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BACK TO MAIN Study Title - Characterization Study of PFOS, Primary Standard Test Control Reference #TCR-000 17-046 PHASE: SOLUBILITY OF P F o S IN NATURALSEAWATER AND AN AQUEOUS SOLUTIO'NOF 3.5% SODIUMCHLORIDE Data Requirement 40 CFR 160.105(b) Author Mark E. Ellefson P'haseCompletion Date Date of signing F'erforming Laboratory 3M EnvironmentalLaboratory 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 STATEMEINT Study Title: Characterizatiori 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: F.ACT-TCR002, Centre Analytical Laboratories Study # 0;!3-021 This phase of the study was conducted in compliancewith Environmental ProtectionAgency (EPA) Good Laboratory Practice (GLIP) Standards 40 CFR 160 with the exceptions in the bulleted list below. Exceptions to GLP compliance: 0 The electronic data systems in use have not been validated and there is not an electronic audit trail of corrections currently available (40CFR 160.130 (e)). Authenticated hardcopies of chromatograrrrs and associated documents will be considered as the original raw data. =@+ark E. lefson, PrincipalAna ytical estigator William K. Reagen, Testing Facility Management Date FACT-TCROO2 (LIMS#E00-1716), Page 2 of 138 BACK TO MAIN QUALITYASSURANCSETATEMENT 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 EnvironmentalLaboratory Quality Assurance Unit (QAU) as indicated in the following table. The findings were reported to the study director and laboratory management. I 4/23/01 -4/26/01 4/26/01 - 4/27/01 1 Data - Draft Phase Report 1 I 1 4 / 2 1 : 4/27/01 4/27/01 a( ,;2b,-O1 I FACT-TCROOS (LIMS#E00-1716), Page 3 of 138 . BACK TO MAIN TABLEOF 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......................................................................................................................................... q7 List of Attachments............................................................................................................................. 17 Signature Page................................................................................................................................... 18 Attachment A: Extraction and Analytical Methods .............................................................................. 19 Attachment 6: Data Summary Tables ................................................................................................ 40 Attachment C: Sample Chromatograms ............................................................................................ 63 Attachment D: Deviations froim the Protocol ...................................................................................... A33 Attachment E: Sample Calculations................................................................................................... 138 FACT-TCROOZ (LIMS #E00.1716). Page 4 of 138 . BACK TO MAIN LIST OF TABLES Table l a. Summary Table of Solubility of PFOS TCR-00017-046 in Natural Seawater.................... 7 Table 1b. Summary Table of Solubiliv of PFOS TCR-00017-046 in an Aqueous solution of 3.5% Sodium Chloride.................................................................................................................. 7 Table 2. Characterizationof the Test Substance .............................................................................. 8 Table 3. Characterization of the Analytical Reference Substances ................................................... 8 Table 4. Test System ........................................................................................................................ 8 Table 5a. Shake Flask Method Preparationfor Natural Seawater.................................................... 9 Table 5b. Shake Flask Method Preparationfor an Aqueous Solution of 3.5% Sodium Chloride.....9 Table 6a. Sample Collection and Preparationfor 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-00017-0. 46 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 :Solubilityof 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-TCROOZ (LIMS tlE00.1716). Page 5 of 138 BACK TO MAIN STUDYINFORMATION Study Director John Flaherty Centre Analytical Laboratory 3048 Research Drive State College, PA 16801 Analytical Chemistry Laboratories Solubility Testing Certificate of Analysis 3M EnvironmentalTechnology 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, Labomtory Manager Mark E. Ellefson, Principal Analyticai lnvestigator 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 Laboratoqr 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-TCROOZ (LIMS #E00-1716), Page 6 o f 138 BACK TO MAIN SUMMARY The solubility of PFOS in naturalseawater and an aqueous solution of 3.5% sodium chloridewas determined quantitatively via the Shake Flask Method. Results are presented in Tables l a and lb: Table l a . Summary Table of Solubility of PFOS TCR-00017-046 in Natural Seawater. I Day 1 I 12.2 pghL I 0.47 I 3.9% I Average Value 12.4 pg/rnL 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 Ib. Summary Table of Solubility of PFOS TCR-00017-046 in an Aqueous solution of 3.5%Sodium Chloride. I I Day 1 I Day 2 I Average Value Excluded 20.0 pg/mL 19.9 pghL 1I I 2.20 I 11.O% 1.31 0.07 0.4% 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-TCROOZ (LIMS #E00-1716), Page 7 of 138 BACK TO MAIN TESTSUBSTANCE PFOS, Test,Control Reference#TCF:-00017-046 Table 2. Characterizationof the Test Substance Re-aystallized by George Moore, 3M Specialty Materials, Bidg. 236-1B-10 Expiration Date I - Storage Conditions 3M Laboratory Identification Number Frozen TCR-00017-046 White Powder 97.9% REFERENCSEUBSTANCE Table 3. Characterizationof the Analytic;al ReferenceSubstances Source Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity Recrystallizedby George Moore, 3M Specialty Materials, Bldg. 236-1510 8/31/01 Frozen TCli-00017-046 White Powder 979% SynQuest Labs Not Available Frozen TCR-00017-047 Lot #Q75-30 White Powder NA 3M, Cottage Grove 12/04/01 Frozen TCR-99030-023 Lot #I a11 ~~ ~~~~~~ I 96.7 TESTSYSTEM Table 4. Test System Source Expiration Date Storage Conditions 3M Laboratory Identification PuritylGrade Ocean Scientific international Salinity = 3.5% EM Science TN-A: 2458 FACT-TCROOZ (LIMS #E00-1716), Page 8 of 138 BACK TO MAIN METHODSUMMARIES The solubility determination of PFOS TCR-00017-046 in natural seawater and aqueous 3.5% NaCl was performed according to 3kl Environmental Laboratory method ETS-8-172.0 "Shake Flask Method; Solubility Determinationof a Test Substance in Various Solvents" as adapted from United States Environmental F'rotection Agency OPPTS 830.7840, "Water Solubility: Column Elution Method; Shake Flask Method" and OECD 105, "Water Solubility" Guidelines. IETS-8172.0 was subsequently revised to irlclude additional informationlclarification. 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 Pertluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-ElectrospraylMassSpectrometry". The approximately solubility of PFOS in natural seawater and in an aqueous solution of 3.5% NaCl 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. PREPARATOMRYETHODS 0 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 Ei g of natural seawater or 3 g of of 3.5% sodium c:hloride 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 i3 temperature-controlledorbital shaker set at approximately 30OC. See the following tables documenting the shake flask method preparation: Table 5a. Shake Flask Method F'reparaiiion for Natural Seawater. 1 >6.5 rng PFOS weighed into tared 15 rnL centrifuge tube 9 - 2 Natural seawater added io centriluge tube such that total weight of 9 PFOS and solvent was approximately between 5.0 5.2 g. 3 Method Blank Preparation- Appri3ximately 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 3O.O0C, rotation speed set at approximately 150 rpm. 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 1:38 BACK TO MAIN 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 ai tared centrifuge tube gravimetrically. 4 Samples sealed with tape, vortex-mixed, and placed in a 12 - temperature-controlled oirbitalshaker set at approximately 3O.O0C, rotation speed set at approximately 150 rpm. 01-29-01 01-29-01 01-29-01 SAMPLECOLLECTIOANND ANALYSIS 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 OC for approximately 24 hours. After this, they were centrifuged and thein had aliquots of supernatant collected. The aliquots wlere diluted using IOOX dilutions (990 pL rnethano1:lO pL sample). The diluted samples were spiked with internal standard (17pL of 15 pg THF'FOS/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 anti Preparation for Study FACT-TCROOZ in Natural Seawater? ere collected and dispensed into Table 6b. Sample Collection and Prepaiationfor Study FACT-TCROOZ in Aqueous 3.5% Sodiium Chloride? FACT-TCROOZ (LIMS #E00-1716), Page 10 of `I 38 BACK TO MAIN 1 At 24,48, and 72 hours of shaking, 3 PFOS+ 4centri- I Day1 I 01-30-01 I solvent, and 1 solvent (method blank) centrifuge f i = l tubes are removedfromihe incubatorand per day equilibratedat 24-25 OC ior approximately24 hours. 2 Aliquots of the supematant (solvent containing dissolved PFOS or sohreiit only fiom the method blanks) were collected arid dispeinsed into 02-01-01 i 1 - autovials. Day3 02-02-01 I 3 The aliquotswere diluted 100Xwith methanol Day 1 01-31-01 (using a dual syringe diluter). Day 2 I 02-01-01 I Day 3 I 02-02-01 I 4 lntemal Standard was added to the 100X sample Day I I 01-31-01 I ' 5 dilutions (17pL of 15 pg 1HPFOSlmL and 15 pg PFBS/mLin methanol). Sampleswere analyzed via HPLCESIMSon HP 1100 LCIMSD Day 2 I 02-02-01 I Day 3 I 02-02-01 I - Day I I 01-31-0i O:!-OI-OI I - Day 2 I 02-0501 0:!-06-01 I - Day 3 I 02-06-01 0:!-07-01 I *Information pertains to sample preparation and dates of final reported data only. ANALYTICAML ETHOD 0 ETS-8-155.0 "Analysis of PotassiumPerfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-ElectrosprayIMassSpectrometry". Diluted samples (Le. diluted supernatants) were analyzed using HPLCIESIMS in the negative ion mode. PFOS levels were evaluated versus calibration standards ranging in concientration from 2.5-1002 ng PFOSIniL. Internal Standard quantification was used to normalize the data. Target ions were 499 m/z (PFOS anion), 427 m/z (deprotonated THPFOS), and 2!99 mIz (PFBS anion). Analytical Equipment Liquid Chromatograph: Hewlett-Palckard" Series 1100 Liquid Chromatograph system Analytical column: Keystone@BetasiP CIS 2x50mm, 5pm particle size Column temperature: Ambient Cycle Time: 9.75 minutes Flow rate: 300pUmin Injection volume: 1OpL Mobile phase components: Solvent A: 2.0 mM ammonium acetate in water Solvent C: Methanol FACT-TCROOP (LIMS #E00-1716), Page 11 of 'I38 BACK TO MAIN Solvent Gradient: Time 0.00 0.50 0.80 3.50 6.50 7.00 9.75 & y 15 % 15 % 60 % 100 % 100 % 15 % 15 % Mass Spectrometer: Hewlett-Packard@Series 1100 APllMass Spectrometer Detector Software: HP ChemStation" 6.0 Fragmentor Voltage: m/z 427=:100V; mlz 499= 140V; m/z 299 = 100 V. Capillary Voltage: 3500 V Gain = 2.0 EMV Mode: Electrospray Negative Gas Temperature: 350 OC Drying Gas: 10.0 L /min. Nebulizer Pressure: 25 psig Analysis Type: Single Ion Monitoring (SIM) ANALYTICARLESULTS Data quality objectives outlined in the! 3M Environmental Laboratory method were met (see Appendix A). 0 Regressions. Quadratic curve fit was applied to calibration standards and sample data to improve quantitationover the concentrationrange appropriate to the data. All calilbration curves had least-square fits of 0.990 or greater (R2 values ranged from 0.9992 - 0,9999). 0 CalibrationStandards. Eleven standards ranging in concentrationfrom approximately 2.5 to 1000 ng PFOSlmL methanol were used for the calibration curves. Calibration curves were run before and after every analytical sequence. 0 Sample Replicates. Sarriples 012201-swPFOS-2.3.1, 012201-swPFOS-2.3.2, 0'12201swPFOS-2.3.3, 01220l-s\~PFOS-2.3.4and naclPFOS.2.2.1were excluded from the reported data using Dixon's Q-Test. 0 ContinuingCalibrationVerification. 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. 0 Limit of Quantitation (LOQ). The LOQ is equal to the lowest standard in the calibration curve (either 2.5, 5.0 or 10.0 nglmL). Table 7a. CalibrationStandard ReprocessingSummary for PFOS in NaturalSeawater. 1002 ng/mL 2!.5 - 1002 nglmL All curve pointswere used.* All curvepointswen?used.* FACT-TCROO2 (LIMS #E00-1716), Page 12 of 138 BACK TO MAIN Table 7b. Calibration Standard Repr'ocessingSummary for PFOS in an Aqueous Solution of 3.5% Sodium Chloride. Day I data: 01-31-01 -02-01-01 5 -501 ng/mL Sntd 2 (2.5 nglmL), and Stnd 13 (1002 ng/rnL) were excluded to better tit the data at the low end of the curve: Day 2 data: - 02-05-01 02-06-01 10 -1 002 ng/mL Stnd 2 (2.5 ng/mL) and Stnd 3 (5.0 ng/mL) was excluded to better tit the data at the low end of the cuNe: Day 3 data: - 02-06-01 02-07-01 Ei - 501 ng/mL Stnd 2 (2.5 ng/mL), and Stnd 13 (1002 ng/mL) were excluded to bettertit the data at the low end of the curve.' ~ ~~~ ~~ ~~ T h e first standard, Stnd 1 (0 nglmL), is not used since there is no response measurable. Blanks. Method blanks (natural seawater or the aqueous solution of 3.5% sodium chlclride taken through the entire sarnple preparation, dilution, and analysis process) provided a measure of laboratory contaimination. Acceptable values for the blanks were less than 50% of the limit of quantitation (LOQ). 0 Solvent blanks (methanol injlections) provided a measure of instrument contamination. Acceptable solvent blanks rriust contain levels of target analyte less than 50% of the limit of quantitation (LOQ). Acceptable solvent blanks were analyzed before each calibration curve. 0 Specificity (according to OPPlrS 830.7840): The solubility determination as stated in the EPA Guidelines follows. 'This method should only be applied to: 0 Pure substance. This study shows a purity of 97.9%. 0 Substances that are stable in water. Hydrolytic studies have been conducted at the 3M Environmental Laboratory showing stability (Report # W1878). DATASUMMARY 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 (LIMS #E00-1716), Page 13'of 138 BACK TO MAIN Table 8a. PFOS TCR-00017-046Solubility in Natural Seawater Data Summarv DW 1 mhifuge Tube #I ~ a 1yh b i f u g e Tube #2 ~ a 1 ymbifuge Tube #3 DW 2 Centrifuge Tube #I Rep 1: 012201-mwPF0S-1.'1.1 Rep2: 012201-~vvPFOS-l:l.2 Rep 3: 012201-~~~PFOS-l.'I.3 - RW4: 012201-~~PFOS-l.'I.4 Rep 1: OI~~OI-SWP-F1.O:!.S1 Rep 2:OI~~OI-SWPF-1.O:!S.2 Rep 3:012201-~~PF-O1.S2!.3 - Rep 4:012201-SWPFOS-1.:!.4 Rep 1:012201-SWPFOS-I.~~.1 Rep 2:012201-MPFOS-1.3.2 Rep 3:012201-SWPFOS-1.3.3 - Rep 4:012201-~PFO-S1.3.4 Rep 1: OI~~OI-SWPF-O2,S'l.l Rep 2:OI~~OI-SNPF-2O.`1S.2 Rep 3:012201-SWPFOS-2.'1.3 Rw,4:OI~~OI-SWPF-O2.S`1.4 DW 2 Centrifuge Tube #2 Rep 1: OI~~OI-SW~P-F2O2.S1 Rep 2: OI~~OI-SWP-F2O2S.2 Rep 3:012201-~PFO-S22.3 Rep 4:OI~~OI-SWP-F2O.S24 Day2 &nt,-jh,ge Tube #3 ~ a 3yCenmge Tube #1 Rep I: 0 1 2 2 0 1 ~ ~ P F O-2S3.1 Rep 2: 012201JHfpK)s- 2 3 2 Rep3: 0 1 2 2 0 1 ~ ~ ~ P F-O23S3 Rep4: 0 1 2 2 0 1 ~ ~ P F O-2S34 Rep 1: 012201-SM'FOS -3,'I.l Rep 2: O I ~ ~ O I - S M P F-O3S.'1.2 Rep 3:012201-~PFO-S3.l.3 Rep4: 012201~rPFOS-3.'1.4 DW 3mbifuge Tube #2 Tube #3 Rep 1: 012201-~rPFOS3.:1.1 Rep 2:012201-~~rPF-O3S.22 Rep 3:012201-SMrPFOS32.3 - Rep 4:012201-~~rPF-O3.:S!.4 Rep 1: 012201-~~rPF-O3.S3.1 Rep 2: 012201-~~rPF-O3S.32 Rep 3:OI~~OI-SMP-F3.O9S.3 Rep 4:012201-~~rPF-O3.S3.4 12.3 12.7 12.6 12 9 11.6 12.0 11.7 11.6 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 15.3 15.8 16.0 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 .O% 11.8 0.10 0.8% 11.9 0.18 1.5% 15.6 * 0.39 2.5% `Excluded via Dixon's Q-Test 14.5 0.10 0.7% 13.3 0.17 1.3% 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 I Rep 1: 012901-natJPFOS-1.1.1 22.2 Day 1 e n m g e Rep 2: 012901-natJPFOS-1.1.2 22.3 Tube #I Rep3: 012901-natJPFOS-1.1.3 21.7 I - Rep4: 012901-natJPFOS-1.1.4 22.8 22.30.45 2.0% oav1 an- Tube #2 I oay1 m Tube #3 m DW 2 Centrifuge Tube # I I DW 2 Tube #2 Rep 1: 012901-natJPFOS-1.2 1 Rep 2 012901-natJPFOS-1.22 Rep3: 012901-natJPFOS-1.23 Rep 4: - 012901-nadPFOS-1.24 Rep I: 012901-natJPFO.S-1.3.1 Rep 2: 012901-natJPFOS-1.3.2 Rep 3: 012901-natPFOS -1.3.3 Rep 4: - 012901-nacJPFOS-1.3.4 Rep 1: 012901~iPFOS-2.1.1 Rep 2: 012901-natiPFOS -2.1.2 Rep 3: 012901-naciPFOS-2.1.3 Rep 4: - 012901-natiPFOS -2.1.4 Rep 1: 012901-nacJPFOS-2.2 1 Rep 2: 012901-natiPFOS -2.2.2 Rep 3: 012901-naciPFOS -2.2.3 Rep4: 012901-natiPFOS -2.2.4 19.8 19.9 19.7 20. I 15.5 16.1 15.7 15.9 21.0 21.4 22. I 24.4 28.1' 20.3 19.9 19.9 19.9" 0.17 0.9% 15.8- d. 26 1.6% 22.2 1.52 6.8% 20.0 0.23 1.2% 'Rep 1excluded via DEton's Q-Test D~~2 mmge Rep 2: 012901-naciPFOS-2.3.2 Tube #3 Rep 3: 012901-naciPFOS -2.3.3 Rep 4: 012901-m1PFOS -2.3.4 18.1 17.9 17.8 17.5 17.8 0.25 1.4% 21.2 I D~~3m e Rep 2: 012901-natiPFOS 3.1.2 20.9 Tube # I Rep 3: 012901-natiPFOS 3.1.3 21.1 Rep4: 012901-nat~PFO.S3.1.4 21.1 21.1 0.13 0.6% Rep 1: 012901-natiPFO.S3.2.1 20.4 I D~~3 centrifuge Tube #2 Rep 2: 012901-natiPFOS 3.2.2 Rep 3: 012901-natiPFOS -3.2.3 20.3 20.1 19.4 20.1 0.45 2.2% Rep 1: 012901-naciPFOS-3.3.1 18.6 18.5 D? 3 centrifuge II Tube#3 Rep 2: 012901-~tiPFOS3.3.2 Rep 3: 0 1 2 9 0 1 ~ i P F O S-3.3.3 - Rep4: 012901-~tiPFOS-3.3.4 ..Triplicates not excludedvia the Q-Test. However,when Ule triplies for solubilitywas therefore excluded. 18.5 18.1 18.6 Day 1 were averaged, the %CV was outslde of the 0.24 1.3% acceptable range. The Day I FACT-TCROOS (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. I I I 7- Day 1 I I I I I Day 2 I I I Day 3 12.2 pglrnL 11.9 pg/mL 13.2p g h L ~~ 0.47 0.07 ~~ 1.30 0.6% --r-7in The solubility of PFOS TCR-0~0017-046in natural seawater was determined to be 12.,4pglmL at 22-23 "C. Table 9b. Summary Table of Solubility of PFOS TCR-00017-046 in an Aqueous solution of 3.5% Sodium Chloride. Excluded 20.0 pglrnL 19.9 pg/rnL Excluded 2.20 1.31 11.O% 6.6% STATISTICAMLETHODS 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 CONCL.USIOIN Under the conditions of the present study, the solubility of PFOS TCR-00017-046 in natural seawater and an aqueous sollution 0%3.5% sodium chloride is 12.4 pglmL at 22-23 "C:and 20.0 pg/mL at 22-24 OC respectively. FACT-TCROO2 (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 (OPPT3) 830.7840 Water Solubility: Column Elution Method; Shake Flask Method. EPA 712-C-96-041 August 1996. 2. OECD 105: Water Solubility. Adopted 27Julyl 1995. LISTOF ATTACHMENTS Attachment A: Extraction and Analytical Methods 0 Attachment B: Data Summary Tables 0 Attachment C: Sample Chromatograms 0 Attachment D: Deviations from the Protocol 0 Attachment E: Sample Calculations ~ ~ ~~ FACT-TCROOZ (LIMS #E00-1716), Page 17 of 1:38 BACK TO MAIN SIGNATURPEAGE We certify that this report is a true and complete representation of the data for this phase of the study: Principal Analytical lnvest!igator William K. Reagen Laboratory Manager Date FACT-TCROOZ (LIMS #E00-1716),Page 18 of 1:38 BACK TO MAIN ATTACHMENAT: EXTRACTIOANND ANALYTICALMETHODS 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 siince it gives more details on the actual prccedures, this new version is presented instead. FACT-TCROOZ (LIMS #E00-1716), Page 19 of 138 BACK TO MAIN 3M ENVIRONME- NT]ALALBORATORY SHAKE FLASKMETHOD::SOLUBILITYDETERMINATIOOFNA TESTSUBSTANCEIN 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 1.0 Scope and Application 1.1 Purpose. According it0 the United States Environmental Protection Ageincy ( 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 (OECDGuideline 105, and OPPTS Guideline 830.7840). The prerequisite to this' method is a preliminaxy screen of the test compound for its approximate solubility level. Refer to ETS-8-170.0 for the preliminary solubility screen test procedures. Initial ETS-8-172.1 Page 1 of 11 T e ~ A ~ ~ ~ ~ 71~6), P~ageg20 o~f I3~8 ~ ~ ~ ~ O O - l 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 METHO~D 2.1 Using the qualitativehemi-quantitativedata 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, dluplica.te, 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 inciibatorhhaker set to 30 "C -I 2 "Cyshaking 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 : l O or higher with a suitable solvent for analysis via LCMS. At approximately 48 hours and 72 hours, the second and third sets, respectively, will be pulled, equilibrated, centrifuged, aliquoted and diluted with a suitable analytical solvent for LCMS analysis. Depending on the analytical range, dilutions may be made using a diluter or syringe to make successive serial dilutjons using a suitable analytical solvent to reach the desired concentration (e.g. 1:10 or higher samp1e:methanoVacetone serial dilutions), and an appropriate internal stmdarcl (e.g. 1HY1H,2H,2Htetrahydroperfluorooctane sulphonic acid (THPFOS)) will be added to the final dilution prior to analysis. Samples are to be analyzed via LCMS a.gainst a standard curve containing the test substance and an appropriate internal standard. 