D 70 5.162 4726155.5 189.2 18.9 18.5 0.24 "0 (0Q) CD TCR-002, 012901-nadPFOS-3.3.3,100X nadPFOS-3.3.3 D. SFM 02-02-01 MEE(MLA) 59 H010206A.M HILL0059.D 71 5.156 4696616.0 185.3 18.5 18.1 1.3% o> O O TCR-002, 012901-nac!PFOS-3.3.4, 100X nadPFOS-3.3.4 Dii. SFM 02-02-01 MEE(MLA) 60 H010206A.M HILL0060.D 72 5.156 4754382.0 189.8 19.0 18.6 Day3 average: std dev: %C.V.: 19.9 ng/mL 1.31 6.6% ng/mL 3M Environmental Laboratory Solubility, S haki Flask Method 5/2/2001 Page 9 of 11 FACT-TCR002 (LIMS #E00-1716), Page 61 of 138 FACT-TCR-002 FACT-TCR002 PFOS Solubility of TCR-00017-46 in 3.5% NaCl Solution Day 1 data source acquisition instrumcnt/sequence: Agilent 1100 HPLC/MSD "Hillary"/H01013l.s Day 2 data source acquisition instrumcnt/sequence: Agilent 1100 HPLC/MSD "Hillary'7H010205.S Day 3 data source acquisition instrument/sequencc: Agilent 1100 HPLC/MSD "Hillary "/H010206.* DATA SUMMARY FOR INDIVIDUAL SAMPLES BACK TO MAIN FACT-TCR002 PFOS Solubility o f TCR-00017-46 in 3.5% NaCl Solution. DAILY AND TOTAL DATA SUMMARIES nadPFOS-2.1.1 naclPFOS-2.1.2 naclPFOS-2.1.3 naclPFOS-2.1.4 nadPFOS-2r2.1 nadPFOS-2.2.2 nadPFOS-2.2.3 nadPFOS-2.2.4 nadPFOS-2.3.1 nadPFOS-2.3.2 nadPFOS-2.3.3 nadPFOS-2.3.4 . nadPFOS-3.1.1 nadPFOS-3.1.2 nadPFOS-3.t.3 r.adPFOS-3.1.4 nadPFOS.3.2.1 nadPFOS-3.2.2 nadPFOS-3.2.3 nadPFOS-3.2.4 nadPFOS-3.3.1 nadPFOS-3.3.2 nadPFOS-3.3.3 nadPFOS-3.3.4 21.4 21.9 22.6 24.9 20.7 20.3 20.3 18.5 18.3 18.2 17.9 21.7 21.3 21.6 21.6 20.8 20.7 20.5 19.8 19.0 18.9 18.5 19.0 21.0 21.4 22.1 24.4 _ ' - 28 1 , . 20.3 19.9 19.9 18.1 17.9 17.8 17.5 21.2 20.9 21.1 21.1 20.4 20.3 20.1 19.4 18.6 18.5 18.1 18.6 3M Environmental Laboratory 22.2 1.52 6.8% 20.0 0.23 . 1.2% 17.8 0.25 1.4% 21.1 0.13 0.6% 20.1 0.45 2.2% 18.5 0.24 1.3% lis rv i n a y x u a U s Um iliai y Average: 20.0 ppm StdDev: 2.20 %CV: 11.0% (Sample 2.2. i excluded via Q-Tcxt) Day 3 data summary Average: 19.9 ppm Std Dev: 1.31 %CV: 6.6% TOTAL data summary Average: 20.0 ppm Std Dev: 0.07 %CV: 0.4% Data from Days 2 and 3 are used. Day 1has been omitted from the calculations. Greyed / yellowed areas have been Solubility, Shake Flask Method 5(272001 Paga 10 of 11 FACT-TCR-002 PFOS in 3.5% NaCI Solution Shake Flask Method BACK TO MAIN Q-TEST Data Calculations: Sample ID: naclPFOS;2.2.T , naclPFOS-2.2.2 naclPFOS-2.2.3 naclPFOS-2.2.4 Sample Cone., Rep1 Sample Clone., Rep2 Sample Clone., !Rep3 Sample Clone., Rep4 r; 281 t, 20.3 19.9 19.9 _ Range: . 8.20 Gap: 7.80 Qobs: 0.95 No. observations: 4 Retain? no Exclude rep 1! Qobserved = gap/range where "gap" is the difference between the questionable data point and the closest value of the data set, and "range" is the difference between the highest and lowest value of the data set. If Qobserved is > Q-tabulated, then the data point may be excluded with 90% confidence. Q-tabulated for 4 observations (or data points) is 0.68. The samples highlighted in yellow in the above table have Q-observed > 0.68, and were therefore excluded from the reported data._______________ 3M Environmental Laboratory Solubility, Shake Flask Method, 5/2/2001 FACT-TCR002 (LIMS #E00-1716), Page 62 of 138 Page 11 of 11 Attachment C: Sample Chromatograms BACK TO MAIN FACT-TCR002 (LIMS #E00-1716), Page 63 of 138 Batch Run # 22 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0022.D TN-A-4740, 04 Dec 00 Injection Date 1/25/01 1:13:34 PM Seq. Line Sample Name MeOH Blank 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\H0125A1.M Last changed 1/29/01 2:28:35 PM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" 22 92 1 10 BACK TO MAIN Sample Name: MeOH Blank Internal Standard Report - ============================:=============:======================Ex0et={;opy of Original Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name Signal 1 ft- Monday', January 29, 2001 2 :15 :31HPM . 1.0000 Initial 1.0000 Instrument 1 1/29/01 2:28:36 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 64 of 138 Page 1 of 3 Batch Run. # 22 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0022.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 [min] ra.tio [ng/mL] ------------|----------- |------------------ |------------------ |------------------ |-|------------ 4.111 - - - 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 Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ------------------ 1 ----------------- ! ---------------------------- 1 ---------------------------- 1 ----------------------------1 - | ------------------- 4.864 - - - 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 - - - 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 Monday, January 29, 2001 2:15:31 PM 1.0000 1.0000- Signal 1: MSD1 299, EIC=298.7:299.7 Peak RetTime # [min] I 1 4.111 Type I Width [min] 0.0000 Totals : Area 0.00000 0.00000 Area % Name 0.0000 PFBS Instrument 1 1/29/01 2:28:36 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 65 of 138 Page 2 of 3 Batch Run # 22 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0022.D Signal 2: MSD1 427, EIC=426.7:427.7 Peak RetTime Type Width Area Area Name # [min] [min] % - -- I--------- I--------- I---------- I--------------- I------------ I............ 1 4.864 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 # [min] [min] % 1__ ____I______ l1_ _-_- I1__________ 1.1. ____ I1I__ 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 Name : MeOH Blan> Instrument 1 1/29/01 2:28:36 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 66 of 138 Page 3 of 3 Batch Run # 38 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0038.D TN-A-4740, 04 Dec 00 Injection Date 1/25/01 4:11:20 PM Seq. Line Sample Name MeOH Blank 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\H0125A1.M Last changed 1/29/01 2:30:01 PM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil Bum 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT 38 92 1 10 p l BACK TO MAIN Sample Name : MeOH Blank Sample ISTD Information: ISTD ISTD Amount Name Instrument 1 1/29/01 2:30:01 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 67 of 138 Page 1 of 3 Batch Run # 38 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0038.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 [min] ratio [ng/mL] ------------------ 1 ----------------- 1 -----------------------------| ---------------------------- 1 ---------------------------- 1 - | ------------------- 4.111 - - - 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 Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ------------------ | ----------------- | -------------------------- - | ---------------------------- | ---------------------------- l - l - ----------------- 4.864 - - - 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 - - - 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 Mondciy, January 29, 2001 2:15:31PM 1.0000 1.0000' Signal 1: MSD1 299, EIC=298.7:299.7 Peak RetTime Type Width Area Area Name # [min] [min] % - -- I----------I--------- I-----------I--------------- I------------ I------- 1 4.111 I 0.0000 0.00000 0.0000 PFBS Totals : 0.00000 Instrument 1 1/29/01 2:30:01 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 68 of 138 Page 2 of 3 Batch Run # 38 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0038.D BACK TO MAIN Sample Name: MeOH Blank Signal 2: MSD1 427, EIC=426.7: 427.7 Peak RetTime Type Width # [min] [min] ___ I_______ i______ i _ _ ____ | 1 4.864 I 0.0000 Area Area Name % ________ 1S______ ___1______________________ 0.00000 0.0000 THPFOS Totals : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 Peak RetTime Type Width # [min] [min] Area 1 5.144 0.0000 0.00000 Totals : 0.00000 Area % Name 0.0000 PFOS 1 Warnings or Errors : Warning : ISTD compound(s) not found *** End of Report *** Instrument 1 1/29/01 2:30:01 PM KLT/MLA FACT-TCR002(LIMS#E00-1716), Page69of138 page 3 of 3 Batch Run # 43 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0122.D TN-A-4740, 04 Dec 00 Injection Date : 1/30/01 12:10:30 PM Seq. Line Sample Name : MeOH Blank Vial Acq. Operator : MLA Inj Acq. Instrument : Hillary Inj Volume Acq. Method : C:\HPCHEM\1\METHCDS\H010129.M Last changed : 1/29/01 1:35:12 PM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010129B.M Last changed : 1/31/01 11:08:44 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate : 122 : 97 :1 : 10 p 1 BACK TO MAIN Scimple Name : MeOH Blank Internal Standard Report ""xcTGopy of O rin ai Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name Signal 1/31/01 11:08:42 AM 1.0000 1.0000 ^ /y --- Initial _____ Daf.8 Instrument 1 1/31/01 11:21:50 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 70 of 138 Page 1 of 3 Batch Run # 43 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0122.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 [min] ratio [ng/mL] ------------| -----------| ---------------- . | ------------------ | ------------------ | - | ------------- 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 [min] ratio [ng/mL] ------------|-----------|------------------ |------------------ |------------------ |-|------------- 4.909 - - - 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 -- Amount Grp Name [ng/mL] I ----------------------------| - | -------------------- - 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 1/31/01 1.0000 1.0000 11:08:42 AM Signal 1: MSD1 299, EIC=298.7 :299 7 Peak RetTime Type Width Area Area Name # [min] [min] % - -- I----------I--------- I-----------I-----------.