Document 85XG6axK6k4gVneL4o60pyKJe

AR226-1030A007 BACK TO MAIN Study Title Solubility Study of Perfluorooctanesulfonate (PFOS), SD-018 and Perfluorooctanesulfonamide (FOSA), SE-027 in Male/Female Human Urine Data Requirement 40 CFR 160.105(b) Author Mark E. Ellefson Phase Completion Date Date of signing Performing Laboratory 3M Environmental Laboratory Building 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Project Identification 3M Environmental Laboratorty Project# E01-0768 3M LIMS#: 25160 (PFOS SD-018), and #25161 (FOSA SE-027) Total Number of Pages 171 BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 Table of Contents Study Information......................................................................................................................................4 S u m m a ry ....................................................................................................................................................5 Purpose......................................................................................................................................................5 Test Substance.........................................................................................................................................5 Reference Substance............................................................................................................................... 6 Test System .............................................................................................................................................. 6 Method Summaries.................................................................................................................................. 7 Preparatory Methods................................................................................................................................ 7 Sample Collection and Analysis.............................................................................................................. 8 Analytical Method..................................................................................................................................... 10 Analytical Results..................................................................................................................................... 10 Data Sum mary..........................................................................................................................................12 Statistical Methods................................................................................................................................... 14 Statement of Conclusion..........................................................................................................................14 R e fe re n ce s................................................................................................................................................ 15 List of Attachments................................................................................................................................... 15 Signature Page..........................................................................................................................................16 Page 2 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01 -0768 List of Tables Table 1a. Summary Table of Solubility of PFOS SD-018 in Urine......................................................... 5 Table 1b. Summary Table of Solubility of FOSA SE-027 in Urine......................................................... 5 Table 2. Characterization of the Test Substance...................................................................................6 Table 3. Characterization of the Analytical Reference Substances..................................................... 6 Table 4. Description of the test system used in this study.................................................................... 6 Table 5. Solubility Screen Test Sample Preparation.............................................................................7 Table 6. Shake Flask Method Preparation for S tudy.............................................................................8 Table 7. Sample Collection and Preparation for Solubility Study ........................................................9 Table 8a. PFOS Calibration Standard Reprocessing Summary............................................................11 Table 8b. FOSA Calibration Standard Reprocessing Summary............................................................ 