3.0 DEFINITIONS 3.1 Method blank: An arialyte-fkee matrix (e.g. methanol, water, or acetone) to which all reagents agree are added in the same volumes or proportions as used in tlhe sample processing. The method blank is used to document contamination resulting fiom the entire sample treatment and analytical process. The method blank is canied through the complete sample preparation, treatment, and analytical procedure. 3.2 Solvent blank: A sample of analyte-free medium (e.g. methanoVwater/acetone solution) that is not taken through the sample treatment process. This blank is used to evaluate instrument and reagent contamhation. 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 rnianner. 3.4 Sample replicates: Replicate samples (two or more) taken from and representative of the same sample source ('2.8. 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 anadytical behavior to the compound(s) ofinterc:st, added to all samples and standards, and carried through the entire measurement process. ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCROO2 (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 WARNINGS 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 solvei~tsin i i 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 13azard 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 sufficientlyrinsed with solvent prior to their usage. 5.0 INTERFERENCES 5.1 Impurities may significantly affect the solubility of the test substance. "lie purity of the test substance should be known and documented prior to starting the preliminary solubility screening procedure. 5.2 Contaminants in solveints, reagents, glassware and other sample processing or analysis hardware may cause in.terference. The routine analysis of laboratory method blanks must ' be used to demonstrate:that fhere is no interference under the conditions of the analysis. 6.0 EQUIPMENT 6.1 Analytical balance sensitive to1 0.1 mg. 6.2 Centrifuge capable of holding 15 mL centrifuge tubes or equivalent. 6.3 Incubator with heatingkooling capabilities. 6.4 Diluter, Hamilton Microlab@.500Series, or equivalent. 6.5 Vortex-mixer. 7.0 SUPPLIES AND MATERIALS 7.1 Thermometer capable of readi ng at least 15 'C-40 OC. 7.2 5-250 mL polypropylene centrifuge tubes, or equivalent. 7.3 Disposable glass graduated pipettes, 1mL to 10mL. 7.4 Disposable glass pastew 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 k 1% of the total volume), 5 pL to 1000 pL. 7.8 Pipette-man manual pipettor. ETS-8-172.1 Soliibility Test: Shake Flask Method FACT-TCROO2 (LIMS #E00-1716), Page 22 of 138 Page 3 of 11 BACK TO MAIN 8.0 SUPPLIES AND MATERIALS 8.1 Methanol (MeOH), PILC/SPEC/GC grade from EM Science, or equivalent. 8.2 Acetone, HPLC/SPEC/GC grade from EM Science or equivalent. 8.3 Water, ASTM Type 1. 8.4 Test substance of known purity. . 8.5 Calcium Chloride Dihydrate, Approximately 99% or better, from Sigma. 8.6 0.01 M CaClz solution, Example: A 0.01 M CaC12 stock solution is prepared by weighmg 1.4 g CaCl2 in a weigh boat and transferring to a 1 L volumetric :flask and diluting to the mark with Milli-QTMwater. 9.0 SAMPLHEANDLING 9.1 Record times of initial preparation, set-up, and sample aliquotinghalysis on a sample preparation sheet or logbook. 9.2 Once the samples have been diluted, they may be analyzed via LCMS. Aliernatively, 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 QUALITYCONTROL 10.1 Shake Flask Sample Triplica~tes.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 accruedl throughout the sample preparation process. The method blank is carried throug,hthe same sample preparation procedures as the three test vessels with test substimce, only no test substance is added throughout the entire procedure. 10.3.2 Solvent Blank. An aliquot of the dilution solvent (Le. methanol) directly analyzed for possible contaminants. The solvent blank is used to document any possible contamination of the solvent(s) used during the sample preparationtprocess, and to detect any instnunentail 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 FIask Method FACT-TCR002 (LIMS #E00-1716),Page 23 of 138 Page 4 of 1 1 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 STANDAIXIZATION 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 preliminay solubility screen test (ETS-8-170.0). 12.1.2 Weigh out test substance into a tared test vessel ( e g 15 mL polypropylene centrifbge tube). 12.1.3 Add the test solvent to the test vessel gravimetrically until the desired volume has been obtained (note: solvents have diflering 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 conlimi that there are undissolved particles. If no particles are present, repeat 12.1.2 with 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 I ,-Rep 2, and - Rep 3; and Day 3, -Rq) 1, -Rep 2, and -Rep 3. Also include the dqy of initial sample prep, the persoii(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. Midshake test vessel to ensure contact between the test substance and the s;olvent. And wrap- the cap With tape. 12.2 Equilibration of samples. 12.2.1 Place all of the test vessels on their side (horizontal) in an orbital incubator set to approximately 30 OC & 2 "Cand rotating at a considerable speed to ensure sufficient contact/mixing between the test substance and solvent. 12.2.2 At approximately 24 bows, four test vessels are removed: three containing test substance labeled "Day l,Repl", "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 actual1temperature) for about a 24 hour period. 12.2.5 After about 24 h'oursof equilibration at 20 "C-26"C, centrifbge the samples until the solution is visibly clear. If micelle formation is suspected, an additional highspeed centrifbgation step may be added (20,000 RCF for approximately 1 hour). The test vessels are n o w ready for dilution. See section 12.3 for fbrther sample preparation. ETS-8-172.1 Solirbility Test: Shake Flask Method FACT-TCROOZ (LIMS #E00-1716), Page 24 of 1:38 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,Replyy"YDay2,Rep2", "Day2,Rep3", and "Di~y2,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,ReplYy, "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 sixface of the solution, it may be necessary to pipette off the top layer of solution (or an aliquot of sample may be centrifbged 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 of pipette to be wed, take into consideration the test substance 's tendency to adsorb to certain materials (i.e. adsorption of test substame to glass or plastic). 12.3.2.2 Prior tci aliquoting sample to the autovial, the pipette tip must be equilibmtedsaturated with the test solution by drawing and gently expelling the test solution in and out of the pipette tip, taking care nol. 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 samp1e: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 T o the final analytical sample, add internal standard at a concentration suitable to the analytical method. 12.3.7 Samples will be analyzed via L C M S against a standard curve of varied, known concentrations of test substance with a constant concentration of internal standard equal to the colncentri~tionin the samples. 13.0 DATAANALYSIASND CALCULATIONS 13.1 Samples will be analyzed via a calibration curve. The amount of test sulxtance 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 individual1entities. 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 based on the individual entities (n) being less than 30: ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCROOZ (LIMS #E00-1716),Page 25 of 138 Page 6 of 11 BACK TO MAIN 13.4 Sample precision will he reported as %RSD (or %CV). Sample precision will be calculated using the following equation: Ah3 X 100 = Sample %RSD where: A= standard deviation of averaged samples B= average of samples I I Sample RPD will be cidculated using the following equation: A-B /((A+13)/2)= Sample RPD where: A= concentration of first replicate B= concentration of second replicate observations 4 5 Qtnbulated, 90% Confidence - Range 0.886 0.679 0.557 14.0 DATAANALYSIASND 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 ilverage and precision is re-calculated and reported without the questionable data .point. Document the non-compliant data on data summary sheets, and include results of the statistical analysis with the final results. 14.1.1 14.1.2 Sample replicate %PLSD'sshould be 45%. If the average of the sample triplicate data is >15% ItSD, evaluate the threevalues 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 fiom 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 lie used in the final reported data. `Theremaining shake flasks for the timepoint shall be used to report the data. 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 of 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 4 5 % for the shake flask method. If this criteria is not met, it may be necessary to re-evaluate the data for possible 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-dilutehe-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 Contrcil Blank. 14.3 Quality Control Blanks: Method and Solvent Blank samples. The level of analyte (test analyte OR internal startdard analyte) shall be less than 50% of the area counts of the LOQ. If background lewels 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 other indicators that either the samples or the instrument contain significant background levels of analyte). 15.0 POLLUTIOPNREVENTIIONAND WASTEMANAGEMENT 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 -0ECD Guideline 105: pp. 1-7, Adoptedl 1995 18.2 United States Environmental Protection Agency. OPPTS 830.7860 Water Solubility (Generator Column Method:).Prevention, Pesticides and Toxic Substances: Fate, Transport and Transfclrmation Test Guidelines. EPA 7 12-C-96-042: pp. 1-17, 1996 18.3 United States Environmental Protection Agency. OPPTS 830.7840 Water Solubility: Column Elution Method; Shtake Flask Method. Prevention, Pesticides anti Toxic ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCROO2 (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 Chernicalhalysis. ed.; W.H. Freeman and Company: New York, 1982; p 70-71. 18.6 Natrella, Mary Gibbons. Tht: Treatment of Outliers. Experimental Statistics, National ` Bureau of Standards Handbook 91; US.Government Printing Office: Washington, D.C., 1963; Pages 17-3, and T-27. 19.0 AFFECTEDDOCUMENTS 19.1 ETS-8-170.0, "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents." 20.0 REVISIONS . Revision Number Reason For Revision 1 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 centrifugationstep was added. Fixed the incorrwt numbering of sections 13.5 through 14.3. Section 14.3, more clearly defined the acceptance criterion for method and solvent blariks. Revision - Date 03-27-01 ETS-8-172.1 Solubility Test: Shake Flask Method FACT-TCROO2 (LIMS #E00-1716),Page 28 of 138 Page 9 of 11 BACK TO MAIN ATTACHMENTA: Example Sample Preparation Sheet @age I of 2). Temperature of Study: 0 .. 3M F o v i r o i Sample preparation worksheet Test Substance: ID& Source: Date: Test Solvent: IDI: Test Vessel: drill Source: Was the solubility screen test performedprior to staff? Y/N lf so, what is the appmxlmate concentretion?ucr/ml -SFMvials IW: "samplelD" samplelDl.l.1 thru -1.1.4 Balance ID: Sample Descrfptlon Dayl, Smpl welght test subrtance added: Thermometer ID Total mass (solute i solvent) added: RoomTemp: a 'Internal Standardaddltlon U U mls IS added to dllutlon factoc 1: Study # Analyst(s): 15hcenlrlfuge lube/Other(spedfy)' "(; Dateilimellnitials: Obse~vrtlonslComment:s A 2 Test Vessels sealed w/ tape? YN Test Vessels sPakerVvortex-mixed? YRJ Q, Y Test vessels placed on orbital Incubator?Y/N IncubatorID: Speed: rpm InitialTemperature: 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 0 rID Visual observations: Datdndnllials: - ETS-8-172.1 Solubility Test:Shake Flask Method Page 10 of 11 BACK TO MAIN ATTACHMENTA CONTINUED (page2 of 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. DaWimdlnlUah: I I Location of samples: Visual observations: I I I "Day 1" Test Vessels Centrifuged: Cent. ID: Temperature of environment 0 RPM or RCF readout duration: ID mia DateJTimellnlUak 1 Visual observations: -Four aliquots from each of the four samples are to be made into glasdplastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution -1: with methanol. Methanol TN-A: Additional dilutions: Dilution factor (test so1ution:methanol): 1: X's how many dilutions: I\I/-S t o r e s a m p l e s a n d extracts Diluter ID u in a cooler at sed until time o f analysis. Amounts used: Cooler ID: ui meihanoi. Cooler Temp: =final dilution factor: 1: 0 DateJTimdlnilials: U..IIaaliipica DatefrimdlniUals: ~ 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. Location of samples: Temperature of environment 0 r ID: Visual observations: Datefrhndlnihals: Visual observations: ,Day 4 h t approx. 24 hoursof equilibration, the 'Day 3' samples are to be aliquotedlextracted. Environment Temp.: Test Vessels Centrifuged: Cent. ID: RPM or RCF readout duration: "(;Them. ID min, Visual observations: I -Four aliquots from each of the four samples are to be made into glasslplastic autovials (also, check autovials for correct labeling). YeSMo DalerrhellnlUals: ETS-8-172.1 Solubility Test:Shake Flask Method Page 11of 11 BACK TO MAIN 3M ENVIRONMEP?TAI, LABORATORY METHOD ANALYSIS OF POTASSIUM PERFLUOROOCTANESULFONATE OR OTHER FLUOROCHEMICIKNLWSASTE STREAM OR WATER EXTRACTUSSING HPLC-ELECTROSPRAYMASPSESCTROMETRY Method Number: ETS-8-155.0 Author: Mark L. Anderson, IVIark E. Ellefson Approved By: Adoption Date: l(/fO/OU Revision Date: Laboratory Manager Date Word 97 ETS-8-155.0 Page 1of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospraymass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 31 of '138 BACK TO MAIN 1.0 SCOPE AND APPLICATION - 1.1 Scope: This method describes tlhe analysis of waste stream or water extracts using HPLC- electrospray/mass spectrometry. 1.2 Applicable Compounds: Fluomchemicals 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 fluorochemicalsor other electrosprayionizable compounds extracted fiom water, using HPLC-electrospraymass 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, dz:= 499 or perfluorooctanoate (PFOA), ndz = 413. 3.0 DEFINITIONS - 3.1 Atmospheric Pressure Ionization (MI):The Micromass Platform LCZ single quadrupole system and other commerciallyaivailable LCMS systems allow for various methods of ionization by utilizing a variety of sources, probes, and interfaces. These include but are not limited to: Electrospray Icmization (ESI), Atmospheric Pressure chemical Ionization (APcI), Thermospray, etc. The ianizatica in these processes occurs at atmosphericpreasure (i.e., not under a vacuum). 3.2 ElectrosprayIonization (ES,ESI): A method of ionization performed at airnospheric pressure, whereby ions in soluticin 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):'ThePlatform LCZ and other commerciallymanlufactured ESNS systems are equipped with a single quadrupole mass selective detector. Ions are selectivelydiscriminated 1)ymass to charge ratio ( d z ) and subsequentlydetected. 3.4 Conventionalvs. Z-spray probe interface: The MicromassPlatform LCZ system utilizes a "Z-spray" conformatioin. 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 coiiventic~naclomponents are not compatiblewith one another, but only with similar systems (i.e., 2:-spray components are compatible with some other Z-spray systems, etc.). Other commercialllymanufacturedESNS systems may have similar features. 3.5 Mass Lynx Software: System softwaredesigned for the specific operation (ofMicromass LCZ Mass spectrometer. Curreiitly 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-8-15 5 .O Page 2 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluomchemicals in Waste Stream or Water Extracts Using KPLC-Electrospray/Mass Spectrometry FACT-TCR002 (LIMS #E00-1716),Page 32 of 138 BACK TO MAIN 4.0 WARNINGS AND CAUTIOlNS 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 pump:sbelow a backpressure of 400 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 interfkrenlces whim analyzing samples, Teflon should not be used for sample ' storage or anypart of instrumentation that comes in contact with the sample c r extract. - 6.0 EOUIPMENT 6.1 Equipment listed below may be modified in order to optimize the system. Document any modifications in the raw data izs 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 colunzn, such as a Betasil C18 column (5Ox2mm, 5 pi711particle size) or equivalent. 7.1.3 Capped autovials or capped 15 mL centrifbge tubes. ETS-8-155.0 Page 3 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Waler Extracts Using HPLC-Electrospray/Mass S,pectrometry 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-QTMwater (ASTM type I), all water used in this method should be Milli-QTM water or equivalent, an.d 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 mA4 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 lhmks (Milli-Q water), two matrix blanks, and solvent standards are prepared during the sample extraction procedure. 9.0 SAMPLHEANDLING - 9.1 Standardsand sample e:xtracts,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 refiigerated a.t approximately4" 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 anailyzed with each sample set to dete:rmine 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 IATiciency. 10.2.2 Matrix spike duplicates are prepared periodically to measure the precision associated with the analysis. 10.2.3 Analyze the matrix spike and matrix spike duplicate (if prepared) in the same run as the original sample. 10.2.4 Matrix spike and matnix spike duplicate concentrations should fkll in th.e 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-ElectrosprayMass Spectromletry FACT-TCROOZ (LIMS #E00-1716), Page 34 of 138 BACK TO MAIN concentration ofthe arialyte. 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 Continuingcalilxation verifications (CCV) are analyzed to veri@the continued accuracy of the calibration curve. 10.3.2 Analyze a mid-range calibration standard after every tenth sample, with a minimum of one per sample set. 10.4 Internal StandardlSuirrogate Standard 10.4.1 An internal standard Q[S)may be used to quantifl the target analytes by establishing a relationship between the ratio of analyte response to IS response and a known concentration OF the arialyte of interest. The IS shouldbe spiked at an amount that will fd1 within Ihe mid-range of the calibration curve. The IS should be added after the extraction process and before analysis. 10.4.2 A surrogate standard rnay 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 CALIBRATIONAND STANDARDIZATION - 11.1 Analyze the standard cimes prior to and following each set of extracts. The average of two standard curvesmay be plotted by linear regression (y = mx + b) weighted l/x, or quadratic fit (y = ax' + bx + c) using MassLynx or other suitable software. The Calibration curves should not be forced through zero. 11.2 If the calibration curve does not meet acceptance criteria perform routine maintenance or prepare a new standard curve (if necessary) and reanalyze. 11.3 For purposes of accuracy when quantitating low levels of analyte, it may be ntxessary to use the low end of the calibration curve rather than the full range. Example: when attemptingto quantitate approximately 10ppb of analyte, generate a calibratica curve consisting of the standards fi-om5 ppb to 100 ppb rather than the full range ofthe 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 of the instrurnent (1'for Tucker), the year (00 for 2000), the month (04 for April), and the day (TO01012for October 12,2000). If more than one list is made on the same clay, use increasing letters of the alphabet startingwith A at the end of the list. ETS-8-155.0 Page 5 of 9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicalsin Waste Stream or Water Extracts Using HPLC-ElectrospraylMass Spectrometry FACT-TCROOZ (LIMS #E00-1716), Page 35 of 1:38 BACK TO MAIN 12.1.1.2 Assign. a metlhod (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 metlhod, 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 $appropriatemasses. A full scan is usually collected in addition to the SIRs. Save acquisition method. ' See the Micromass MassLynx GIJIDE 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 carrycwer. 12.2 Using the Autosampler/CohimnHeater 12.2.1 Place sample vials into the sample tray according to the sample list prqmred in Section 12.1.1. 12.2.2 Attach the propz 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 HP1 LOO 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 pUmin. 12.1.1.3 Cycle time = 10.0 minutes 12.1.1.4 Mobile phase components: Solvent A 2.0 mM Ammonium Acetate Solvent B: Methanol (MeOH) Solvent Gradient: Time (min.1 0.00 1.oo 4.50 8.00 8.50 10.0 - % B 5.00 'Yo 5.00 'Yo 95.0 Yo 95.0 % 5.00 'Yo stop ETS-3-155.0 Page 6 of9 Analysis of Potassium Perfluorooctanesulfonateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrosprayhlass S:pectrometry FACT-TCROOS (LIMS #E00-1716), Page 36 of 1:38 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 of the Micromass Platform LCZ ' Electrospray/M:assSpectrometer". 