-- I----------- I------- 1 4.111 I 0.0000 0.00000 0.0000 PFBS Totals : 0.00000 BACK TO MAIN Sample Name: MeOH Blank Instrument 1 1/31/01 11:21:50 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 71 of 138 Page 2 of 3 Batch Run # 43 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0122.D BACK TO MAIN Sample Name: MeOH Blank Signal 2: MSD1 427, EIC=426.7 :427.7 Peak RetTime Type Width # [min] [min] I i __ i ______ i I II I 1 4.909 I 0.0000 Area Area Name % __ I_1________ I1 __________ __________ 0.00000 0.0000 THPFOS Totals : 0.00000 S i g n a l 3 : MSD1 4 9 9 , E I C = 4 9 8 .7 : 4 9 9 . 7 Peak RetTime # [min] 1 1 5.144 Type Width [min] _l__ 0.0000 Area _____ 1 0.00000 Area Name % ______ I1_____ ________________ 0.0000 PFOS Totals : 0.00000 1 Warnings or Errors : Warning : ISTD compound(s) not found *** End of Report *** instrument 1 1/31/01 11:21:50 AM KLT/MLA FACT-TCR002 (LIMS#500-1716), Page72of 138 page 3.of 3 Batch Run # 41 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0041.D TCR-002, 012201-swPFOS-1.4.2, 100X Dii. Method Blank, SFM 01-24-01 MEE (MLA) Injection Date : 1/25/01 4:44:42 PM Seg. Line Sample Name : swPFOS-1.4.2 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\H0125A1.M Last changed : 1/29/01 2:30:17 PM 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: swPFOS-1.4.2 41 22 1 10 f il Instrument 1 1/29/01 2:30:18 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 73 of 138 Page 1 of 2 Batch Run # 41 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0041.D BACK TO MAIN Sample Name : swPFOS-1.4.2 Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution ,: Sample ISTD Information: ISTD ISTD Amount Name # _______I I 1 [ng/mL] 254.00000 PFBS 2 254.40000 THPFOS Signal Monday, 1.0000 1.0000 January 29, 2001 2:15:31 PM 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 2.23757e6 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 ---[-m--i-n--]---| ----------- | ------------------ | ratio ------------------ 4.941 PBA+ I 1.13828e6 1.00000 Amount Grp Name [ng/mL] 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] ------------| -----------l . _ ---------------| ------------------ | ------------------ | . _ | ------------ 5.144 - - - PFOS Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : Calibrated compound(s) not found *** End of Report *** Instrument 1 1/29/01 2:30:18 PM KLT/MLA FACT-TCR002 (LIMS#E00-1716), Page 74 of 138 Page 2 of 2 Batch Run # 22 of 59 Data File C :\HPCHEM\l\DATA\H010126\HILL0158.D TCR-002, 012201-SwPFOS-l.4.3, 100X Dil. Method Blank, SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 7:11:01 PM Seq. Line Sample Name Acq. Operator swPFOS-2.4.3 MLA 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\H010126C.M Last changed : 1/30/01 2:52:45 PM by KLT/MLA . (modified after loading) PFOS Analysis Column: C18 Betasil Sum 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" BACK TO MAIN Sample Name: swPFOS-2.4.3 158 61 1 10 p i /i/y A p Instrument 1 1/30/01 2:52:45 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 75 of 138 Page 1 of 2 Batch Run # 22 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0158.D Internal Standard Report BACK TO MAIN Sample Name: swPFOS-2.4.3 Sorted By : Calib. Data Modified : Multiplier : Dilution .: Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] Signal Tuesday, January 30, 2001 2:27:34 PM 1.0000 1.0000 --- 1--------------1------------------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 [min] ratio [ng/mL] Il 1 _ 1 ________ 11__ 11 _____ ______ 4.112 VBA+ I 2.05076e6 1.00000 254.00000 PFBS __ Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type [min] Area Amt/Area ratio Amount Grp Name [ng/mL] . Il 1 1 11 4.924 PBA+ I 1.12624e6 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type [min] Il 5.142 Area - Amt/Area ratio i - Totals without ISTD(s) : Amount [ng/mL] ___ - Grp Name |-|- -- PFOS 0.00000 - 2 Warnings or Errors : Warning : Calibration warnings (see. calibration table listing) Warning : Calibrated compound(s) not found *** End of Report *** Instrument 1 1/30/01 2:52:45 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 76 of 138 Page 2 of 2 Batch Run # 22 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0101.D TCR-002, 012201-SWPFOS-3.4.3, 100X Dil. Method Blank, SFM 01-26-01 MEE(MLA) Injection Date 1/30/01 8:16:24 AM Seq. Line Sample Name swPFOS-3.4.3 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acg. Method C :\HPCHEM\1\METHODS\H010129.M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C :\HPCHEM\l\METHODS\HO10129 B .M Last changed 1/31/01 11:08:44 AM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil Sum 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT : 101 : 53 :1 : 10 BACK TO MAIN Sample Name: swPFOS-3.4.3 Instrument 1 1/31/01 11:20:03 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 77 of 138 Page 1 of 2 Batch Run # 22 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0101.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 1/31/01 1.0000 1.0000 11:08:42 AM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ------------------ | ----------------- | ---------------------------- 1 ----------------------------| ---------------------------- | - | ------------------- 4.111 VBA+ I 1.81230e6 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] - - - -- I--------I--------------- I--------------- I--------------- l " l ---------- 4.909 PBA+ I 1.00441e6 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 - - - 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 : swPFOS-3.4.3 Instrument 1 1/31/01 11:20:03 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 78 of 138 Page 2 of 2 Batch Run # 46 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0046.D TCR-002, 012201-SwPFOS-1.1.2, 100X Dii. SFM 01-24-01 MEE(MLA) Injection Date 1/25/01 5:40:19 PM Seq. Line Sample Name swPFOS-1.1.2 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\H0125A1-M Last changed 1/29/01 2:30:45 PM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil Eium 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT BACK TO MAIN Sample Name: swPFOS-1.1.2 46 32 1 10 t il Exact Copy ei ur : 1" M iai U m - L Instrument 1 1/29/01 2:30:45 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 79 of 138 Page 1 of 2 Batch Run # 46 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0046.D BACK TO MAIN Sample Name: swPFOS-1.1.2 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 Monday', 1.0000 1.0000 January 29, 2001 2:15:31 PM Signal 1: MSD1 299, EIC=298.7 :299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] . -------- 1------- 1 - .............I-........... - I - .............. i - i --------- 4.111 VBA+ I 2.15890e6 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-]-- I------- I------------- I---r--a-t-i--o---- -[-n-g--/-m-L-]---- l - l --------- 4.927 VBA+ I 1.11676e6 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 VBA+ 3.91905e6 1.45546e-l 129.93889 PFOS Totals without ISTD(s) : 129.93889 **" End of Report *** Instrument 1 1/29/01 2:30:45 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 80 of 138 Page 2 of 2 Batch Run # 53 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0053.D BACK TO MAIN Sample Name : sv/PFOS-1.2.2 TCR-002, 012201-swPFOS-1.2.2, 100X Dii. SFM 01-24-01 MEE(MLA) Injection Date 1/25/01 6:58:14 PM Seq. Line Sample Name swPFOS-1.2.2 Vial Acq. Operator MLA inj Ac q . 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\METHCDS\H0125A1.M Last changed 1/29/01 2:31:22 PM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betcisil 5um 50X2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" : 53 : 36 :1 : 10 ill Exact Copy of Or.n' ^ / i j A - ........ i n ' -- - Instrument 1 1/29/01 2:31:23 PM KLT/MLA FACT-TCR002 (LIMS #EOO-1716), Page 81 of 138 Page 1 of 2 Batch Run # 53 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0053.D BACK TO MAIN Sample Name: swPFOS-1.2.2 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' Monday, 1.0000 1.0000 January 29, 2001 2:15:31 PM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type [min] Area Amt/Area ratio Amount Grp Name [ng/mL] ------------------ | ----------------- | ---------------------------- | -- ------------------- I ----------------------------l - l ------------------- 4.109 VBA+ I 2.14016e6 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] - -- -- I-------- I--------------- I--------------- I---------------l - l ---------- 4.939 VBA+ I 1.11329e6 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 PVA+ 3.70294e6 1.45288e-l 122.93840 PFOS Totals without ISTD(s) : 122.93840 *** End of Report *** Instrument 1 1/29/01 2:31:23 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 82 of 138 Page 2 of 2 Batch Run # 57 of 79 Data File C:\HPCHEM\1\DATA\H010125\HILL0057.D TCR-002, 012201-swPFOS-l.3.1, 100X Dii. SFM 01-24-01 M E E (MLA) Injection Date 1/25/01 7:42:55 PM Seq. Line Sample Name swPFOS-1.3.1 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\1\METHODS\H01012 5.M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C :\HPCHEM\1\METHODS\H0125A1.M Last changed 1/29/01 2:31:44 PM 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: swPFOS-1.3.1 57 39 1 10 il 350000 300000 -i 250000 200000 -3 150000 100000 50000H 0 --i---------- 1 MSD1 427, EIC=426.7:427.7 (H010125\HILL.0057.D) API-ES, Neg, SIM, Frag: Var mir Exact Copy ot Original Instrument 1 1/29/01 2:31:45 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 83 of 138 Page 1 of 2 Batch Run # 57 of 79 Data File C:\HPCHEM\l\DATA\H010125\HILL0057.D BACK TO MAIN Sample Name: swPFOS-1.3.1 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 Monday, 1.0000 1.0000 January 29, 2001 2:15:31 PM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt./Area Amount Grp Name [min] ratio [ng/mL] ----------1............ i .................... i ---------------1................ - i - - i .............. 4.109 VBA+ 1 2 . 17183e6 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] ------------|----------- |------------------ |------------------ |----------------- |-|------------- 4.939 VBA+ I 1.12792e6 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] ------------------ ! ----------------- 1 ---------------------------- , ---------------------------- 1 ---------------------------- l - l -------------------- 5.142 PVA+ 3.79790e6 1.45346e-l 124.50482 PFOS Totals without ISTD(s) : 124.50482 *** End of Report *** Instrument 1 1/29/01 2:31:45 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 84 of 138 Page 2 of 2 Batch Run # 25 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0161.D BACK TO MAIN Sample ame: .i .: TCR-002, 012201-SWPFOS-2.1.1, 100X Dii. SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 7:44:28 PM Seq. Line Sample Name SWPFOS-2.1.1 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\l\METHODS\HO1012 6C.M Last changed 1/30/01 2:53:00 PM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil Bum 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT 161 63 1 10 L nstsal u/ Instrument 1 1 / 3 0 / 0 1 2 : 5 3 : 0 1 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 85 of 138 Page 1 o f 2 Batch Run # 25 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0161.D . Internal Standard Report BACK TO MAIN Sample AMCX111C O W f l 'V U 4* 4. X Il 1 Il 1 Il 1 li I Il I Il 1 Il II Il II Il II Il II Il II Il II Il II Il II Il II Il II Il II Il II Il II Il II Il II Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] 1 1_______| __________________________| ________ 1 254.00000 PFBS _ 2 254.40000 THPFOS Signal Tuesday 1.0000 1.0000 January 30 , 2001 2:27:34 PM Signal 1: MSD1 299, EIC=298.7 :299.7 RetTime Type [min] Area 4.108 VBA+ I 2.07348e6 Amt/Area Amount Grp Name ratio [ng/mL] 1| _____________ |1 ! 1 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] 1_________| ________ |1 1_________________| 4.924 PBA+ I 1.11620e6 1_________________ | 1.00000 254.40000 i 1 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7 :499.7 RetTime Type Area Amt/Area Amount [min] ratio [ng/mL] _____________| 1______ | 1______________ _ | 1___________________ 5 .1 4 4 WA+ 3 .3 7 9 5 8 e 6 1 .5 B 4 7 7 e - l 1 2 2 .0 6 8 7 5 Grp Name 1 PFOS ----------------------------- Totals without ISTD(s) : 122.06875 1 Warnings or Errors : Warning : Calibration warnings (see calibration table listing) *** End of Report *** Instrument 1 1/30/01 2:53:01 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 86 of 138 Page 2 of 2 Batch Run # 28 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0164.D TCR-002, 012201-SWPFOS-2.1.4, 100X Dii. SFM 01-25-01 MEE(MLA) Injection Date 1/27/01 8:17:52 PM Seq. Line Sample Name swPFOS-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\H01012 6 C .M Last changed 1/30/01 2:53:16 PM by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" . : 164 : 66 :1 : 10 BACK TO MAIN Sample Mame ; wrruo'4 .j_.ft Exact Copy o f 0 ; ; ' "ji z f If initial Instrument 1 1/30/01 2:53:16 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 87 of 138 Page 1 of 2 Batch Run # 28 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0164.D BACK TO MAIN Sample Name: swPF0S-2.1.<: 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 Tuesday, January 30, 2001 2:27:34 PM 1 .0 0 0 0 1 .0 0 0 0 Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area Amount Grp Name [min] ratio [ng/mL] ------------------ |----------------- |---------------------------- |----------------------------|----------- --------------- |-|-------------------- 4.112 VBA+ I 2.03714e6 1.00000 254.00000 PFBS Totals without ISTD(s) : . 0.00000 Signal 2: MSD1 427, EIC=426.7:427.7 RetTime Type [min] Area Amt/Area ratio Amount Grp Name [ng/mL] - - -- I - ------------- I ----------------------------I ---------------------------- I ---------------------------- l - l -------------------- 4.928 VBA+ I 1.10630e6 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] ------------------ 1 ----------------- 1 -----------------------------1 ----------------------------) -- ---------------- | - - | -------------------- 5.145 W A + 3.33404e6 1.58453e-l 121.48330 PFOS Totals without ISTD(s) : 121.48330 1 Warnings or Errors : Warning : Calibration warnings (see calibration table listing) *** End of Report *** Instrument 1 1/30/01 2:53:16 PM KLT/MLA. FACT-TCR002 (LIMS #E00-1716), Page 88 of 138 Page 2 of 2 Batch Run # 33 of 59 Data File C:\HPCHEM\l\DATA\H010126\HILL0169.D TCR-002, 012201-SWPFOS-2.2.2, 100X Dii. SFM 01-25-01 M E E (MLA) Injection Date 1/27/01 9:13:46 PM Seq. Line Sample Name swPFOS-2.2.2 ' Vial Ac q . Operator MLA Inj Acq. Instrument Hillary Inj Volume A cq. Method C :\HPCHEM\1\METHC)DS\H010125 .M Last changed 1/25/01 9:13:04 AM by MLA Analysis Method C :\HPCHEM\1\METHODS\H010126C.M Last changed 1/30/01 2:53:42 PM 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: swPFOS-2.2.2 169 68 1 10 toltiaS JX.Vf i Instrument 1 1/30/01 2:53:43 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 89 of 138 Page 1 of 2 Batch Run # 33 of 59 Data File C:\HPCHEM\1\DATA\H010126\HILL0169.D BACK TO MAIN Sample Name: swPFOS-2.2.2 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 Tuesday, 1.0 000 1.0 000 January 30, 2001 2:27:34 PM Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area' Amount Grp Name [min] ratio [ng/mL] ------------|-----------|------------------ |------------------ |------------------ |-_|------------- 4.109 VBA+ I 2.01151e6 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--]-------- |-|-------------------- 4.925 PBA+ I 1.10297e6 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 VBA+ 3.38154e6 1.58541e-l 123.65462 PFOS Totals without ISTD(s) : 123.65462 1 Warnings or Errors : Warning : Calibration warnings (see calibration table listing) *** End of Report *** Instrument 1 1/30/01 2:53:43 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 90 of 138 Page 2 of 2 Batch Run # 25 of 59 Data File C:\HPCHEM\l\DATA\H010129\HILL0104.D TCR-002, 012201-SWPFOS-3.1.1, 100X Dii. SFM 01-26-01 MEE(MLA) Injection Date 1/30/01 8:49:51 AM Seq. Line Sample Name swPFOS-3.1.1 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\H010129B.M Last changed 1/31/01 11:08:44 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 : 104 : 61 :1 : 10 BACK TO MAIN Sample Name: swPF0S-3.1.i Instrument 1 1/31/01 11:20:18 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 91 of 138 Page 1 of 2 Batch Run # 25 of 59 Data File C:\HPCHEM\l\DATA\H010129\HILL0104.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # [ng/mL] - -- I----------------- r I--------- 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/31/01 1 .0 0 0 0 1 .0 0 0 0 11:08:42 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 1.79360e6 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] ------------| ----------- | ------------------ | ------------------ | ------------------ | _ _ | ------------ 4.909 PBA+ I 9.89058e5 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 + 3.60619e6 1.59134e-l 147.60707 PFOS Totals without ISTD(s) : 147.60707 *** End of Report *** BACK TO MAIN Sample Name: swPFOS-3.1.1 Instrument 1 1/31/01 11:20:18 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 92 of 138 Page 2 of 2 Batch Run # 28 of 59 bata File C:\HPCHEM\1\DATA\H010129\HILL0107.D BACK TO MAIN Sample Name : swPFOS-3.1.4 TCR-002, 012201-SWPFOS-3.1.4, 100X Dii. SFM 01-26-01 MEE(MLA) Injection Date 1/30/01 9:23:14 AM Seq. Line Sample Name swPFOS-3.1.4 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method C :\HPCHEM\1\METHC)DS\H010129 .M Last changed 1/29/01 1:35:12 PM by MLA Analysis Method C :\HPCHEM\1\METHODS\HO1012 9B.M Last changed 1/31/01 11:08:44 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" 107 64 1 10 Exact Copy ef ,/ih Snitia! L il Instrument 1 1/31/01 11:20:33 AM KLT/MLA FACT-TCR002 (LIMS#E00-1716).Page93of138 Page i of 2 Batch Run # 28 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0107.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 1/31/01 11:08:42 AM 1.0 000 1.0 000 Signal 1: MSD1 299, EIC=298.7:299.7 RetTime Type Area Amt/Area - Amount Grp Name [min] ratio [ng/mL] ...........- i ---------1..............