12 Table 9a. PFOS SD-018 Solubility in Urine Data Sum mary................................................................. 13 Table 9b. FOSA SE-027 Solubility in Urine Data Sum m ary................................................................. 13 Table 10a. Summary Table of Solubility of PFOS SD-018 in Urine....................................................... 14 Table 10b. Summary Table of Solubility of FOSA SE-027 in Urine........................................................14 Page 3 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 Study Information Analytical Chemistry Laboratories Solubility Testing 3M Environmental Technology and Safety Services (ET&SS) 3M Environmental Laboratory Bldg. 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Dr. William K. Reagen, Laboratory Manager Mark E. Ellefson, Principal Analytical Investigator Kristin L. Terrell, Analytical Chemist Mark L. Anderson, Analytical Chemist Cindy M. Carlson, Analytical Chemist Sponsor 3M Environmental Laboratory 935 Bush Avenue Building 2-3E-09 St. Paul, MN 55106 Dr. William K. Reagen Experimental Dates Experimental Start Date: 23 April 2001 Experimental Termination Date: 01 May 2001 Archives R eserve sa m p le s o f the reference standards w ill be m aintained by the 3M E nvironm ental Laboratory. All study data and a copy of the final report are archived by the 3M Environmental Laboratory. Page 4 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 S ummary The approximate solubility of Perfluorooctanesulfonate (PFOS) and Perfluorooctanesulfonamide FOSA in human urine was determined by performing a solubility screen test, followed by a quantitative solubility determination via Shake Flask Method. Results are presented in table 1a and 1b: Table 1a. Summary Table o f Solubility of PFOS SD-018 in Urine. S a m plin g E ven t Day 1 Day 2 Day 3 Average Value PFOS S o lu b ility in U rine (C o r r ec ted for S t d . P u r ity) 302pg/mL 325 pg/mL 287 pg/mL 305 pg/mL Standard Deviation 12 40 30 14 %CV 4% 12% 10% 5% The solubility of PFOS SD-018 in urine was determined to be 305 pg/mL at 23-24 C. Table 1b. Summary Table o f Solubility of FOSA SE-027 in Urine. S a m plin g E ven t FOSA S o lu b ility in U rine Day 1 Day 2 Day 3 Average Value ; 2.56 pg/mL 2.88 pg/mL 2.61 pg/mL 2 . 6 8 ng/m L Standard Deviation 0.38 0 .1 2 0.05 0.18 % cv 15% 4% 2% 7% The solubility of FOSA SE-027 in urine was determined to be 2.68 pg/mL at 23-24 C. Purpose The purpose of this solubility study was to determine the solubility of PFOS and FOSA in urine. Test Substance PFOS, Test Control Reference #SD-018 and FOSA, Test Control Reference # SE-027 Page 5 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Table 2. Characterization of the Test Substance T est Substance PFOS Source Expiration Date Storage Conditions 3M Laboratory Identification Number Physical Description Purity 98-0211-0888-5 08/31/01 Frozen SD-018 White powder 86.9% FOSA R. Buckanin, 3M Not Available Frozen SE-027 White powder/chunks To Be Determined Reference Substance Table 3. Characterization of the Analytical Reference Substances R eference S ubstance PFOS FOSA THPFOS PFBS Source Re-crystallized by George Moore, 3M Specialty Materials, Bldg. 236-1B-10 R. Buckanin, 3M SynQuest Labs Pat Savu, 3M Expiration Date 01-01-2010 Not Available Not Available Not Available Storage Conditions Frozen Frozen Frozen Frozen 3M Laboratory Identification Number TCR-00017-46 SE-027 TCR-00017-047 Lot #Q75-30 Primary Standard, TCR99030-23 (L-7038, F-8442); Lot 101 Physical Description White Powder White powder/chunks White Powder White Powder Purity 97.9% To Be Determined * The purity o f THPFOS and PFBS (currently being determined by Centre Analytical Laboratory) will not affect any analytical findings since it is used as a reference substance only. T est System Table 4. Description of the test system used in this study TEST SYSTEM/SOLVENT Source Expiration Date Storage Conditions 3M Laboratory Identification Number P urity/G rade H u m a n U r in e Lampire 03-16-05 Frozen TN-A 4822 Normal Male/Female Urine Page 6 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Method Summaries The solubility determination of PFOS SD-018 and FOSA SE-027 in urine was performed according to 3M Environmental Laboratory methods ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents;" and ETS-8-172.1 "Shake Flask Method; Solubility Determination of a Test Substance in Various Solvents" as adapted from United States Environmental Protection Agency OPPTS 830.7840, "Water Solubility: Column Elution Method; Shake Flask Method" and OECD 105, "Water Solubility" Guidelines. All analyses were performed according to the 3M Environmental Laboratory method ETS-8-155.0 "Analysis of Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry". The Solubility Screen Test Method (ETS-8-170.1) was used to determine the solubility range of PFOS SD-018 and FOSA SE-027 in