12.4.2 Check the solvent lever1in reservoirsand 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, disassemblethe probe and replace the stainlesssteel 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 Obserfe droplets coming out of the tip of the probe. A fine mist should be expelled with1 no nebulizing gas leaking around the tip of the 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 instrumentuses tliese parametersat the followingsettings. These:settingsmay change in order to optimize the response: 12.4.6.1 Drying gas 250-425 literhour 12.4.6.2 ESI ne:bulizing gas 10-15 literdhour 12.4.6.3 HPLC constant flow mode, flow rate 10 - 500 pIfmin 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 applicableinformationand storeit in the study binder with copies taped into the instrument run logbook. 12.4.7.1 All colpies 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 DATAANALYSIS AND C:ALCUILATIONS 13.1 Calculations: 13.1.1 Calculatematrix spike percent recoveries using the followingequation: ETS-8-155.0 Page 7 of 9 Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicalsin Waste Stream or Water Extracts Using HPLC-Electrosprayhlass Spectrometry FACT-TCR002 (LIMS #E00-1716), Page 37 of 138 BACK TO MAIN % Recovery = Observed Result - Backnound Result x 100 Expected Result 13.1.2 Calculate percent difference using the following equation: % Difference= Exiiected Conc. - Calculated Conc. x 100 Expected Conc. 13.1.3 Calculate actual concentration of analyte in matrix (pg/mL): On-Column Concentration o.~g/mL)x Dilution Factors = Calculated Concentration 14.0 METHODPERFORMANCE 14.1 The Limit of Quantitation (LO@ 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 < ?hthat of the lowest standard used in the calibration curve. 14.3 The coefficient of determination(2)value for the calibration curve must be greater than or equal to 0.980. 14.4 Continuing Calibration Verification (CCV) percent recoveries must be f 30% of the standard concentration. 14.5 Internal Standard recoveries should be within k 50% of the spiked concentration. 14.6 If criteria listed in this method performance section are not met, maintenance may be performed on the system and :jamples reanalyzed or other actions as determined by the analyst. Document all ;actionsin 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 PREXEWMON AND WASTE MANAGEMENT 15.1 Sample extract waste and flanunable solvent is disposed in high BTU containtas, and glass pipette waste is disposed in bIoken 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 metliod, integration method, sample name, extraction date, dilution factor (if applicable), and analyst. 16.2 Print the tune page, sample list, and acquisition method fiom MassLynx and other applicable information to include in the appropriate study folder. Copy these pages and tape into the instrument runlog. 16.3 Plot the calibration curve then print these graphs and store in the study folder. ETS-8-155.0 Page 8 of 9 Analysis of Potassium Perfluorooctanesulhnate or Other Fluorochemicals in Waste Stream or Wa.ter Extracts Using HPLC-ElectrosprayMass Spectrometry FACT-TCROOP (LIMS #E00-1716),Page 38 of '138 BACK TO MAIN 16.4 Print data integrationsummary, integration method, and chromatograms,from MassLynx, and store in the study folder. 16.5 Summarize data using suitabl'esoftwareand store in the study folder. 16.6 Back up electronicdata to appropriate medium. Record in study notebookthe file name and location of backup electrcaic data. 17.0 ATTACHMENTS 17.1 None - 18.0 REFEXENCES - - 18.1 Platform LCZ User's Guide, bdicromass UK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.2 MassLynx NT User's Chide, lvlicromassUK Limited,Tudor Road, Altrimham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kingdom. 18.3 MassLynxNT Guide To Data Acquisition,MicromassUK Limited, Tudor Road, Altrincham, WA14 5RZ; or Floats Road, Wythenshawe M23 9LZ; United Kirtgdom. 18.4 ETS-9-36.0, "Operation and Maintenanceof the Micromass PlatformLCZ Electrosprayhlass Sprectrometer". 19.0 AFFECTEDDOCUMENTS 19.1 None 20.0 REVISIONS Revision Number. - Reason For Revision - Revision - Date ETS-8-155.0 Page 9 of9 Analysis of Potassium Perfluorooctimesulfc~nateor Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrosprayh4ass Spectrometry FACT-TCROOZ (LIMS #E00-1716), Page 39 of 138 ATTACHMENBT: DATASUMMARTYABLES BACK TO MAIN FACT-TCROOZ (LIMS #E00-1716), Page 40 of 138 BACK TO MAIN TCR-002, 012201-~~PFOS-1.4.41,00X Dil. WPFOS-1.4.4 Method Blank. SFM 01-24-01 MEE(ML4) MeOH Blank TN-A-4740. 04 Dec 00 TCR-002.012201-swPFOS-1.1.1,100DXil. SWPFOS-1.1.1 SFM 01-24-01 MEE(MLA) TCR-OOL, 012201-swPFOS-1.1.2, 100X Dil. S W P F O S - ~ .S~F.M~ 01-24-01 MEE(ML4) TCR-OOZ.012201-swPFOS1.1.3, 1OOX Dil. SWPFOS-1.1.3 SFM 01-24-01 MEE(ML4) TCR-002, 012201-wPFOS-1.1.4. 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 100X Dil. TCR-002.012201-swPFOS-1.2.1,10D0ilX. SWPFOS-1.2.1 SFM 01-24-01 MEE(MLA) TCRM)2, 012201-~wPFOS1.2.2,1OOX 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(ML4) TCR-002, 012201-swPFU5-i2.4, i K X Dii. SWPFOS-1.2.4 SFM 01-24-01 MEE(ML4) MeOH Blank TN-A-4740. 04 Dec 00 TCR-00Z,012201-swPFOS-1.3.1,100XDil. SWPFOS-1.3.1 SFM 01-24-01 MEE(MLA) TCR-002,012201-swPFOS1.3.2.IMlX Dil. SWPFOS-1.3.2 SFM 01-24-01 MEE(ML4) TCR-002,012201-swPFOS-1.3.3, 100X Dil. SWPFOS-1.3.3 SFM 01-24-01 MEE(ML4) TCR-002,Ol 2201-SWPFOS-.13.4, IOOX Dil. s~PFOS-1.3.4SFM 01-24-01 MEE(MIA) 01003-07-09 100.2ppb PFOS. CCV MeOH Blank TN-A4740. 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 1Oppb PFOS 01003-07-05 25ppb PFOS 0100507-06 40ppb PFOS 01003-07-07 50.lppb PFOS 01003-07-08 75.lppb PFOS 01003-07-09 100.2ppb PFOS i J j X M 7 - i G 252,:ppb pFcs 01003-07-11 01003-07-12 01003-07-13 MeOH Blank MeOH Blank 400.8ppb PFOS 501.0ppb PFOS 1002.0ppb PFOS TN-A-4740. 04 Dec 00 TN-A-4740. 04 Dec 00 43 H0125Al.M HILL0043.D 24 44 H0125Al.M HILLW44.D 93 45 H0125Al.M HILL0045.D 31 46 H0125Al.M HILL0046.D 32 47 H0125Al.M HILL0047.D 33 48 H0125A1.M HILL0048.D 34 49 H0125Al.M HILL0049.D 9 50 H0125Al.M HILL0050.D 93 51 H0125Al.M HILL0051.D 93 52 HO125Al.M HILL0052.D 35 63 ?e 54 H0125Al.M HILL0054.D 37 55 H0125Al.M HJLL0055.D 38 56 H0125Al.M HILL0056.D 94 57 H0125AI.M HILL0057.D 39 58 H0125Al.M HlllW58.0 40 59 H0125Al.M HILL0059.D 41 60 H0125Al.M HILL0060.D 42 61 H0125Al.M HILL0061.D 9 62 H0125Al.M HlLL0062.D 94 63 H0125Al.M HILL0063.D 94 64 H0125Al.M HlLL0064.D 94 65 H0125Al.M HILL0065.D 1 66 H0125Al.M HILL0066.0 2 67 H0125Al.M HILL0067.D 3 68 H0125Al.M HILL0068.D 4 69 H0125A1.M HlLL0069.D 5 70 H0125Al.M HILL0070.D 6 71 H0125Al.M HILL0071.D 7 72 H0125Al.M HILL0072.D 8 73 H0125Al.M HILL0073.D 9 74 H0125Al.M HILL0074.D 10 75 H0125A1.M HILL0075.D 11 76 HOIZAI.M n i u ~ 7 6 . 0 12 77 H0125Al.M HILL0077.D 13 78 H0125Al.M HiLL0078.D 94 79 H0125Al.M HILL0079.D 95 4.11 2,194,236.0 0.00 0.0 4.11 2,102,494.3 4.11 2.1 58.897.3 4.11 2.209.667.8 4.11 4.1 1 0.00 0.00 2.201.234.8 2,265,761.0 0.0 0.0 4.11 2,127,831 .O A 11 2.140.157.8 4.11 2,234,175.8 4.11 0.00 2.1 33.1 77.8 0.0 4.11 2,171,835.0 4.11 2,169,104.3 4.11 2,169,278.8 4.11 4.il 0.00 0.00 0.00 4.11 4.11 4.11 4.1 1 4.11 4.11 4.11 4.11 4.11 4.11 4.1 1 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,i54.0 2,213,476.0 2,203,661.3 0.0 0.0 254.0 0.0 254.0 254.0 254.0 254.0 254.0 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 0.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 IC. n La." 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 4.85 4.86 4.86 0.00 0.00 1,141,147.0 0.0 1,112.681.4 1,116.756.6 1.1 19,839.4 1,126,401.0 1,118.630.0 0.0 0.0 1,118,494.1 1,113.286.9 1.141.315.6 l,izi,!33i.i 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 1,103.58 1.8 1,145,372.3 1.132,338.8 1,155,401 .O 1.134.933.8 1.146.786.6 1.137.&23.9 1.132,096.5 1.1 30,818.8 1,132,445.8 I,!!5.520.0 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 5.14 0.00 0.00 4,009,264.5 3.109.402.5 0.0 0.0 131.9 102.2 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 .c3. 1I.* 0.00 3,507,278.5 0.0 !!%A 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.o00.9 0.0 0.0 2.0% 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% S o h b f i . Shake Fbrk Mamod 5117RWl FACT-TCRQR RAW DATA Agilenl 1100HPLC/MSD "Hillary" Acquistion Run: H010126 PFOS in Natural Seawater Shake Flask Method Day 2 Raw Data BACK TO MAIN MeOH Blank 01003-07-01 0100%07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-0(1 0100307-07 01003-07-08 0100307-09 01003-07-10 01003.07-11 0100307-12 01003-07-13 MeOH Blank MeOH Blank MeOH Blank MeOH Blank TN-A-4740. 04 Dec 00 Oppb PFOS 2.5ppb PFOS 5ppb PFOS loppb PFOS 25ppb PFOS 40ppL ;os 5O.lppb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.0ppb 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 2 H010126C.M HILL0138.D 98 3 H010126C.M HILL0139.D 46 4 H010126C.M HILL0140.D 47 5 H010126C.M HILL0141.D 48 8 H010126C.M HILL0142.D 49 7 H010126C.M HILL0143.D 50 8 HOiOiZ6C.M HllL0144.D 51 9 H010126C.M HILL0145.D 52 10 HOlO126C.M HILL0146.D 53 11 HO10126C.M HILL0147.D 54 !2 HnlOl26C.M HILLO148.D 55 13 H010126C.M HILL0149.D 56 14 HO10126C.M HILLOl5O.D 57 15 H010126C.M HILLOl51.D 58 16 H010126C.M HILL0152.D 98 17 H010126C.M HILL0153.D 98 18 H010126C.M HILL0154.D 99 19 H010126C.M HILL0155.D 99 TCR-002. 012201-SWPFOS-2.4.1.l00X Dil. swPFOS-2.4.1 Method Blank. SFM 01-25-01 MEE(ML4) 20 H010126C.M HILL0156.D 59 TCR-002. 012201-SWPFOS-2.4.21, 00X Dil. SWPFOS-2.4.2 Method Blank. SFM 01-2501 MEE(ML4) 21 H010126C.M HILL0157.D 60 TCR-002. 012201-~~PFOS-1.4.310. 0X Dil. swPFOS2.4.3 Method Blank. SFMOi-25-01ME(MLA) 22 H010126C.M HILL0158.D 61 TCR-002.012201-swPFOS-2.4.4, 100X Dil. SWPFOS-2.4.4 Method Blank. SFM 01-25-01 MEE(MLA) 23 H010126C.M HILL0159.D 62 MeOH Blank TN-A-4740. 04 Dec 00 24 H010126C.M HILL0160.D 99 TCR-002,01220l-s~PFOS-2.1.1. 100X Dil. SWPFOS-2.1.1 SFM 01-2501 MEE(MLA) 25 H010126C.M HILLO161.D 63 TCR-002. 012201-SWPFOS-2.1.2, 100X Dil. swPFOS-2.1.2 SFM 01-2501 MEE(MLA) 26 H010126C.M HILL0162.D 64 TCR-002,012201s~PF0S-2.1.130.0X Dil. SWPFOS-2.1.3 SFM 01-2501 MEE(MLA) 27 H010126C.M HILL0163.D 65 TCR-002.012201-~~PFOS-2.1.41,00X Dil. swPFOS-2.1 .4 SFM 01-25-01 MEE(MLA) 28 H010126C.M HILL0164.D 66 0100307-09 100.2PPD PFOS, CCL' 29 H010126C.M HILL0165.D 54 MeOH Blank TN-A-4740, 04 0%00 30 H010126C.M HILL0166.D 99 MeOH Blank TN-A-4740. 04 Dec 00 31 H010126C.M HILL0167.D 100 TCR-002,012201-~wPFOS-2.2.1.100X Dil. swPFOS.2.2.1 SFM 01-25-01 MEE(MLA) 32 H010126C.M HILL0168.D 67 TCR-002. 012201-SWPFOS-2.2.2,100XDI. SWPFOS-2.2.2 SFM 01-25-01 MEE(MLA) 33 H010126C.M HILLO169.D 68 TCR-002. 012201-SWPFOS-2.2.3l0, 0X Dil. SWPFOS-2.2.3 SFM 01-25-01 MEE(MLA) 34 H010126C.M HILL0170.D 69 TCR-002. 012201-SWPFOS-2.2.4,100X Dil. SWPFOS-2.2.4 SFM 01-25-01 MEE(MLA) 35 H010126C.M HILL0171.D 70 MeOH Blank TN-A-4740, 04 Dec 00 36 H010126C.M HILL0172.D 100 0.00 4.1 1 4.11 4.11 4.11 4.11 4.11 4:: 4.11 4.11 4.11 4.11 4.1 1 4.11 0.00 0.00 0.00 0.00 0.0 2096939.6 2130418.5 2141519.8 2104440.5 2090968.0 2091922.9 10?512? 6 2114582.0 2099818.0 2100878.0 2115iOi.3 2092776.1 2112700.5 0.0 0.0 0.0 0.0 4.11 2043336.4 4.11 2117351.0 4.1 1 2050763.3 4.11 2056015.4 0.00 0.0 4.1 1 2073482.0 4.11 2018667.1 4.1 1 2037984.0 4.11 2037142.3 4.11 2060367.5 0.D 0.00 0.0 4.11 1998534.4 4.11 2011509.9 4.11 2076255.3 4.11 2085483.0 0.00 0.0 0.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 254.0 nci n L-." 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 0.0 254.0 254.0 254.0 254.0 0.0 M, bM.F)..X U.W Y17Ra31 0.00 4.92 4.92 4.93 4.92 4.92 4.93 4.93 4.93 4.93 4.93 4.9 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 4.92 000 0.00 4.92 4.92 4.92 4.92 0.00 0.0 1174597.3 1173146.4 1194294.9 1183290.1 1189051.O 1167906.5 1188761.4 1169898.0 1168198.0 1160032.3 1144943.4 1149592.4 1110896.4 0.0 0.0 0.0 0.0 1126808.I 1132002.3 1126241.6 1129527.3 0.0 1116196.9 1111698.8 1107790.4 1106298.8 1155895.6 0.0 0.0 1 107285.0 1102966.4 1119362.8 1109671.5 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 5.14 5.14 5.14 5.14 5.14 5.14 5% 5.14 5.14 5.14 5.14 5.14 0.00 0.00 0.00 0.00 0.0 0.0 81704.0 159329.1 284697.0 760289.3 1195676.5 ._ 1513715.1 o n-rncn, &&-,I"-. 2934306.3 7028210.5 10446112.0 12728626.0 22114552.0 0.0 0.0 0.0 0.0 0.0 0.0 2.2 4.7 8.9 24.8 40.2 50.2 76.6 100.9 251.9 392.0 488.4 993.7 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 0.0 0.00 0.0 0.0 5.14 3379581.8 122.1 5.14 3307267.8 119.9 5.14 3271451.3 119.0 5.15 5.14 0.00 0.00 3334039.3 2889710.8 0.0 0.0 121.5 100.2 0.0 n "_n " 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.O% 0.2% 0.2% 1.9% 0.7% 0.6% 2.2% 2.9% 0.8% 0.0% BACK TO MAIN FAfT-TCRm2 TCR-002,012201-swPFOS-2.3.1, 100X Dil. SWPFOS-2.3.1 SFM 01-2501 MEE(MLA) 37 H010126C.M HILL0173.D 71 TCR-002. 012201-swPFOS-2.3.2. 100X Dil. WPFOS-2.3.2 SFM 01-25-01 MEE(MLA) 38 H010126C.M HILL0174.D 72 TCR-002. 012201-swPFOS-2.3.3.100X Dil. SWPFOS-2.3.3 SFM 01-2501 MEE(MLA) 39 H010126C.M HILL0175.D 73 TCR-002. 012201-SWPFOS-2.3.4. 1OOX Dil. SWPFOS-2.3.4 SFM01-2501 MEE(Ml-4) 40 H010126C.M HILL0176.D 74 01003-07-09 100.2ppb PFOS. CCV 41 H010126C.M HILL0177.D 54 MeOH Blank TN-A-4740. 04 DS 00 42 H010126C.M HILL0178.D 100 MeOH Blank TN-A-4740. 04 DeC 00 43 H010126C.M HILL0179.D 100 MeOHBlank TN-A-4740. 04 Dec 00 44 H010126C.M HILL0180.D 90 01003-07-01 Oppb PFOS 45 H010126C.M HILL018l.D 46 0100347-02 2.5ppb PFOS 46 H010126C.M HILL0182.D 47 01003-07-03 5ppb PFOS 47 H010126C.M HlLL0183.D 46 01003-07-04 lOppb PFOS 48 H010126C.M HILL0184.D 49 01003-07-05 25ppb PFOS 49 H010126C.M HILL0165.D 50 01003-07-06 40ppb PFOS 50 H010126C.M HILL0186.D 51 Oiw54iG .eW ,. .,.p-"pk'y "" DCnr I I 51 H010126C.M HILL0187.D 52 0100347-08 75.lppb PFOS 52 HO10126C.M HILL0186.D 53 010050749 100.2ppb PFOS 53 H010128C.M HILL0189.D 54 0100347-10 01003-07-11 01003-07-12 250.5ppb PFOS 400.8ppb PFOS 501.0ppb PFOS -54 H010126C.M HILLO19O.D 55 cc un!n!ZX M HILL0191.D 56 56 H010126C.M HILL0192.D 57 0100347-13 MeOH Blank 1002.0ppb PFOS TN-A-4740. 04 Dec 00 57 H010126C.M HILL0193.D 58 58 H010126C.M HILL0194.D m MeOH Blsnk TN-A-4740. 04 Dec 00 50 HO10126C.M HILLOl95.D 90 4.11 2060058.4 4.1 1 2075784.8 4.11 1989603.4 4.11 4.11 0.00 0.00 0.00 4.11 4.11 4.11 4.1 1 4.11 4.11 4.11 4.: i 4.11 4.11 4.11 4.11 4.11 0.00 0.00 2027539.0 2098973.5 0.0 0.0 0.0 2101871.5 2121610.3 2147140.8 2105029.8 2099930.5 2102480.8 2091009.0 208S7~.3 2089134.0 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 2C.d.n 254.0 254.0 254.0 254.0 254.0 0.0 0.0 4.93 4.93 4.93 4.92 4.92 0.00 0.00 0.00 4.92 4.03 4.93 4.92 4.93 4.92 4.92 A 93 4.03 4.03 4.92 433 4.92 0.00 0.00 1103978.5 1111200.3 1098706.6 1114992.9 1156568.0 0.0 0.0 0.0 1160805.3 1178425.8 1180347.3 1157096.3 1170934.4 1157883.0 1159863.6 1153828.9 1148130.8 1134578.9 1112226.0 ..,.nc.7 D Il"=.rl,." 1082718.6 0.0 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 %A ..A. 254.4 0.0 0.0 5.14 4200268.0 5.14 4266221.O 5.14 4350663.0 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 14 5.14 0.00 0.00 4451651.5 2959959.5 0.0 0.0 0.0 0.0 83007.1 152217.0 277895.2 735110.4 1160993.9 1481490.6 2222884.0 2895124.5 6880929.5 10583437.0 12823226.0 21835648.0 0.0 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 iui.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% a An, 1.,n 0.7% 2.4% 1.9% 1.O% .. RAW DATA Agilent 1100 HPLClMSD "Hillary" Acquistion Run: HOlOl29 PFOS in Natural Seawater Shake Flask Method Day 3 Raw Data BACK TO MAIN MeOH Blank 01003-07-01 01003-07-02 01003-07-03 01003-07-04 "#..MIn7 nC. lV V C y l -v1 01003-07-06 01003-07-07 01003-07-08 01003-0749 01003-07-10 01003-07-11 01003-07-12 01003-07-13 MeOH Blank MeOH Blank MeOH Blank MeOH Blank TN-A-4740. 04 Dec 00 Oppb PFOS 2.5ppb PFOS 5ppb PFOS 10ppb PFOS 25;:k PFQS 40ppb PFOS 50.lppb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.0ppb PFOS 1002.0ppb PFOS TN-A4740, 04 DeC 00 TN-A-4740. 04 DeC 00 TN-A-4740. 04 D S 00 TN-A-4740, 04 Dec 00 TCR-002, 012X)l-mPFOS-3.4.1. l00X Dil. SWPFOS-3.4.1 Method Blank. SFM 01-26-01 MEE(MLA) TCR-002.012201-SWPFOS-3.4.120,0X Dil. sWPFOS-3.4.2 MethodBlank. SFM 01-26-01MEE(MLA) TCR-002. 012201-sWPFOS-3.4.3,100X Dil. sWPFOS-3.4.3 Method Blank. SFM 01-26-01 MEE(MLA) TCR-002. 012201-SWPFOS-3.4.4,100X Dil. swPFOS-3.4.4 Method Blank, SFM 01-26-01 MEE(MLA) MeOH Blank TN-A4740. 04 Dec 00 TCR-002,O12201-~~PFOS-3.1.1l0.0X Dil. MFOS-3.1 .ISFM 01-26-01 MEE(MLA) TCR-002. 012201-SWPFOS-3.1.2,l00X Dil. MFOS-3.1.2 SFM 01-26-01 MEE(MLA) TCR-002, 012201-SWPFOS-3.1.3,1WX Dil. SFM 01-26-01 MEE(MLA) MFOS-3.1.4 01003-07-09 MeOH Blank MeOH Blank TCR-002, O12201-~~PFOS-3.1.410. 0X Dll. SFM 01-26-01 MEE(MLA) 100.2ppb PFOS, CCV TN-A-4740. 04 DeC 00 TN-A-4740, 04 Dec 00 TCR-002, 012201-SWPFOS-3.2.1.1OOX Dil. swPFOS.3.2.1 SFM 01-26-01 MEE(MLA) TCR-002.012201-SWPFOS-3.2.2. IOOX Dit. sWPFOS-3.2.2 SFM 01-26-01 MEE(MLA) 2 H010129B.M HILL0081.D 95 3 H010129B.M HILL0082.D 1 4 H010129B.M HILL0083.D 2 5 H010129B.M HILL0084.D 3 6 H010129B.M HILL0085.D 4 7 H0101298.M HILLW86.D 5 8 H010129B.M HILL0087.D 6 9 H010129B.M HILL0088.D 7 10 H010129B.M HILL0089.D 8 A., I K x ! ! 2BB.rn U!LLnnSnD 9 12 H010129B.M HILL0091.D 10 13 H010129B.M HILL0092.D I 1 14 H010129B.M HILL0093.D 12 15 H010129B.M HILL0094.D 13 16 H010129B.M HILL0095.D 96 17 H010129B.M HJLL0096.D 96 18 H010129B.M HILL0097.D 96 19 H010129B.M HILL0098.D 96 20 H010129B.M HILL0099.D 51 21 H010129B.M HILLO1OO.D 52 22 H010129B.M HILLO1O1.D 53 23 H010129B.M HILLO1OZ.D 54 24 H010129B.M HILLO103.D 97 25 H010129B.M HILL0104.D 61 26 H010129B.M HILLO105.D 62 27 H010129B.M HILL0106.D 63 28 H010129B.M HILL0107.D 64 29 H0101298.M HILLOIO8.D 9 30 H0101296.M HILL0109.D 97 31 H010129B.M HILLO1lO.D 97 32 H010129B.M HILLO1ll.D 65 33 H010129B.M HILLO1IP.D 66 0.00 4.11 4.11 4.11 4.11 4.11 i.ii 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 1.842.994.6 1.857.425.3 1.866.181.9 --- 1,845,838.8 1,855,556.4 A n-7 4 1,01), (VLL.. 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 0.0 254.0 254.0 254.0 254.0 254.0 254.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 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 1,031,596.8 1,036,276.1 1,060.254.5 1,039,973.3 1,037,191.3 1. M I,723.2 1,040,650.0 1,035,925.8 1,041,005.9 1,018.wu.i 1,012,298.0 1,006,363.1 963,085.4 0.0 0.0 0.0 0.0 4.92 1.010.853.3 4.91 1.006.413.9 4.91 1,004,414.6 4.91 0.00 1,006,855.0 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 4.91 996,1842 4.91 994.797.9 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 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.z 5.14 5.14 5.14 0.00 0.00 0.00 0.00 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 S.284.821.5 9,555.366.0 11,624,301 .O 20,656,982.0 0.0 0.0 0.0 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 0.00 0.0 5.14 3.606.191.8 5.14 3399,729.5 5.14 3,632.102.3 5.14 5.14 0.00 0.00 3,656,226.8 2,644,160.3 0.0 0.0 5.14 3,371.343.3 5.14 3298,727.8 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 0.0 0.0 0.0 0.0 0.0 147.6 146.1 148.3 148.2 101.0 0.0 0.0 136.7 133.9 15.6% 12.2% 13.7% 2.4% 0.8% 0.41 2.3% 0.9% 1 7% 0.4% 0.9% 0.7% 1.6% P a p 5 Of 11 BACK TO MAIN TCR-002,012201-~~PFOS-3.2.130,0X Dil. SWPFOS-3.2.3 SFM 01-26-01 MEE(MLA) TCR-OOP. 012201-SWPFOS-3.2.4,1WX Dil. SWPFOS-3.2.4 SFM 01-2601 MEE(MLA) MeOH Blank TN-A-4740. 04 Dec 00 TCR-002,012201-swPF0S-3.3.1, l00X Dil. 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) TCROOZ, 012201-SWPFOS-3.3.3,100X Dil. JWPFOS-3.3.3 SFM 01-26-01 MEE(MLA) TCR-002.01 2201-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-A4740. 04 Oac00 01003-07-01 Oppb PFOS 01003-07-02 2.5ppb PFOS 01003-07-03 5ppb PFOS 0 , ~ *'"-p-~pA " aci ne ~ r l "V 01003-07-05 25ppb PFOS 01003-07-06 40ppb PFOS 01003-07-07 50.lppb PFOS 01003-07-08 75.lppb PFOS 01003-07-09 100.2ppb PFOS 01003-07-10 250.5ppb PFOS 2 01003-07-11 400.8ppb PFOS 01003-07-12 501.0ppb PFOS 1 01003-07-13 1002.Oppb PFOS 0 MeOHBlank TWA-4740. 04Dec00 MeOHBlank TN-A-4740. 04Dec00 0 N 34 H010129B.M HILL0113.D 67 35 H010129B.M HILL0114.D 68 36 H010129B.M HILLO115.D 97 37 H010129B.M HILLOll6.D 69 38 H010129B.M HlLLO117.D 70 39 H010129B.M HILLO118.D 71 40 H010129B.M HILLO11S.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 4.C0 H C ! C ! ! ~ S B . ~!.wni24.~ 1 46 H010129B.M HILL0125.D 2 47 H010129B.M HILL0126.D 3 48 H010129B.M HlLLOl27.D 4 49 H010129B.M HILLO128.U 5 50 H010129B.M HILL0129.D 6 51 H010129B.M HILL0130.D 7 52 H010129B.M HlLLOl31.D 8 53 H010129B.M HILL0132.D 9 54 H010129B.M HlLLOl33.D 10 55 H010129B.M HILL0134.D I 1 56 H010129B.M HILL0135.D 12 57 H010129B.M HILL0136.D 13 58 HO10129B.M HILL0137.D 98 59 H010129B.M HlLLOl38.D 98 4.11 4.11 0.00 4.71 4.11 4.11 4.11 4.11 0.00 0.00 0.00 4.11 4.11 4.11 4.11 4.ii 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 1,808.923.3 1,817,528.4 1,823,151.8 0.0 0.0 0.0 1,797,068.0 1,807.103.9 .1,806.916.9 1,808.355.9 V"0 cn-0 rsr=G,.r.r-." 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 7 . i...~n 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.Yi 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,I76.3 254.4 983.479.1 0.0 254.4 0.0 987,376.1 254.4 990,274.6 254.4 SS5.121 .I 254.4 992.1 11.4 1,039,414.1 0.0 0.0 0.0 1.041.622.9 ~ -.eI .,. e .I .WO,SLJ.O 1,054,742.1 1,046,836.9 1.048.370.6 1.042.1 50.7 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 0.0 0.0 254.4 *LE.2" 7.7 1 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 254.4 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 5.14 0.00 0.00 0.00 0.00 E..!'