-- i ....................i ....................i - i----------- 4.109 VBA+ I 1.82894e6 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] ------------|----------- |------------------ |------------------ |------------------ |-|----- 4.911 PBA+ I 9.98892e5 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] ----------- | ---------- | ----------------- | ----------------- | ----------------- l - l - -- -- 5.142 W A + 3.65623e6 1.59152e-l 148.19823 PFOS Totals without ISTD(s) : 148.19823 *** End of Report *** BACK TO MAIN Sample Name: swPFOS-3.1. Instrument 1 1/31/01 11:20:33 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 94 of 138 Page 2 of 2 Batch Run # 32 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0111.D BACK TO MAIN Sample Name : s w p f o . 3 . 2.1 TCR-002, 012201-SWPFOS-3.2.1, 100X Dii. SFM 01-26-01 MEE(MLA) Injection Date 1/30/01 10:07:52 AM Seq. Line Sample Name swPFOS.3.2.1 Vial Acq. Operator MLA Inj Acq. Instrument Hillary Inj Volume Acq. Method . .. . Last changed : 1/29/01 1:35:12 PM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010129B.M Last changed : 1/31/01 11:08:44 AM by KLT/MLA (modified after loading) PFOS Analysis Column: Cl8 Betasil Bum 50X2 mm Eluents : Methanol and 2 mm Ammonium, Acetate Reprocessed on "Dioana" KLT 111 65 1 10 Instrument 1 1/31/01 11:20:54 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 95 of 138 Page 1 of 2 Batch Run # 32 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0111.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 1/31/01 1.0 000 1.0 000 11:08:42 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 1.82761e6- 1.00000 254.00000 PFBS Totals without ISTD(s) : 0.00000 Signal 2: MSD1 427, EIC=426.7 :427.7. RetTime Type Area Ami:/Area Amount Grp Name [min] ratio [ng/mL] ------------| ----------- , ------------------ | ------------------ | ------------------ | __| ------------- 4.912 PBA+ I 9.96184e5 1.00000 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Type Area Ami:/Area ---[-m--i-n--]---| ----------- | ------------------ | ratio ------------------ S.143 W A + 3.37134e6 1.58803e--l Amount Grp Name [ng/mL] ------------------------ 1 - 1 -------------------- 136.72210 PFOS Totals without ISTD(s) : 136.72210 *** End of Report *** BACK TO MAIN Sample N a m e : s w p f u s . 3 . 2 . 1 Instrument 1 1/31/01 11:20:54 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 96 of 138 Page 2 of 2 Batch Run # 37 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0116.D BACK TO MAIN Sample Name: swPFOS-3.3.l TCR-002, 012201-SWPFOS-3.3.1, 100XD1. SFM 01-26-01 MEE(MLA) Injection Date 1/30/01 11:03:41 AM Seq. Line Sample Name swPFOS-3.3.1 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\H010129B.M Last changed 1/31/01 11:08:44 AM by KLT/MLA (modified after loading) PFOS Analysis Column: Cl 8 Bet asil 5um 50X2 mm Eluents : Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" . KLT : 116 : 69 :1 : 10 /xl MSD1 427, EIC=426.7:427.7 (H010129\HILL0116.D) API-ES, Neg, SIM, Frag: Var 225000 j 200000-i 175000H 150000j 125000 -j 1ooooo -i 75000j 50000 j 25000 -j n ___________________ , _____________ I P; jd - _ teilia! _ d A r lL ___ Date f ju y l j l Instrument 1 1/31/01 11:21:20 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 97 of 138 Page 1 of 2 Batch Run # 37 of 59 Data File C:\HPCHEM\1\DATA\H010129\HILL0116.D Internal Standard Report Sorted By : Calib. Data Modified : Multiplier : Dilution : Sample ISTD Information: ISTD ISTD Amount Name # Cng/mL] 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/31/01 1.0 000 1.0 000 11:08:42 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 1.76373e6 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] ------------------|-----------------|---------------------------- |---------------------------- |----------------------------|-|------------------- 4.912 VBA+ I 9.87376e5 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 + 2.90941e6 1.5B231e-l 118.61261 PFOS Totals without ISTD(s) : 118.61261 *** End of Report *** BACK TO MAIN Sample w a r n e : s w f o s - 3 . 3 . 1 Instrument 1 1/31/01 11:21:20 AM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 98 of 138 Page 2 of 2 Batch Run # 22 of 79 Data File C:\HPCHEM\1\DATA\H010205\HILL0022.D TM-A-47 55, 05 Feb 01, exp:2005. Injection Date 2/5/01 6:07:45 PM Seq. Line 22 Sample Name MeOH Blank Vial 92 Acq. Operator Acq. Instrument Acq. Method MLA Inj Hillary Inj Volume C :\HPCHEM\1\METHODS\H010205.M 1 10 /il Last changed 2/5/01 2:09:33 PM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010205A.M Last changed 2/9/01 3:37:04 PM by MLA (modified after loading) :in run C2,c3,c4,c5, c7 and CI3 perf luoronated carboxylic acids BACK TO MAIN Sample Name: MeOH Blank Internal Standard Report Sorted By : CaLib. Data Modified : Multiplier Dilution : : Sample ISTD Information: ISTD ISTD Amount Name :r [ p p b ] Retention Time Friday, February 09, 2001 3:22:24 PM 1.0000 1.0 000 Exae Copy 'Cl V), /il$ - Initial Date Instrument 1 2/9/01 3:37:04 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 99 of 138 Page 1 of 2 Batch Run # 22 of 79 Data File C:\HPCHEM\l\DATA\H010205\HILL0022.D TL -A-17 55, 05 Feb 01, exp:2005. Injection Date : 2/5/01 6:07:45 PM Seq. Line : 22 Sample Name : MeOH Blank Vial : 92 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 l Acq. Method : C:\HPCHEM\1\METHODS\H010205.M Last changed : 2/5/01 2:09:33 PM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010205A.M Last changed .: 2/9/01 3:37:04 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids BACK TO MAIN Sarnpj. amc ; n e u n XciXIK 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EIC=426.7:427.7 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] 4.121 1 W A + 4.821 2 5.158 3 W A + 1.29920e4 - 1.31270e4 0.00000 ########## -- 0.00000 0.00000 PFBS THPFOS PFOS Tecals without ISTD(s) : 2.53242e-12 2 Warnings or Errors : Warning : ISTD compound(s) not found Warning : Negative results set to zero (cal. curve intercept), (PFOS) * * * End of Report *** Instrument 1 2/9/01 3:37:04 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 100 of 138 Page 2 of 2 Batch ;un # 50 of 79 Data r'.le C:\HPCHEM\l\DATA\H010205\HILL0050.D Ti: A-4755, 05 Feb 01, exp:2005. Injection Date 2/5/01 11:19:11 PM Seq. Line 50 Sr. -pie Name MeOH Blank Vial 93 Ac ;. Operator Ac Instrument MLA Hillary Inj Inj Volume 1 10 nl Ac i. Method C :\HPCHEM\1\METHC)DS\H010205 .M L? :jt changed 2/5/01 2:09:33 PM by MLA Ar ;lysis Method C :\HPCHEM\1\METHODS\H01020 5A .M Lc.rt changed 2/9/01 3:39:25 PM by MLA (modified after loading) Si 1 run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids BACK TO MAIN Sample-- ----- MSD1 299, EIC=298 7:299.7 (H0102D5\HILL0050.D) API-ES, Neg, SIM, Frag: Var Internal Sta.ndard Report Sc cted By : Cc, Lib. Data Modified : Multiplier : D.i Lution : Sample ISTD Information: IS I'D ISTD Amount Name Cppb] Retention Time Friday, February 09, 2001 3:22:24 PM 1.0 000 1.0 000 j-i M- ^ niilaS @1 y m i /,/) Instrument 1 2/9/01 3:39:25 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 101 of 138 Page 1 of 2 Batch ,;un # 50 of 79 Data I Lie C:\HPCHEM\l\DATA\H010205\HILL0050.D TI -A-4755, 05 Feb 01, exp:2005. Irjection Date : 2/5/01 11:19:11 PM Seq. Line : 50 Sample Name : MeOH Blank Vial : 93 Acq. Operator : MLA Inj : 1 A c q . Instrument : Hillary Inj Volume : 10 f i l Acq. Method : C:\HPCHEM\l\METHODS\H010205.M La.-31 changed : 2/5/01 2:09:33 PM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010205A.M Last changed : 2/9/01 3:39:25 PM by MLA (modified after loading) Sin run C2,c3,c4,c5, c7 and C3 perfluoronated carboxylic acids BACK TO MAIN Samp_ 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7: 299.7 Signal 2: MSD1 427, EIC=426.7:427.7 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] .118 1 VVA+ :.821 2 5.161 3 PBA+ 1 30096e4 2 60.08472 0.00000 ########## - 0.00000 0.00000 PFBS THPFOS PFOS Tc'als without ISTD(s) 2.53242e-12 2 Warnings or Errors : Warning : ISTD compound(s) not found Warning : Negative results set to zero (cal. curve intercept), (PFOS) *** End of Report *** Instn L'.ent 1 2/9/01 3:39:25 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 102 of 138 Page 2 of 2 Batch Run # 22 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0022.D TN-A-4755, 05 Feb 01, exp:2005. Injection Date : 2/6/01 3:46:36 PM Seq. Line : 22 Sample Name : MeOH Blank Vial : 96 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 i l Acq. Method : C:\HPCHEM\l\METHODS\H010206.M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed .: 2/7/01 1:14:17 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids BACK TO MAIN Sample Name: MeOH Blank Instrument 1 2/7/01 1:14:17 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 103 of 138 Page 1 of 2 Batch Run # 22 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0022.D TN-A-4755, 05 Feb 01, exp:20CI5. Injection Date 2/6/01 3:46:36 PM Seq. Line : 22 Sample Name MeOH Blank Vial : 96 Ac q . Operator MLA Inj : 1 Acq. Instrument Hillary Inj Volume : 10 i l Acq. Method C :\HPCHEM\1\METHODS\H010206.M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010206A.M Last changed 2/7/01 1:14:17 PM by MLA (modified