urine. Incremental amounts of urine were added to PFOS and FOSA neat material and a qualitative determination of the solubility point was made. The screen test indicated a solubility of PFOS in urine of less than 200 pg/mL, and FOSA in urine of less than 200 pg/mL at 23 C. Therefore the Shake Flask Method was used for the quantitative determination of PFOS and FOSA solubility in urine. Detailed descriptions of the Solubility Screen Test Method and Shake Flask methods used in this study are located in Attachment A. Preparatory Methods ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents." This method is a prerequisite to the shake flask method and gives an estimate of the solubility point of the test substance in the solvent of choice. Approximately ten milligrams of PFOS/FOSA was weighed into glass vials, and varying amounts of urine were added in a step-wise fashion. After each urine addition, the vials were shaken, sonicated, and observed for particulate. When particulate was observed in a final volume of 2 mL of urine (approximately 5000 pg/mL) for both PFOS and FOSA, the final step of the screen test was initiated. Approximately 10 mg PFOS/FOSA was placed into a 100 mL volumetric flask and urine was added in a step-wise fashion up to 50 mL (with shaking, v o rte x-m ixin g , sonica ting , and o b se rva tio n s fo r pa rticu la te in betw een). D ue to fine particulates present in the urine, it was difficult to tell the difference between urine that did and did not have the test substance in it. This indistinguishable difference between FOSA and PFOS in urine and a urine blank sample was determined to be the stopping point for the screen test. The approximate solubility of PFOS and FOSA in urine at 23 C was 200 pg/mL. This concentration estimation was used as a starting point for the shake flask method, and as a guide to determine the amount of dilution necessary to bring the final sample concentration into the analytical range of method ETS-8-155.0 (approximately 2.5 - 1000 ng test substance/mL). Table 5. Solubility Screen Test Sample Preparation S tep 1 2 3 C en tr ifu g e T u b es P r epa r a tio n 10 mg test substance weighed into tared 4.0 mL glass screw-capped vial 0.1 mL of urine added to glass screw-capped vial Following the addition of urine, vial was capped, shaken vigorously and vortexed, and sonicated. Mixing and sonication times recorded on the worksheet. Page 7 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Table 5. Solubility Screen Test Sample Preparation S tep 4 5 6 7 8 C en tr ifu g e T u b es P r ep a r a tio n Sample checked visually for undissolved particles of the test substance. (If all of the test substance is dissolved, the solubility is determined to be greater than 10% (mass/volume) and no additional solubility testing is required. If a portion of the test substance remains undissolved, additional dilutions are performed using the appropriate solvent.) Observation made: undissolved particles present... continue to step 5. Step 2 repeated with total volume of urine of 0.5,1, and 2 mL, respectively. Following urine addition, vial was shaken, sonicated, and observed for particulate. Following the final urine addition to bring the volume of urine to 2 mL, there was still undissolved PFOS and FOSA. The screen test method would therefore be continued to step 7. Approximately 10 mg PFOS/FOSA were weighed into 100 mL volumetric flasks and urine was added stepwise up to 50 mL. Following each addition of urine the flask was capped, vortex-mixed, sonicated, and allowed to settle. The appearance of urine without test substance looked about the same as urine with PFOS or FOSA at 50 mL. The concentration of urine was approximately 200 pg/mL and there was still particulate. The shake flask method shall be used for the quantitative determination of PFOS/FOSA solubility in urine. ETS-8-172.1 "Shake Flask Method: Solubility Determination of a Test Substance in Various Solvents." Approximately 10 mg test substance was weighed into a tared 15 mL plastic centrifuge tube. Urine was added gravimetrically to approximately 4.7-5 g (approximately 5 mL if density of urine is assumed to be approximately 1 g/mL). For each test substance study, nine centrifuge tubes were prepared, along with three method blanks (tubes with 5 g 0.5 g urine only). The centrifuge tubes were placed in a temperature- controlled orbital shaker set at approximately 30 C. See the following table documenting the shake flask method preparation: Table 6. Shake Flask Method Preparation for Study S tep C en tr ifu g e T u b e P r ep a r a tio n R eplic a tes 1 0.010 g PFOS/FOSA weighed into tared 15 mL centrifuge tube 9 PFOS/ 9 FOSA 2 Urine added to centrifuge tube such that total weight of PFOS/FOSA and urine is approximately 5 g. 9 PFOS/ 9 FOSA 3 Method Blank Preparation- Approximately 5 g urine added to a 3 PFOS/ tared centrifuge tube gravimetrically. 