! 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 3,043,574.5 2,664,370.3 0.0 0.0 0.0 0.0 73,997.4 134.066.8 248.733.9 653,704.9 1.053.882.6 1,323,609.8 1,972,099.5 2.618.876.0 6,271,318.5 9,627.486.0 11,622.508.0 20,749,418.0 0.0 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 59.8 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% Vm."0 0m, 0.2% 1.7% 1.2% 0.7% 0.7% 0.6% 0.6% SMUbW, Shake h s k M o d 511711001 FACT-TCRWZ PFOS in Seawater Day 1 Hillary. H010125 BACK TO MAIN swpFos-.l ' TCR-002.012201-swPFOS-1.1.1lO,OX Dil. 45 H0125A1.M HILL0045,D 3, SFM 01-24-01 MEE(MLA) TCR-002, 012201-swPFOS-1.1.2, IOOX Dil. 46 H0125A1,M HILL0046,D 32 swpFos-1'1'2 SFM 01-24-01 MEE(MIA) L. 1...T,,-.,,,,, SP!?FOS-I.I.~ TCR-002 012201-SWPFOS-1.1.3,lOOX Dil. 47 H0125A1,M HILL0047,D 33 >tM -_..-a U 1-Lq-U I IV~LL{W-, SWPFOS-1.1.4 -. .. - TCR-002, 012201-~~PFOS-1.1.4lO, OX CCM ni.qq-ni MEECMLAI Oil. 48 H0125A1,M HILL0048,D 34 TCR-OO2,012201-swPFOS-1.2.1. lOOX Dil. 52 H0125A1,M HILL0052,D 35 swpFos-12'1 SFM 01-24-01 MEE(MLA) TCR-002, O ~ ~ ~ O I - S W P F O S -lOI .O~X. ~D,il. 53 H0125A1,M HILLO053,D 36 swpFos-122 SFM 01-24-01 MEE(MLA) TCR-002, 012201-swPFOS-1.2.3, 100X Dil. 54 H0125A1,M H,LL0054,D 37 swpF0s-1'2'3 SFM 01-24-01 MEE(MLA) TCR-002,012201-~~PFOS-214. lOOX DII 55 H0125A1 HILL0055 38 swpFos-1.2 SFM 01-24-01 MEE(MLA) T C R - O O ~ , O ~ ~ ~ O ~ - S W P3F1O,lOSO- ~X 011 57 H0125A1 HILL0057 39 swpFos-l 3'1 SFM 01-24-01 MEE(MLA) TCR-002, 012201-~~PFOS3-l2, lOOX DII 58 H0125A1 HILL0058 40 swpFos-' SFM 01-24-01 MEE(MLA) TCR-002, OI~~OI-SWPFOS3-I3, lOOX DII 59 H0125A1 HILL0059 41 swpFos-l SFM 01-24-01 MEE(MLA) . S wnr rr unoC- a u - . TCR-002,012201-~WPFOS-13 4, 1OOX DII. 6o H0125A1 HILL0060 42 SFM 01-24-01 MEt(MlA) 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5 14 5 14 5 14 5 14 5 14 3,780,994 3,919,051 3,895.319 4,009,265 3,576,570 3,702,940 3,689,193 3,597,279 3,797,897 3,862,722 3.785.649 3,743,934 125.7 129.9 128.8 131.9 118.0 122.9 119.4 1184 124 5 128 2 127 2 126 I Day I average: std dev: %C.V.: 12.6 13.0 12.9 13.2 11.8 12.3 11.9 11 8 12 5 12 8 12 7 12 6 12.3 12.7 12.6 12.9 11.6 12.0 11.7 11 6 12 2 12 5 12 4 12 3 12.2 &nL 0.47 3.9% 12.6 0.25 2.0% 11.7 0.19 1.6% 12 4 0 13 10% Solubilly-Shake Flask Melhod 5/17RW1 Pa00 7 of 11 FACT-TCRWZ PFOS in Seawater Day 2 Hillary. H010126 BACK TO MAIN TCR-002, 012201-SWPFOS-2.1.1, lOOX Dil. 25 H010126C,M HILL0161,D 63 swpFos~2~1~S1FM 01-25-01 MEE(MLA) TCR-002, 012201-SWPFOS-2.1.2,lOOX Dil. 26 H010126C.M HILL0162,D 64 swpFos-2'1'2 SFM 01-25-01 MEE(MLA) swpF0s-2'1'3 TECFRM-0c0!-2p,*0-1c!22M01E-ES(WMlP_FnO) S-2.1.3l,OOX Dil. 27 H0,0126C,M HILL0163,D 65 TCR-002, 012201-swPFOS-2.1.4, lOOX Dil. 28 H010126C.M HILL0164,D 66 swpF0s-2.1'4 SFM 01-25-01 MEE(MLA) TCR-002, 012201-SWPFOS-2.2.1.100X Dil. 32 H010126C,M HlLL0168,D 67 swpFos'2'2.1 SFM 01-25-01 MEE(MLA) TCR-OO2,012201-swPFOS-2.2.2, lOOX Dil. 33 H010126C,M HILL0169,D 68 swpFos-2'2'2 SFM 01-25-01 MEE(MW TCR-002, 012201-SWPFOS-2.2.3,lOOX Dil. 34 H010126C,M HILLO170,D 69 swpF0s-2'2.3 SFM 01-25-01 MEE(MLA) TCR-002, 012201-SWPFOS-2.2.4.l O O X Dil. 35 H010126C,M HILL0171,D 7o swpF0s-2'2'4 SFM 01-25-01 MEE(MLA) TCR-002,01220l-~~PFOS-32.1, lOOX DII. 37 H010126C HILL0173 71 swpFos-2 3'1 SFM 01-25-01 MEE(MLA) TCR-002,01220l-~~PFOS3-2.2.100X 011. 38 H010126C.M HlLL0174 72 swPF0s-2'3'2 SFM 01-25-01 MEE(MLA) CR-O02~012201-~wPFOS2. 5.14 5.14 5.14 5.15 5.14 5.14 5.14 5.14 5 14 5 14 3379582 3307268 3271451 3334039 3367553 3381545 3372613 3277744 4200268 4268221 122.1 119.9 119.0 121.5 122.6 123.7 121.5 119.0 154 6 156 2 12.2 12.0 11.9 12.1 12.3 12.4 12.1 11.9 15 5 15 6 11.9 11.7 11.7 11.8 12.0 12.1 11.8 11.7 15 2 15 3 ?.-*- I Day 2 average: I stdde": I %C.V.: 11.9 VgglrnL 0.07 0.6% 11.8 0.10 0.8% 11.9 0.18 1.5% 15 6 0 39 I Solubaiy-Shake Flask Method 5/17/2001 Plpc 8 of 11 FACT-TCRW2 4. PFOS in Seawater Day 3 Hillary. H010129 BACK TO MAIN TCR-002,012201-swPFOS-3.1.lO1O,X Dil. 25 H010129B,M HILLo104,D 61 swpF0s9.1'1 SFM 01-26-01 MEE(MLA) TCR-002, 012201-swPFOS-3.1.2, lOOX Dil. 26 H010129B,M HILL0105,D 62 swpF0s-3'1'2 SFM 01-26-01 MEE(MLA) ..--,.., WwPFOS-3.1.3 TCR-0_02.. 012201-swPF~OS,-3.1.3, IOOX Dil. 27 H010129B.M HILL0106,D 63 YFM Ul-26-U I I V I K E ~ I Y I ) ,.."_. - TCR-002.012201-swPF0S-3.1.4,100XDil. 28 H010129B,M HILL0107.D swPFoS-3.1.4 c c b i - . n4.9fi-m U F F ~ M ~ A ! 64 "I \.. TCR-002,012201-swPFOS-3.2.1, IOOX Dil. 32 H0,0129B,M HLILO~llD 65 swpF0s'3'2'1 SFM 01-26-01 MEE(MLA) TCR-002.012201-swPF0S-3.2.2,100X Dil. 33 H010129B,M HILLO112,D 66 swpFos32'2 SFM 01-26-01 MEE(MLA) TCR-002,012201-swPF0S-3.2.lO3O,X Dil. 34 H010129B,M HILL0,13,D 67 swpF0s-3.2'3 SFM 01-26-01 MEE(MLA) TCR-002.012201-SWPFOS-3.2.4, lOOX Dil. 35 H010129B,M HILL0114,D 68 swpF0s-3'2'4 SFM 01-26-01 MEE(MLA) TCR-002,012201-swPFOS-3.3.11O,OX Dil. 37 H010129B,M H,LL0116.D 69 swpF0s-3'3'1 SFM 01-26-01 MEE(MLA) TCR-002, 012201-SWPFOS-3.3.2,lOOX Dil. 38 H010129B,M H,LL0117,0 7o swpF0s-3'3'2 SFM 01-26-01 MEE(MLA) TCR-OO2.012201-swPFOS-3.3.3IO,OX Dil. 39 H0,a,29B.M H,LLa,,B,D 71 swpF0s-3.3'3 SFM 01-26-01 MEE(MLA) _ _ _ _ - - swrtus-a.J.4 TCR-002, 012201-swPFOS-3.3.4, 100X Dil. 4o H010129B,M HILLOl19,D 72 SFM 01-26-01 MEE(MLA) 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 5.14 3,606.192 3,599,730 3,632,102 3,656,227 3,371,343 3,298,728 3,367.698 3,367.747 2,909,406 3,057,539 2,972,588 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 14.8 14.6 14.8 14.8 13.7 13.4 13.6 13.8 11.9 12.4 12.0 12.4 14.5 14.3 14.5 14.5 13.4 13.1 13.3 13.5 11.7 12.1 11.7 12 1 14.5 0.10 0.7% 13.3 0.17 1.3% 11.9 0.23 1.9% Solubikty-ShakeFhsk Method , Y17Rw1 Page 8 of 11 FACT-TCROOP FACT-TCROO2 PFOS Solubility of TCR-00017-46 in Seawater Day 1 data source acquisition instrumentlsequenee: Agilent 1100 HPLCMSD "Hillrry"R1010125.s Day 2 data source acquisitioninstrument/sequence: Agilent 1100 HPLCMSD "HiIIary"R1010126.s Day 3 data source acquisitioninstrumentkequence: Agilent 1100 HPLCMSD "HilIary"R1010129.s DATA SUMMARY FOR INDIVIDUAL SAMPLES BACK TO MAIN SWPFOS-I.~.~ 13.0 12.1 SWPFOS-1.1.3 12.9 12.6 SWPFOS-1.1.4 13.2 12.9 -c.w..DFQS-1 2 1 11.8 11.6 SWPFOS-1.2.2 12.3 12.0 SWPFOS-1.2.3 11.9 11.7 SWPFUS-1.2.4 1. D 11.0 !!.5 0.25 2.0% 11.7 I .6% 0.19 I FACT-TCROO2 PFOS Solubility of TCR-00017-46 in Seawater. DAILY AND TOTAL DATA S MMARIES )av 1 data summary Average: 12.2 ". # n.... n 1-- 3LU Y C V . V . t l - %cv:- 3.9% ppm SWPFOS-1.3.1 12.5 12.2 12.4 SWPFOS-1.3.2 12.8 12.5 0.13 SWPFOS-1.3.3 12.7 12.4 1 .O% SWPFOS-1.3.4 12.6 12.3 SWPFOS-2.1.1 12.2 11.9 11.8 )av 2 data summary Average: 11.9 ~ Std Dev:- 0.07 - %CV- 0.6% ppm . (Sample 3 acludcd via Q-Tat) SWPFOS-2.1.2 12.0 11.7 0.10 SWPFOS-2.1.3 11.9 11.7 0.8% SWPFOS-2.1.4 12.1 11.8 SWPFOS-2.2.1 12.3 12.0 11.9 SWPFOS-2.2.2 12.4 12.1 0.15 lay 3 data summary Average: 13.2 ppm _ Std_De_v: -1.30 - %CV:- 9.8% SWPFOS-2.2.3 12.1 11.8 1.5% cwPFnS-7 7 A 11.9 11.7 4 0 Y TOTAL data summary Average: 12.4 ppm ~ Std Dev:- 0.71 %cV: 5.7% SWPFOS-3.1.1 14.8 14.5 14.5 UI 0 SWPFOS-3.1.2 14.6 14.3 0.10 4 SwPFOS-3.i .3 !4.8 14.5 0.7% d w SWPFOS-3.1.4 14.8 14.5 0) swPFOS.3.2.1 13.7 13.4 13.3 SWPFOS-3.2.2 13.4 13.1 0.17 SWPFOS-3.2.3 13.6 13.3 1.3% SWPFOS-3.2.4 13.8 13.5 SWPFOS-3.3.1 11.9 11.7 11.9 SWPFOS-3.3.2 12.4 12.1 0.23 SWPFOS-3.3.3 12.0 11.7 1.9% qwPFOS-3 3 4 12.4 12.1 Solubility-Shake Flask Msllmd , 5/17ROO1 Pwe 10 of 11 FACT-TCR-002 - PFOS in Seawater Shake Flask Method BACK TO MAIN Q-TEST Data Calculations: !SampleID: SWPFOS-2.1 SWPFOS-2.2 SWPFOS-2.3 Sample Conc., Rep1 Range: 3.70 Gap: 3.60 Qobs: 0.97 N0. observations: Exclude sample set SWPFOS-2.3 - Qobserved = gap/range where "gap" is the difference between the questionabledate 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 Q- observed 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 highligh,tedin yellow in the above table have Q-observed > 0.88, from the reported data. - - 3M Environmental Laboratory Solubility, Shake Flask Method, 5/17/2001 FACT-TCROOZ (LIMS #E00-1716), Page 51 ad 138 Page 11 of 11 FACT-TCR-002 RAW DATA Agilent 1100 HPLClMSD "Hillary" Acquistion Run: H010131 PFOS in 3.5%NaCl Solution Shake Flask Method Day 1 Raw Data BACK TO MAIN MeOH Blank 01003-07-13 01003-07-13 MeOH Blank MeOH Blank .w.-,Tr\vY, 0l3nl, I "llll.. 01003-07-01 0 1003-07-02 01003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-1 1 0100367-12 01003-07-13 MeOH Blank MeOH Blank MeOH Blank 01003-07-01 01003-07-02 01003-07-03 01003-07-04 0 1003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 ..-.,au- IlJu3-1u-I-4I"L 01003-07-13 MeOH Blank MeOH Blank MeOH Blank nadPFOS-1.4.1 nadPFOS-1.4.2 TN-A4740, 04 Dec 00 1002.0ppb PFOS 1002.0ppb PFOS TN-A4740, 04 Dec 00 TN-A4740, 04 Dec 00 TN-.A.-A7AO. 04 Dec 00 Oppb PFOS 2.5ppb PFOS 5ppb PFOS IOppb PFOS 25ppb PFOS 40ppb PFOS 50.lppb PFOS 75.fppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.0ppb PFOS 1002.0ppb PFOS TN-A4740, 04 Dec 00 TN-A4740, 04 Dec 00 TN-A-4740, 04 Dec 00 Oppb PFOS 2.5ppb PFOS 5ppb PFOS lOppb PFOS 25ppb PFOS 40ppb PFOS 5O.lppb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS SO? .Oppb PFOS 1002.0ppb PFOS TN-A-4740. 04 Dec 00 TN-A-4740, 04 Dec 00 TN-A-4740. 04 Dec 00 TCR-002,012901-nadPFOS-1.4.1. loOX Dil. Method Blank, SFM 01-3101 MEE(MLA) TCR-002,012901-nadPFOS.4-.I2, IOOX Dil. Method Blank, SFM 01-3101 MEE(MlA) ' 2 HO10131A.M HILL0002.D 91 0.000 0.0 0.0 0.000 0.0 0.0 5.156 7224.9 0.9 3 HO10131A.M HILL0003.D 13 4.121 2143601.3 301.1 4.821 993486.1 250.7 5.206 22127404.0 0.0 4 HO10131A.M HILL0004.D 13 4.121 2124774.3 305.6 4.821 970509.3 250.7 5.206 21844558.0 0.0 5 HOIO131AM HlU0005.D 91 4.1 19 11608.7 0.0 0.000 0.0 0.0 5.156 8180.2 0.9 6 H010131A.M HILL0006.D 91 4.117 12030.3 0.0 0.000 0.0 0.0 5.160 3006.9 0.9 7 H010131A.M HILL0007.D 91 4.118 11730.2 0.0 0.000 0.0 0.0 5.161 7961.4 0.9 8 H010131AM HlLL0UUB.D i 4.12; "nro?oc q LW-tWll"." 250.5 4.821 1060946.9 250.7 5.157 12540.2 1.3 9 H010131A.M HILL0009.D 2 4.122 2093037.3 270.5 4.823 1080061.5 250.7 5.152 87037.7 4.0 10 HOlOl3lAM HILLOO1O.D 3 4.118 2110525.8 269.8 4.822 1091921.6 250.7 5.162 155338.9 6.4 .4 II H3:9!3?A.M H!?Lnn?I 0 4 4.119 2097033.9 268.2 4.819 1091357.9 250.7 5.155 283237.4 10.9 12 H010131A. M HlLLOOl2. D 5 4.118 2087465.6 266.3 4.822 1094229.1 250.7 5.161 72: 16?.4 2C.8 13 HO10131AM HILL0013.D 6 4.121 2089456.8 268.0 4.821 1088254.4 250.7 5.157 1153655.3 42.2 14 H010131AM HlLL0014.D 7 4.118 2089359.4 268.0 4.819 1087986.1 250.7 5.155 1443086.4 52.8 15 H010131A.M HILL0015.D 8 4.115 2087226.1 264.3 4.823 1102227.4 250.7 5.159 2167099.3 78.4 16 HO10131A.M HILL0016.D 9 4.122 2097466.5 264.9 4.822 1105173.9 250.7 5.158 2856232.3 103.6 17 H010131A.M HILL0017.D 10 4.119 2091827.3 264.0 4.820 1105860.1 250.7 5.156 6777085.5 256.7 18 H010131A.M HlLLOOl8.D 11 4.118 2081840.1 262.9 4.819 1105371.5 250.7 5.232 10322257.0 411.4 19 HOl0131AM HILL0019.D 12 4.119 2127462.5 270.6 4.820 1097313.3 250.7 5.240 12413629.0 517.0 20 HOIO131A.M HlLL0020.D 13 4.121 2128281.3 277.4 4.821 1070927.4 250.7 5.200 22093346.0 1319.8 21 HO10131A.M HlLL0021.D 92 4.119 11259.9 0.0 0.000 0.0 0.0 5.163 4968.3 0.9 22 H010131A.M HILL0022.D 92 4.121 11279.0 0.0 0.000 0.0 0.0 5.165 6091.6 0.9 23 H010131AM HlLL0023.D 92 4.122 11475.7 0.0 0.000 0.0 0.0 5.158 7088.3 0.9 24 HO10131A.M HILL0024.D 1 4.119 2095800.8 254.9 4.819 1147396.9 250.7 5.155 8761.4 1.2 25 HO1013lAM HILL0025.D 2 4.119 2092956.8 253.9 4.819 1150438.9 250.7 5.155 85318.9 3.7 26 H010131A.M HILL0026.D 3 4.121 2136092.8 255.4 4.622 1167485.3 250.7 5.g58 158275.4 6.1 22.1 27 HOIO131AM HILL0027.D 4 4.119 2134188.0 254.6 4.819 1169935.9 250.7 5.156 294889.3 10.6 6.1 28 HO10131A.M HILL0028.D 5 4.121 2101620.5 251.3 4.821 1167190.9 250.7 5.158 731035.8 25.2 0.3 29 H010131A.M HILL0029.D 6 4.122 2118756.3 254.2 4.822 1163371.8 250.7 5.158 1194338.3 40.9 2.0 30 H010131AM HILL0030.D 7 4.117 2094413.3 250.6 4.821 1166273.0 250.7 5.161 1473480.0 50.3 0.4 31 HOlOl31A.M HILL0031.D 8 4.118' 2107698.3 253.3 4.819 1161204.9 250.7 5.155 2231440.0' 76.6 1.9 32 H010131AM HILL0032.D 9 4.118 2107941.5 253.2 4.822 1161693.0 250.7 5.162 2926687.3 101.0 0.7 33 H010131AM HILL0033.D 10 4.118 2085320.1 251.0 4.822 1159443.8 250.7 5.162 6886002.0 248.1 -1.0 34 H010131AM HILL0034.D 11 4.118 2104751.3 260.1 4.822 4129470.5 250.7 5.218 10541540.0 411.2 2.6 35 HOlO131AM HILL0035.D 12 4.121 2089080.4 254.8 4.821 1144288.3 250.7 5.157 12617936.0 501.1 0.0 36 HOlOl3lAM HILL0036.D 13 4.i2i 2132ioc.5 270.5 4.821 1096943.1 250.7 5.164 22841106.0 1346.3 37 HO1013lAM HILL0037.D 92 4.118 11790.3 0.0 0.000 0.0 0.0 5.161 4108.8 0.9 38 HO1013lAM HILL0038.D 92 4.119 8487.4 0.0 0.000 0.0 0.0 5.155 7473.4 0.9 39 HO10131AM HILL0039.D 93 0.000 0.0 0.0 0.000 0.0 0.0 5.162 6551.3 0.9 40 H010131AM HILL0040.D 21 4.117 2022771.3 250.5 4.821 1126861.6 250.7 5.161 4319.0 1.0 41 252.9 4.819 1111055.0 250.7 5.156 2599.3 1.o BACK TO MAIN FACT.TCR-002 TCR-002, 012901-nadPFOS-1.43. IOOX Dil. Method Blank. SFM 01-31- nadPFOS-1.4.3 01 MEE(MLA) 42 H010131A.M HILL0042.D 23 4.119 2083439.9 259.2 4.819 1121788.5 250.7 5.155 8289.1 1.2 TCR-002,012901-nadPFOS-1.4.4, IOOX D1. Method Blank. SFM 01-31- nadPFOS-1.4.4 01 MEE(MLA) 43 HO10131A.M HILL0043.D 24 4.119 2038687.6 257.2 4.820 1106088.3 250.7 5.163 4842.2 1.o MeOH Blank TN-A-4740, 04 Dec 00 44 H010131A.M HILL0044.D 93 4.121 12652.4 0.0 0.000 0.0 0.0 5.158 5851.6 0.9 TCR-002, 012901-nadPFOS-1.1 .I, naclPFOS-1.1.1 IOOX Dil. SFM 01-31-01 MEE(MIA) 45 HOlOI3IA.M HILL0045.D 31 4.119 2044713.0 263.8 4.820 1081767.8 250.7 5.156 5915846.0 227.0 TCR-002, 012901-nadPFOS-I.I.2. nadPFOS-1.1.2 IOOX Dd. SFM 01-31-01 MEE(MLA) 46 HOlOl3lAM HILLOM6.D 32 4.118 2043153.5 267.1 4.822 1067474.3 250.7 5.162 5851699.5 227.5 TCR-002, 012901-nadPFOS-1.1.3, nadPFOS-1.1.3 IOOX Dl. SFM 01-31-01 MEE(MLA) 47 HO10131A.M HILL0047.D 33 4.119 2047704.3 263.1 4.820 1086182.9 250.7 5.156 5827699.0 222.4 TCR-002, 012901-nadPFOS-I.1.4. nadPFOS-1.1.4 IOOX Did. SFM 01-31-01 MEE(MLA) 48 HOI0131A.M HILLO048.D 34 4.118 2040932.9 266.2 4.822 1070219.3 250.7 5,162 5990611.0 232.7 01003-07-09 100.2ppb PFOS, CCV 49 H010131A.M HILL0049.D 9 4.121 2112425.0 251.0 4.822 1174724.8 250.7 5.158 2899438.8 98.9 -1.3 MeOH Blank TN-A-4740, 04 Doc 00 50 HOlOI3IA.M HILL0050.D 93 4.118 11531.6 0.0 0.000 ' 0.0 0.0 5.162 1726.1 0.9 !kQ!E!& TN-A-4740. 04 Dec 00 51 HO 1013IA.M HILL0051.0 93 4.118 8666.6 0.0 0.000 0.0 0.0 5.161 6133.9 0.9 TCR-002, 012901-nadPFOS-1.2.1, nadPFOS1.2.1 lOOX Dil. SFM 01-31-01 MEE(MLA) 52 HOlOI31A.M HILL0052.D 35 4.118 1995595.9 261.8 4.819 1063811.5 250.7 5.155 5222047.5 202.2 TCR-002,012901-nadPFOS-1.2.2. nadPFOS-1.2.2 lOOX Dl. SFM 01-3147 MEEihfiAj .eId - 36 4.119 2011646.8 265.8 4.819 1056323.1 250.7 5.155 5201276.0 202.9 TCR-002, 012901-nadPFOS-1.2.3, nadPFOS-1.2.3 IOOX Dll. SFM 01-31-01 MEE(MLA) 54 HO10131A.M HILL0054.D 37 4.118 1994192.1 261.7 4.822 1063676.3 250.7 5.162 5192852.5 201.0 TCR-002, 012901-nadPFOS-1.2.4, nadPFOS-1.2.4 IOOX Dil. SFM 01-31-01 MEE(MLA) 55 HO10131A.M HILL0055.D 38 4.118 1986943.1 261.5 4.822 1060499.5 250.7 5.161 5269990.5 204.9 MeOH Blank TN-A-4740. 04 Dec 00 56 H010131A.M HILL0056.D 94 4.120 9279.7 0.0 0.000 0.0 0.0 5.156 6002.4 0.9 TCR-002, 012901-nadPFOS-I.3.1, nadPFOS-1.3.1 IOOX oil. SFM 01-31-01 MEE(MIA) 57 HO1013IA.M HILL0057.D 39 4.118 1922033.9 250.0 4.819 1073103.1 250.7 5.155 4172225.8 158.1 TCR-002,012901-nadPFOS-I .3.2, nadPFOS-1.3.2 IOOX D1. SFM 01-31-01 MEE(MLA) 58 HO1013IAM HILLOO58.D 40 4.118 1988949.3 258.8 4.822 1072507.3 250.7 5.161 43 17565.0 164.0 TCR-002.012901-nadPFOS-1.3.3, nadPFOS-1.3.3 IOOX D1. SFM 01-31-01 MEE(MLA) 59 H010131AM HILL0059.D 41 4.121 1991271.4 261.3 4.821 1063607.5 250.7 5.157 4187921.5 160.2 TCR-002. 012901-nadPFOS-1.3.4, nadPFOS-1.3.4 100X D1. SFM 01-31-01 MEE(MLA1 60 HO1013IA.M HILL0060.D 42 4.120 1982020.0 262.7 4.821 1052995.8 250.7 5.157 4194090.0 162.2 01003-07-09 100.2ppb PFOS, CCV 61 HOlOI3IA.M HILl0061.D 9 4.121 2055678.9 249.3 4.821 1150774.1 250.7 5.157 2847996.0 99.1 -1.1 MeOH Blank TN-A-4740, 04 D ~0c0 62 H01013IAM HILL0062.D 94 4.121 9943.1 0.0 0.000 0.0 0.0 0.000 0.0 0.0 MeOH Blank TN-A-4740, 04 D ~ 0c0 63 H010131A.M HILL0063.D 94 4.119 11681.8 0.0 0.000 0.0 0.0 5.156 6434.6 0.9 MeOH Blank TN-A-4740. 04 D ~0c0 64 HO10131A.M HILL0064.D 94 4.122 11540.1 0.0 0.000 0.0 0.0 0.000 0.0 0.0 01003-07-01 Oppb PFOS 01003-07-02 2.5ppbPFOS . 01003-07-03 5ppb PFOS 65 H010131A.M HILL0065.D I 4.120 2041874.0 245.9 4.820 1159008.5 250.7 5.156 8746.7 1.2 66 HOI0131A.M HILL0066.D 2 4.119 2069020.8 245.7 4.819 1175189.9 250.7 5.155 80179.2 3.5 67 HO1013IAM HlLL0067.D 3 4.118 2081127.1 244.2 4.822 1189579.9 250.7 5.162 150817.4 5.8 15.3 01003-07-04 IOppb PFOS 68 HOlOl3lAM HILL0068.D 4 4.119 2070209.8 244.3 4.819 1182606.9 250.7 5.156 286563.4 10.2 2.3 01003-07-05 25ppb PFOS 69 HOI0131A.M HlLL0069.D 5 4.120 2059409.9 243.5 4.821 1180256.6 250.7 5.157 720880.0 24.6 -2.1 01003-07-06 40ppb PFOS 70 H010131AM HILL0070.D 6 ' 4.119 2080276.8 245.4 4.820 1183280.5 250.7 5.156 1170613.4 39.4 -1.7 iiiOiX-C7-67 :3.:ppb PfOS 71 HOlOl31AM HILL0071.D 7 4.118 2077642.6 244.2 4.819 1187313.3 250.7 5.155 1480991.4 49.6 -0.9 01003-07-08 75.lppb PFOS 72 HO10131A.M HILL0072.0 8 4.119 2084619.8 246.0 4.879 .4"1.-114 1 I IDLJQI. I & .=A.)".I -I 5.?55 2ens32.n 73 5 -2.2 01003-07-09 100.2ppb PFOS 73 HO1013IA.M HILL0073.D 9 4.119 2089444.1 245.3 4.819 11886503 250.7 5.155 2894335.8 97.5 -2.7 01003-07-10 250.5ppb PFOS 74 HOlOl3lAM HILL0074.D 10 4.120 2067633.0 247.4 4.821 1166542.9 250.7 5.157 6910958.0 247.4 -1.2 01003-07-1 1 400.8ppb PFOS 75 HOlOI31A.M HILL0075.D 11 4.115 2096577.1 255.5 4.822 1145464.9 250.7 5.159 10501242.0 402.7 0.5 01003-07-12 501.0ppb PFOS 76 HO1013IA.M HILL0076.D 12 4.120 21 13937.3 255.7 4.820 1154010.9 250.7 5.219 12580502.0 494.2 -1.4 01003-07-13 1002.0ppb PFOS 77 H010131A.M HILL0077.D 13 4.120 2036590.3 253.5 4.821 1121090.4 250.7 5.164 23094802.0 1314.3 MeOH Blank TN-A-4740. 04 DW 00 78 HOI0131AM HILL0078.D 95 4.120 8770.0 0.0 0.000 0.0 0.0 5.157 7282.3 0.9 MeOH Blank TN-A-4740, 04 Dec 00 79 H010131A.M HlLL0079.D 95 4.119 11212.9 0.0 0.000 0.0 0.0 5.155 6371.0 0.9 FACT-TCRMIP RAW DATA Agilent 1100 HPLClMSD "Hillary" Acquistion Run: H010205 PFOS in 3.5% NaCl Solution Shake Flask Method Day 2 Raw Data BACK TO MAIN MeOH Blank 01003-07-13 01003-07-13 MeOH Blank MeOH Blank ".. MeOH Blank u 1V V S U l -v1.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 01003-07-1I 01003-07-1 2 01003-07-13 MeOH Blank MeOH Blank MeOH Blank nadPFOS2.4.1 nadPFOS2.4.2 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. Unp-_yL " rnrr"hUC 2.5ppb PFOS 5ppb PFOS 10ppb PFOS 25ppb PFOS 4Oppb PFOS 50.lppb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 5Ol.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 IOppb PFOS 25ppb PFOS 4Oppb PFOS 5O.Ippb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.0ppb 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. TCR-002,012901-nadPFOS-2.4.1, IOOX Di.Method Blank, SFM 02-01-01 MEE(MLA) TCR-002. 012901-nadPFOS2.4.2. lOOX Dil. M e t h d Blank, SFM 02-01-01 MEE(MLA) 2 H010205A.M HILL0002.D 3 H010205A.M HILL0003.D 4 H010205A.M HILL0004.D 5 H010205A.M HILL0005.D 6 H010205A.M HILL0006.D 7 H010205A.M HILL0007.D 8 un?n2n5.A.M YKLnnoR n 9 H010205A. M HILL0009.D 10 H010205A.M HILLOO1O.D 11 H010205A.M HILLOO1l.D 12 H010205A.M HILL0012.D 13 H010205A.M HILL0013.D 14 H010205A.M HILL0014.D 15 H010205A.M HILL0015.D 18 H010205A.M HILL0016.D 17 H010205A.M HILL0017.D 18 H010205A.M HILL0018.D 19 H010205A.M HILL0019.D 20 H010205A.M HILL0020.D 21 H010205A.M HILL0021.D 22 H010205A.M HILL0022.D 23 H010205A.M HILL0023.D 24 H010205A.M HILL0024.D 25 H010205A.M HILL0025.D 26 HO10205A. M HILL0026.D 27 H010205A.M HILL0027.D 28 H010205A.M HILL0028.D 29 ii010205A.M HILL0029.D 30 H010205A.M HILL0030.D 31 H010205A.M HILL0031.D 32 H010205A.M HILL0032.D 33 H010205A.M HILL0033.D 34 H010205A.M HILL0034.D 35 H010205A.M HILL0035.D :e iiOi0205A.M iiiiLi;036.E 37 H010205A.M HILL0037.D 38 HO10205A. M HILL0038. D 39 H010205A.M HILL0039.D 91 13 13 91 91 ' 91 1 2 3 4 5 6 7 8 9 10 11 12 13 92 92 92 1 2 3 4 5 6. 7 . 8 9 10 11 1. ,.2I ) 92 92 93 4.119 4.121 4.118 4.121 4.118 4.121 4.120 4.119 4.122 4.119 4.118 4.120 4.117 4.121 4.120 4.121 4.118 4.119 4.118 4.119 4.121 4.120 4.119 4.122 4.121 4.117 4.121 4.119 4.120 4.121 4.119 4.121 4.118 4.118 1440 7 .I I" 4.121 4.118 4.119 9599.3 1774643.6 1808354.9 9271.7 12252.3 13494.0 1837110.1 1829781.3 1874887.3 1836290.8 1854312.5 1834995.5 1865783.1 1861396.1 1811954.0 1848057.6 1811635.1 1874128.5 1919553.6 13717.4 12992.0 12346.2 1888101.0 1894234.6 1897593.9 1880741.9 1869055.4 1881326.5 1896198.5 1845975.0 1871880.4 1880987.0 1871845.4 1881822.5 3895748.5 13125.2 13076.4 8488.4 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 2ce.2 0.0 0.0 0.0 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 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 988284.3 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 ?