after loading) Sim run C2,c3,c4 ,c5, c7 and CfJ perfluoronated carboxylic acids BACK TO MAIN Sample Name: MeOH Blank 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EIC=426.7 :427.7 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Sig Type [min] Area Amt/Area Amount Grp Name ratio . [ppb] 4.105 1 W A + 4.819 2 5.155 3 W A + 1.24766e4 - 6796.12695 0.00000 ########## -- 0.00000 1.42633e-l PFBS THPFOS PROS Totals without ISTD(s) 1.42633e-l 1 Warnings or Errors : . Warning : ISTD compound(s) not found *** End of Report *** Instrument 1 2/7/01 1:14:17 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 104 of 138 Page 2 of 2 Batch iun # 40 of 79 Data rile C:\HPCHEM\1\DATA\H010205\HILL0040.D T'1-002, 012 901-naclPFOS-2.4.1, lOOXDil. Mi shod Blank, SFM 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.4.1 Injection Date : 2/5/01 9:27:53 PM Seq. Line : 40 S. nple Name : naclPFOS-2.4.1 Vial : 21 A {. Operator : MLA. Inj : 1 A. i . instrument : Hillary Inj Volume : 10 jlI A: Method : C:\HPCHEM\l\METHODS\H010205.M L; st changed . : 2/5/01 2:09:33 PM by MLA A.: alysis Method : C:\HPCHEM\l\METHODS\H010205A.M List changed : 2/9/01 3:38:35 PM by MLA (modified after loading) S In run C2 ,c3 ,c 4 ,c5 , c7 and CEI perl:luoronated carboxylic acids Internal Standard Report Si..:;ted By Ci Lib. Data Modified M. Ltiplier D Lution S. nple ISTD Information: I; rD ISTD Amount Name 4 t p p b ] Retention Time Friday, February 09, 2001 3:22:24 PM 1.0 0 0 0 1.0 0 0 0 Instr nenu 1 2/9/01 3:38:36 PM MLA FACT-TCR002 (UNIS #E00-1716), Page 105 of 138 Page 1 of 2 Batch J.un & 40 of 79 Data Lie C:\HPCHEM\1\DATA\H010205\HILL0040.D T 1-002, 012901-naclPFOS-2.4.1, lOOXDil. M< shod Blank, SFM 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.4.1 1: j ec: ion Date : 2/5/01 9:27::53 PM Seq. Line : 40 S. nple Name : naclPFOS-2.4.1 Vial : 21 A i . Operator : MLA Inj : 1 A {. Instrument : Hillary Inj Volume : 10 jlI A i . Method : C:\HPCHEM\1\METHODS\H010205.M L st changed 2/5/01 2:09:33 PM by MLA Ai A l y s i s Method : C:\HPCHEM\1\METHODS\H010205A.M L. st changed : 2/9/01 3:38:35 PM by MLA (modified after loading) S n r m C2 ,c3 ,c 4 ,c5 , c7 and C8 perf luoronated carboxylic acids 250.70000 THPFOS S.gnal 1: MSD1 299, EIC=298.7 :299.7 Signal 2: MSD1 427, EIC=426.7 :427.7 signal 3: MSD1 499, EIC=498.7 :499.7 R-cTine Sig Type .ninj Area Amt/Area ratio Amount Grp Name [ppb] i.l\9 1.8.9 3.155 1 W A + 1.94355e6 5.81750e-l 2 PVA+ I 1.04252e6 1.00000 3 W A + 8906.63379 0.00000 271.89463 PFBS 250.70000 THPFOS 0.00000 PFOS T' cals without ISTD(s) : 271.89463 1 .Warnings or Errors : W .m i ng : Negative results set to zero (cal. curve intercept), (PFOS) *** End of Report *** Instr nene 1 2/9/01 3:38:36 PM MIA FACT-TCR002 (LIMS #E00-1716), Page 106 of 138 Page 2 of 2 Batch 3.un ft 42 of 79 Data Lie C:\HPCHEM\1\DATA\H010205\HILL0042.D T .1-0 J2 , 012 901-naclPFOS-2.4.3, 100X Dil. M: 1 hod Blank, SFM 02-01-01 MEE (MLA). BACK TO MAIN Sample Name: naclPFOS-2.4 .2 I: jection Date : 2/5/01 9:50:09 PM Seq. Line : 42 S' .nple Name :naclPFOS-2.4.3 Vial : 23 A jperator :MLA Inj : 1 A {. .instrument : Hillary Inj Volume : 10 i l A 1 . Method :C:\HPCHEM\1\METHODS\H010205.M L jt changed .:2/5/01 2:09:33 PM by MLA A ilycis Method :C:\HPCHEM\l\METHODS\H010205A.M L it changed :2/9/01 3:38:45 PM by MLA (modified after loading) S n run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids MSD1 299, EIC=298.7:299.7 (H010205\HILL0042.D) API-ES, Neg, SIM, Frag: Var Internal Standard Report cted By : C. L i b . Data Modified : M Ltip'lier : D ..ut ion : :ipla ISTD Information: I. i'D ISTD Amount Name [ppb] Retention Time Friday, February 09 1.0000 1.0000 PM Insti-.-.lent 1 2/9/01 3:38:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 107 of 138 Page 1 of 2 Bate h Mur !l 42 of 79 Data L i e C:\HPCHEM\1\DATA\H010205\HILL0042.D T .1-002, 012 901-naclPFOS-2.4.3, 100X Dii. H' shod Blank, SFM 02-01-01 M E E (MLA) BACK TO MAIN Sample Name: naclPFOS-2.4.3 1. jection Date 2/5/01 9:50:09 PM Seq. Line 42 S nple Name naclPFOS-2.4.3 Vial 23 A' q. Operator MLA Inj 1 A '. q . Instrument Hillary Inj Volume 10 A q. Method : C:\HPCHEM\l\METHODS\H010205.M L e t changed 2/5/01 2:09:33 PM by MLA A: ilvsis Method : C:\HPCHEM\l\METHODS\H010205A.M L. st changed : 2/9/01 3:38:45 PM by MLA (modified after loading) S ' r .in C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 250.70000 THPFOS S.gnal 1: MSD1 299, EIC=298.7 :299.7 Signal 2: MSD1 427, EIC=426.7 :427.7 S gnal 3: MSD1 499, EIC=498.7 :499.7 R'.tTime Siq Type Area Amt/Area Amount Grp Name ;nin ; ratio [ppb] i1_-i1_____ 1 1! 1____ _ I1_ 1I_ __ 1. I :7 1 W A + 1.93318e6 5.81750e-l 272.07681 PFBS 1.821 2 PBA+ I 1.03627e6 1.00000 250.70000 THPFOS 5.131 3 PPA+ 5505.63037 0.00000 0.00000 PFOS T. cals without ISTD(s) : 272.07681 1 darnings or Errors : W. rning : Negative results set to zero (cal. curve intercept), (PFOS) *** End of Report *** Inst: en . 1 2/9/01 3:38:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 108 of 138 Page 2 of 2 Batch Run # 41 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0041.D TCP.-002, 012901-naclPFOS-3.4.2, 100X Dil. Method Blank, SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-3.4 .; Injection Date 2/6/01 7:17:53 PM Seq. Line 41 Sample Name naclPFOS-3.4.2 Vial 52 Acq. Operator MLA . Inj 1 A c q . Instrument Hillary Inj Volume 10 l Acq. Method C :\HPCHEM\1\METHODS\H010206.M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C :\HPCHEM\3.\METHODS \H010206A .M Last changed 2/7/01 1:15:46 PM by MLA (modified cLfter loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids Instrument 1 2/7/01 1:15:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 109 of 138 Page 1 of 2 Batch Run # 41 of 79 Data File C:\HPCHEM\1\DATA\H0102C6\HILL0041.D TCR-002, 012901-naclPFOS-3.4.2, 100X Dil. Method Blank,.SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-3.4. Injection Date 2/6/01 7:17:53 PM Seq. Line 41 Sample Name naclPFOS-3.4.2 Vial 52 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 1 0 l l Acq. Method C :\HPCHEM\ l\METHODS\H010206 .M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C :\HPCHEM\ 3.\METHODS\H010206A .M Last changed 2/7/01 1:15:46 PM by MLA (modified eilfter loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EIC=426.7 :427 7 Signal 3: MSD1 499, EIC=498.7 :499 i RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] 4.106 4.820 5.156 1 W A + 2.00919e6 6.10461e-l 290.41323 2 PVA+ I 1.05881e6 1 0 0 0 0 0 250.70000 3 PPA+ 3730.26538 3.15106e-l 2.78313e-l PFBS THPFOS PFOS Totals without ISTD(s) : 290.69154 * * * End of Report *** Instrument 1 2/7/01 1:15:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 110 of 138 Page 2 of 2 Batch Run # 43 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0043.D TCR-002, 012901-naclPFOS-3.4.4, 100X Dil. Method Blank, SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-3.4. Injection Date : 2/6/01 7:40:11 PM Seq. Line : 43 Sample Name : naclPFOS-3.4.4 Vial : 54 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 i l Acq. Method : C :\HPCHEM\l\METHODS\H010206 .M Last changed .: 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed : 2/7/01 1:15 :55 PM-by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids ISTD ISTD Amount Name # [ppb] Instrument 1 2/7/01 1:15:56 PM MLA FACT-TCR002 (LIMS#E00-1716), Page 111 of138 Page 1 0 f 2 Batch Run # 43 of 79 Data File C:\HPCHEM\l\DATA\H010206\HILL0043.D TCR-002, 012901-naclPFOS-3.4.4, 100X Dil. Method Blank, SFM 02-02-01 MEE (MLA) BACK TO MAIN Sample Name: naclPFOS-3.4 .c Injection Date : 2/6/01 7:40:11 PM Seq. Line : 43 Sample Name : naclPFOS-3.4.4 Vial : 54 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 /xl Acq. Method : C:\HPCHEM\1\METHODS\H010206.M Last changed .: 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\l\METHODS\H010206A.M Last changed : 2/7/01 1:15:55 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EIC=426.7:427.7 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] 4.105 4.819 5.156 1W A + 1.97953e6 6.10461e-l 288.63083 2PBA+ I 1.04962e6 1.00000 250.70000 3PBA+ 3744.80615 3.13083e-l 2.80034e-l PFBS THPFOS PFOS Totals without ISTD(s) 288.91086 *** End of Report *** Instrument 1 2/7/01 1:15:56 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 112 of 138 Page 2 of 2 Batch :-;ur* # 45 of 79 Data : Lie C:\HPCHEM\l\DATA\H010205\HILL0045.D T;.7-092, 012901 -naciPFOS-2.1.1, 100X Dii. S: >i 02-01-01 m e e (m l a ; BACK TO MAIN Sample Name: naclPFOS-2.1. I: jeceion Date o ';p :- Marne 2/5/01 10:23:33 PM naclPFOS-2.1.1 Seq. Line Vial 45 31 -- . operator MLn Inj 1 A. Instrument Hillary Inj Volume 10 A [. Method : C :\HPCHEM\1\METH:ODS\H010205 .M L :t changed 2/5/01 2:09:33 PM- by MLA A: .ilysis Method : C :\HPCHEM\1\METHODS\H010205A.M L,, st changed : 2/9/01 3:39:00 PM by MLA (modified after loading) S .:n run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids MSD1 299, EIC=2S8.7:299.7 (H010205\HILL.0045.D) API-ES, Neg, SIM, Frag: Var CO Internal Standard Report S ::ted By C, Lib. Data Modified M- :.tiplier D Lon S. r.ple ISTD Information: Il t d ISTD Amount Name :f [ppb] . Retention Time Friday, February 09, 2001 3:22:24 PM 1.0 000 1.0 000 lustrimene 1 2/9/01 3:39:01 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 113 of 138 ip ) page x o f 2 Batch .:ur: # 45 of 79 Data Lie C:\HPCHEM\1\DATA\H010205\HILL0045.D T' 7-002, 012901-naclPFOS-2.1.1, 100X Dil. S: /; 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.1. I. jeccion Date : 2/5/01 10:23:33 PM Seq. Line : 45 S; iple Name : naclPFOS-2.1.1 Vial : 31 Acq. Operator : MLA Inj : 1 A q. Instrument : Hillary Inj Volume : 10 /zl Acq. Method : C:\HPCHEM\l\METHODS\H010205.M Lest changed .: 2/5/01 2:09:33 PM by MLA A: Jilysis Method : C:\HPCHEM\1\METHODS\H010205A.M Lest changed : 2/9/01 3:39:00 PM by MLA (modified after loading) S ,i ran C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 250.70000 THPFOS Signal 1: MSD1 299, EIC=298. :299.7 SL :jnal 2: MSD1 427, EIC=42S. :427.7 S.gnal 3: MSD1 499, EIC=498. :499.7 RctTime Sig Type Area min] . --------- - - I --------- | --------------- 4.118 1 W A + 1.95449e6 4.819 2 PBA+ I 1.01804e6 5.15 5 3 VVA+ 5.3 6024e6 Amt/Area ratio 5.81750e-l 1.00000 1.622:53e-l Amount Grp Name [ppb] 280.00194 PFBS 250.70000 THPFOS 214.17458 PFOS Tc cals without ISTD(s) : 494.17652 *** End of Report *** Instr 1 2/9/01 3:3 9:01 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 114 of 138 Page 2 of 2 Batch hurt # 46 of 79 Data : Lie C:\HPCHEM\1\DATA\H010205\HILL0046.D T 7.