3 FOSA 4 Samples sealed with tape, vortex-mixed, and placed in a 12 PFOS temperature-controlled orbital shaker set at approximately 30.0 C, /12 FOSA rotation speed set at approximately 150 rpm. Da t e (s ) Performed 04-23-01 04-23-01 04-23-01 04-23-01 Sample Collection and A nalysis On each of Days 1, 2, and 3 (approximately 24, 48 and 72 hours after initial sample preparation) three centrifuge tubes (3 containing PFOS and 3 containing FOSA) and a method blank were removed for analysis. The centrifuge tubes with PFOS and FOSA in urine, and method blanks (urine only) were allowed to equilibrate at 23-24 C for 24 hours, centrifuged, and aliquots of Page 8 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 supernatant were collected. For the PFOS samples, aliquots were first diluted 100X (990 pL methanol: 10 pL sample), and then diluted further to 1,000X (900 pL methanol: 100 pL sample). For the FOSA samples, aliquots were diluted 10X (900 pL methanol: 100 pL sample). Final dilutions were spiked with internal standard (17 pL of 15 pg THPFOS and PFBS/mL) and every fourth sample replicate was spiked with 4 pL test analyte (25.05 pg/mL PFOS, 24 pg/mL FOSA). Samples were analyzed via HPLC/ES/MS according to analytical method ETS-8-155.0. Four injections (three samples and one sample spike) of each sample were performed. The following table describes the sample collection and preparation regimen: Table 7. Sample Collection and Preparation for Solubility Study S tep P rocedure R eplic a tes 1 At 24,48, and 72 hours, 3 test substance + urine, and 1 urine (method blank) centrifuge tubes per PFOS and FOSA are removed from the incubator and equilibrated at 23-24 C for approximately 24 hours. 2 Aliquots of the supernatant (urine containing dissolved test substance or urine only from the method blanks) were collected and dispensed into autovials. 3a PFOS The PFOS aliquots were diluted 100X with methanol (using a dual syringe dilutee 990 |j.L methanol, 10 pLsample), followed by a second dilution of 10X (900 pL methanol, 100 pLsample) for a final dilution factor of 1,000X. 17 pL THPFOS and PFBS solution at 15 pg/mL in methanol were then added to the final dilutions, and every fourth sample was spiked with 4 |xL 25.05 ng/mL PFOS 4 centri fuge tubes per day for PFOS and FOSA Day1 Day2 Day3 4 per centrifuge tube per FOSA and PFOS Day1 Day2 Day3 Day 1 Day 2 Day 3 3b FOSA 4 The FOSA aliquots were diluted 10X with methanol (using a dual syringe dilutee 900 pL methanol, 100 pLsample), 17 pL THPFOS and PFBS solution at 15 pg/mL in methanol were then added to the final dilutions, and every fourth sample was spiked with 4 pL 24 pg/mL FOSA. Samples were analyzed via HPLC/ES/MS on HP 1100 LC/MSD Day 1 Day 2 Day 3 Day 1 Day 2 Day 3 D a te (s ) P erfo rm ed 04-24-01 04-25-01 04-26-01 04-24-01 04-25-01 04-26-01 04-26-01 05-01-01 04-26-01 04-26-01 04-26-01 05-01-01 04-26-01 PFOS: 05-01-01/FOSA: 04 26-01 PFOS: 04-30-01/FOSA: 05 0 1 -0 1 Page 9 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 A nalytical Method ETS-8-155.0 "Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry". Diluted samples (i.e. diluted supernatants) were analyzed using HPLC/ES/MS in the negative ion mode. PFOS levels were evaluated versus calibration standards ranging in concentration from 2.5-1000 ng PFOS/mL. FOSA levels were evaluated versus calibration standards ranging in concentration from 2.5-1000 ng FOSA/mL. Internal Standard quantification was used to normalize the data. PFBS was chosen as the internal reference standard to quantify the data, THPFOS was added as an optional internal standard during preparation for analysis, but was not used to quantify the data. Target ions were 499 m/z (PFOS anion), 498 m/z (FOSA anion), 427 m/z (THPFOS anion), and 299 m/z (PFBS anion). Analytical Equipment Liquid Chromatograph: Hewlett-Packard Series 1100 Liquid Chromatograph system Analytical column: Keystone BetasilTM C182x50mm, 5pm particle size Column temperature: Ambient Cycle Time: 10 minutes Flow rate: 300pL/min Injection volume: 10pL Mobile phase components: Solvent A: 2.0 mM ammonium acetate in water Solvent C: Methanol Solvent Gradient: Time %C 0.00 15% 0.50 15% 0.80 60% 3.50 100% 6.50 100% 7.00 15% 10.00 Stop M ass S p e c tro m e te r: Hewlett-Packard Series 1100 API/M ass Spectrom eter D etector Software: HP ChemStationTM 6.0 Fragmenter Voltage: m/z 299=100 V; m/z 427=100 V; m/z 499= 140 V; m/z 498=80 V Capillary Voltage: 3500 V Gain = 2.0 EMV Mode: Electrospray Negative Gas Temperature: 350 C Drying Gas: 10.0 L /min. Nebulizer Pressure: 25 psig Analysis