@3nn?2.e 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 5.156 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 5.158 5.157 5.157 5.156 5.255 5.162 5.204 5.162 5.157 5.162 5.155 3212.3 19985400.0 20450016.0 18446.0 4197.1 7831.2 11402.0 86371.4 142977.5 266736.0 697003.3 1123236.8 1391739.1 2083089.4 2734341.5 6425435.5 9833563.0 11816095.0 21038770.0 8349.7 13127.0 9888.0 12737.3 91752.4 161460.5 286824.4 716901.5 1151040.3 1455018.6 2161271.8 2786907.8 6624594.0 10062423.0 12373037.0 22023792 0 13229.0 7287.5 3465.8 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 1027 6 0.0 0.0 0.0 -12.5 -0.4 2.8 4.6 4.7 3.3 1.1 2.6 1.1 26 40 H010205A.M HILL0040.D 21 4.119 1943546.6 271.9 4.819 1042521.5 250.7 5.155 8908.6 0.0 41 H010205A.M HILL0041.D 22 4.119 1900756.8 263.2 4.819 1053132.4 250.7 5.155 16638.0 0.0 Paw 3 of 11 BACK TO MAIN FACT-TCROOZ nadPFOS-2.4.3 nadPFOS-2.4.4 MeOH Blank nadPFOS-2.1.1 nadPFOS-2.1.2 nadPFOS-2.1.3 nadPFOSQ.1.4 01003-07-09 MeOH Blank MeOH Blank nadPFOS2.2.1 naciPFOS-2.2.2 nadPFOS-2.2.3 nadPFOS-2.2.4 MeOH Blank nadPFOS-2.3.1 nadPFOS-2.3.2 nadPFOS-2.3.3 nadPFOS-2.3.4 01003-07-09 MeOH Blank MeOH Blank MeOH Blank 01003-07-01 01003-07-02 01003-07-03 01003-07-04 0 1003-07-05 01003-07-06 n!003-07-n7 0 1003-07-08 0 1003-07-09 01003-07-10 01003-07-11 01003-07-12 01003-07-13 MeOH Blank MeOH Blank TCR-OO2,012901-nadPFOS-2.4.3,1 OOX Dil. Method Blank, SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.4.4, IOOX Dit. Method Blank, SFM 02-01-01 MEE(MLA) TN-A-4755. 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-2.1.1. IOOX Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.1.2, IOOX Di. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.I.3, f OOX Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.1.4. IOOX Dit. SFM 02-01-01 MEE(MLA) 100.2ppb PFOS, CCV TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755. 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-2.2.1, 1OOX Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.2.2. IOOX Dii. s&i, ij&oi-iji GEEjUsj TCR-002, 012901-nadPFOS-2.2.3. IOOX Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.2.4, IOOX Dil. SFM 02-01-01 MEE(MLA) TN-A-4755. 05 Feb 01, exp:2005. TCR-002, 012901-nadPFOS-2.3.1, IOOX Dit. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.3.2. IOOX DI. SFM 02-01-01 MEE(MLA) TCR-002,012901-nadPFOS-2.3.3. IOOX Dil. SFM 02-01-01 MEE(MLA) TCR-002, 012901-nadPFOS-2.3.4, IOOX Dil. SFM 02-01-01 MEE(MLA) 100.2ppb PFOS, CCV 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 4Oppb PFOS 512 4pph PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.0ppb PFOS 1002.0ppb PFOS TN-A-4755. 05 Feb 01. exp:2005. TN-A-4755. 05 Feb 01, exp:2005. 42 H010205A.M HILL0042.D 23 43 H010205A.M HILL0043.D 24 44 H010205A.M HILL0044.D 93 45 H010205A.M HILL0045.D 31 46 H010205A.M HILL0046.D 32 47 H010205A.M HILL0047.D 33 48 H010205A.M HILL0048.D 34 49 H010205A.M HILL0049.D 9 50 H010205A.M HILL0050.D 93 51 H010205A.M HILLO051.D 93 52 H010205A.M HILL0052.D 35 5; Ie"C 54 H010205A.M HILL0054.D 37 55 H010205A.M HILL0055.D 38 56 H010205A.M HILL0056.D 93 57 H010205A.M HILL0057.D 39 58 H010205A.M HILL0058.D 40 59 H010205A.M HILL0059.D 41 60 H010205A.M HILL0060.D 42 61 H010205A.M HILL0061.D 9 62 H010205A.M HILL0062.D 93 63 H010205A.M HILL0063.D 94 64 H010205A.M HILL0064.D 94 65 H010205A.M HILL0065.D I 66 H010205A.M HILL0066.D 2 67 H010205A.M HILL0067.D 3 68 H010205A.M HILL0068.D 4 69 H010205A.M HILL0069.D 5 70 H010205A.M HILL0070.D 6 71 HO10205A.M HILL0071.D 7 72 H010205A.M HILL0072.D 8 73 H010205A.M HILL0073.D 9 74 H010205A.M HILL0074.D 10 75 H010205A.M HILL0075.D 11 '76 H010205A.M HILL0076.D 12 77 H010205A.M HILL0077.D 13 78 H010205A.M HILL0078.D 94 79 H010205A.M HILL0079.D 94 4.117 1933177.9 272.1 4.821 1036265.4 250.7 5.161 5505.6 0.0 4.120 4.118 4.118 4.119 4.119 4.119 4.120 4.118 4.118 4.119 7 1 .e.I ICI 4.117 4.118 4.121 4.119 4.121 4.118 4.119 4.120 4.120 4.122 4.119 4.121 4.120 4.117 4.122 4.121 4.120 4.123 4.119 4.121 4.122 4.120 4.118 4.121 4.119 4.121 1981495.4 8589.0 276.1 0.0 1954489.6 280.0 1995386.6 283.3 1973433.0 282.4 1916815.9 1907227.4 13009.6 13189.6 275.8 255.0 0.0 0.0 1966392.4 :S7505.8 280.2 279.3 1880691.9 267.8 1976344.5 12975.6 280.9 0.0 1949027.0 276.7 1899727.9 270.5 1893792.4 267.5 1925417.8 1878686.8 9121.0 12767.6 8712.4 1859950.3 1851090.0 1863924.8 1858022.6 1826781.8 1873868.3 1789390.1 1851189.0 1895202.0 1881744.3 1806523.5 1874440.5 1874729.0 13199.4 12154.5 272.4 250.2 0.0 0.0 0.0 243.4 240.7 238.1 240.7 236.4 246.3 230.6 239.7 246.7 242.8 240.8 248.7 252.1 0.0 0.0 4.820 0.000 1046513.6 0.0 250.7 0.0 4.819 1018035.8 250.7 4.820 1027304.7 250.7 4.819 1019282.8 250.7 4.820 4.820 0.000 0.000 1013776.3 IO90911.0 0.0 0.0 250.7 250.7 0.0 0.0 4.820 1023456.4 250.7 4..8?8 ?922278?.8 259.7 4.821 1024368.3 250.7 4.819 0.000 1026108.8 0.0 250.7 0.0 4.819 1027143.3 250.7 4.822 1024350.2 250.7 4.822 1032577.4 250.7 4.819 4.821 0.000 0.000 0.000 4.821 4.820 4.821 4.822 4.821. 4.821 4.820 4.820 4.822 4.822 4.821 4.822 4.821 0.000 0.000 1031034.4 1095013.0 0.0 0.0 0.0 1114555.1 1121590.6 1141707.3 1125752.9 1126887.1 1109607.5 1131681.9 1126242.4 1120633.3 1130160.4 1093945.6 1099099.3 1084462.3 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 5.162 5.155 5.156 5.155 5.156 5.1.57 5.161 5.162 5.156 -c.4.K--4 5.160 5.155 5.158 5.155 5.158 5.162 5.155 5.157 5.157 5.158 5.155 5.158 5.156 5.161 5.158 5.157 5.157 5.152 5.156 5.158 5.158 5.220 5.211 5.213 5.156 5.165 5787.1 1716.6 5360243.5 5515177.0 5645223.0 6158368.0 2803938.5 2060.1 2302.3 7113649.5 5223sc.n 5134239.0 5143755.5 7253.0 4691219.0 4632432.0 4642529.5 4582600.5 2811571.O 7782.5 6500.7 5702.5 8455.8 88443.7 158514.7 268391.2 71 1128.3 1137256.0 1464379.4 2179371.O 2826115.3 6735983.0 10220093.0 12558129.0 22272594.0 10110.2 4001.3 0.0 0.0 214.2 218.6 225.9 249.0 101.5 0.0 0.0 287.2 2n7.2 203.4 203.4 0.0 184.5 182.6 181.5 179.4 101.4 0.0 0.0 0.0 0.0 1.3 3.6 7.6 23.2 38.9 49.7 75.6 99.5 244.0 394.5 492.0 977.2 0.0 0.0 1.3 1.2 -24.4 -7.7 -3.0 -0.8 0.5 -0.7 -2.6 -1.6 -1.8 -2.5 SduMuty,Shake f l u k Mehod YMWl FACT-TCRMIZ RAW DATA Agilent 1100 HPLClMSD "Hillary" Acquistion Run: H010206 PFOS in 3.5% NaCl Solution Shake Flask Method Day 3 Raw Data BACK TO MAIN 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 0 1003-07-03 01003-07-04 01003-07-05 01003-07-06 01003-07-07 01003-07-08 01003-07-09 01003-07-10 01003-07-11 $?$03-07-Q 01003-07-13 MeOH Blank MeOH Blank MeOH Blank nadPFOS-3.4.1 nadPFOS-3.4.2 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 FFOS 25ppb PFOS 40ppb PFOS 50.lppb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS 501.0ppb 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 5O.lppb PFOS 75.lppb PFOS 100.2ppb PFOS 250.5ppb PFOS 400.8ppb PFOS SO1 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-nadPF0S-3.4.11.00x Dil. Method Blank, SFM 02-02-01 MEE(ML.4) TCR-002,012901-nadPFOS-3.4.2. IOOX Dil. Method Bfank. SFM 02-02-01 MEE(MLA) 2 H010206A.M HJLL0002.D 95 3 H010206A.M HILL0003.D 13 4 H010206A.M HILL0004.D 13 5 H010206A.M HILL0005.D 95 6 H010206A.M HILL0006.D 95 87 HH0U1i0O20P6UA6.MA,fHiEI;Li;Lv0^0v07^.vD^u".c95 9 H010206A.M HILL0009.D 2 10 H010206A.M HILLOO1O.D 3 I! H010206A.M HILLOO1l.D 4 12 HOI0206A.M HILL0012.D 5 13 H010206A.M HILL0013.D 6 14 H010206A.M HILL0014.D 7 15 H010206A.M HILL0015.D 8 16 H010206A.M HILL0016.D 9 17 H010206A.M HILL0017.D 10 18 H010206A.M HILL0018.D 11 19 H010206A.M HILL0019.D 12 20 H010206A.M HILL0020.D 13 21 H010206A.M HILL0021.D 96 22 H010206A.M HILL0022.D 96 23 H010206A.M HILL0023.D 96 24 HO10206A.M HILL0024D 1 25 H010206A.M HILL0025.D 2 26 H010206A.M HILL0026.D 3 27 HO10206A.M HILL0027.D 4 28 H010206A.M HILL0028.D 5 29 H010206A.M HILLO029.D 6 30 H010206A.M HILL0030.D 7 31 H010206A.M HILL0031.D 8 32 H010206A.M HILL0032.D 9 33 H010206A.M HILL0033.D 10 34 H010206A.M HILL0034.D 11 35 H010206A.M HILL0035.D 12 36 H010206A.M HlLL0036.D i3 37 H010206A.M HILL0037.D 96 38 H010206A.M HILL0038.D 96 39 H010206A.M HILL0039.D 97 40 H010206A.M HILL0040.D 51 41 H010206A.M HILL0041.D 52 4.104 9621.8 0.0 0.000 0.0 0.0 5.162 1366.8 0.1 4.108 1891799.6 299.3 4.822 967438.5 250.7 5.208 22423620.0 1538.4 4.108 1887421.0 288.1 4.823 1002759.7 250.7 5.208 21458074.0 1251.5 4.105 13291.9 0.0 0.000 0.0 0.0 5.155 10494.2 0.1 4.105 13218.0 0.0 0.000 0.0 0.0 5.156 . 3099.5 0.1 4.105 12931.8 0.0 0.000 0.0 0.0 5.155 7381.7 0.1 4.?!?-? !nnn?E;! . 3 266.2 4.822 1039861.I 250.7 5.162 12818.6 0.6 4.106 1870716.5 268.4 4.821 1066850.1 250.7 5.157 86415.2 3.3 4.106 1907032.1 267.0 4.821 1092983.6 250.7 5.157 158469.1 5.7 4.106 4.108 1843009.6 1847886.0 264.6 264.4 4.820 4.822 1065255.5 1089764.8 250.7 25ii.i 5.156 273021.3 10.0 ac ..,CaO0 708?43.3 -9-6.- R 4.105 1841950.1 262.6 4.820 1073389.1 250.7 5.156 1155762.5 42. I 4.104 1852270.8 262.2 4.822 1081077.6 250.7 5.162 1429296.4 51.8 4.106 1849483.9 263.2 4.820 1075265.0 250.7 5.156 2158608.0 79.2 4.106 1833357.3 261.5 4.820 1072851.6 250.7 5.156 2797833.8 103.5 4.106 1780889.1 251.6 4.820 1083292.4 250.7 5.240 6612530.5 252.6 4.104 1870953.8 272.3 4.822 1051607.1 250.7 5.183 10170355.0 420.9 4.104 1863719.8 267.6 4.822 1065822.9 250.7 5.211 12424400.0 523.9 4.102 1820228.4 266.8 4.820 1044313.8 250.7 5.180 22065096.0 1219.6 4.107 12848.0 0.0 0.000 0.0 0.0 5.158 3335.9 0.1 4.105 12476.6 0.0 Q.000 0.0 0.0 5.155 6796.1 0.1 4.104 12057.4 0.0 0.000 0.0 0.0 5.162 6750.2 0.1 4.107 1840212.0 257.8 4.821 1092359.3 250.7 5.157 12639.4 0.6 0.0 4.105 1846254.5 256.1 4.820 1103289.0 250.7 5.156 89759.2 3.3 0.0 4.105 1865722.9 253.7 4.819 1125402.9 250.7 5.155 159703.8 5.6 12.3 4.108 1863265.3 257.9 4.822 1105801.0 250.7 5.158 268012.6 9.5 -5.0 4.104 1894610.1 262.2 4.822 1105694.1 250.7 5.162 713836.3 25.2 0.3 4.105 1661333.8 258.4 4,819 1102618.5 250.7 5.155 1132725.6 40.1 0.1 4.106 1830163.8 252.4 4.821 1109924.9 250.7 5.157 , 1441188.8 50.8 1.5 4.106 1851626.5 256.3 4.820 1105607.3 250.7 5.156 2124345.5 75.7 0.7 4.105 1833460.3 253.8 4.819 1105475.6 250.7 5.155 2806380.8 100.7 0.5 4.106 1855395.4 256.2 4.821 1108144.0 250.7 5.157 6668410.0 248.7 -0.7 4.106 1858516.4 262.0 4.821 1085765.9 250.7 5.241 9982846.0 397.2 -0.9 4.104 1891111.4 265.7 4.022 1089443.1 250.7 5.197 12576619.0 517.8 3.4 4.iiX :s:9519.9 2n.2 4.822 1045348.4 250.7 5.169 22259990.0 1238.9 0.0 4.107 12090.8 0.0 0.000 0.0 0.0 5.165 6525.8 0.1 4.104 11984.1 0.0 0.000 0.0 0.0 5.161 , 6927.2 0.1 4.107 11526.1 0.0 0.000 0.0 0.0 0.000 0.0 0.0 4.108 1926670.8 278.3 4.823 1059642.9 250.7 5.152 8463.8 0.5 4.106 2009192.8 290.4 4.820 1058807.8 250.7 5.156 3730.3 0.3 BACK TO MAIN FACT-TCROOZ TCR-002, 012901-nadPFOS3.4.3, 1OOX Dil. Method Blank, SFM 02-02-01 nadPFOS-3.4.3 MEE(MLA) 42 HOl0206A.M HILL0042.D 53 TCR-002. 012901-nadPFOS-3.4.4. 100X Dil. Method Blank, SFM 02-02-01 nadPFOS3.4.4 MEE(MLA) 43 H010206A.M HILL0043.D 54 MeOH Blank TN-A-4755, 05 Feb 01. exp:2005. 44 H010206A.M HILL0044.D 97 TCR-002, 012901-naclPFOS3.1 .l.1OOX nadPFOS3.1.I Dil. SFM 02-02-01 MEE(MLA) 45 HO10206A. M HILL0045D 61 TCR-002. 012901-nadPFOS3.1.2, lOOX nadPFOS3.1.2 Di. SFM 02-02-01 MEE(MLA) 46 H010206A.M HILL0046.D 62 TCR-002. 012901-nadPFOS3.1.3. lOOX nadPFOS-3.1.3 Dil. SFM 02-02-01 MEE(MLA) 47 H010206A.M HILL0047.D 63 TCR-002. 012901-nadPFOS-3.1.4, lOOX nadPFOS-3.1.4 Dil. SFM 02-02-01 MEE(MLA) 48 H010206A.M HILL0048.D 64 01003-07-09 MeOH Blank MeOH Blank 100.2ppb PFOS, CCV TN-A-4755, 05 Feb 01, exp:2005. TN-A-4755, 05 Feb 01, exp:2005. ' 49 H010206A.M HILL0049.D 9 50 H010206A.M HILL0050.D 97 51 H010206A.M HILL0051.D 97 TCR-002, 012901-nadPFOS-3.2.1. 1OOX nadPFOS-3.2.1 Dl. SFM 02-02-01 MEE(MLA) 52 H010206A.M HILL0052.D 65 . ./ TCR-002. 012901-nadPFOS-3.2.2, lOOX na.c.. ir-rCuAwI .x-L1.L mil "1,. "errl .w. A" n3 . n. ..CC/,", VL-VL-" I '.'Lb\'." &\ 5 1 HningotiA M HILL0053 D 66 TCR-002, 012901-nadPFOS-3.2.3, 100X nadPFOS-3.2.3 Dil. SFM 02-02-01 MEE(MLA) 54 H010206A.M HILL0054.D 67 TCR-002. 012901-nadPFOS-3.2.4. 1OOX nadPFOS-3.2.4 Dil. SFM 02-02-01 MEE(MLA) MeOH Blank TN-A-4755. 05 Feb 01, exp:2005. ' 55 H010206A.M HILL0055.D 68 56 H010206A.M HILL0056.D 97 TCR-002. 012901-nadPFOS-3.3.1, 1OOX nadPFOSJ.3.1 Dil. SFM 02-02-01 MEE(MLA) 57 HO10206A.M HILL0057.D 69 TCR-002. 012901-nadPFOS3.3.2. lOOX nadPFOS3.3.2 Dil. SFM 02-02-01 MEE(MLA) 58 H010206A.M HILL0058.D 70 TCR-002, 012901-nadPFOS-3.3.3, 1OOX nadPFOS3.3.3 Dil. SFM 02-02-01 MEE(MLA) 59 H010206A.M HILL0059.D 71 TCR-002. 012901-nadPFOS-3.3.4, 100X nadPFOS-3.3.4 Dil. SFM 02-02-01 MEE(MLA) 60 H010206A.M HILL0060.D 72 01003-07-09 100.2ppb PFOS. CCV 61 H010206A.M HILL0061.D 9 MeOH Blank MeOH Blank MeOH Blank 01003-07-01 01003-07-02 01003-07-03 01003-07-04 01003-07-05 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 2.5ppbPFOS . 5ppb PFOS 1Oppb PFOS 25ppb PFOS 62 H010206A.M HILL0062.D 98 63 H010206A.M HILL0063.D 98 64 H010206A.M HILL0064.D 98 65 H010206A.M HILL0065.D 1 66 H010206A.M HILL0066.D 2 67 H010206A.M HILL0067.D 3 68 H010206A.M HILLOO68.D 4 69 H010206A.M HILL0069.D 5 01003-07-06 e!en3-G-n? 01003-07-08 40ppb PFOS Snlppb PFOS 75. Ippb PFOS 70 H010206A.M HILL0070.D 6 71 H010206A.M HILL0071.D 7 72 H010206A.M HILL0072.D 8 01003-07-09 100.2ppb PFOS 73 H010206A.M HILL0073.D 9 01003-07-10 250.5ppb PFOS 74 H010206A.M HILL0074.D 10 01003-07-1 1 400.8ppb PFOS 75 H010206A.M HILL0075.D 11 01003-07-12 01003-07-1 3 MeOH Blank MeOH Blank 501.0ppb PFOS 1002.0ppb PFOS TN-A-4755, 05 Feb 01. exp:2005. TN-A-4755. 05 Feb 01. exp:2005. 76 H010206A.M HILL0076.D 12 77 H010206A.M HILL0077.D 13 78 H010206A.M HILL0078.D 98 79 H010206A.M HILL0079.D 98 4.106 2025762.9 292.3 4.821 1060565.4 250.7 5.157 7621.1 0.4 4.105 1979531.4 288.6 4.819 1049618.8 250.7 5.156 3744.8 0.3 4.106 11598.8 0.0 0.000 0.0 0.0 5.157 5353.4 0.1 4.104 1986989.8 298.8 4.822 1017566.9 250.7 5.162 5394307.0 217.1 4.104 1903896.9 281.9 4.822 1033535.4 250.7 5.161 5387695.5 213.3 4.105 1903997.0 283.7 4.820 1027231.4 250.7 5.156 5409418.0 215.6 4.107 2028305.4 305.1 4.821 1017373.9 250.7 5.158 5367317.5 216.0 4.107 1828271.5 250.2 4.821 1118280.8 250.7 5.157 2840861.5 100.7 0.5 0.000 0.0 0.0 0.000 0.0 0.0 5.155 7618.2 0.1 0.000 0.0 0.0 0.000 0.0 0.0 5.162 8197.7 0.1 4.104 1998596.6 297.3 4.819 1028671.3 250.7 5.155 5247156.5 208.4 4.105 2000593.5 298.4 4.819 1025976.1 250.7 5.155 5202058.5 207.1 4.107 2000672.9 299.4 4.821 1022749.9 250.7 5.157 5144285.5 205.3 4.105 0.000 1891713.3 0.0 280.7 0.0 4.819 0.000 1031479.1 0.0 250.7 0.0 5.155 5.155 5024824.0 6650.2 198.5 0.1 4.106 1896904.9 285.8 4.821 1015830.9 250.7 5.157 4756814.0 190.3 4.104 1956381.6 295.0 4.822 1015064.3 250.7 5.162 4726155.5 189.2 4.106 1902701.1 283.0 4.820 1028884.6 250.7 5.156 4696616.0 185.3 4.105 1894214.3 284.8 4.820 1017989.3 250.7 5.156 4754382.0 189.8 4.106 1756132.8 242.7 4.820 1107496.5 250.7 5.156 2809160.5 100.6 0.4 0.000 0.0 0.0 0.000 0.0 0.0 5.155 6589.1 0. I 4.104 11876.2 0.0 0.000 0.0 0.0 0.000 0.0 0.0 0.000 0.0 0.0 0.000 0.0 0.0 5.156 5586.4 0.1 4.105 1780994.1 245.2 4.819 1111747.3 250.7 5.156 12076.9 0.6 0.0 4.105 1755939.4 236.5 4.819 1136281.3 250.7 5.155 88457.2 3.1 0.0 4.104 1814153.1 241.7 4.822 1148491.8 250.7 5.161 156107.9 5.4 7.7 4.104 1790839.6 239.8 4.821 1143103.6 250.7 5.161 274913.9 9.4 -5.7 4.106 1788983.0 243.8 4.821 1122996.1 250.7 5.157 709161.8 24.6 -1.9 4.105 1770309.1 240.0 4.820 1129011.3 250.7 5.156 1158373.6 40.1 0.0 -- - 4.106 1832118.0 248.1 4.821 1130353.5 250.7 5.157 1436545.9 49.8 -0.7 4.106 1799289.3 243.7 4.820 1129984.5 250.7 5.156 2i6080i.O 13.0 0.6 4.104 1739000.9 235.3 4.819 I131132.6 250.7 5.155 2826039.5 99.0 -1.2 4.108 1788427.6 246.5 4.822 1110432.5 250.7 5.194 6744845.5 251.3 0.3 4.104 1755005.4 248.1 4.822 1082374.3 250.7 5.162 10142755.0 406.0 1.3 4.105 1787929.6 244.5 4.819 1119100.9 250.7 5.155 12195626.0 483.6 -3.5 4.107 1830473.3 263.4 4.822 1063516.4 250.7 5.193 22142466.0 1185.0 0.0 0.000 0.0 0.0 0.000 0.0 0.0 5.156 2995.9 0. I 4.106 11785.3 0.0 0.000 0.0 0.0 5.156 1708.9 0. I FACT7CRMIZ PFOS in 3.5% NaCl Solution Day 1 Hillary. H010131 BACK TO MAIN P a p 7 01 11 FACT-TCR-002 PFOS,in 3.5% NaCl Solution Day 2 Hillary. H010205 BACK TO MAIN TCR-002.012901-nadPFOS-2.1.1. IOOX 45 H010205A.M HILL0045,D 31 5.155 5360243.5 214.2 21.4 nadPFoS-2.1.1 Dil. SFM 02-01-01 MEE(MLA) TCR-OO2,012901-nadPFOS-2.1.210.0X 46 H010205A.M HILL0046,D 32 5.156 5515177.0 218.6 21.9 nadPFoS-2`1.2 Dil. SFM 02-01-01 MEE(MLA) TCR-002.012901-nadPFOS-2.1.3, 1OOX 47 H010205A,M HILL0047.D 33 5.155 5645223.0 225.9 22.6 nadPF0S-2'1'3 Dil. SFM 02-01-01 MEE(ML4) TCR-002,012901-nadPFOS-2.1.I4O,OX 48 H010205A,M HILL0048,D 34 5.156 6158368.0 249.0 24.9 nadPF0S-2'1.4 Dil. SFM 02-01-01 MEE(MLA) 21 .o 22.2 21.4 1.52 22.1 6.8% 24.4 TCR-002, 012901-nadPFOS2.2.2,lOOX 53 H010205A,M H,LL0053.D 36 5.155 5223066.0 207.2 20.7 20.3 0.23 nadPFoS2'2'2 Dil. SFM 02-01-01 MEE(MLA) TCR-002,012901-nadPFOS-2.2.3. IOOX 54 H010205A.M HILL0054,D 37 5.160 5134239.0 203.4 20.3 19.9 1.2% nadPF0S-2`2`3 Dil. SFM 02-01-01 MEE(MW 5 InadPF0s-Z'2'4 TCR-002,012901-nadPFOS2.2.4. Dil. SFM 02-01-01 MEE(MLA) IOOX 55 H010205A,M HILL0055,D 38 5.155 5143755.5 203.4 20.3 19.9 lnadPF05-2.3.1 TCR-002.012901-nadPFOS-2.3.1.IOOX Dil. SFM 02-01-01 MEE(MLA) 57 H010205kM HILL0057.D 39 5.155 4691219.0 104.5 18.5 18.1 17.8 lnadPF0s-2'3'2 TCR-002.012901-nadPFOS-2.3.2, Dii. SFM 02-01-01 MEE(MLA) 1oOX 58 H010205A,M HlLL0058,D 4o 5.158 4632432.0 182.6 18.3 17.9 0.25 TCR-002. 012901-nadPFOS2.3.3, IOOX 59 H010205kM H,LL0059,D 4, 5.162 4642529.5 181.5 18.2 17.8 1.4% lnadp~os-2.3.3 Dil. SFM 02-01-01 MEE(ML4) TCR-OO2,012901-nadPFOS2.3.4. 1oOx 6o H010205kM HILL0060,D 42 5.155 4582600.5 , 179.4 17.9 17.5 Inadp~os-2.3.4 Dil. SFM 02-01-01 MEE(MLA) SdubWy.Shake fluk Mehod 5,ZrZWI FACT-TCR-002 BACK TO MAIN PFOS in 3.5% NaCl Solution Day 3 Hillary, 010206 InadPFOSJ'l'l TCR-002,012901-nadPFOS-3.1.1,10OX Dil. SFM 02-02-01 MEE(ML4) TCR-002,012901-nadPFOS-3.1.2. 100X (nadpF0S-3.1.2 Dil. SFM 02-02-01 MEE(MLA) nadPFOS-3.1.3 TCK-UUS. uii90i-nadiYcS3.7.3, Dil. SFM 02-02-01 MEE(MLA) 45 H010206AM HILL0045.D 6l 46 Holo206A,M HILL0046.D 62 47 H010206A.M HlLLOU47.b 63 5.162 5.161 5.i56 5394307.0 5387695.5 54094!8.!? 217.1 213.3 2!5E TCR-002, 012901-nadPFOS-3.2.1,lOOX 52 H010206A,M HlLL0052,D 65 (nadPF0SJ.2'2 TCR-002,012901-nadPFOS-3.2.2,lOOX Di. SFM 02-02-01 MEE(MtA) I ~ ~ ~ P F o s - J . ~ . ~ TCR-002,0+2901-nadPFOS-3.2.3. Dil. SFM 02-02-01 MEE(MLA) lOOX TCR-002.012901-nadPFOS-3.2.4.lOOX ( ~ ~ c J P F o s - JD. ~il. .S~FM 02-02-01 MEE(MLA) TCR-OO2,012901-~dPFOS3.3.lO1,OX I n a d ~ ~ o s - 3 - 3 .D1il. SFM 02-02-01 MEE(Mu) TCR-002,012901-nadPFOS-3.3.2.lOOX Jnadp~os-3.3.2 Dil. SFM 02-02-01 MEE(MLA) TCR-002.012901-nadPFOS3.3.3, IOOX Di. SFM 02-02-01 MEE(MLA) TCR-002,012901-nadPFOS-3.3.4. IOOX I 53 H010206A,M HILL0053,D 66 54 H010206kM HILL0054,D 67 55 H010206A,M H,LL0055.D 68 ST H010206A,M HILL0057.D 69 58 H010206AM HlLLO058.D 7o 59 H010206/*M HILL0059,D 71 6o HO10206A,M HILL0060,D 72 5.155 5.155 5.157 5.155 5.157 5.162 5.156 5.156 5247156.5 208.4 5202058.5 207.1 5t44265.5 205.3 5024824.0 198.5 4756814.0 190.3 4726155.5 189.2 4696616.0 185.3 4754382.0 1 189.8 avenge: std dev: 21.7 21.2 21.3 20.9 21.6 21.1 21.6 21.1 20.8 20.4 20.7 20.3 20.5 20.1 19.8 19.4 19.0 18.6 18.9 18.5 18.5 18.1 19.0 18.6 19.9 p@mL 1.31 21.1 0.13 0.6% 20.1 0.45 2.2% 18.5 0.24 1.3% P.* a Of 11 BACK TO MAIN FACT-TCROOZ PFOS Solubility of TCR-00017-46 in 3.5% NaCl Solution Day 1 data source acquisition inrtrument/aequence: Agilent 1100 HPLClMSD "Hillrry"WO10131.s Day 2 data source acquisition instrument/scqucnce: Agilent 1100 HPLCMSD "Hilluy"WO1OZOS.s Day 3 data source acquisition instrumcnt/requutcc: Agilcnt 1100 HPLClMSD"Hillary"W010206.s DATA SUMMARYFOR INDIVIDUAL SAMPLES FACT-TCROOZ PFOS Solubility of TCR-00017-46 in 3.5% NaCl Solution. naclPFOS-2 1 1 naclPFOS-2 1 2 naclPFOS-2 1 3 naclPFOS-2 1 4 naclPFOS-2.2.2 naclPFOS-2.2.3 naclPFOS2.2.4 naclPFOS2.3.1 naclPFOS2.3.2 naclPFOS-2.3.3 naclPFOS-2.3.4 naclPFOS-3.1.1 naclPFOS-3.1.2 naclPFOS3.1.3 - - r l O C A P a. 4 A llPUl I "Y-"...- naclPFOS.3.2.1 naclPFOS-3.2.2 nadPFOS-3.2.3 IW~PFOS-3.2.4 nadPFOS-3.3.1 nadPFOS-3.3.2 nacIPFOS-3.3.3 naclPFOS-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 is o 3M EnvkmmonW Laboratory 21 0 21 4 22 I 24 4 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 22 2 I52 6 8% 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% 1 Averave: 20.0 PPm StdDev: 2.20 %CV 11.0% (Sample2.2.1 cxcluded viaQ-Tut) Dav 3 data summary -- Average: 19.9 StdDev: 1.31 PPm - %CV: 6- .6% rOTAL data summary Average: 20.0 PPm -- StdDev: 0.07 -- %CV: 0.4% Z t a from Days 2 and 3 arc wed. lay 1 has been omitted ftom the calculations. FACT-TCR-002 PFOS in 3.5%NaCl Solution Shake Flask Method BACK TO MAIN -- Q-TEST DlataCalculations: Sample ID: -- Sample Conc., Rep1 Sample Conc., lRep2 Sample Conc., IRep3 Sample Conc., !Rep4 . Range: Gap: Qsbs: No. observations: Retain? naclPFOS-2.2.3 naclPFOS-2.2.4 20.3 19.9 19.9 8.20 7.80 0.95 4 no Exclude rep I! L- 9 Qobserved = gaplrange!where "gap" is the difference between the questionable data point and the closest value of the data s e t , and "range" is the difference between the highest and lowest value of the data set. If C!observed is > Q-tabulated, then the data point may be excluded with 9O?h 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-TCROOZ (LIMS #E00-1716), Page 62 of 138 Page 11 of 11 ATTACHMENcT: SAMPLE CHROMATOGRAMS BACK TO MAIN FACT-TCROOP (LIMS#E00-1716), Page 63 of 138 Batch Run # 22 of 79 Data File C:\HPCHEM\l\DATA\HOl0125\HILL0022.D BACK TO MAIN Sample Name: MeOH Blank T._.N_.- .A_.- .4_.7.-4.0-.,-._. ._0.4_. ._D.e._.c._.0_.0._. ._. ._. _. ._. .-.-.-.-. -. .-.-.-.-.-.-.-.-.-. -. .-.-.-.-.-.-.-.-.-. .-.-.-.-.-.-.-.-.