-002 , 012901-naclPFOS-2.1.2, 100X Dil. SIM 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.1.2 I; ;ection Date : 2/5/01 10:34:39 PM Seq. Line : 46 S ;:p:e Name : naclPFOS-2.1.2 Vial : 32 A ;. Operator : MLA Inj : 1 A. .{. Instrument : Hillary Inj Volume : 10 /il A Method : C:\HPCHEM\l\METHODS\H010205.M 1 :t changed 2/5/01 2:09:33 PM by MLA A. 1 1ysis Method : C:\HPCHEM\l\METHODS\H010205A.M L: ..;t changed : 2/9/01 3:39:05 PM. by MLA (modified after loading) S a run C2,c3,c4,c5, c7 and CO peri:luoronated carboxylic acids MSD1 299, EIC=298.7:299.7(H010205\HILL0046.D) API-ES, Neg, SIM, Frag: Var 00000 i50000 00000 50000 - 0 rCD- MSD1 499, E!C=498.7:499.7(H010205\HILL0046.D) API-ES, Neg, SIM, Frag: Var : 1 JOOOOO -j i w 'J00000 ; '00000 I JOOOOO 1:00000 I o05 : o ...... 0 Internal Standard Report Sc rted By CrLib. Data Modified Mu t Lplier D: ..ution Sample ISTD Information: ISTD ISTD Amount Name : [ppb] Retention Time Friday, February 09, 2001 3:22:24 PM 1 .0 0 0 0 ' 1.0 000 Instrument 1 2/9/01 3:39:06 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 115 of 138 min --i---------- r" mir Page 1 of 2 Batch ;,ur: # 46 of 79 Data I Lie C:\HPCHEM\1\DATA\H010205\HILL0046.D TCP-002, 012901-naclPFOS-2.1.2, lOOXDil. SF -i 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.1 . ' Injection Date 2/5/01 10:34:39 PM Seq. Line 46 Sample Name naclPFOS-2.1.2 Vial 32 Acg. Operator MLA Inj 1 Ac . Instrument Hillary Inj Volume 10 Ac ;[. Method : C :\HPCHEM\l\METHODS\H010205 .M Lc.: i t changed : 2/5/01 2:09:33 PM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010205A.M Last changed : 2/9/01 3:39:05 PM by MLA (modified after loading) Sin run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.'; : 2 9 9 . 7 Signal 2: MSD1 427, EIC=426.'; : 4 2 7 . 7 Signal 3: MSD1 499, ETC=498.'; : 4 9 9 . 7 ReiTime Sig Type [m in] Area Amt/Area ratio Amount Grp Name [ppb] !.119 ' 1 W A + 1.99539e6 5.81750e-l 4.8.20 2 PVA+ I 1.02730e6 1.00000 5 .156 3 W A + 5.51518e6 1.62412e-l 283.28167 250.70000 218.59113 PFBS THPFOS PFOS Tccals without ISTD(s) : 501.87280 *** End of Report *** Instrument 1 2/9/01 3:39:06 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 116 of 138 Page 2 of 2 Batch :;uii # 48 of 79 Data File C:\HPCHEM\1\DATA\H010205\HILL0048.D TCP-002, 012901-naclPFOS-2.1.4, 100X Dii. SF: 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2 1 4 '' In iection Date 2/5/01 10:56:54 PM Seq. Line 48 Samp e Name Ac . Operator Ac :j. Instrument A Method naclPFOS-2.1.4 Vial MLA Inj Hillary Inj Volume C :\HPCHEM\1\METHODS\H010205 .M 34 1 10 Li .;t changed . 2/5/01 2:09:33 PM by MLA Ar 11. sis Method C:\HPCHEM\1\METHODS\H010205A.M Laut changed 2/9/01 3:39:15 PM by MLA (modified after loading) S:i :i run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids Internal Standard Report Sl :ted By : Ci i b . Data Modified : Mi Lplier : D.: .union : Staple ISTD Information: ISTD ISTD Amount Name ? [ppb] Retention Time Friday, February 09, 1.0000 1.0000 Instruiert 1 2/9/01 3:39:16 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 117 of 138 Page 1 of 2 Batch ,-u.. # 43 of 79 Data i C:\HPCHEM\1\DATA\H010205\HILL0048.D TC - 02, 012 901-naclPFOS-2.1.4, 100XD1. SI 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.1.4 Injection Date 2/5/01 10:56:54 PM Seq. Line : 48 Sample Name naclPFOS-2.1.4 Vial : 34 Acq. Operator MLA Inj : 1 Acq. Instrument Hillary Inj Volume ! 10 Acq. Method C :\HPCHEM\1\METHODS\H010205 .M Ls.;t changed 2/5/01 2:09:33 PM by MLA Analysis Method C :\HPCHEM\1\METHODS\H010205A.M Loot changed 2/9/01 3:39:15 PM by MLA (modified after loading) Sim run C2,c3,c4 c 5 , c7 and C8 perfluoronated carboxylic acids 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EIC=426.7:427.7 Signal 3: MSD1 499, EIC=498.7:499.7 Re .Time Sig Type . [min] Area Amt/Area ratio Amount Grp Name [ppb] :..19 ..220 i .156 1 VBA+ 1 91S82e6 5.81750e-l 275.75855 2 PVA+ I 1 013 78e6 1.00000 250.70000 3 PBA+ 6 15837e6 1.63487e-l 248.97829 PFBS THPFOS PFOS Tc-cals without ISTD (s) : ' 524.73683 *** End of Report *** Instri ment 1 2/9/01 3:39:16 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 118 of 138 Page 2 of 2 Batch Run # 53 of 79 Data File C:\HPCHEM\1\DATA\H010205\HILL0053.D TCR-002, 012901-naclPFOS-2.2.2, lOCIXDil. SFM 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.2.2 Injection Date : 2/5/01 11:52:35 PM Seq. Line : 53 Sample Name : naclPFOS-2.2.2 Vial : 36 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 /I Acq. Method : C:\HPCHEM\l\METHODS\H010205.M Last Changed : 2/5/01 2:09:: 33 PM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010205A.M Last changed : 2/9/01 3:39::40 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and Cfi perfluoronated carboxylic acids ISTD ISTD Amount Name # [ppb] Instrument 1 2/9/01 3:39:41 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 119 of 138 Page 1 of 2 Batch Run # 53 of 79 Data File C:\HPCHEM\1\DATA\H010205\HILL0053.D TCR-002, 012901-naclPFOS-2.2.2, 100XD1. SFM 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.2. Injection Date 2/5/01 11:52:35 PM Seq. Line 53 Sample Name naclPFOS-2,,2.2 Vial 36 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 10 Acq. Methoa C :\HPCHEM\1\METHODS\H010205 .M Last changed . 2/5/01 2:09:33 PM by MLA Analysis Method C :\HPCHEM\1\METHODS\H010205A.M L.ist change! 2/9/01 3:39:40 PM by MLA (modified after loading) S ;.m run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EI=426.7: 427.7 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Sig Type [min] Area ------------------ I - - ; -----------------I - 4.119 1 7VA+ 1 .89751e6 4.819 2 PVA+ I 1 .02378e6 5.155 3 W A + 5 .223 07e6 Amt/Area ratio 5.81750e-l 1.00000 1.61.999e-l Amount Grp Name [ppb] 270.31266 250.70000 207.19812 PFBS THPFOS PFOS Totals without ISTD (s) : 477.51078 ** * End of Report *** Instrument 1 2/9/01 3:39:41 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 120 of 138 Page 2 of 2 Batch Run # 54 of 79 Data ile C:\HP:HEM\1\DATA\H010205\HILL0054 .D TCR-002, 012 901-naclPFOS-2.2.3, lOOXDil. SFM 02-01-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-2.2 .: Injection Date 2/6/01 12:03:44 AM Seq. Line 54 Sample Name naclPFOS-2.2.3 Vial 37 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 10 Acq. Method C :\HPCHEM\1\METHODS\H010205.M Lcist changed 2/5/01 2:09:33 PM by MLA Analysis Method' C:\HPCHEM\l\METHODS\H010205A.M Last changed 2/9/01 3:39:45 PM by MLA (modified after loading) Sim run 02,03,04,05, c7 and C8 perfluoronated carboxylic acids MSD 299, E!C=298.7:299.7 (H010205\HILL0054.D) API-ES, Neg, SIM, Frag: Var 300000 250000 d 200000 150000J 225000 200000 175000d 150000 125000 100000 75000 d 50000 MSD1 499, EIC=498.7:499.7 (H010205\HILL0054.D) API-ES, Neg, SIM, Frag: Var 900000 800000 1 700000 ] I 600000 500000 4 I 400000 4 1 300000 j 200000 4 oo 100000 I o 0 -> , 8__________ mi T 8 mi Internal Standard Report Sorted By C..lib. Data Modified Multiplier D.lution Sample ISTD Information: ISTD ISTD Amount Name # [ppb] Retention Time Friday, February 09, 2001 3:22:24 PM 1.0000 1.0000 Instrument 1 2/9/01 3:39:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 121 of 138 Page 1 of 2 Batch Run # 54 of 79 Data rile C:\HPCHEM\1\DATA\H010205\HILL0054.D TAR-002, 01'_:901-naclPFOS-2.2.3;, lOOXDil. SiM 02-01-17 MEE(MLAj BACK TO MAIN Sample Name: naclPFOS-2.2.3 . Injection Date : 2/6/01 12:03:44 Seq. Line : 54 Sample Name :naclPFOS-2.2.3 Vial : 37 Acq. Operator :MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 /I Acq. Method :C:\HPCHEM\1\METHODS\H010205.M Last changed :2/5/01 2:09:33 PM by MLA Analysis Method ':C:\HPCHEM\1\METHODS\H010205A.M L.iSt changed :2/9/01 3:39:45 PM by MLA . (modified after loading) Sim run C2,c3,c4,c5, c7 and Cii perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298. :299.7 Signal 2: MSD1 427, EIC=426. :427.7 signal 3: MSD1 499, EIC=498. :499.7 RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] 4.117 1 7BA+ 1.880 69e6 5.81750e-l 4.821 2 VVA+ I 1.02437e6 1.00000 5.160 3 TVA+ 5.13424e6 1.61860e-l 267.76401 PFBS 250.70000 THPFOS 203.38226 PFOS Totals without ISTD(s) : 471.14627 *** End of Report *** Instrument 1 2 7/01 3:39:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 122 of 138 Page 2 of 2 Batch Run # 46 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0046.D TCR-002, 012901-naclPFOS-3.1.2, 100X Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-3.l .: Injection Date : 2/6/01 8:121:35 PM Seg. Line : 46 Sample Name : naclPFOS-3.1.2 Vial : 62 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 jlI Acq. Method : C:\HPCHEM\1\METHODS\H010206.M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed : 2/7/01 1:16:10 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids ISTD ISTD Amount Name # [ppb] Instrument 1 2/7/01 1:16:10 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 123 of 138 Page 1 of 2 Batch Run # 46 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0046.D TCR-002, 012901-naclPFOS-3.1.2, 100X Dii. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naciPFOS-3.1.2 Injection Date 2/6/01 8:13:35 PM Seq. Line 46 Sample Name naclPFOS-3.1.2 Vial 62 Acq. Operator MLA Inj 1 Acq. Instrument Hillary ' Inj Volume 10 Acq. Method : C:\HPCHEM\1\METHODS\H010206.M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed : 2/7/01 1:16:10 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 1 25Q.70000 THPFOS Signal 1: MSD1 299, EIC=298.7 :299.7 Signal 2: MSD1 427, EIC=426.7 :427.7 Signal 3: MSD1 499, EIC=498.7 :499.7 RetTime Sig Type [min] Area Amt/.Area ratio Amount Grp Name [ppb] 4.104 1 VBA+ 1.90390e6 5 .10461e-l 281.92266 4.822 2 PVA+ I 1.03354e6 1.00000 250.70000 5.161 3 W A + 5.38770e6 1.63206e-l 213.28895 PFBS THPFOS PFOS Totals without ISTD(s) 495.21161 *** End of Report * * * Instrument 1 2/7/01 1:16:10 PM MIA FACT-TCR002 (LIMS #E00-1716), Page 124 of 138 Page 2 of 2 Batch Run # 48 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0048.D TCR-002, 012901-naclPFOS-3.1.4, 100X Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: i m i r r w - j . i . ! Injection Date : 2/6/01 8:35:51 PM Seq. Line : 48 Sample Name : naclPFOS-3.1.4 Vial : 64 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 l Acq. Method : C :\HPCHEM\1\METHODS\H010206 .M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\l\METHODS\H010206A.M Last changed : 2/7/01 1:16:19 E'M by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids Sample ISTD Information: ISTD ISTD Amount Name # [ppb] Instrument 1 2/7/01 1:16:19 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 125 of 138 Page 1 of 2 Batch Run # 48 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0048.D TCR-002, 012901-naclPFOS-3.1.4, 100X Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample H,, Injection Date : 2/6/01 8:35:51 PM Seq. Line : 48 Sample Name : naclPFOS-3.1.4 Vial : 64 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 f i l Acq. Method : C:\HPCHEM\l\METHODS\H010206.M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed : 2/7/01 1:16:19 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1 : MSD1 299, EIC=298.7:299.7 Signal 2 : MSD1 427, EIC=426. 7:427.7 Signal 3 : MSD1 499, EIC=498.7:499.7 RetTime [min] 4.107 4.821 5.158 Sig Type Area 1 W A + 2..02831e6 2 PVA+ I 1 .01737e6 3 W A + 5,.36732e6 Amt/Area Amount Grp Name ratio [ppb] 1 1__________ I1_ I1_____ _ 6.10461e-l 305.11576 PFBS 1.00000 250.70000 THPFOS 1.63334e-l 216.02714 PFOS Totals without ISTD(s) : 521.14289 *** End of Report *** Instrument 1 2/7/01 1:16:19 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 126 of 138 Page 2 of 2 Batch Run # 52 of 79 Data File C:\HPCHEM\l\DATA\H010206\HILL0052.D TCR-002, 012901-naclPFOS-3.2.1, 100X Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Nu,,.. Injection Date : 2/6/01 9:20:29 PM Seq. Line : 52 Sample Name : naclPFOS-3.2.1 Vial : 65 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p i Acq. Method : C:\HPCHEM\1\METHODS\H010206.M Last Changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed : 2/7/01 1:16:38 PM by MLA (modified after loading) Sim run C2(c3,c4,c5, c7 and C8 perfluoronated carboxylic acids ISTD ISTD Amount Name # [ppb] Instrument 1 2/7/01 1:16:38 PM MIA FACT-TCR002 (LIMS #E00-1716), Page 127 of 138 Page 1 of 2 Batch Run # 52 of 79 Data File C :\HPCHEM\1\DATA\H010206\HILL0052 .d TCR-002, 012901-naclPFOS-3.2.1, 100X Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Numu . uau a.c ckjj --o . . Injection Date 2/6/01 9:20:29 PM Seq. Line 52 Sample Name naclPFOS-3.2.1 Vial 65 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 1 0 i l l Acq. Method C :\HPCHEM\1\METHODS\H010206.M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C :\HPCHEM\1\METHODS\H010206A .M Last changed 2/7/01 1:16:38 PM by MLA (modified after loading) Sim run C2,c3,c4,c5( c7 and C8 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7:299.7 Signal 2: MSD1 427, EIC=426.7:427.7 Signal 3: MSD1 499, EIC=498.7:499.7 RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] 4.104 4.819 5.155 1 W A + 1 99860e6 S.10461e-1 297.34485 2 PVA+ I 1 02867e6 1.00000 250.70000 3 W A + 5 24716e6 1.62979e-l 208.41657 PFBS THPFOS PFOS Totals without ISTD ( S ) : 505.76142 *** End of Report *** Instrument 1 2/7/01 1:16:38 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 128 of 138 Page 2 of 2 Batch Run # 54 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0054.D TCR-002, 012901-naclPFOS-3.2.3, 100X Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Ne... Injection Date 2/6/01 9:42:48 PM Seq. Line 54 Sample Name naclPFOS-3.2.3 Vial 67 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 1 0 l l Acq. Method C :\HPCHEM\1\METHODS\H010206.M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C :\HPCHEM\1\METHODS\H010206A.M Last changed 2/7/01 1:16::47 PM by MLA (imodaifrixeda afrtrer lxoadaing)j Sim run 02,03,04,05, c7 and C8 perfluoronated carboxylic acids ISTD ISTD Amount Name # [ppb] Instrument 1 2/7/01 1:16:48 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 129 of 138 Page 1 of 2 Batch Run # 54 of 79 Data File C:\HPCHEM\l\DATA\H010206\HILL0054.D TCR-002, 012901-naclPFOS-3.2.3, lOCIXDil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample N aiuc i n a t . x r i v o " j . , o Injection Date : 2/6/01 9:42:48 PM Seq. Line : 54 Sample Name : naclPFOS-3.2.3 Vial : 67 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 i l Acq. Method : C:\HPCHEM\1\METHODS\H010206.M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1\METHODS\H010206A.M Last changed : 2/7/01 1:16:47 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C3 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, E I C = 2 9 8 . 7 : 2 9 9 . 7 Signal 2: MSD1 427, E I C = 4 2 6 . 7 : 4 2 7 . 7 Signal 3: MSD1 499, E I C = 4 9 8 . 7 : 4 9 9 .7 RetTime Sig Type [min] Area Amt/Area ratio Amount Grp Name [ppb] 4.107 4.821 5.157 1 W A + 2 00067e6 6.10461e-l 299.37708 2 PVA+ I 1 02275e6 1.00000 250.70000 3 W A + 5 14429e6 1.62835e-l 205.33247 PFBS THPFOS PFOS Totals without ISTD ( S) : 504.70955 *** End of Report *** Instrument 1 2/7/01 1:16:48 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 130 of 138 Page 2 of 2 Batch R u n # 5 9 of 79 Data File C:\HPCHEM\1\DATA\H010206\HILL0059.D TCR-0 0 2 , 012901-naclPFOS-3.3.3, 100X Dii. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample N _. _ .. .______ Injection Date 2/6/01 10:38:35 PM Seq. Line 59 Sample Name naclPFOS-3.3.3 Vial 71 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 1 0 p i Acq. Method C:\HPCHEM\1\METHCDS\H010206.M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C:\HPCHEM\1\METHODS\H010206A.M Last changed 2/7/01 1:17:11 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and CEi perfluoronated carboxylic acids MSD1 299, EIC=298.7:299.7 (H0102D6\HILLCI059.D) API-ES, Neg, SIM, Frag: Var 300000 . % 250000 200000 150000- 100000- 00 50000 - 0 - : d____ _ _ Internal Standard Report Sorted By Calib. Data Modified Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name # [ppb] Retention Time Wednesday, February 07, 2001 12:53:59 PM 1.0000 1.0000 -- - I ----------------------------------- I ---------------- Instrument 1 2/7/01 1:17:11 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 131 of 138 H Page 1 of 2 Batch Run # 59 of 79 Data File C:\HPCHEM\l\DATA\H010206\HILL0059.D TCR-002, 012901-naclPFOS-3.3.3, 100X Dii. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Nall Injection Date 2/6/01 10:38:35 PM Seq. Line 59 Sample Name naclPFOS-3.3.3 Vial 71 Acq. Operator MLA Inj 1 Acq. Instrument Hillary Inj Volume 10 p i Acq. Method C :\HPCHEM\1\METHODS\H010206.M Last changed 2/6/01 11:47:54 AM by MLA Analysis Method C :\HPCHEM\1\METHODS\H0102 06 A .M Last changed 2/7/01 1:17:11 PM by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and C8 perfluoronated carboxylic acids 1 250.70000 THPFOS Signal 1: MSD1 299, EIC=298.7 :299.7 Signal 2: MSD1 427, EIC=426.7 ::427.7 Signal 3: MSD1 499, EIC=498.7 :499.7 RetTime Sig Type [min] Area . Amt/Urea ratio Amount Grp Name [ppb] 4.106 4.820 5.156 1 VBA+ 1 90270e6 6.10461e-l 283.01915 2 PVA+ I 1 02888e6 1.00000 250.70000 3 W A + 4 69662e6 1.61909e-l 185.28658 PFBS THPFOS PFOS Totals without ISTD ( S ) : 468.30573 *** End of Report *** Instrument 1 2/7/01 1:17:11 PM MLA FACT-TCR002 (LIMS#E00-1716),Page 132of138 Page 2 of 2 Attachment D: Deviations from the Protocol BACK TO MAIN FACT-TCR002 (LIMS #E00-1716), Page 133 of 138 MAI. 11. UD Utili filivi RUMIMI AL LAB l Jfi W BACK TO MAIN Record of Deviation i. Identification tuid[y7ProjectNo. "............... TCR-002 G^afionType:.... D SOP " 'tf^ethoif'DEquipmentProcedure '' (Cheek one) Protocol Other: """ "" Document Nwnbei:: ETS-8155.0 <15ate(s)ofoccurrence: 01 ian 01 to 07 Feb 01 II. Dwtcription: RequiredProcedure/procesii: ET3-8-I55.0 scctionl0.2.1 states, "Matrixspikes areprepared for each sample set andanalysed] <jete'rmme~tficmatrixeffect onthe recovery efficiency." "Swtion 10213 states, "anllyze andthematfix'splicedu^cale ( ifprepared)~m the samerunasthe original sample ,________ ____ _____ ____ __ ........... 4 K i l l UMfcl* 4 Actual Procedurc/pxocess: Thematrixspikeswerenotprepared, therefore,they werenot IMMIMM* I A . M I M I I 4 4 4 M M r . ....................-- -- - r. > . . 1 1 1 4 4 M U I .........................-- -- I - . 4 mmm m , 444MM4M t # m - IIIItNAu 111, Actions Taken; ..... (tech as amendmentissued, SOPrevision, etc.) ........ .... TlieTS-S-iSiTdmethbdliasBeenrevisedsothatmatrixspikesdonotni^'toBeprepared whenmereisnoneed. 'RecordedBy' | Date: /V. ImpactonStudy/ Project UM jRG15mict onthst^ ^ T s'^ lactoFa mat^spike'.ib-ILSs, no beanhgf<>--**=------- S` ^4 ontKcfinal rsuts._T)i imiibrais'wefldefined'andcharwteriiedT'iliematrixspeistually nofpossible in tHs study silicethi: matrixis Baturatedwiththeanalyteofinterest. * " AuuttfhfioorriizzpeddByy~:((SSttudyyDiirreeccttoorr / ProjectLj -------- ---- K Gl ................. .............. .. 3A iEnvironm ental Laboratory Deviation No, RECEIVED TIME MflV.17. 2 !28PM FACT-TCR002 (LIMS #E00-1716), Page 134 of 138 s 'd ees'ON bH ItDIlAIbNy 3dlN3D Ud9I:P 1002'I`AbW M i, il. LUUi i.JJIili UH l lWIWWi'U AL LAJJ L JL UJ TTOt BACK TO MAIN Record of Deviation /. Identification StudyTProject'No.......... .......... TCR-002 I^iation typeT (Checkone) SOP.........Method Equipmentfifocedure ' Protocol Other: ......... ........ . jDocuinentN u m b i w f f f i ..... ........ Date(3)ofowurrcnceibl Jah6rto'07Feb0f II. Description: RequiredProcedure/process: J3TS-8-155.0section 10.1.2 states, "Analyze amethodblankand amatoxti8mi5idrto eachcaliSziidoncurve. riMtoMblIMVMS "* m tw m > -- - Hi. Actual Procedure/process: Inthis experiment, themethodandmatrix blanksare essentiallythe same. The"method/matnxblankswerenotmibelore^thecafibrS^a^es.._TTae"m^Sp^ _ b la n k s were rana&r tHe&it ca lib ratio n curve." ....... . ' "' , > U I M lb Ik It W titllllll- I4|i * ` P III. Actions Token: (suchas amendmenUssued, SOPrevision, etc.) .... ........... the ET^-li~-T5~$.0methodhits'Si^arreviseirso tHat^ methodandmaHxlilanksS'e to bVrain afterthe first calibrationcurve. ~ '" RecordedBy: ibMMiMliirt- - jDate: .... "" IV. Imped on Study/Project the iinpaiwdrthfs de^HohonlSrstudy IsmiiaiimSrtlSe^placimert bearing ohthe resufts. See (directive-Action. ' " ...................... . . . . .......... -iin ** It llim b lM . n "................. AuthonziedBy: (Sw$Birectr /ProjectLead)......... 'Diile:........ Q ljiJ d ^ I s //? fo 3M Environmental Laboratory Form ETS-4-8.0 Delation No. (w igm d by Study Director or Project Lead it the end of study or project) RECEIVED^ TIME WY. 17. 2>:28PM FACT- QP.-H16), Page 135 of .138 WldPI :p 1002`T 'tW mi. j i. uni iJbM-- w m m m n i r n r w NO. 5 BACK TO MAIN Record of Deviation Study/ ProjectNo? I. Identification TCR-002 DeviatonTyp: (Check one) 'SOP $ Method qm^nt^cedre " Protocol Other: Docm'atNumber: TS-S-$37# i D a t ^ orSSSiiri^: Ti Tto II. Description: OT Required Procedure/procesa: Indealingwiththestandardcurve, the curvejnuathave coffclntofdetermination(r2) valuegreaterthan'orequalto 0.980 andindividual curve " TOintsrousthive `PeroentDeviaticma' eq^td less than+/-J6% ... ..... Actual Proccdure/process: In some cases, highand/orlowcurvepointswere eliminated so that the? valiw^^'m eet the catena, iho&erca^ curvepoints were _ " eliminated, "theywerenotwitliinthe+/-3^ "accuracyreqremrits Whendus"was don,.... the curvepoints)gbctedfiindthctaa^) ticn'\iw~ifcrtated "Sheet5'........... " ..... ................ .......... . ....... .. ' ' ................ IlifUowingriiist'ofali cv^eponteaffectedandthresbnswh^ '' "3OTaCDay2, {^W6i05A)7fiointsHZLLoW5"95^/0066and66B'7.... .... y :s% i?iC T % T ^ ^ -- ----- ------------------- AlibithesepointswereexcludedtoprovideahottrBtoverthermge'appropriatetothedata. ~ III. Actions Taken: (suchos amendment issued, SOPrevision, etc.) T^elM Environment^MihdTEtS-8-l55:0wasamendedtotahlntoltccounttheeitmmktion oicurvepoints. CurveTis maybeoinitte3"bithelollbwmgreasons:' ` ` (Comments arebulletedas theywouldamear onthesumma^sheets.) ^ ^ 0) "High/lowcurvepointswere excludedto provide abetterfit ovwthe range appropntfeto the data.'* ^ ^_ __ (2) `I c ^ e v d p ^ these pointswere " " excluded from the curve to disqualOy a datarange that may have heh signMcntly affectcdl&y backgroundleyel^ '" "_1~ ............l.,, " " jPV^^^wci^epoint(ii)wereexcludedastfccy werenbtwitESnthe^/-30% accuracy.... " reqmremehts ofthemethod'whenthecumswere'vaiutfedoveTarange^propriatet the data?1 ...... . .................... ............... ......................... Recorded'By: , .......... '""TS5 r a fe IV. Impact on tudy/ Project Theelimination'f curvepointshit'dapositiyem^ct onthis'study"If curvepoi^wer not elimmatedrthnthecurves wbulTnotbeascurate. .......... " 1 Authored By: (St\^~tyinct#r /ProjectLeod) ; DateT j J r /z j/q " '3 M Environm ental Laboratory Form ETS-4-8,0 Deviation No. (UAgoed by Study Dirotor or Projct Lead it the end ofuMly orpiqjcct) RECEIVED TIME MAY. 17, 2 : 28PM FACT-TCR002 (LIMS#E00-1716), Page 136 of138 E 'd EES `ON tn "IbDIlAltNt 3dlN33 WdST :V T002`ZT-AbW a i i t NO, BACK TO MAIN Record of Deviation ~ I, identification Stiiiiy/ProjectNo..... ....... ............. .................. ... _ _..... TCR.002..................... .......... D^ationType: ...0 SOF......iSMethod~0EquipmentProcedure (Checkone) Protocol Other; i)cmentNumber: ETS-Ii-i72Tf fDate(s)Foceiience:22"Jjalto07Fe6"01 II. Description: RequiredProcedure/process: ETS-8-172.1indicatesthatascreentestmustbeperformed , M w a jM M u w . 1 . .m m i h w * * -- -- . a < -- m m > u w i i w . m m m * ------- -- . i m i . i - - . mem priorto the shakeflaskmethod. __ T ^ a . > , , VIWHAU>i> i mmmi II> . M.U1Unil - - W lI - t P*m # I ActualProcedure/proccss: Intheseawaterand3.5%NaCIportionsofthisstudy.thescreen testwashotlSne. .... . .. ......... IIM M ifM ial I til. Actions Taken: . lamaaaui * * * * -- in . . .. .mummi l" * - . . . .kMini , , , t 11 Notes to File werewrittenconcerningthis issue. ~~ * la a a iin ^Jll * ******I^TUVM RecordeaBy -- " */V!( M IIW NIMi*' 1 0% m m i . I i i w u k . w i i m ; Date:-- ^ waM.Ml >` . IV. Impsct on Study/Project s' Thereis minimal impact onthis studyby not doing screeningteats inthese matrices.__--------- iiimi-iia* IhescreentestswerenotdcinelreiauseoftwomainreasiiiT^itwasnotTdnetoconserve'*"'" xnatcmyr^d'2-thesolubilityofPFSwasalreadyknownSr^teranditvrai'alsolmown ' lEattfiesoliiKGtywould'detaeasem seawaterid 3.5%NIf....................... . .......... tK^ ..............[Date:......... ........ * - Q .l Q i * L d . ! s r /;? 4 > / 3M Environm ental Laboratory R FC E IV ET TTMT MFIY. 17. p d ees ow 2!:28PM FACT- Deviation No. 1Q-1I.16J, Page 137 ^ 1002^1 *AbW BACK TO MAIN Attachment E: Sample Calculations 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: _ nx 1 _ -Where n is the number of observations, and x is sample concentration. Average/Standard Deviation /%R8D example calculations: Sample ID Rep1 Rep 2 Rep 3 Rep 4 Concentration ng/mL 647.9 723.4 723.0 717.3 Calculations Average (647.9+723.4+723.0+717.3)/4= 702.9 Std Dev (see above equation)= 36.8 %RSD (36.8/702.9)= 5.2% Data that did not meet acceptance criteria as described in the OPPTS and OECD guidelines was excluded using statistical justification provided by Dixon's Q-test. A data point may be excluded if "Qobserved"is greater than "Q tal3ulated"with 90% confidence. Q obServed= gap/range where "gap" is the difference between the questionable data point and the closest value of the data set, and "range" is the difference between the highest and lowest value of the data set. Q-tabulated (90% confidence) for 4 observations (or data points) is 0.679 and for 3 observations is 0.886. Q-Test Example (Shaded number represents the suspected outlier): Description pg/mL Sample Cone., Rep1 607.1 Sample Cone., Rep2 591.7 Sample Cone., Rep3 626.1 Sample Cone., R e p 4 ^ ^ ^ ^ $ J 8 ^ ^ ^ Range (Rep4-Rep2): 2057.14 Gap (Rep4-Rep3): Cnhseirved (Range/Gap): No. observations: 2022.66 0.98 4 Retsiin? no Q-Test example conclusion: Since Qobserved0.98, was greater than Qtabulalad, 0.679, rep 4 may be excluded. FACT-TCR002 (LIMS #E00-1716), Page 138 of 138