Type: Single Ion Monitoring (SIM) A nalytical Results Data quality objectives outlined in the 3M Environmental Laboratory method were met (see Appendix A). Page 10 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Regressions. Quadratic curve fit was applied to calibration standards and sample data to improve quantitation over the concentration range appropriate to the data. All calibration curves had least-square fits of 0.980 or greater (R2 values ranged from 0.9993-0.9998). Calibration Standards. Twelve standards ranging in concentration from approximately 2.5 to 1000 ng/mL PFOS/FOSA in methanol were used for the calibration curves. Calibration curves were run before and after every analytical sequence. Calibration standards were also evaluated for accuracy, and were consistently < 30% difference from the expected value. Lab Control Spikes. 1 mL methanol was spiked with 4 pL 25.05 pg/mL PFOS spike solution, and another 1 mL was spiked with 4 pL 24 pg/mL FOSA spike solution, (the same 25 ppm spike solutions spiked into every fourth replicate for sample recoveries). The lab control sample was used to evaluate the recovery of the test substance in methanol only. Recoveries for PFOS ranged from 89-90%, and recoveries for FOSA ranged from 103-111% for Days 1,2, and 3. Matrix Spikes. Matrix spikes were prepared to demonstrate any possible matrix affects (i.e. signal suppression or enhancement) from the urine. Matrix spike recoveries for PFOS and FOSA samples were as follows: 30% with the following PFOS sample exceptions: 042301-PFOS-3.1.4MS (65%), 042301-PFOS-2.1.4 (52%), 042301-PFOS-2.2.4 (135%), 042301-PFOS-2.3.4 (53%). The MS samples from day 2 were done with a 5 uL syringe that seemed to have a loose plunger, therefore giving erratic results. Excluding the Day 2 PFOS spike recoveries may be disregarded. Overall, there appears to be no significant difference between Lab Control Spikes (test analyte spiked into methanol only) and Method Blank (test analyte spiked into urine only), or Sample Spikes (test analyte spiked into urine samples containing test analyte). Sample Replicates. Samples were within the 15% precision requirement. Continuing Calibration Verification. For quantitative determinations, a mid-level matrix calibration check was analyzed every ten samples to monitor instrumental drift, with a limit of 30% deviation of the target concentrations. Limit of Quantitation (LOQ). The LOQ is equal to the lowest standard in the calibration curve. See tables 8a and 8b for the calibration curve ranges used in the study. Table 8a. PFOS Calibration Standard Reprocessing Summary Data S ub Batch, A nalysis Date Calibration S tandards Day 1 data: PFOS: 5-501 ng/mL Day 2 data: PFOS: 10-501 ng/mL Day 3 data: PFOS: 5-501 ng/mL Standards not used, reason for exclusion 2.5 & 1000 ng/mL since only 10 calibration levels may be reprocessed using Target data analysis software. 2.5 & 1000 ng/mL since only 10 calibration levels may be reprocessed in Target. 5 ng/mL std. was disabled because the 5 ng/mL CCVs did not meet the 30% accuracy requirement. (Data at the high end of the curve passed all criteria). 2.5 & 1000 ng/mL since only 10 calibration levels may be reprocessed in Target. Page 11 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Table 8b. FOSA Calibration Standard Reprocessing Summary Data S ub Batch, A n a l y s is D a t e C a l ib r a t io n S t a n d a r d s D ay 1 a n d 2 data: FOSA: 10-499 D ay 3 data: Blanks. FOSA: 10-499 S t a n d a r d s n o t u s e d , r e a s o n f o r e x c l u s io n 2.5, & 1000 ng/mL were not used as calibrants since Target allows 10 levels only. The 5 ng/mL standard was disabled due to an elevated level of FOSA in some blank samples. 2.5,5, & 1000 ng/mL standards were excluded/disabled to remain consistent with Day 1 and 2 data. Method blanks (urine taken through the entire sample preparation, dilution, and analysis process) provided a measure of laboratory contamination. Acceptable values for the blanks were less than 50% of the limit of quantitation (LOQ). Method blank samples for Day 3 FOSA had a level of FOSA (20, 18, and 15 ng FOSA/mL on column) that was most likely due to FOSA dust in the analytical balance on the day of initial prep of the centrifuge tubes. Method blank samples from Days 1 and 2, a diluter blank, and internal standard blank ruled out all other possible forms of contamination. Therefore since it was determined that the FOSA was not in the urine prior to the sample preparation, this finding (i.e. FOSA in the day 3 method blank samples) is inconsequential. Solvent blanks (methanol injections) provided a measure of instrument contamination. Acceptable solvent blanks must contain levels of target analyte less than 