-. -. - - - - - - - - - - - - - - - - Injection Date : 1/25/01 1:13:34 PM Seq. Line : 22 Sample Name : MeOH Blank vial : 92 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl ACq. Method : C:\HPCHEM\l\METHODS\HOl0125.M Last changed : 1/25/01 9:13:04 AM by MLA Analysis Method : C:\HPCHEM\l\METHODS\H0125Al.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" LT - MSDl 299, EIC=298.7:299.7 (H0101:!5VllLL0022.D) API-ES, Neg, SIM, Frag: Var I 250000: 4 : 2000 1500 { 1000 ; 500 __r 2 4 6 MSDl 427. ElC426.73427.7 ( H 0 1 0 1 ~ 0 0 2 2 . D ) API-ES. Neg, SIM, Frag:Var 8 min 12000 7 10000 7 8000 : 6000 1 4000 7 2000 7 -------o I- --- I 3000 I 2000 L < 1500 1000 I L,~-LJ-L+-l\.iRr Instrument 1 1/29/01 2:28:36 PM :KLT/M:LA FACT-TCROOP (LIMS#E00-1716), Page 64 oi 138 Page 1 of 3 Batch Run # 22 of 79 Data File C:\HPCHEM\l\DATA\HOlOl25\HILL0022.D - - - - I#- - - - - - - - - - -[- -n) -g- -/- - m- - L- - l- - - - - - - - - - - - - - - - 1 254.00000 PFBS 2 254.40000 THPFOS Totals without ISTD(s) : 0.00000 BACK TO MAIN Sample Name: MeOH Blank Totals without ISTD(s) : 0.00000 Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : ISTD compound(s) not found Sorted By Calib. Data Modified : Multiplier Dilution Signa.1 Mondaly, January 29, 2001 2:15:31 PM 1.0000 1.0000~ Signal 1: MSDl 299, EIC=298.7:299.7 Peak RetTime Type Width ----1#-------1-[--m--i-1n--l-----1.-----.-----1------[--mini 1 4.111 I 0.0000 Area 0,00000 Totals : 0.00000 Area Name % I ..................... 0.0000 PFBS Instrument 1 1/29/01 2:28:36 PM KLT/MLA FACT-TCROOS (LIMS #E00-1716), Page 65 of 138 Page 2 of 3 Batch Run # 22 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILLOO22.D Totals : 0.00000 Signal 3 : MSDl 499, EIC=498.7:499.7 1 Warnings or Errors : Warning : ISTD compound(s) not found BACK TO MAIN Sample Name: MeOH Blanb Instrument 1 1/29/01 2:28:36 PM :KLT/MLA FACT-TCROOP (LIMS #E00-1716), Page 66 of 138 Page 3 of 3 Batch Run # 38 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILL0038.D TN-A-4740, 04 Dec 00 _________--_--_-_-----_--______________-_-----------------.----.------.----.------------------------------------------------------------------ Injection Date : 1/25/01 4:13.:20 I'M Seq. Line : Sample Name : MeOH Blank Vial : Acq. Operator : MLA Inj : Acq. Instrument : Hillary Inj Volume : Acq. Method : C:\HPCHEM\l\,METHODS\HOlOl25.M Last changed : 1/25/01 9:13:04 AM by MLA Analysis Method : C:\HPCHEM\l\,METHODS\H0125Al.M Last changed : 1/29/01 2:30:01 I'M by KLT/MLA (modified after .l!oading) PFOS Analysis Column: C18 Betasil 5um SOX2 mm Eluents: Methanol and 2 mm Amnioniunn Acetate Reprocessed on I1Dioana" KLT MSDl 299, EIC=298.7:299.7 (H0101m l 0 3 8 . D ) API-ES, Neg, SIM, Frag: Var 38 92 1 10 p l BACK TO MAIN Sample Name: MeOH Blank 1 12000 : 10000 1 8000 : 6000 : 4000 : 2000 7 0 -- I I( I I I I -_--------- - I , I I I I I II I I ,I I I I I 2 4 6 8 mir Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name Signa.1, Monda.y, January 29, 2001 2:15:31 PM 1.O O C ~ O 1. O O C l O Instrument 1 1/29/01 2:30:01 PM PLT/MIA FACT-TCROOZ (LIMS#E00-1716), Page 67 of 138 Page 1 of 3 BACK TO MAIN Sample Name: MeOH Blank Totals without ISTD(s1 : 0.00000 Signal 2: MSDl 427, EIC=426.7:427.'7 Totals without ISTD(s1 : 0.ooooo Signal 3: MSDl 499, EIC=498.7:499.7 Totals without ISTD(s) : 1 Warnings or Errors : Warning : ISTD compound (s) not found 0.00000 Multiplier Dilution 1.0000 1.0000' Signal 1: MSDl 299, EIC=298.7:299.7 Totals : 0.00000 Name Instrument 1 1/29/01 2:30:01 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716),Page 68of 138 Page 2 of 3 Batch Run # 38 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25'~HILLf~O38.D Signal 2: MSDl 427, EIC=426.7:427.7 Peak RetTime Type - -#- - I - -[-m-i-n-l- - - - - - - 1 4.864 I Totals : 0.00000 Signal 3: MSDl 499, EIC=498.7:499.7 Totals : 0.00000 1 Warnings or Errors : Warning : ISTD compound(8) not found BACK TO MAIN Sample Name: MeOH Blank Instrument 1 1/29/01 2:30:01 PM KLT/E'ILA FACT-TCR002 (LIMS #E00-1716), Page 69 of 138 Page 3 of 3 Batch Run # 43 of 59 Data File C:\HPCHEM\1\DATA\HOlOl29\HILLOl22.D BACK TO MAIN Sample Name: MeOH Blank TN-A-4740, 04 Dec 00 ===P==I============p========p==x=151========================~=============== Injection Date : 1/30/01 12:10:30 PM Seq. Line : 122 Sample Name : MeOH Blank Vial : 97 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p l Acq. Method : C:\HPCHEM\l\METHC~DS\HOl0129.M Last changed : 1/29/01 1:35 :12 F'M by M L A Analysis Method : C:\HPCHEM\l\METHClDS\HOl0129B.M Last changed : 1/31/01 11:C18:44AM by KLT/MLA (modified after 1.oading) PFOS Analysis Column: C18 Betasil 5um 50x2 mm Eluents: Methanol and 2 mm Ammonium Acetate I: :Reprocessed on "Dioana" KLT MSDl 299, ElC=298.7299.7( H O l O l ~ l 1 2 2 . D )API-ES, Neg, SIM, Frag: Var I 2000 4 12000 : 10000 1 8000 1 6000 : 4000 : 2000 : 0 -7 I 1- I I ,. _A_-- ~ - - - - - I I Instrument 1 1/31/01 11:21:50 MI KLT/'MLA FACT-TCROO2 (LIMS #E00-1716). Page 70 of 138 Page 1 of 3 Batch Run # 43 of 59 Data File C:\HPCHEM\1\DATA\HolOl29\HILLOl22.D Signal 1: MSDl 299, EIC=298.7:299.7. Totals without ISTD(s) : 0.00000 ~~ ~ ~~ BACK TO MAIN Sample Name: MeOH Blank Totals without ISTD(9) : 0.00000 Totals without ISTD(S) : 0* 00000 1 Warnings or Errors : Warning : ISTD compound(s) not found Sorted By Calib. Data Modified : Multiplier Dilution Signal 1/31/01 11:08:42 AM 1.0000 1.0000 Signal 1: MSDl 299, EIC=298.7:299.7 Totals : 0.~30000 Instrument 1 1/31/01 11:21:50 AM KLT/MLA 4 FACT-TCROOZ (LIMS #E00-1716),Page 71 of 138 Page 2 of 3 Batch Run # 43 of 59 Data File C:\HPCHEM\1\DATA\HOlOl29\HILLOl22.D Totals : 0.00000 Signal 3: MSDl 499, EIC=498.7:499.7 Totals : 0.00000 1 Warnings or Er-rors : Warning : ISTD compound(s) not: fomid BACK TO MAIN Sample Name : MeOH Blank Instrument 1 1/31/01 11:21:50 AM IGT/MLA FACT-TCROOZ (LIMS #E00-1716),Page 72 of 138 Page 3 of 3 Batch Run # 41 of 79 Data File C:\HPCHEM\1\DATA\HolOl2S\HILL0041.D BACK TO MAIN Sample Name: swPFOS-1.4.2 TCR-002, 012201-swPFOS-1.4.2, lOOX Dil. Method Blank, SFM 01-24-01 MEE:(MLA) -_---------------_---------_-_---------------------.----.----~----------------------------------------------------------------------- Injection Date : 1/25/01 4:44.:42 PM Seq. Line : 41 Sample Name : SWPFOS-1.4.2 Vial : 22 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl Acq. Method Y C:\HPCHEM\l\,METHODS\HOl012.5M Last changed : 1/25/01 9:13:04 AM by M L A Analysis Method : C:\HPCHEM\l\,METHC)DS\H0125Al.M Last changed : 1/29/01 2:30:17 I'M by KLT/MLA (modified after loading) PFOS Analysis Column: C18 Betasil Eium 50x2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on flDioanalf LT MSDI 299, ElC=298.7:299.7 (HOIOI25WlLLOO41.D) API-ES, Neg, SIM, Frag: Var i350000 300000 250000 I I I , i L MSDI 427, , ElC426.7427.27 I (H010125vllLL(~04.1D) A4PI-ES, Neg, SIM, Frag: Var 6 ,, I ~, , 8 , , , mir~ 250000 : 200000 : 150000 : 100000 : 50000 : Instrument 1 1/29/01 2 :30 :18 PM KLT/MIA FACT-TCROOS (LIMS#E00-1716), Page 73 of '138 Page 1 of 2 Batch Run # 41 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILLOO4l.D BACK TO MAIN Sample Name : swPFOS-1.4.2 Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name ----I#-------------I[--n---g---/---d--I---,--------- 1 254.00000 PFBS 2 254.40000 THPFOS Signal M:onday,January 29, 2001 2:15:31 PM 1.0000 1.0000' Signal 1: MSDl 299, EIC=298.7:299.7 Totals without ISTD(s) : 0.00000 Signal 2 : MSDl 427, EIC=426.7 :427.'7 Totals without ISTD(s) : 0.00000 Signal 3: MSDl 499, EIC=498.7:499.7 Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : Calibrated compound(s) n.ot found Instrument 1 1/29/01 2:30:18 PM ICLT/MI;A FACT-TCROOZ (LIMS#E00-1716),Page 74 of 138 Page 2 of 2 Batch Run # 22 of 59 Data File C:\HPCHEM\1\DATA\HO1012;\HILIJO158.D BACK TO MAIN Sample Name: swPFOS-2.4.3 TCR-002, 012201-SWPFOS-1.4.3, lOOX Dil. Method Blank, SFM 01-25-01 ME$ (MLA) ....................................................................... Injection Date : 1/27/01 7 : l : L : O l I?M Seq. Line : 158 Sample Name : SWPFOS-2.4.3 Vial : 61 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p1 Acq. Method ,: C:\HPCHEM\l'\METHODS\HOl0125 .M Last changed : 1/25/01 9:1:%:04AM by MLA Analysis Method : C:\HPCHEM\l'\METHODS\HOl0126C.M Last changed : 1/30/01 2:5:1:45 I?M by KLT/MLA (modified a:Eter :Loading) PFOS Analysis Column: C18 Betinsil !Sum 50x2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on ffDioanalf L" KLT MSDl 299, ElC=298.7:299.7 (H010126VllLLO158.D) API-ES, Neg, SIM, Frag: Var I 300000 250000 I 2 4 6 MSDl 427, ElC426.73427.7 (HOl0126\HILLO158.D) API-ES, Neg, SIM, Frag: Var A 200000 1 150000 1 100000 1 50000 : 2 MSDl 499, ElC=498.7:499.7 (HOlOl2S\HILL.Ol58.D) 250012000 4 6 API-ES, Neg, SIM, Frag: Var 8 mir, I 8- mip Instrument 1 1/30/01 2:52:45 PM ICLT/MLA FACT-TCROO2 (LIMS#E00-1716), Page 75 of 138 Page 1 of 2 Batch Run # 22 of 59 Data File C:\HPCHEM\l\DATA\HOlO126\HILLO1S8.D BACK TO MAIN Sample Name : SwPFOS-2.4.3 Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name ----I#-------------I[---n--g--/--f--.i--l---.--------- 1 2S4.00000 PFBS 2 254.40000 THPFOS Signal ?'uesda.y, January 30, 2001 2:27:34 PM 1..O O O C ~ 1..O O O C l Totals without ISTD(s) : 0.00000 Signal 2: MSDl 427, EIC=426.7:427.'7 Totals without ISTD(s) : 0.00000 Totals without ISTD(s) : 0.00000 2 Warnings or Errors : Warning : Calibration warnings (see.calibration table listing) Warning : Calibrated compound (s) not found Instrument 1 1/30/01 2:52:45 PM lKLT/M:LA FACT-TCROO2 (LIMS #E00-1716),Page 76 of'138 Page 2 of 2 Batch Run # 22 of 59 Data File C:\HPCHEM\1\DATA\HO1Ol29~~HILLOlOl.D BACK TO MAIN Sample Name: swPFOS-3.4.3 4 300000 I 250000 I 200000 '$ 150000 L 100000 4 50000 1 0-: 200000 150000 1 4q5 ,>!" I I I Instrument 1 1/31/01 11:20:03 AM KLT/1\ILA FACT-TCROOP (LIMS #E00-1716), Page 77 of 138 Page 1 of 2 Batch Run # 22 of 59 Data File C:\HPCHF,M\1\DATA\HOlol29\HILLOlOl.D Sorted By E: ignal. Calib. Data Modified : 3./31/01 11:08:42 AM Multiplier 3.. 0000 Dilution I.. 0000 Sample ISTD Information: ISTD ISTD Amount Name - - -#- I - - - -[-n-g-/-m-L-l- - - I - - - - - - - - - - . - - - - - . . - - - - - - - - - 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.'7 Totals without ISTD(s) : 0.00000 BACK TO MAIN Sample Name : swPFOS-3.4.3 Totals without ISTD(s) : 0.00000 Signal 3: MSDl 499, EIC=498.7:499.7 RetTime tminl 5.144 Type Area - mt/Are:a ratio - Totals without ISTD(s) : Amount [ng/m~l - G r p Name PFOS 0.00000 1 Warnings or Errors : Warning : Calibrated compound(s) :not found Instrument 1 1/31/01 11:20:03 Ab1 KLTIMLA FACT-TCROOZ (LIMS #E00-1716),Page 78 of 138 Page 2 of 2 Batch Run # 46 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILLOO46.D BACK TO MAIN Sample Name : swPFOS-1.1.2 -f 300000 I 250000 I 150000 I 100000 I 50000 I #B" \\!' 2 600000 500000 L 400000 I 300000 I 200000 I 100000 I 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\1\DATA\HOlOl25\HILLOO46.D BACK TO MAIN Sample Name: swPFOS-1.1.2 Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Infoimation : ISTD ISTD Amount Name ----I-#------------I--[---n---g---/.--m--.~.---l------ 1 254.00000 PFBS 2 254.40000 THPFOS Signal. Monday, January 29, 2001 2:15:31 PM 1..OOOCI 7.. OOOCl Totals without ISTD(s) : 0.00000 Totals without ISTD(s1 : 0.00000 Totals without ISTD(s) : 129.93889 Instrument 1 1/29/01 2:30:45 PM KLTIYILA FACT-TCROOZ (LIMS #EOO-1716),Page 80 of138 Page 2 of 2 Batch Run # 53 of 79 Data File C:\HPCHEM\1\DATA\HO10125~,HILL0053.D BACK TO MAIN Sample Name: swPFOS-1.2.2 350000 300000 250000 200000 150000 100000 50000 ~ 1 qd5 &J* I - 200000 150000 100000 50000 2 MSDl499, ElC=498.7:499.7 ( H O l m . L O O 5 3 . D ) I I 4 6 API-ES, Neg, SIM, Frag: Var 600000 { < 500000 200000 5 4 100000 I a m Instrument 1 1/29/01 2:31:23 PPI KLTjMLA FACT-TCR002 (LIMS #EOO-1716), Page 81 of 138 Page 1 of 2 Batch Run # 53 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILI~OO53.D BACK TO MAIN Sample Name: swPFOS-1.2.2 Sorted By !;igna:l' Calib. Data Modified : Monday, January 29, 2001 2:15:31 PM Multiplier :L. 0000 Dilution :1. 0000 Sample ISTD Information: ISTD ISTD Amount Name - -#- - I - - -C-n-g-/-m-L-I- - - - I. . . . . . . . . . . . . . . . . . . . . . . . . 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 RetTime [minl 4.109 VBA+ 12.14016e6 1.00000 254.00000 Totals without ISTD(s1 : 0.00000 Signal 2: MSDl 427, EIC=426.7:427.7 RetTime Type - -[m-i_nl_ _I -_- - - - - . 4.939 VBA+ I Totals without Amount - -[-n_g/-f-i-l- - - 254.40000 0.00000 Signal 3: MSDl 499, EIC=498 .'I :499.7 RetTime Type [minl Area &nt /Area ratio Amount [ng/mLl ~ r p Name Instrument 1 1/29/01 2:31:23 PM KLT/MLA FACT-TCROO2 (LIMS#E00-1716), Page 82 of 138 Page 2 of 2 Batch Run # 57 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILL0057.D BACK TO MAIN Sample Name : SWPFOS- 1.3.1 350000 300000 250000 200000 150000 100000 50000 0, 250000 200000 150000 100000 600000 L 500000 I < 400000 3 300000 200000 I 100000 : nv ,- ' q+@ $Q' 1. ___ I/ Q p' I r I Instrument 1 1/29/01 2:31:45 PM KLT/WLA FACT-TCROO2 (LIMS #E00-1716), Page 83 of 138 Page 1 of 2 Batch Run # 57 of 79 Data File C:\HPCHEM\1\DATA\HOlOl25\HILLOO57.D BACK TO MAIN Sample Name: swPFOS-1.3.1 Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name ----I#------------[-I-n---g--/---a--l-------------- 1 254.00000 PFBS 2 254.40000 THPFOS Signal Monday, January 29, 2001 2:15:31 PM 1.0000 1.0000 Signal 1: MSDl 299, EIC=298.7:299.7 RetTime Type - -[r-n-i-n-l - I - - - - - 4.109 VBA+ I Totals without ISTD(s) : G r p Name 0.00000 Signal 2: MSDl 427, EIC=426.7 :427.'7 RetTime Type [minl Area Amt/Arein ratio Amount G r p Name [ng/mLl Signal 3: MSDl 499, EIC=498.7:499.7 RetTime Type [minl 5.142 PVA+ Area 3.79790e6 Amt/Area ratio 1.45346e-1 Amount G r p Name [ng/mLl 124.50482 PFOS Totals without ISTD(s) : 124.50482 Instrument 1 1/29/01 2:31:45 PM ICLT/MI;A FACT-TCROOP (LIMS #E00-1716),Page 84 of 138 Page 2 of 2 Batch Run # 25 of 59 Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ ~ ~ ; \ H I L ~ J O ~ ~ ~ . D BACK TO MAIN Sample Name: swPFOS-2.1.: J 250000 : 200000 7 150000 1 100000 : 50000 : 0 A I , I ~- 600000 I 500000 I 400000 1 < 300000 200000 I 100000 1 0- I 2 Q90% +?bP' I I I I 6 b mil Instrument 1 1/30/01 2:53:01 PM KLT/MLA FACT-TCROO2 (LIMS #E00-1716), Page 85of 138 Page 1 of 2 Batch Run # 25--0f59 Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ ~ ~ \ H I L ~ J O ~ ~ ~ . D BACK TO MAIN Sample Name: swPFOS-2.1.1 Sorted By Signal Calib. Data Modified : Tuesday, January 30, 2001 2:27:34 PM Multiplier :t. 0000 Dilution :t. 0000 Sample ISTD Information: ISTD ISTD Amount Name ----I#-------------[ng/m~l I - - - - _ _ _ _ _ _ _ _ _ _ _ _ _ _ - - - - - - 1 254.00000 PFBS 2 254.40000 THPFOS Totals without ISTD(s) : 0.00000 Signal 2: MSDl 427, EIC=426.7:427.'7 RetTime - -[-m-in-l- - Totals without ISTD(s) : 0.00000 Totals without ISTD(s) : 122.06875 1 Warnings or Errors : Warning : Calibration warnings (see calibration table listing) 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\1\DATA\HOlOl26~\HILI~Ol64.D BACK TO MAIN Sample Name: swPFOS-2.1.4 TCR-002, 012201-swPFOS-2.1.4, lOOX Dil. S--F--M-----0-1-----2--5------0-1---M--E---E--(-M---L--A--)-----.-------.--.-------.--------------------------------------------------- Injection Date : 1/27/01 8:15':52 I'M Seq. Line : 164 Sample Name : SWPFOS-2.1.4: Vial : 66 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl Acq. Method : C:\HPCHEM\l\,METHODS\HOlOl2.5M Last changed : 1/25/01 9:13:04 IN by M L A Analysis Method : C:\HPCHEM\l\,METHC)DS\HOlOl26C.M Last changed : 1/30/01 2:53:16 I'M by KLT/MLA (modified after 1-oading) PFOS Analysis Column: C18 Betasil Ejum 50x2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on "Dioana" KLT - MSDI 299, ElC=298.7:299.7 (H0101:26VllLL0164.D) API-ES, Neg, SIM, Frag: Var 300000 I 250000 I 200000 I 150000 I - 2 4 6 MSDl 427, ElC=426.7:427.7 (H010126VllLL0164.D) API-ES. Neg, SIM, Frag: Var 200000 7 150000 1 100000 7 50000 : 0 -j\ 2 MSDl 499,EIC=498.7:499.7(H010126VIILLol64.D) 4 6 MI-ES. Neg. SIM, Frag: Var 8 min 8 min 400000 : 300000 { 200000 1 100000 L 0: I _ , \ , , , , , , , Instrument 1 1/30/01 2:53:16 PM KLT/MLA FACT-TCR002 (LIMS #E00-1716), Page 87 of 1138 Page 1 of 2 Batch Run # 28 of 59 Data File C:\HPCHEM\1\DATA\HOlOl2~6\HILL0164.D BACK TO MAIN Sample Name : swPFOS-2.1.r Sorted By Signa.1 Calib. Data Modified : Tuesdlay, January 30, 2001 2:27:34 PM Multiplier 1.0000 Dilution 1.0000 Sample ISTD Information: ISTD ISTD Amount Name - - -#- I - _ _[- n- -g-/-m- _~l_ _ - I . . . . . . . . . . . . . . . . . . . . . . . . . 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 RetTime Type Area wit/ A r ea - -[-m_in- l- _ I - - _ _ _ _ ---------- I - -r- a- -t-i-o- - - 4.112 VBA+ I 2.03714e6 1.00000 Totals without ISTD(s) : Signal 2: MSDl 427, EIC=426.7:427.7 RetTime Type [minl Area Amt/Area ratio G r p Name Signal 3 : MSDl 499, EIC=498.7:499.7 1 Warnings or Errors : Warning : Calibration warnings (see calibration table listing) 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\1\DATA\HOlOl2~\HILI~O~69.D BACK TO MAIN Sample Name : swPFOS-2.2.2 TCR-002, 012201-SWPFOS-2.2.2,lOOX Dil. SFM 01-25-01MEE(MLA) ............................................................................... Injection Date : 1/27/01 9:13:46 I'M Seq. Line : 169 Sample Name : SWPFOS-2.2.I; Vial : 68 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl Acq. Method : C:\HPCHEM\l\,METHODS\HOlOl25.M Last changed ': 1/25/01 9:13:04 AM by M L A Analysis Method : C:\HPCHEM\l\,METHC)DS\HOl0126C.M Last changed : 1/30/01 2:53:42 I'M by KLT/MLA (modified after 1.oading) PFOS Analysis Column: C18 Betasil Eium 50x2 mm Eluents: Methanol and 2 mm Ammonium Acetate Reprocessed on llDioanall 300000 ~ 250000 4 200000 4 150000 100000 4 50000 L 1 , Q@ ,p' I. 200000 1 150000 1 100000 1 50000 - 2 4 6 MSDl 499,ElC=498.7:499.7( H 0 1 0 1 ~ ) 1 6 9 . D ) API-ES, Neg. SIM, Frag: Var - 500000 1 400000 7 300000 1 200000 : 100000 I - -0 \ \ QQ05 1% $3' I i, ,) \, , 8 mid i'! j I &- !initial &A?&- L k? ( > 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 # 3 3 of 59 Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ ~ I ~ \ H I L : L O ~ ~ ~ . D BACK TO MAIN Sample Name : swPFOS-2.2.2 Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name - - - - #I - - - - - - - - - - -[- -ng/fil 1 254.00000 PFBS 2 254.40000 THPFOS Signal Tuesday, January 30, 2001 2:27:34 PM '1. 0000 :1. 00013 Signal 1: MSDl 299 EIC=298.7:299.'7 Totals without ISTD(s) : 0.00000 1 Warnings or Errors : Warning : Calibration warnings (see calibration table listing) . Instrument 1 1/30/01 2:53:43 PM KLT/MUI FACT-TCR002 (LIMS #E00-1716), Page 90 of 138 Page 2 of 2 Batch Run # 25 of 59 Data File C:\HPCHEM\1\DATA\HO10129\HILlLO104.D BACK TO MAIN Sample Name: swPFOS-3.1.1 300000 L 250000 < 200000 150000 I 100000 < 50000 200000 : 150000 : 100000 1 50000 1 0 h 600000 < 500000 400000 I 300000 < 200000 100000 \ &@ ,.?h!' 8 4% I I ee' J\ Instrument 1 1/31/01 11:20:18 AM I(LT/MLA FACT-TCROO2 (LIMS #E00-1716), Page 91 of 138 Page 1 of 2 Batch Run # 25 of 59 Data File C:\HPCHEM\1\DATA\HOlOl29\HILLOlO4.D Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name - -#- - I - - -[-n-g-/-m-t-l- - - - 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1/31/01 11:08:42 AM 1.0000 1.0000 Signal 1: MSDl 299 EIC=298.7:299.7 BACK TO MAIN Sample Name: swPFOS-3.1.1 Totals without ISTD(s) : Signal 2: MSDl 427, EIC=426.7:427.7 RetTime Type Area ---[--m--iI-n--l---I----------l---------- 4.909 PBA+ I 9.89058e5 Amt/Area ratio 1.00000 Totals without ISTD(s) : Signal 3: MSDl 499, EIC=498.'7:499.7 RetTime Type Area Amt/Area ----[--m-Ii--n--l--I----------l----------l----------l--l-----------------r- atio 5.144 W A + 3.60619e6 1.59134e-1 Amount G r p Name [ng/mLl 147.60707 PFOS Totals without ISTD(s) : ' 147.60707 Instrument 1 1/31/01 11:20:18 AM KLT/MLA FACT-TCROO2 (LIMS #E00-1716), Page 92 of 138 Page 2 of 2 Batch Run # 28 of 59 .Data File C:\HPCHEM\1\DATA\HOlOl29\HILI~OlO7.D BACK TO MAIN Sample Name : swPFOS- 3 .1. 4 J 300000 q&5 ,.?6"* 250000 L 200000 L 150000 I I 100000 I I I - 1, 50000 I I 0; - - I , I I I I I 200000 1 150000 : 100000 : 50000 7 + 600000 500000 I 400000 G 300000 I 100000 < 0; Instrument 1 1/31/01 11:20:33 AM KLT/MLA FACT-TCR002 (LIMS#E00-1716), Page 93 of 138 Page 1 of 2 Batch Run # 28 of 59 Data File C : \ H P C H E M \ ~ \ D A T A \ H ~ ~ ~ ~ ~ ~ ~ \ H I ~ J L ~ ~ ~ ~ . D BACK TO MAIN Sample Name: swPFOS-3.1. Sorted By Signal Calib. Data Modified : . 1/31/01 11:08:42 AM Multiplier 1.0000 Dilution 1.0000 Sample ISTD Information: ISTD ISTD Amount Name - - - -#I - - - - - - - - - - -[- - ng/m~l I - - - - - - - - - _ - - - - , - - - - - - - ---- 1 254.00000 PFBS 2 254.40000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 4.109 VBA+ 11.82894e6 Totals without ISTD(s) : 1.00~300 0.00000 Signal 2: MSDl 427, EIC=426.7:427.7 RetTime Type Area knt /Area - -[-m-in-l- - I - - - - - - I - - - - - - - - - - I - - . :ratio -----._-- 4.911 PBA+ I 9.98892e5 1.00000 Totals without ISTD(s) : Amount G r p [ng/m~l 0.00000 Name Signal 3: MSDl 499, EIC=498.'7:499.7 RetTime Type Iminl Area knt /Area :ratio ' Instrument 1 1/31/01 11:20:33 AM KLT/IYLA FACT-TCROOP (LIMS #E00-1716), Page 94 of 138 Page 2 of 2 Batch Run # 32 of 59 Data File C:\HPCHEM\1\DATA\HOlOl29\HILI~Olll.D BACK TO MAIN Sample Name: swPFOS.3.2.1 TCR-002, 012201-~wPFOS-3.2.1,lOOX Dil. S----F--_M----0---1_---_--2--6-------0---1---_M--E_-E--_-(-_M-.L-_-A-_-)-._=_----------------------------.