50% of the limit of quantitation (LOQ). Acceptable solvent blanks were analyzed before each calibration curve. Specificity (according to OPPTS 830.7840): The solubility determination as stated in the EPA Guidelines follows. This method should be applied to: Pure substance. Purity of PFOS SD-018 has been determined to be 86.9%. The purity of FOSA SE-027 has yet to be determined. Since it is possible that impurities may exist in the FOSA, and the PFOS SD-018 is 86.9% pure, the reported solubility may be greater than that of a pure substance. Substances that are stable in water. Hydrolytic studies have been conducted for P FO S T C R -00017-46 (prim ary standard m aterial, R eport # W 1878) and FO S A (Project #EL-1132) at the 3M Environmental Laboratory showing stability. Data S ummary Tables 9a and 9b summarize individual sample data. Representative chromatograms are presented in Attachment C. The table displays PFOS and FOSA concentrations for individual injections. Also included are the average concentrations for each Centrifuge Tube replicate, standard deviation, and % coefficient of variation. Page 12 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Table 9a. PFOS SD-018 Solubility in Urine Data Summary S a m p l e ID SD-018 PFOS UG/m L C o r r e c te d fo r P urity Day 1 Centrifuge Tube#1 Day 1 Centrifuge Tube #2 Day 1 Centrifuge Tube #3 Day 2 Centrifuge Tube #1 Day 2 Centrifuge Tube #2 Day 2 Centrifuge Tube #3 Day 3 Centrifuge Tube #1 Day 3 Centrifuge Tube #2 Day 3 Centrifuge Tube #3 042301-PFOS-1.1.1 Smp 042301-PFOS-1.1.2 Dup 042301-PFOS-1.1.3 Trip 042301-PFOS-1.2.1 Smp 042301-PFOS-1.2.2 Dup 042301-PFOS-1.2.3 Trip 042301-PFOS-1.3.1 Smp 042301-PFOS-1.3.2 Dup 042301-PFOS-1.3.3 Trip 042301-PFOS-2.1.1 Smp 042301 -PFOS-2.1.2 Dup 042301-PFOS-2.1.3 Trip 042301-PFOS-2.2.1 Smp 042301 -PFOS-2.2.2 Dup 042301-PFOS-2.2.3 Trip 042301 -PFOS-2.3.1 Smp 042301-PFOS-2.3.2 Dup 042301-PFOS-2.3.3 Trip 042301-PFOS-3.1.1 Smp 042301-PFOS-3.1.2 Dup 042301-PFOS-3.1.3 Trip 042301 -PFOS-3.2.1 Smp 042301-PFOS-3.2.2 Dup 042301-PFOS-3.2.3 Trip 042301-PFOS-3.3.1 Smp 042301-PFOS-3.3.2 Dup 042301-PFOS-3.3.3 Trip 286 325 323 292 289 284 314 301 302 305 412 356 289 288 263 332 338 345 262 287 259 302 352 312 286 257 270 A verage ug/m L S td Dev %COEFFICIENT OF VARIATION 311 2 2 .0 7% 288 4.0 1% 306 7.2 2% 358 54 15% 280 15 5% 338 7 2% 269 15.4 6% 322 26.5 8% 271 14.5 5% Table 9b. FOSA SE-027 Solubility in Urine Data Summary S a m p l e ID SE-027 FOSA ug/m L C o r r e c te d fo r P urity Day 1 Centrifuge Tube #1 Day 1 Centrifuge Tube #2 Day 1 Centrifuge Tube #3 Day 2 Centrifuge Tube #1 Day 2 Centrifuge Tube #2 Day 2 Centrifuge Tube #3 042301 -FOSA-1.1.1 Smp 042301-FOSA-1.1.2 Dup 042301-FOSA-1.1.3 Trip 042301-FOSA-1.2.1 Smp 042301-FOSA-1.2.2 Dup 042301-FOSA-1.2.3 Trip 042301-FOSA-1.3.1 Smp 042301-FOSA-1.3.2 Dup 042301-FOSA-1.3.3 Trip 042301-FOSA-2.1.1 Smp 042301-FOSA-2.1.2 Dup 042301-FOSA-2.1.3 Trip 042301-FOSA-2.2.1 Smp 042301-FOSA-2.2.2 Dup 042301-FOSA-2.2.3 Trip 042301-FOSA-2.3.1 Smp 042301-FOSA-2.3.2 Dup 042301-FOSA-2.3.3 Trip 3 ^3 2.23 2.13 3.09 3.13 3.12 2.48 2.33 2.30 3.17 2.96 2.91 2.98 2.80 2.69 2.89 2.79 2.75 A verage ug/m L Std Dev % C oefficient of variation 2.18 4.6 % RPD (Rep 1 excluded from calc.) 3.11 0.0 1% 2.37 0 .1 4% 3.02 0 .1 5% 2.82 0 .1 5% 2.81 0 .1 3% Page 13 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 Day 3 Centrifuge Tube#1 Day 3 Centrifuge Tube #2 Day 3 Centrifuge Tube #3 042301-FOSA-3.1.1,Smp 042301-FOSA-3.1.2, Dup 042301 -FOSA-3.1.3, Trip 042301-FOSA-3.2.1, Smp 042301-FOSA-3.2.2, Dup 042301-FOSA-3.2.3, Trip 042301 -FOSA-3.3.1, Smp 042301-FOSA-3.3.2, Dup 042301 -FOSA-3.3.3, Trip 2.69 2.51 2.60 2.57 2.61 2.51 2.63 2.74 2.60 2.60 0 .1 3% 2.56 0 .1 2% 2 .6 6 0 .1 3% The average PFOS and FOSA concentrations and standard deviations for each day, as well as the final overall average for all non-excluded replicates and time points were as follows: Table 10a. Summary Table of Solubility of PFOS SD-018 in Urine. Sa m plin g Eve n t PFOS S o lu b ility in U rin e Standard Day 1 Day 2 (C o r r ec ted fo r P ur ity) 302 pg/mL 325 pg/mL Deviation 12 40 Day 3 287 pg/mL 30 Average Value 305 pg/mL 14 The solubility of PFOS SD-018 in urine is 305 pg/mL at 23-24 C. %CV 4% 12% 10% 5% Table 10b. Summary Table of Solubility of FOSA SE-027 in Urine. S a m plin g E ven t F O S A S o l u b il it y in U r in e Standard Day 1 (C o rrec ted fo r P urity) 2.56 pg/mL Deviation 0.38 Day 2 Day 3 2.88 pg/mL 2.61 pg/mL 0 .1 2 0.047 Average Value 2.68 pg/mL 0 .2 The solubility o f FOSA SE-027 at 23-24 C is 2.68 ng/mL. %CV 15% 4% 2% 7% Attachment B contains data summary tables. Statistical Methods Statistical methods included calculating means and standard deviations. Outlier data points were excluded using Dixon's Q-Test. Refer to Attachment E for formulas and example calculations. Statement of Conclusion Under the conditions of the present study, the solubility of PFOS SD-018 in urine is 305 pg/mL at 23-24 C. The solubility of FOSA SE-027 at 23-24 C is 2.68 pg/mL. Page 14 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 References 1. Fate, Transport and Transformation Test Guidelines Office of Prevention, Pesticides and Toxic Substances (OPPTS) 830.7840 Water Solubility: Column Elution Method; Shake Flask Method. EPA 712-C-96-041, August 1996. 2. OECD 105: Water Solubility. Adopted 27July, 1995. List of Attachments Attachment A: Extraction and Analytical Methods Attachment B: Data Summary Tables Attachment C: Sample Chromatograms Attachment D: Deviations from the Protocol Attachment E: Sample Calculations Page 15 of 171 Signature Page BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 We certify that this report is a true and complete representation of the data for this phase of the study: Principal Analytical Investigator William K. Reagen Laboratory Manager --------- o /o * A / Date Page 16 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E01 -0768 Attachment A: Extraction and A nalytical Methods Page 17 of 171 3M Environmental Laboratory BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents Method Number: ETS-8-170.1 Adoption Date: 09/08/00 Effective Date: 03/14/01 Approved By: William K. Reagen, Laboratory Manager // / Mar^ K Ellefson, Project Le; Date Date 1.0 Scope and Application_________________________________________________________ 1.1 tpATdhP((ifonOoEpeihuggrtmTptEereehhcepSCnr)lEeormyoc-fDmtP8soyhsisoAe)-nrpeo(1lm.aoaUvl7CatuueiAip2Snnboonn.rdclgl0ndteEeuc)lsOomsPtoiieimofnhrAEssndliaitupCnt)invoEnibatDaianerlginbnrrudltygiieesdtittcoscioysuuosttal.thomslnuttuaeeeelbdAuersMdsiOyttb.lsdihai,einordtlotIwgyglsihidfvtoatyhotisvepnleoidunirgiscsnaezbtterh(saliaiettEin,llhtmwailfignTtyetooyieoi,SnlrgnCrltod-uafhftob8uufirholdeb-yre>aur1teynhomttt7leo1hieut1ns1n0hert.tte0l'0ehi2siEEs%n)neogUlcgsewlu/toutn(dLetiaimnbininltoitoil(eddneal1nmbiidest0tcthesnMyhiaS/pcacivutdstteypeaosCetsimmetlhotfoeudeao)etsfomrh,dttscmpEhoetoeeehaoni)lrprdnne.udtvaraedab,tieSittirinelsioSholioreimnahntcmnrykamvoiaiewknemonneesaFidefnplrFall<tyotDaashlbuslase1eaeknsoPv0dkspnlrMe'u2osorelMbeolgctetueriop/eteleLbchismtqbttihsoyilu(eaeoiod1tirnndys0ytsit.e 1.2 Compatible Analytes. Test substance and degradation products for solubility testing. ETS-8-170.1 Solubility Determination: Screen Test Method Page 1of9 Page 18 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 1.3 oAtchceerpstoalbvelentM(s)atorficineste.reAstq.ueous (e.g. Milli-Q water, 0.01M CaCl2), Acetone, Methanol, or 2.0 Summary of Method___________________________________________________________ 2.1 hthtddmgaiodlpaPsa1heonulpnieair2igrrlsseiggscatbspdo/nnetssehrdbhmsrvwloubeoorsosouolitimmltuLelymatouaoaxvevfenbnpl.rtkiseieoesi,nencssmia.nno.ssrct,dweIeraltaaaamftiAtausOniicencthrttftncbheehiyactdhyetnlgotleel1xeildeeoe2cyeihCrSisn,eLt-svamsthtao5oo1dean1haoee1ll0olasen20rddluemuu0teulrr.dv.pmbb5m0.tfbisdilprpiinniaeonRiarlmimlgrAmlulsiosslinei.teevtststtLLydso)syeclyfoe.esoA.fudu-fsonloensD4tl.ufrtrTftotiirltetdtteomsve;hmliMihtesosvntnooeeitareitelLtenntralvmsareaslnmct.hkutemaogoetosaeaen1bclalItsnbhdtsviathseyfhtLon,tsadtsiepnatoabneasstsbinhwgihontdorsgtneteibsvreteiclioeacowuevsianreuynsrsdrevneneteneiehiiunsanrtlocontfwdailehitataelnntfrbiikqboto-sosseavseee1cuehussansddiea0aiaoooilscfsdrunopd0rnlulhlce1iytavvonptaydieba0psiaeleefldt.locueik0Ldndoizths,cnpnh,tesImmtopi,tvdaa.eofedhttnalivehneoLvntelarWsfrh(otodeeiltioh/2Eca.igerrwadvtcloetmaprTlre,umoelaAeiddtpsetSgtxwleashiiLtursadhdszt-(ooeemimr8Es.deanoexisaua-dsgTritnetI1nipbxaeoosemhtfSp7dptsnrlopssitfutr-i1raadltphftcaoa8eolt.itpsneeilt0prle-vxuflophlo1rc)aoliaisnecnrel.aos7emrwpuvododusab2stpbesxIkaniteoas.vuhsifnrs0itdcleobsmooe(taltts)ercaoynhlsxllitvinyaulnwoottleniecasvttmmcnbfreihdon1steoveclaeeli0eaencldryaettasfteteicfbrnmtueufroopityo1itertlpdlsvnaecoryin0gmluinaeryurrstsiftbmrgtooss1issiliwndscea5oiofgat5iteldshlnatgtetskureienohseent1istotccofsidtgth0ioe.rnt0,eno>r 33..10 TsoDelsvetefsniutnbwitsitilaolnbncese_d._e_Ate_r_lmi_q_iun_ie_dd_.o__r_s_o_li_d_m__a_t_e_ri_a_l_f_o_r_w__h_ic_h__th__e_r_e_la_t_iv__e_s_o_l_u_b_il_i_ty__in__a__sp_e_c_i_f_ie_d___ 3.2 Tmasoenesldtvthvesanaonrtloivmole,unasaytn.sidanTlcathlcmueedtamoetnrabiectu.reitsxis(teon.gow.th0lii.cm0h1itMtehdeCttoeasCatlqs2u(uaeqb)o)su;tasannmcdeaotorrifgciaennst,iecrinesscotlluvisdeininntgtmroAadSturTicceMeds.,TTiynhpceelutIedsWint gater 44..10 WHaeranltihngasnadnSdafCeatyuWtioarnnsings: . ______________________________________ 4.1.1 pWroetaerctthioenparot