------.---.--.---.-.--.-.--.......................... Injection Date : 1/30/01 10:07:52 AM Seq. Line : 111 Sample Name : SWPFOS.3.2.3. Vial : 65 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p1 Acq. Method : C:\HPCHEM\l\,METHODS\HOl0129.M Last changed .: 1/29/01 1:3Ei:12 I'M by MLA Analysis Method : C:\HPCHEM\l\,METHODS\HOl0129B.M Last changed : 1/31/01 11:08:44 AM by KLT/MLA (modified after I~oading) PFOS Analysis Column: C18 Betasil Ejum 50x2 mm Eluents: Methanol and 2 mm Amnioniunn,Acetate Reprocessed on llDioanall KLT MSDl 299, ElC=298.7:299.7 (HOlOl:29VllLL(llll.D) API-ES, Neg. SIM,Frag: Var 250000 1 200000 < r 150000 100000 1 50000 L - 0 < d 200000 1 150000 1 100000 : 50000 : 0 7- 600000 < 500000 400000 I 300000 1 200000 I I - k@ \$/ , I I I 4% Q Q`?t Instrument 1 1/31/01 11:20:54 AM I(LT/MI;A FACT-TCROO2 (LIMS #E00-1716), Page 95 of 138 Page 1 of 2 Batch Run # 32 of 59 Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ ~ ! ~ \ H I L I L L O ~ ~ ~ . D Sorted By Calib. Data Modified : Multiplier Dilution Sample ISTD Information: ISTD ISTD Amount Name ----I#-------------I[--n---g---/--,-m---1~----------- 1 254.00000 PFBS 2 254.40000 THPFOS !3 igna:l :L/31/13111:08:42 AM :1. 0008 :1. 0000 Signal 1: MSDl 299, EIC=298.7:299.'7 Totals without ISTD(s) : Signal 2: MSDl 427, EIC=426.7:427:7, 0.00000 Totals without ISTD(s) : 0.00000 BACK TO MAIN Sample Name : swPFOS .3.2.1 Totals without ISTD(s1 : 136.72210 Instrument 1 1/31/01 11:20:54 AM KLT/MLA FACT-TCROOP (LIMS #E00-1716), Page 96 of 138 Page 2 of 2 ~~~~~~~~~ Batch Run # 37 of 59 Data File C:\HPCHEM\1\DATA\HO10129\HIL:L0116.D TCR-002, 012201-swPFOS-3.3.1, lOOX Dil. SFM 01-26-01 MEE (MLA) BACK TO MAIN Sample Name: SWPFOS-3.3.1 Injection Date : 1/30/01 11:03:41 AM Seq. Line : 116 Sample Name : SWPFOS-3.3.1 Vial : 69 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p1 Acq. Method : C:\HP~M\l\METHODS\HOl0129.M Last changed .: 1/29/01 1:35:12 PM by MLA Analysis Method : C:\HPCHEM\l\METHODS\HOl0129B.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" 250000 200000 < I50000 I 100000 1 50000 I 0 1-A ' 4Q5 $8 i , I I 225000 200000 175000 150000 125000 100000 75000 50000 2 4 6 MSDl 499,ElC=498.7:499.7( H O l O . ~ O 1I6.D) API-ES. Neg. SIM, Frag: Var 500000 400000 { 300000 200000 100000 Q I:$' 'r 8 rnir Instrument 1 1/31/01 11:21:20 AM KLT/M:LA FACT-TCROO2 (LIMS #EOO-I716), Page 97 of 138 Page 1 of 2 Batch Run # 37 of 59 Data File C:\HPCHEM\1\DATA\HO10129\HILIJOl16.D Sorted By Calib. Data Multiplier Dilution Sample ISTD Modified : Information: Name Signal. 3./31/01 11:08:42 AM 3.. 0000 3.. 0000 BACK TO MAIN Sample Name : swPFOS-3.3.1 Totals without ISTD(s) : 0.00000 Signal 2: MSDl 427, EIC=426.7:427.'7 Totals without ISTD(s) : 118.61261 Instrument 1 1/31/01 11:21:20 AM KLT/MLA FACT-TCROOP (LIMS #E00-1716). Page 98 of 138 Page 2 of 2 BACK TO MAIN Sample Name: MeOH Blank _ _ MSDI 299, ElC=298.7:299.7 (H010205VllLL0022.D) API-ES.Neg, SIM, Frag: Var I I 2500 2000 I 1500 1060 500 I r- I I I 1 - 2 4 6 MSDI 427, ElC=426.7:427.7 ( H 0 1 0 2 ~ 0 0 2 2 . 0 )API-ES, Neg, SIM, Frag: Var 14000 12000 1 I -; 10000 ! 8000 6000 4000 2000 I - 0 - - - ---- I , I I I .____cI__.I I I - -~ 2 4 6 MSDI 499, ElC=498.7:499.7 (HO10205VllLL11022.D) API-ES,Neg, SIM, Frag: Var I i 2000 -; 1750 1500 i 1250 1000 750 I . - I 500 , 250 \,- --.. ,~ L 2 4 6 I 8 mil / 1 8 mil 8 min 1nstr::inent 1 7/9/01 3:37:04 PM MLA FACT-TCROO2 (LIMS #E00-1716), Page 99 of '138 Page 1 of 2 BACK TO MAIN 250.70000 THPFOS Sygnal 1: MSDl 299, EIC=298.7:299.7 Signal 2: MSDl 427, EIC=426.7:427.7 Signal 3: MSDl 499, EIC=498.7:499.7 RetTime Sig Type Area Amt/.&ea Amount ~ r p Name -...i-m---iI-n-I]------I----------I----------I----------I--I--------------- ratio [PPbl 4.121 1 W A + 4.821 2 1.299- 20e4 0.- 00000 #####-##### PFBS THPFOS 5 . 1 5 8 3 WA+ 1.31270e4 0.00000 0.00000 PFOS T c . c a l s without ISTD(s) : 2.53242e-12 2 Warnings or Errors : Warning : ISTD compound(s1 not found Warning : Negative results set to zero (cal. curve intercept), (PFOS) Instrvient 1 2/9/01 3:37:04 PM MLA FACT-TCROOP (LIMS #E00-1716), Page 100 of 138 Page 2 of 2 BACK TO MAIN I I 14000 12000 -i 10000 4 8000 1 -0 60001 2 4000' 11 2000L 1 ' 0{-> __-- ------ -Iy-I - __I_ _L - _ _ --I_ I I i 1 I I j 1 ._ I 2 _. 6 I I 8 mir InstrL .:ent1 2 / 9 / 0 1 3:39:25 PM MIA FACT-TCROO2 (LIMS #E00-1716), Page 101 of 138 Page 1 of 2 BACK TO MAIN 250.70000 THPFOS Siynal 1: MSDl 299, EIC=298.7:299.'7 Signal 2: MSDl 427, EIC=426.7:427.'7 Signal 3 : MSDl 499, EIC=498.7:499.7 RetTime Sig Type Area Amt/ikea Amount G r p Name ---[--i--iIi--n~]------I----------~----------~----------~--~-------------r--at.io [PPbl 'I .118 1 VVA+ .821 2 1.161 3 PBA+ 1.3099Ge4 2060.08472 0.- 60000 ########## - 0.00000 0.00000 PFBS THPFOS PFOS Tc ' als without ISTD(s) : 2.53242e-12 2 :!arnings or Errors : wL-~'- ~.nin:gISTD compound(s) not found Warning : Negative results set to !zero (cal. curve intercept), (PFOS) I n s t r i !<nt 12/9/01 3:39:25 PM MLA FACT-TCR002 (LIMS #E00-1716),Page 102 of '138 Page 2 of 2 BACK TO MAIN MSDl 299, ElC=298.7:299.7 (H0102!06\H0022.D) 42500 API-ES, Neg, SIM, Frag: Var 12000 4 10000 4 8000 4 6000 { 4000 I I 2000 I 0: _-____--- --- p P I J I I I Batch Run # 22 of 79 Data File C:\HPCHEM\1\DATA\HO10206\HILIJO022.D Sample TN-A-4755, 05 Feb 01, exp:2005. ___________--_-_--_-_--_-_--_________-_--_-_----------.--------.-.-----~--------------------------------------------------------- Injection Date : 2/6/01 3:46:36 PEI Seq. Line : 22 Sample Name : MeOH Blank Vial : 96 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl Acq. Method : C:\HPCHEM\l\,METHODS\HOlO206.M Last changed : 2/6/01 11:4:1:54 AM by MLA Analysis Method ,: C :\HPCHEM\l\,METHODS\H010206A.M Last changed : 2/7/01 1:14::17PM by MLA (modified aliter :loading) Sim run C2,c3,c4,c5, c7 and Ctl perfluoronated carboxylic acids ...................................................................... BACK TO MAIN Name: MeOH Blank 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 Signal 2: MSDl 427, EIC=426.7:427.*? Signal 3: MSDl 499, EIC=498.7:499:? RetTime Sig Type Area Amt/Area Amount G r p Name ---[--m--i1-n-1l------1----------~.-----.-----~----------~--~-------------.--ratio . [ppbl 4.105 1 W A + 4.819 2 1.247- 66e4 0.-00000 #####-##### PFBS THPFOS 5.155 3 W A + 6796.12695 0.t30000 1.42633e-1 PFOS Totals without ISTD(s) : 1.42633e-1 1 Warnings or Errors : . Warning : ISTD compound(s) not found Instrument 1 2/7/01 1:14:17 PM MLA FACT-TCROOS (LIMS#E00-1716),Page 104 of 138 Page 2 of 2 Batch ?un # 40 of 79 Data :ile C:\HPCHEM\1\DATA\HOlO205\HILI~O04O.D BACK TO MAIN Sample Name: naclPFOS-2.4.1 T' i-002, 012901-naclPFOS-2.4.I, 1OClX Dil. Mt :hod Blank, SFM 02-01-01 MEE:(MLA) =_============================:=====:================================== Ir jection Date : 2/5/01 9:27:53 PFI Seq. Line : 40 S c rlple Name : naclPFOS-2.4 .l Vial : 21 1"- 4 . Jperator : MLA Inj : 1 F. 1. ,nstrument : Hiilary Inj Volume : 10 pl A. x. Iilethod : C : \HPCHEM\1\,METHODS\HO10205.M L, ;t rhanged : 2/5/01 2:09:33 PPI by MLA C. i l y ;is Method : C:\,HPCHEM\l\,METHC)DS\HO10205A.M Lc ;t zhansed : 2/9/01 3:38:35 PEI by MLA ~blsD1 299, EIC=29g-i 299.7 ( H 0 1 0 2 i ~ l 0 4 0 . D ) API-ES. Neg, SIM, Frag: Var , , rn :ooooo 5OOLJ oooco v- Tt I 50060 000b0 0) 1 500G0 2 l , () - - - _ - _______ v- 8 I I - 2 4 6 MSDi 427, EIC=426 7 427.7 ( H 0 1 0 2 ~ 1 0 4 0 . D ) API-ES, Neg, SIM, Frag:Var rn i a '50000 'OOO('0 ' z 8 500LO 0) r I 8 min d oooco ' I 500!!0 (D 12 0 L ,.! I r\ __ I I- I I I - 2 4 6 MSDI 499, EIC=b98 7 499.7 ( H 0 1 0 1 ~ i D 0 4 0 . D ) API-ES, Neg. SIM, Frag: Var (X v) 1 ; 1200 + I 10( r l I I --Ad+v 846C0O0 I, ,I - -4' '+--v.?.,, -' 200 I I- I I I I 8 mir I 2 4 6 6 mir -_. . __ . SI.. j.-te-iBy c, Lib. Data Modified : Retention Time Friday, February 09, 2001 3: M Ltiplier 1.0000 D ..ut- on s. npl- ISTD Information: 1.0000 +I. XI ISTD Amount Name - - I _ _[_P_P_bl_ _ _ - _ _ _ ~ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ Instr .ien: 1 2/9/01 3:33:36 PM MLA FACT-TCROOZ (LIMS #E00-1716), Page 105 of 138 Page 1 of 2 Batch tun 2 40 of 79 Data :le C :\HPCHEM\1\DA~A\HOlO205\HILI~004.0D Sample! T 1 - 0 0 2 , 012901-naclPFOS-2.4.I, lOOX Dil. M: :hod Blank, SFM 02-01-01MEIC(MLA) = .............................................................. I.. jec-i.onDate : 2/5/01 9:27::53PM Seq. Line : 40 S . nple Name : naclPFOS-2.4.1 Vial : 21 A. 1. Cperator : MLA Inj : 1 A .f. Lnstrument : Hillary Inj Volume : 10 p 1 f . 4 . ?iethod : C :\HPCHEM\l'~METHODS\HO10205.M L ;t changed ,: 2/5/01 2:09:33 PM by MLA Ai. lysis Method : C:\HPCHEM\l'\METHODS\HOl0205A.M L. .;t changed : 2/9/01 3:38:35 PI4 by MLA (modified after :Loading) s 7 r.,nC2,c3,c4,cS,c7 and C13 perfluoronated carboxylic acids =. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . BACK TO MAIN Name: naclPFOS-2.4.1 I. 250.70000 THPFOS S . p a l 1: MSDl 299, EIC=298.7:299.'7 S gnal 2: M S D l 427, EIC=426.7:427.'7 S'.jnal 3 : M S D l 499, EIC=498.7:499.'7 R i-Til:s Sig Type Area Amt/Area Amount G r p Name - _iii-n!- -1--1------1----------~----------~----------~--~-------r---a--t---io [PPbl 1.19 1 W A + 1.94355e6 15.817150e-1271.89463 PFBS 4.8 9 2 PVA+ I 1.04252e6 1.00000 250.70000 THPFOS i . 1 J 5 3 W A + 8906.63379 0.00000 0.00000 PFOS T, zals without ISTD(s) : 271. a9463 1 Jari1.ings or Errors : W -nii,g : Negative r e s u l t s set to zero (cal. curve intercept), (PFOS) Instr nen-. 1 2/9/01 3:38:36 PM MIA FACT-TCR002 (LIMS #E00-1716), Page 106 of 138 Page 2 of 2 BACK TO MAIN I I . MSDl 299, ElC=298.7:299.7 (H010:!05WlLL0042.D) :ooooo-i 1500C0 API-ES, Neg, SIM, Frag: Var ooouo 500' 0 : ooc i, 1 500r0 ' (D ! " I . 0 . . I_ I I -- I 2 4 6 h;lSDI 427, E I C = 4 2 G ~ 7 : ~ 2 7 ~ ~ - 0 0 4 2AP. ID-ES), Neg, SIM, Fmg: Var 8 mir I__ 2 4 6 MSDl 499, EIC=498.7:499.7( H O l C ~ l L 0 0 4 2 . D ) WI-ES, Neg, SIM, Frag: Var 8 mi BACK TO MAIN I. 2 5 0 . 7 0 0 0 0 THPFOS S gnal 1: MSDl 299, EIC=298.7:299.7 S p a l 2: MSDl 427, EIC=426.7:427.'7 S 3nal. 3: MSDl 499, EIC=498.7:499.7 T :ais without ISTD(s) : 272.07681 1 ,larnings or Errors : h I-ning : Negative r e s u l t s set to zero (cal. curve intercept), (PFOS) Instr ,ieR: 1 2/9/01 3:38:46 PM MLA FACT-TCROOZ (LIMS #E00-1716), Page 108 of 138 Page 2 of 2 BACK TO MAIN 250000 e 200000 z 150000 : 100000 2 5 0 0 0 0 ~ !? 250000 1 200000 : 150000 1 100000 1 : 50000< 8 0 ,2 1400 1 1200: I - r 9 li I I H R -----... I Instrument 1 2/7/01 1:15:46 PM M:LA FACT-TCROO2 (LIMS #E00-1716), Page 109 of 138 Page 1 of 2 Batch Run # 41 of 79 Data File C:\HPCHEM\1\DATA\HO102C16\HI18LO041.D Samp:Le TCR-002, 012901-naclPFOS-3.4.2, 100X Dil. Method Blank,.SFM 02-02-01 ME:E(MLA) ....................................................................... 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 : 10 pl Acq. Method : C:\HPCHEM\I.\MET[ODS\HO10206.M Last changed . : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\1.\METCODS\HO10206A.M Last changed : 2/7/01 1:15:46 I'M by MLA (modified after loading) _Si_m__r_un__C_2_,c_3__,__c_4_,__c__5__,__c-__7----a--n---d-----C--!-8----.p.-e---r---f--l-.u.---o-r-o--n-a-t-e--d--c--a-r-b-o--x-y-l-i--c--a--c-i-d-s------ BACK TO MAIN Name: naclPFOS-3.4. 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 Signal 2 : MSDl 427, EIC=426.ir:427 .,7, Signal 3: MSDl 499, EIC=498.7:499.,7 Ret Time [minl ------- 4.106 4.820 5.156 Sig Type Area Amt/Area mount _ _ I _ _ _ _ _ _ I - - - - - - - - _ -I -_r_at_io..-_I -----[--P-P-bl- - - 1 WA+ 2.00919e6 6.10461e-1 290.41323 2 PVA+ 11.05881e6 1.,00000 250.70000 3 PPA+ 3730.26538 3.15106e-1 2.78313e-1 G r p Name PFBS THPFOS PFOS Totals without ISTD(s1 : 290.69154 Instrument 1 2/7/01 1:15:46 PM MLA FACT-TCROOS (LIMS #E00-1716), Page 110 of 138 Page 2 of 2 BACK TO MAIN Batch Run # 43 of 79 Data File C:\HPCHEM\1\DATA\HOlO206\HILL0043.D Sample Name: naclPFOS-3.4.. TCR-002, 012901-naclPFOS-3.4.4,lOOX Dil. Method Blank, SFM 02-02-01 MEE(MLA) ..................................................................... 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 p1 Acq. Method : C:\HPCHEM\l\METHODS\HO10206.M Last changed . : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\l\METH:ODS\HO10206A.M Last changed : 2/7/01 1:15:55 F'M.by MLA (modified a.fter loading) Sim run C2,c3,c4,cSIc7 and C!8 perfluoronated carboxylic-acids ................................................................... Instrument 1 2/7/01 1:15:56 PM MLA FACT-TCROO2 (LIMS#E00-1716), Page 111 of 138 Page 1 of 2 BACK TO MAIN 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.'7:299.7 Signal 2: MSDl 427, EIC=426.'7:427.7 Signal 3: MSDl 499, EIC=498.'7:499.7 RetTime Sig Type Area Amt/Area Amount G r p Name --[-m-i-n-]- 1--1------1----------1---------- ra,tio I- - -[-P-Pb-l- - - - 1 - - 1 _ - - - _ - - - _ _ _ - _ _ - 4.105 1 W A + 1.97953e6 6.10.461e-1 288.63083 PFBS 4.819 2 PBA+ I 1.04962e6 1.00000 250.70000 THPFOS 5.156 3 PBA+ 3744.80615 3.13083e-1 2.80034e-1 PFOS Totals without ISTD(s1 : 288.91086 Instrument 1 2/7/01 1:15:56 PM M:LA FACT-TCROOP (LIMS #E00-1716)P,age 112of 138 Page 2 of 2 BACK TO MAIN Batch :..UTL # 45 of 79 Data ' :le C:\HPCHEM\1\D~~TA\HOlO205\HILL0045.D Sample Name: naclPFOS-2.1.: 7 ? . - 5 ! 3 2 , 012901-naciPFOS-2.1.1,lOOX Dil. _~S ..I 6 7 - 0 1 - 0 1 MEE(MLA) - _.________ __ _________ __ _________ __ ___--_--_-_--_--_--_--_----------------------------------------------------------------------------- I: jerzion Date : 2/5/01 10:23:33 PM Seq. Line : 45 r' ,i; -. iJarne : ni.::lPFOS-2.1.1 Vial : 31 I: .i. iperator : MLr. Inj : 1 A .{. Instrument : Hillary Inj Volume : 10 pl A .;. Method 1 :t changed : C:'\HPCHEM\l\METH:ODS\HO10205.M . : 2/5/01 2:09:33 PM. by MLA f.. il;/sis Method : C:\HPCHEM\l\METH:ODS\HO10205A.M L, st changed : 2/9/01 3:39:00 FM by MLA (modified after loading) S . : n run C2,c3,c4,c5,c7 and C8 perfluoronated carboxylic acids = 1============================rl=====Ip=========================== v- ' '50000 T. I 50C30 2 I j ,500~0 ? s Ioos(J0 ' i 50000 I 1 - J 0 \ I Batch ..'id!-: fi 4 5 of 79 BACK TO MAIN Data ..:le C:\HPCHEM\1\DATA\HOlO205\HILL0045.D Samp1.e Name: naclPFOS-2.1. T''.-G02, 012901-naclPFOS-2.1.1,lOOX Dil. S , 'j 63-01-01 MEE(MLP.1 _- _._._.-______________ ____________-__-_--_---_--_---_--_---_---_--_---_--_---_--_---_--_---_--_---_- _________------------------------ 1:jeccion Date : 2/5/01 10:23:33 PM Seq. Line : 45 S: i p l e Name : naclPFOS-2.1.1 Vial : 31 P.c ' 4 . Operator : MLA Inj : 1 P. I[. Instrument : Hillary Inj Volume : 10 p1 P.'.-1. Method : C:',HPCHEM\l\METHODS\HO10205.M L:.stchanged . : 2/5/01 2:09:33 PM by MLA A: 31ysi.s Method : C:\HPCHEM\l\METHODS\HO10205A.M L; s t changed : 2/9/01 3:39:00 PM by MLA (modified after loading) s ,I L - G n c2,c3,c4,c5,c7 and C8 perfluoronated carboxylic acids =~1================================================================== 2 5 G . 7 0 0 0 0 TilPFOS S .rial 1 : MSDl 299, EIC=298.7:299.7 S jnal 2: MSDl 427, EIC=426.7:427.7 S gnal 3: MSDl 499, EIC=498.7:499.7 RcLTime Sig Type Area - *_i_iin.]-'--I------I----------l----------l---------- ~ . ~ , 18 W A + 1.95449e6 I. 2 PBA+ I 1.01804e6 ; . I 5 5 3 VVA+ 5.36024e6 Amt/Area rat io 5.81750e-1 1.00000 1.62253e-1 Amount G r p Name [PPbl I--+------------ 280.00194 PFBS 250.70000 THPFOS 214.17458 PFOS TC::ais without ISTD(s) : 494.17652 Insti- ,,e!.:1 2/9/01 3:33:01 PM WLA FACT-TCROOZ (LIMS #E00-1716), Page 114 of 138 Page 2 of 2 BACK TO MAIN Batch :,.un +I46 of 79 Data : :.ICF :\HPCHEM\1\DATA\HOlO205\HILI~OO46.D Sample! Name: naclPFOS-2.1.2 T ?.-CO2, 012901-naclPFOS-2.1.2, l0OX Dil. S: 11. 92-01-01 MEE (MLA) - _.. ____________________________________--_--_-_--_----------.--.----------------------------------------------------------------- Ii Iection Date : 2/5/01 10:34:39 PM Seq. Line : 4 6 C ;:p e Name : naclPFOS-2.3..2 Vial : 32 E. I . 'lperator : MLA Inj : 1 A < 4. instrument : Hillary Inj Volume : 10 p1 A : . !/lethod : C :\HPCHEM\l\,METHODS\HO10205.M L "i -hanged .: 2/5/01 2:09::33PEI by MLA f.. il,ais Method : C:\HPCHEM\l\,METHC)DS\HO10205A.M L..;t changed : 2/9/01 3:39::05PM.by MLA (modified after Iloading) s - '1_1 _ru_n _C_~_,_C _~ _, _C ~_,_cC7_$_an,_d_Ct_j _pe_rf_l-u-o-r-o-n-a-t-ed--c-a-r-b-o-x-y-l-i-c--ac-i-d-s------------------------- __ i MSDI 299,ElC=298.7:299.(7HolO205\HILLOO46.D)API-ES,Neg, SIM,Frag:Var I I ~00000 II ' 50000 ~000i)O, 5ocoo 9' ym 0 1 0 __ - I ~ J J 1 , I - _ _2 _ _ _ _ _ ~ 4 6 ~ W X ~42I7,2c7.427.7(H010205\HILL0046.D) API-ES,Neg, SIM, Frag:Var , I 8, , , , min " I 'Y- ' I I 1 - -2 MSDI 499.Ci498.7:z99.7 ~100000 4 6 (H010i105Vl1LL~D046.D)API-ES,Neg, SIM.Frag:Var :oouoo ~100000 j I \ I , :ooooo ' I 8 rnin 1nstrr:e:it 1 2/9/01 3:39:06 PM MLA FACT-TCROOZ (LIMS#E00-1716),Page 115of 138 Page 1 of 2 BACK TO MAIN 250.70000 THPFOS Si j n a l 1: MSDl 299, EIC=298.'7:299.7 S j gnal 2: MSDl 427, EIC=426.'7:427.7 Si - p a 1 3 : M S D l 499, EIC=498.'7:499.7 S i g Type Area Amt/Area Amount Grp Name _ - / - _ _ _ _ _ I _ - _ _ _ _ _I__ -_r_a_t-i-'o_ _ _I - __[-P-P_bl_ - _ -- -I _ _ - - _ - _ _ _ - _ _ _ _ - 1 INA+ 1.99539e6 5.81'750e-1 283.28167 PFBS 2 PVA+ I 1.02730e6 1.00000 250.70000 THPFOS 3 W A + 5.51518e6 1.62412e-1 218.59113 PFOS Tc z a l s without ISTD(s) : 501.87280 I n s t x i e , ~ t1 2/9/01 3 : 3 9 : 0 6 PM M:LA FACT-TCROOZ (LIMS #E00-1716), Page 116 of 138 Page 2 of 2 BACK TO MAIN r blSD1 299, EIC=298.7.299.7( H 0 1 0 2 ~ 1 0 4 8 . D ) API-ES, Neg, SIM, Frag:Var ~'-00000 :"3ouoo , i .'00G00 -1 500'30 1 -. I ,I I I I 2 4 6 MSDi -427, ElC=426.7:?27.7( H 0 1 0 2 ~ 0 0 4 8 . D ) API-ES, Neg, SIM, Frag:Var I a mini --I I I 2 4 6 M S D l 499, ElC=49~~49~.(H0104'05VllLL0048.D)API-ES, Neg, SIM, Frag:Var -1 E "-'00000 Ik I ::ooi)oo -' I 8 min SC :ted By C; i.i!. Data Modified : M :: iplier D L: :ion S; ;ip i.e ISTD Information: 15I'D ISTD Amount Name Retention Time Friday, February 09, 2001 3 1.0000 1.0000 Instrt..ie:-.1t 2/9/01 3:39:16 PM MLA FACT-TCROOZ (LIMS #E00-1716), Page 117 of 138 Page 1 of 2 BACK TO MAIN Batch . L... # 4ii of 79 Data i ..L': C:\E?PCHEM\1\DATA'\HOlO205\HILL0048.D Samp:Le Name: naclPFOS-2.1.4 T: - 02, 0:2901-naclPPOS-2.1.4, lOOX Dil. SI _- _- ____________________--_------------------------------------------- I i2-01-91MEE(MLA) .____________________---------------------------------------------- Irjeition Date : 2/5/01 10:56:54 PM Seq. Line : 48 Sa.::pleName : naclPFOS-2.1.4 Vial : 34 Ac.;. Operator : MLA Inj : 1 Acq. Instrument : Hillary I n j Volume : 10 p l Ac'i. Method : C:\HPCHEM\l\METHODS\HO10205.M L s . : t changed .: 2/5/01 2:09:33 PM by MLA Ar.'il;/iss Ele thod : C :\HPCHEM\l\METHODS\HOlO205A.M L;:.;t changed : 2/9/01 3:39:15 PM by MLA (iriodified after loading) S__ ?_._'1 __I:u_n___C_2_,__c_3_,__c_4_,__c_5_,_c_7___a_n_d__C_8___p_e_r_f-_l-u-o-r-o-n-a-t-e-d--ca-r-b-o-x-y-l-i-c--a-c-i-d-s----------------------- 250.70000 THPFOS S i . j n a l 1: MSDl 299, EIC=298.7:299.7 S i \ j n a l 2: MSDl 427, EIC=426.7:427.7 S i g n i l 3: MSDl 499, EIC=498.7:499.7 R e - T i m e Sig Type Area Amt/Area Amount G r p Name - [I1i!-I]_.-I _ _ - _ - - I _ --------i----------I------r---a-lt---i--o-------------- [PPbl 1 9 - VBA+ 1.91682e6 5.81750e-1 275.75855 PFBS b 2 0 2 PVA+ I 1.01378e6 1 . 0 0 0 0 0 250.70000 THPFOS 8 / 5 6 3 PBA+ 6.15837e6 1.63487e-1 248.97829 PFOS Tc_a:s w i t h o u t ISTD(s) : 524.73683 Instri cnt 12/9/01 3:39:16 PM MLA FACT-TCROOS (LIMS #E00-1716),Page 118 of 138 Page 2 of 2 Batch Run # 53 of 79 BACK TO MAIN Data File C : \HPCHEM\1\DAT>.\~~HOl0205\HILI10053.D Sample Name: naclPFOS-2.2.2 TCR-002, 012901-naclPFOS-2.2.2, 1OC)X Dil. SFM 02-01-01 MEE(MLA) ....................................................................... 1:-jectionDate : 2/5/01 11:5;!:35 I'M Seq. Line : 53 Snmple Name : naclPFOS-2.2.2 Vial : 36 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl Acq. Method : C:\HPCHEM\l\,METHODS\HOlO205.M L:,st changed .: 2/5/01 2:09::33PM by M L A Arialysis Method : C :\HPCHEM\l\,METHODS\H010205AM. Last changed : 2/9/01 3:39::40PM by MLA (modified after Iloading) S_:_'._mr_un_C_2_,c_3_,c_4_,_c__5_,_c_7___an__d__C__tt __pe__r_f-l-_u-o__r_o_n_-a-t--e-_d---c--a--r--b--o--x--y-l--i--c----a--c-i--d--s--------------------------------------------------- Batch Run # 5 3 rJf 79 BACK TO MAIN Data File C:\HFCHEM\1\DATA\HO10205\HIIJLO053.D TCR-002, 012901-naclPFOS-2.2.2,l O O X Dil. SampILe Name: naclPFOS-2.2. S_?M__02_-_01_-_E1_M_EE_(_ML_A_),____--_-------_------------------------------------------------ 1r:jection Gate : 2/5/01 11:52:35 PM Seq. Line : 53 Sample Name : naclPFOS-2,, 2.2 Vial : 36 Acq. Operator : MLA Inj : 1 A c q . Instrwnent : Hillary Inj Volume : 10 p 1 A c q . Methoc : C : \HPCHEM\:L\METIIODS\H010205 .M Last changed . : 2/5/01 2:0!3:33 I?M by MLA Analysis Mr'lhod : C:\HPCHEM\:L\METIODS\H010205A.M L , ,s t change 2 : 2 / 9 / : j 1 3:3!3:40 I?M by MLA (mo& f i e d after loading) s 1.m run c2,c3,c4,c5, c7 and (28 perfluoronated carboxylic acids .................................................................... 1 250.70000 THPFOS Signal 1: M S D l 299, EIC=298.'7:299.7 Signal 2: M S D l 427, EIC=426.'7:427.7 Signal 3: N S D 1 499, EIC=498.'7:499.7 RetTime S i g Type Area - [_m-i- -n_l) - _ ------I----------I---------- 4.119 1 N A + 1.89751e6 4.819 2 PVA+ I 1.02378e6 5.155 3 GVA+ 5.22307e6 AmtIArea Amount G r p Name ratio I_ -[-P_Pb_l- - - -I- - ] - - - - - - - - - - - - - - - 5.81'750e-1 270.31266 PFBS 1.00000 250.70000 THPFOS 1.61999e-1 207.19812 PFOS Tctals without ISTD(s) : 477.51078 Instr-ment 1 2/9/01 3:39:41 PM MLA FACT-TCROO2 (LIMS #E00-1716), Page 120 of 138 Page 2 of 2 Batch Run # 54 f2f 79 BACK TO MAIN Data ile C:\HE : H E M \ ~ \ D ~ ~ T ~ . : H O ~ O ~ C I S \.HDI L L ~ ~ ~ ~ TCR-002, 012901-naclPF3S-2.2.3,lCiOX Dil. Sample Name: naclPFOS-2.2. S__.__M___0--_2_-__0__1_--__0__1_M__E_E___(__M__L-A-_-)_____--_-._-__---_.-_---_--_---_---_--_---_--_---_--_---_--_---_--_- _______-------------------------- I.jection CJte : 2/6/01 12:C13:44 AM Seq. Line : 54 .Sa.mple Name : naclPFOS-2.2.3 Vial : 37 A - q . Operator : MLA Inj : 1 A q . Instrument : Hillary Inj Volume : 10 p 1 A -9. Methoc, : C:\HPCHEM\I.\METHODS\HO10205.M Letst changed : 2/5/01 2:09:33 P M by MLA A , , a l y s i s Method : C:\HPCHEM\l.\METHODS\H010205A.M Last changed : 2/9/01 3:39:45 P M by MLA (modified after loading) s m run c2,c3,c4,c5,c7 and C!6 perfluoronated carboxylic acids ______________________________--_-_--_-----_------._---------.--------.-------------------------------------------------------- r MSD; 299, ElC=298.7:299.7(H01O m - 0 0 5 4 . D ) 1 ' 300000 1 250000 7 200000 , 1 150000 4 100000 50000, i ; m API-ES,Neg, SIM, FBg:Var 1 Instr>:.ment 1 2,'9/01 3:39:46 PM M L A FACT-TCROOS (LIMS #E00-1716), Page 121 of 138 Page of BACK TO MAIN 1 2 5 0 . ! O O O O THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 Sjgnal 2: MSDl 427, EIC=426.7:427.7 Signal 3: MSDl 499, EIC=498.7:499.'7 RetTime Sig Type Area Amt/lkea Amount Grp Name min] - ----- -- 1 - - - _ _ - - - - -. -r- a- -t-i.o- - - - - I -[-P-P-b-l - - - - - l - - - - - - - - - - ~ - - - - - - . - - 4.117 1 .'BA+ 1.88069e6 !j. 817!jOe-1 267.76401 PFBS 4.821 2 VVA+ I 1.02437e6 1.00000 250.70000 THPFOS 5.160 3 :VA+ 5.13424e6 :L. 618tjOe-1 203.38226 PFOS Totals without ISTD ( s ) : 471.14627 1nstr.ment 1 2 1 / 0 1 3:39:46 PM MLA FACT-TCR002 (LIMS #E00-1716), Page 122 of 138 Page 2 of 2 BACK TO MAIN 300000 I 250000 L 200000 L 150000 I 100000 L : 50000: 0, ,zI n I I I - L I I 2 200000 y 150000 1 100000 y 50000: t- - - - oE X I - I v) LL F I n a * __ Instrument 1 2/7/01 1:16:10 PM MLA FACT-TCROO2 (LIMS #E00-1716), Page 123 c d 138 Page 1 of 2 Batch Run # 46 of 79 BACK TO MAIN Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ O ~ ~ \ H I L ~ J O O ~ ~ . D Sample Name: naclPFOS-3.1.2 TCR-002, 012901-naclPFOS-3.1.2, 1OOX Dil. SFM 02-02-01 MEE(MLA) _.._.._.._.._._.._.._.._._.._.._.._._.._.._.._._.._.._..-.-.-.-.-.-.-.-..-.~..~.-..-.-.-...~..-.-.-.-.-.-.-.-.-..-.-.-.-.--------------------- 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 pl Acq. Method : C:\HPCHEM\1'~METHODS\HO1020.6M Last changed : 2/6/01 11:4'7:54 AM by M L A Analysis Method : C:\HPCHEM\l'\METHODS\HO10206A.M Last changed : 2/7/01 1:16:10 PIY by MLA (modified a:Eter :Loading) Sim r u n C2,c3,c4,c5, c7 and C13 perfluoronated carboxylic acids ....................................................................... 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.'7 Signal 2: MSDl 427, EIC=426.7:427.'7 Signal 3: MSDl 499, EIC=498.7:499.'7 RetTime Sig Type Area Amt/,wea - -[-m-in-l- - - - I - - - - - - I - - - - - - - - - - l - - - - r- a- -t-i-o- 4.104 1 VBA+ 1.90390e6 15.10461e-1 4.822 2 PVA+ I 1.03354e6 1.00000 5.161 3 W A + 5.38770e6 1.63206e-1 Totals without ISTD(s) : 495.21161 Instrument 1 2/7/01 1:16:10 PM MIA FACT-TCROO2 (LIMS #E00-1716), Page 124 of 138 Page 2 of 2 ~ ~~ Batch Run # 48 of 79 BACK TO MAIN Data File C:\HPCHEM\1\DATA\HOlO206\HILL0048.D Sample Name: naclPFOS-3.1.~ TCR-002, 012901-naclPFOS-3.1.4, lOOX Dil. S_FM__0_2-_0_2-_01_M-_E-E__(_M_L_-A_)_____________-_-------------------------------------------------------------------------------------- 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 p l Acq. Method : C:\HPCHEM\l\METH:ODS\HO10206.M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\l\METH~ODS\HO10206A.M Last changed : 2/7/01 1:16:19 E'M by MLA (modified a.fter loading) Sim run C2,c3,c4,c5,c7 and C!8 perfluoronated carboxylic acids __________________-___-_--_____--_-_--_------.---------.--.---------.------------------------------------ ------------ 1 .A 300000 I 250000 L 200000 I -1 . ,g 150000I 100000 i 50000< 3 0.. -d L I , I I I I 250000 : 200000 : 150000 : 100000 : 50000: - - - - - :o : x I- -r v) 2' E I 2; d __ I 3 ~~~ ~~~ ~~ Batch Run # 48 of 79 Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ O ~ \ H I L I J O O ~ ~ . D TCR-002, 012901-naclPFOS-3.1.4, l O O X Dil. SFM 02-02-01 MEE(MLA) Sample ........................................ Injection Date : 2/6/01 8:35:51 PM . Seq. Line : 48 Sample Name : naclPFOS-3. :I. 4 Vial : 64 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 pl Acq. Method : C :\HPCHEM\1'\METHODS\H010206.M Last changed : 2/6/01 11:4'7:54 AM by MLA Analysis Method : C:\HPCHEM\l'\METHODS\HO10206A.M Last changed : 2/7/01 1:16:19 PIY by MLA (modified after loading) Sim run C2,c3,c4,c5, c7 and CB pereluoronated carboxylic acids ======I=====l======PP======pI=====Ip======================================= BACK TO MAIN Name: naclPFOS-3.1.4 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 Signal 2: MSDl 427, EIC=426.7:427.7 Signal 3: MSDl 499, EIC=498.7:499.7 RetTime Sig Type Area Amt/Area Amount G r p Name - -[r-n-in-l_ _I - _ I - - - - - - - _ - - - - - - - - I - _ r- -a-t-i-o- - - I_ -[_P-Pb-l- - - - -- _ I _ _ _ - _ _ _ - _ _ _ _ _ _ _ 4.107 1 W A + 2.02831e6 6.10461e-1 305.11576 PFBS 4.821 2 PVA+ I 1.01737e6 1.00000 250.70000 THPFOS 5.158 3 W A + 5.36732e6 1.63334e-1 216.02714 PFOS Totals without ISTD(s) : 521.14289 Instrument 1 2 / 7 / 0 1 1:16:19 PM M;LA FACT-TCROOZ (LIMS #E00-1716), Page 126 of 138 Page 2 of 2 Batch Run # 52 of 79 Data File C : \ H P C H E M \ ~ \ D A T A \ H O ~ O ~ O ~ \ H I L I J O O ~ ~ . D TCR-002, 012901-naclPFOS-3.2.I, 1OOX Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-3.2.1 .......................................................................... Injection Date : 2/6/01 9:20,:29PFll Seq. Line : 52 Sample Name : naclPFOS-3.2.1 Vial : 65 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p l Acq. Method : C:\HPCHEM\l\~METHODS\HOl020.6M Last changed : 2/6/01 11:4'1:54 AM by MLA Analysis Method : C:\HPCHEM\l\~METHODS\HO10206A.M Last changed : 2/7/01 1:16:38 PI3 by MLA (modified after :Loading) . Sim run C2,c3,c4,c5, c7 and CI3 perfluoronated carboxylic acids ......................................................................... - v) < 300000 I 250000 4 200000 150000 100000 I ; 50O0Oi ,$ O. - Lt - I I - 250000 50 =00 200000 150000 I 1oooooj 0 I , , , ,? Instrument 12/7/01 1:16:38 PM MIA FACT-TCROO2 (LIMS #E00-1716), Page 127 of 138 Page 1 of 2 Batch Run # 52 of 79 Data File C:\HPCHEM\1\DATA\HOlO2O~;\HILI~OO52.D TCR-002, 012901-naclPFOS-3.2.1, 1OOX Dil. SFM 02-02-01 MEE(MLA) BACK TO MAIN Sample Name: naclPFOS-3.2.1 ................................................................. Injection Date : 2/6/01 9:20:29 Pi4 Seq. Line : 52 Sample Name : naclPFOS -3 - 2.1 Vial : 65 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p1 Acq. Method : C:\HPCHEM\1'\METHODS\HO10206.M Last changed : 2/6/01 11:4'7:54 j2M by MLA Analysis Method .: C: \HPCHEM\l'\METHODS\HO10206A.M Last changed : 2/7/01 1:16:38 Pl4 by MLA (modified a:Eter :Loading) Sim run C2,c3,c4,c5, c7 and C13 perfluoronated carboxylic acids _ __ ________________-_-_--_-_--_-----------_-_ --_-_ --_-_.~_-_-_--.._-_--_-_--_-.-_-_ --_-_ ------------------------------------------------------ 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.'7 Signal 2: MSDl 427, EIC=426.7:427.'7 Signal 3: MSDl 499, EIC=498.7:499.'7. RetTime Sig Type Area Amt/;Wea - -[-m-in-l- - 1 - _ 1 - _ - - - - I ----------I----------l---------r- atio 4.104 1 W A + 1.99860e6 15.10461e-1 4.819 2 PVA+ I 1.02867e6 1.lDOOOO 5.155 3 W A + 5.24716e6 1.629'79e-1 Amount G r p Name IPPbl I-+-------------- 297.34485 PFBS 250.70000 THPFOS 208.41657 PFOS Totals without ISTD(s) : 505.76142 Instrument 1 2/7/01 1:16:38 PM MLA FACT-TCROO2 (LIMS #E00-1716),Page 128 of 138 Page 2 of 2 Batch Run # 5 4 of 79 Data File C:\HPCHEM\1\DATA\HO10206\HILL0054.D TCR-002, 012901-naclPFOS-3.2.3, lOOX Dil. Sample SFM 02-02-01 MEE(MLA) ...................................................................... Injection Date : 2/6/01 9:42:48 PPI Sample Name : naclPFOS-3.2,3. Seq. Line : 54 Vial : 67 Acq. Operator : MLA Inj : 1 Acq. Instrufient : Hillary Inj Volume : 10 p1 Acq. Method : C:\HPCHEM\l\,METHODS\HOlO20.6M Last changed : 2/6/01 11:47:54 AM by MLA Analysis Method : C:\HPCHEM\l\,METHC)DS\HO10206A.M Last changed : 2/7/01 1:16::47PM by MLA (modified after Itoading) Sim run C2,c3,c4,cS,c7 and CI3 perfluoronated carboxylic acids ........................................................... BACK TO MAIN Name: naclPFOS-3.2.3 MSDl 299, ElC=298.7:299.7 (HO10206VllLL0054.D) API-ES, Neg, SIM, Frag:Var II v, , 300000 i 250000 200000 150000 i4 JI 100000 2 IMSDl 427, ElC=426.7:427.7 (H010:!06VllLL0054.D) 250000 200000 150000 100000 500004 8d 4 6 API-ES, Neg, SIM, Fmg: Var I/ 8 rnin Batch Run # 54 of 79 Data File C:\HPCHEM\1\DATA\HOlO2Oi\HILI~OO54.D Sample! TCR-002, 012901-naclPFOS-3.2.3, l O O X Dil. SFM 02-02-01 MEE(MLA) ....................................................................... Injection Date : 2/6/01 9:42::48PPI Sample Name : naclPFOS-3 .:!.3 Seq. Line : 54 Vial : 67 Acq. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p l Acq. Method : C:\HPCHEM\l'~METHODS\HO10206.M Last changed : 2/6/01 11:4'7:54 AM by MLA Analysis Method :. C :\HPCHEM\l'\METHODS\HO10206A.M Last changed : 2/7/01 1:16:47 PI4 by MLA (modified a:Eter :Loading) Sim run C2 ,c3,c4 ,c5 , c7 and C 8 perEluoronated carboxylic acids _______________________________- -_______- ----------------,--,--------.--.-------------------------------------------------------------------- - BACK TO MAIN Name: naclPFOS-3.2.3 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7:299.7 Signal 2: MSDl 427, EIC=426.7:427.7 Signal 3: MSDl 499, EIC=498.7:499.7 RetTime Sig Type Area Amt/Area - _[m_in_]_1_--1-_-----1----------1----------1----------1--1------r--a--t--i---o 4.107 1 W A + 2.00067e6 6.1046J.e-1 4.821 2 PVA+ I 1.02275e6 1.00000 5.157 3 W A + 5.14429e6 1.62835e-1 Amount G r p Name [PPbl 299.37708 250.70000 205.33247 PFBS THPFOS PFOS Totals without ISTD(s) : 504.70955 Instrument 1 2/7/01 1:16:48 PM M L A FACT-TCR002 (LIMS#E00-1716),Page 130 of 138 Page 2 of 2 Batch Run # 59 of 79 - Data File C:\HPCHEM\1\DATA\HOlO206\HILL0059.D Sample TCR-002, 012901-naclPFOS-3.3.3, l O O X Dil. SFM 02-02-01 MEE(MLA) ..................................................................... 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 1 Acq. Method : C:\HPCHEM\l\METHC~DS\HO10206.M Last changed : 2/6/01 11:47:54 $24 by MLA Analysis Method ; C:\HPCHEM\l\METHC~DS\H010206A.M Last changed : 2/7/01 1:17:11 PPI by MLA (modified after loading) Sim run C2,c3,c4,c5,c7 and C8 perfluoronated carboxylic acids ....................................................................... BACK TO MAIN Name: naclPFOS-3.3.3 r - -MSDl 299, ElC=298.7:299.7 (HOlO206WlLLClO59.D) 1 300000 I 250000 I 200000 jI API-ES, Neg, SIM, Frag: Var i x 150000 100000 50000 oJ-->.o ~ - t I I I- I I -- 2 4 6 MSDl 427, ElC=426.7:427.7 (HOlO:!O6WlLL0059.0) API-ES, Neg, SIM, Frag:Var -1 I 8 mir p 200000 - n i I 150000 0 * a 100000 11. s; I L x - o - I I- I I I _-_ 2 4 6 8 mi MSDl 499, ElC=498.7:499.7 ( H O l C m L 0 0 5 9 . D ) WI-ES, Neg, SIM, Frag:Var 900000 j 1 800000 1 700000 1 9 600000 -1 500000 400000 300000 200000 100000 0 ' Is!, 12v) n (D ln 7 ln - I 2- J\ I I I 4 6 8 I K 0? '. $ Batch Run # 59 of 79 Data File C:\HPCHEM\1\DATA\HOlO206\HILL0059.D Sample TCR-002, 012901-naclPFOS-3.3.3,lOOX Dil. SFM 02-02-01MEE(MLA) ..................................................................... Injection Date : 2/6/01 10:38:35 PM Seq. Line : 59 Sample Name : naclPFOS-3.3.3 Vial : 71 Acy. Operator : MLA Inj : 1 Acq. Instrument : Hillary Inj Volume : 10 p1 Acq. Method : C:\HPCHEM\l\METHC~DS\HOlO206.M Last changed : 2/6/01 11:47':54 P&l by M I A Analysis Method ,: C:\HPCHEM\l\,METHODS\H010026A.M Last changed : 2/7/01 1:17:11 PPI by MLA (modified after 1.oading) Sim run C2,c3,c4,c5, c7 and CEIperfluoronated carboxylic acids ==============================:=====:================================== . BACK TO MAIN Name: naclPFOS-3.3.3 1 250.70000 THPFOS Signal 1: MSDl 299, EIC=298.7::299.7 Signal 2: MSDl 427, EIC=426.7:427.7 Signal 3: MSDl 499, EIG498.7 :499.'? RetTime Sig Type Area ----[-m--1-i'1n--l----1----------1.-----.-----1---------- 4.106 1 VBA+ 1.90270e6 4 . 8 2 0 2 PVA+ 11.02888e6 5.156 3 W A + 4.69662e6 Amt/Area Amount G r p Name ratio IPPbl I-+-------------- 6.1046le-1 283.01915 PFBS 1.00000 250.70000 THPFOS '1.61969e-1 185.28658 PFOS Totals without ISTD(s) : 468.30573 Instrument 1 2/7/01 1:17:11 PM MIA FACT-TCROO2 (LIMS #E00-1716), Page 132 a4 138 Page 2 of 2 ATTACHMENDT: DEVIATIONFRISOM THE PROTOCOL BACK TO MAIN FACT-TCR002 (LIMS#E00-1716),Page 133 (of 138 Record of Devlatlon BACK TO MAIN %af7'&0ject No. ..-, ........ . .. .... >, U.,..... -I_. . ...--,... ,....Ib . .--, .......... ",I.# .. I-.. ,- ......- t"l.,...'L".. ..I ....... ... ..... T...C.. R=002 .... ..-, .... . ,*II.I,U~ ,.-I- lllnl "&e: Deviation ...- ... 0 SOP' '-'- E#%&xi 0 Equipmait pro-c.-.e..dure ....-l..l-......,Y- , , , , , r , ..I..-"........-, .. ...".. ...... ............ - . . ...... (Cheakone) O ' h C O I 0 otilor: .....,,,1 .,.. -..... ...---.. ibocumont Number ETS.8-155.0 .........-.....(. : T h ....I-.- (9) o f occurrence:01 -.a _-."..........I hn ... I--., .-... 01 to 07 Feb 01-' .... ,...-.. ........ ,- ....-.-.-. .,...,..,I I* -..a, ..... ....",.I ......------. -1. ...-e I ......-- .. .. ...... .....-,, -..-,,, CIYI.... I . , ll"Y,l .............. I.II,U,UII.... .--I. ................ . *",."..... "-1. .......... ....- . ...-*...CI%#'. ._.._"_.. .. ... .. ..., I...-,.,.....IIY"L. -..-.-- 4 - "I".. 1"m. m .Y""..........*.r.. --,a,. I. .Ac_tu.,a"l.,R. owdurc,@. ocess..:.....T...h..e..nud..-r.i-x-.s p...h...e..w. ere..n...o..t.pr.e..p..a.r.e4 t.h...d..-.ore..>.t,hey.w.....e...r.e...not . . _...,I,uan-. I-."-. 11.1 I UI LY," I. . 1- "1.11 . ........ .. ....-... ...... ... . --.- ..... 111- ,.I,. .....--- Y t Y Y Y " ........-...... -c.* ..* ._". l.,. I .I*.._ .. ... .......... .... .....-*..-- . . ... . . -.----~,.,..I- *....lly I..._._ --,.. .-.............-..I . -.-.I-. ...._..I... -IC-........".-.. ............tii&iT&y.-...-.-.... eaniiat.ed. . ... .......................... possible in................ .n..o.t -,.-.n., *It"ltl(..(*l(l....l.... hw.e thci*ma. t.ri.xi.s . ...a ...._I_. --..I.-.., ..-IIYI..l. with the anal* of interest, .. Y I - ..-~l.~..l....,.lllll..l #..1111 ....I-- ........ %-.. .- I I 1 I ' BACK TO MAIN . ,, SbdyT h j e c t No. -- - Record of DevCallon I. / d ""...,...-...........,.-...... ..-.. ew . --. -,,. .... .I-...... .......... Y*la.-...... ....* t l ... TCIR-002 Is.o-p". ............. ..Tyfi?"' ~eviat~on .... ...l...,'Dll' mor: (Check one) ..*".U ..... .......a_-.... ....*-. .....**... ..e,--- .--... l#Methoh Eq~pzIlent~cedllrc 0I)rotocol a ..."". . .I., .. ...... -.. . . I.._* .. .--....... II Or" DocumentN&!&c~%n:&ll55.0 1 . 1 , - - ..-. ............... ....................... I- Date@)ofoccuxrcncc: 01 Jan 01to 07 Feb I I .bi.an. k.S. -- ...,-.- ","&,,,-e"i." the .i.%.s.i..-d%" &o- n-....... .,..c..-uI,r-.v..e......~,-..., .. I".*. ........ .>,*,rnU,~., .............. -.......... ....1-11,,.,.,.... ,...............-.. .........111- ........ .- .__.... ,. . .,.,. ......- Recorded By: . .--. . ,..-.".. " W _--I I.._. . ................ .. .............e-. ..I.._, I. .... ........ .... ....-.-- ,111"- ...--- u I.*. .I_._ . ,.,..I a"- .. .I .......... ... . I"..,. "I*- .........---. ... .....- YC-.-..---..-..l.ll... -.-.--.-. ............. ---.-.. .... bate: ... I*-.-."-... i a"",,-- ...-.---..-, .I..."ll..Y ! I .-.-".". ... .-..-,, I--,- The i.m....p..a..ct o f b f s deviatlon.oris:-.U.sY .tY .u...)d.II.y...-.is ... .......................... *----.. ..\.llillY,II E._.. .,...I--. ....................... .-..-... ..... b e a t i n g o n ~ . ~ ~ ~ : _ S e e ! ~ O ~. . ~ ~ ~ ~ ~I oI..n....,........... ........... .....I I I ~ U I I , . , ~."....... --... ......................... ---- . I'II"..YI ....... .--..,.--..........I I I Y . ....... I"_. 'i BACK TO MAIN 1 Record of DeviatSon - - -. .......... ........ ........... I I _.. . No. / Project Study **- .u, I .N. '*- --- M,., .I ....... -- TCRs-o0p102fl . q ~ p e ~ h a E ... .... . ............ ... ........ 4 , IUS, ,Type: Deviation 1-11 ....--.-., Ll",,. MethodI-,. .-..---,, Y,, 11.11. .-. ....."0, ........ (Check om) 0 Protocol fl Other - ! . ~ ~ ~ ~ ~ ~ . N ..----. ~ .-* ~IC ! D.*~.3.*o-m-.m"-.c-i E T ~ .~csr~Ts.oli.tia' ~8,-je&-~o-r. i ~ . 1 I/, Oweription: ;.- &-uor4-..-Gr98ii .......... . I& 3'0%. (?) I I .Rc..o..e&.qcuylizrnetd ProA c, ed. u.. rY dpr...o..c..w. r: In de...a...l..i..n. g withthe s h d d e w e , the cuingrsvdde-&m"we- t havea --. I "_"I.. .... ,.*. ol, W.t' .... Qrsatcr I. .--........ ... ............ .......... ........ . . . ..-_ .--.... , points ###,,a must -11,. have 'Perc.e..n. t I>eviations' esubljria'or ihsn +/- I,&- .-., I ", 1 1 1 1 . .-. I 'MI,"" IIIU... ""WYWI -(I I.._. Io., *mu. ,.*I. Y . ..... -.. 4th 1 I .A&citu"al P~ro~ced.ure~/Dm. cw~: ~In B~O= ~cas~es. h.i& m=;a.j-n@d~/orl~owd tm heo *.-p..leo~i.r .n-t'-s..w..cerep~e.o.lii.tm.a.~..s.i-n.wa~at.ee.d~80 ~ , ... . """ ..... ......- .....................-.-.- ..a&&&-&. .....I C . . *.D .......... --....... d b w d , t~ not . . . I , _ they ere the +/-M . - . - . I . accuracy menthis -I,.. I..... requitemente, was dono, "".-*-..-_I 3 l a I I i :i I I ........... ......... . . ...... ....... . . . .-. ...--. . ... WOiiKiid -'.*... i D m I .,,,.-,,- -..-..... .. I... ",'*# "T....." ......... *,. -...- "..* ' S h a ' i i i ~ d o on f -I . l.. clnve p o i m brei a posi.l-w*-..c unpact on &a stu- -d-.y. :'-Fiukpom.s~were ._.^I not elii&iit~*&~-k be as accur.a..t.e... ,..1*1.1., ... ...-...- "I,. . . . --.I. tlrrn .--.,. 111"". I.., [ d7h I I I E C E I V U ) T I E my. 17. 2:28PPl FACT-TCROOZ (LIMS#E00-1716).Page 136 of 138 E ' d EES'ON Wl lW3IlAlWNW 3 U N 3 3 WdST:P TBBZ'LT'AUW IRecord of Deviation BACK TO MAIN ry.. . ,",,I ...Y-- ...........- .-e. ..............-..-. -... ,--. ....ll,C ...._. ....." . .l .... .-.. .-. Std~~Phject ...--- s.dF........ .... . .... ...,I.,-,, ,..a,YI ....-.- Deviation''I)pe: .... ,..a4 II..... ..-.I.." .-up .......-....-............I - ..._I IBMethod 0Equpnart Procedure 111.- a mcborrcr) 0 m : o l other: --__ . ---,, "...-.--."*,1411,.."L.L "."CL.",..-..'.L-l..-r.I -.a".--.,-,-* .-L..-m". -......... ............. . .-- .. .. .. -----. .. . .*.a" . ...-.-............I....-... ,.-..I. I.....L.YY.I. -,. YO., .......I.. I..."- 1 ..... ...... .... ... .... -.. .. ................ I ,-,.. "I* ..-a ---.. I- I , . .. . .a,-. t.*-. I- ~....."1111"... .. I,",..,, *..1"."l..... .... In .. ... and portions ofthis ActualProcedurc/prccss: the seawater 3.5% NaCl study, I --. I-V . I-.-" .",YW ----m-.,,-C,.C2----.--. -..e-,., the s ~ l r c c ~ ~ .. I - - - r r u ~ * I , C U , r . * - - - - . ............. ......... ......- ............ .... was not-a~i-n.-e.........-~.,....----. ,.--...... test I'YY,II""I.., ...... ..I.._ -.-, I,*,... ....... . ........... .. --1".1. .... I-..-...... ...1 1........ ,11011.- ...... ..,-... .1.,1111"(1., . I - -,,,,.l. 11.1. -I- .,Y." .. . . ..... , W I , d U " , ,I *--a ........ 1 . 1 " . -.-.-a . ...--....... I l l a.1111 ........-... 11111"1.1.... .---.. .III.CIIIII.' ... ...... .......- ............. ...*. . . ............ ............ ... 111. Actlonr Taken: ..... I . N . . " , I... ........ . I #I*",. .. .......... . thi..s............. . . . Notes...t.o-.F.-i-l.e were v d t e.-c~-o-.~n. w..i..n..g.,.,..,,.. mue. lllL .-111 -..-I .-..,- ,.I"-*. - . . . . ....... . ............ ...... .. IIWIU... ..... .-.--. " Y Y I I 4 ' . . . .--..--.. .,1." ."..-.. . (""1, I.-.... .---. _I.... .., ... ............... ...- -I.-. I-..... lY ! --....... . ..... .... Lead uyp".w.. ...=---- ,I--.. .... .-r.--. &&mzed By: (slucbMtcat9r /.Pr&ct 1 1 . 1 , .. -.--.-. 1 1 . 1 1 1 8 .... .-*. ............... BACK TO MAIN ATTACHMENET: SAMPLEC:ALCULATIONS Mean and standard deviation were calculated using functions provided in Microsoft E.xcel@ 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 entitiles Standard deviation was calculated using the following equation: -Where n is the number of observations, and x is sample concentration. Sample ID Repl Rep 2 Rep 3 Rep 4 iConcentration dmL 647.9 723.4 723.0 717.3 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% Q-Test Example (Shad'ednumber represents the suspected outlier): Clescription Samiple Conc., Repl Samiple Conc., Rep2 591.7 1Range (Rep4-Rep2):1 GaD IRem4-Re~3kI 2057.14 2022.66 Q-Test example excluded. FACT-TCROOZ (LIMS #E00-1716), Page 138 of 138