paellrtliambeas.ttire for all parts of these procedures. Wear gloves and eye 4.1.2 pHraoncdeldeuarell. solvents in a hood for all parts of the described sample preparation 4.1.3 pFaocrkpiontgenmtiaatlerhiaazlsa,rdansdof3MeacEhncvhieromnimcaelnutasel dL,arbeoferarttoorym'satCerhieaml siacfaeltHy adzaatardshReeevtsie,w. 4.1.4 No mouth pipetting is allowed. ETS-8-170.1 Solubility Determination: Screen Test Method Page 2 of 9 Page 19 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 4.2 Cautions: 4.2.1 mGleatshsawnoarletoinrewdhuiccehtshteanpdoasrsdibsialirteyporfepacacreiddesnhtaolucldonbteamtriipnlaetiroinn.sed with acetone and 55..10 IntIetmseptrusfureibtrisetesannmcceaeyss_hs_oig_un_ld_if_ibc_ea_n_kt_nl_yo_wa_fn_f_ea_cn_td_th_de_o_cs_ou_lmu_be_ni_lt_iet_yd__op_rfi_toh_re_t_ote_s_stt_as_ru_tib_ns_gt_a_tnh_ce_e_.s_cT_re_he_en_ip_nu_g_ri_pty_ro_oc_ef_d_thu_er_e_._ 6.0 Equipment____________________:______________________________________________ 6.1 Analytical balance sensitive to 0.1 mg. 6.2 Vortex mixer. 6.3 Sonicating device. 7.0 Supplies and Materials___________________________________________________ 7.1 Disposable glass graduated pipettes, 1mL to 100 mL. 7.2 Disposable glass Pasteur pipettes and rubber bulbs. 7.3 Glass beakers, various sizes. 7.4 2.5 mL-4 mL glass screw-top vial. 7.5 Glass volumetric flasks, 10 mL to 1000 mL. 7.6 10 pL-1000 pL PipettemanTM manual pipettor and plastic pipette tips, or equivalent. 8.0 Reagents and Standards__________________________________________________ 8.1 Methanol (MeOH), HPLC/SPEC/GC grade from EM Science, or equivalent. 8.2 Acetone, HPLC/SPEC/GC grade from EM Science or equivalent. 8.3 Water, ASTM Type I, or equivalent. 8.4 Calcium Chloride Dihydrate, Approximately 99% or better, from Sigma or equivalent. 8.5 Dm0.i0ah1rykMdwraiCttehaiMCnlia2l,lwiA-Qei0TMg.0h1wbaMotaetrC.aanCdlt2rastnoscfkersroinlugtitoonais1pLrevpoaluremdebtryicwfelaigskhianngd1d.5ilugtiCnagCtlo2the 8.6 Test substance of known purity. 9.0 Sample Handling______________________________________________________________ 9.1 Record times of initial preparation and dilution on a sample preparation sheet or logbook. 9.2 Oexntcraecttheed,ptrheelismcirneaernytetessttsinamg hpalessbseheonucldombepldeitsepdosaendd itnhteoatphperporporpiaetrewinafsotermstarteioamn .is ETS-8-170.1 Solubility Determination: Screen Test Method Page 3 of 9 Page 20 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 10.0 Quality Control____________________________________________________________________ 10.1 Not applicable. 11.0 Calibration and Standardization__________________________________________________ 11.1 Tspheecicfoicmaptioounns.ds of interest must be of known characterization according to laboratory 11.2 All equipment used, such as the analytical balance, should be calibrated daily prior to use. 12.0 Procedures__________________________________________________________________ 12.1 Solubility screen. 12.1.1 Westqaueniidgvaharlde1ni0zte.mdgRperceop1rmdshgteheoet)fw.teesitghsutb(rsetafenrcetoinattotacah4mmenLt gAlafsosrsacnreewx-atmopplveiaolfoar 12.1.2 Asudbdstsaonlcvee.nt (e.g. water, methanol, acetone) according to the table below to the test 4 mL vial or equivalent Total vaodludmede(smolLv)e.n..t Approximate Solubility (pg/mL)... adSdo0iltv.i1oennt1 100000 adSdo0iltv.i5oennt2 20000 adSdoiltv1ioennt3 adSdoilt2vioennt4 10000 5000 12.1.3 FmtrRoeoeimlnacllouaolritownedwssin.,otgbchVoseaenidrsstduvoiniaaltuultilioetyoinonacndsohdftoeoincsnoksgtlehvftsoeteolrneslvtut,afenonvndrdotiuasratsprceodcxtlioovzmree5dddiixmnppgraaienprtptuopitcrsetolhhsexeesbie.mateI.bfafooturevenleydmci1sha5sakorisltnev.gceoIdotnbmtdesssea,tyrvssobaunetbiiosnctnaeastcne.ecs2es-a5ry 12.1.4 Itcd"(hfEoheeantiTeglctlSrehemp-slny8tati-rrnss1taueiot7cdbil2louset.ntbo0sa.l)nedbwc,Bie"seies>ladcol1nailb0svdues%esno,euoltvs(thmehfeeudseanrtastcohesfos/tendvetrirceomtetlteeuhnasrmetttmriefnaeiittgr)nhi.soeeitnsTtashrihpoeseeplqv>artueo1ecinscxr0ettuimdparsa.gudat/bdetmesitstLiasooon,lnulctuhbeobeifsliilhs1tihyat0yla0lpkabopenieLdnflrtat.edhsgoekHacrusomdomweeludteehbvnaoietsldrti,htyeifis 12.1.5 twIefsettihgsehuttbe(ssrtteafnseucrbetsoitnaatnotctaeacdh1i0md0enmnotLtAdgifsloassroslavnveoeilxnuamtmheeptrl2iecmoflfLaasoksftoasrnodlevaqerunditiv,zaewldeenpitgr.hepR1es0hcmoeergdt).the1 mg of 12.1.6 Apaaplrdlepodprwaosrpotahrltiveiaoettnneetsastahmcseocoeolutu.rntdtiionongftstooolstvehetetnltet.a.bARlesebcdeoelrsodcwraibltloeodtbhisenetr1ev2sa.tt1is.ou3n,bssvtaoanrntdceexprtmoocidxeed,lusivorenesrictoahnteet,haend ETS-8-170.1 Solubility Determination: Screen Test Method Page 4 of 9 Page 21 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 100 mL volumetric flask or equivalent Solvent addition 1 Solvent addition 2 Solvent addition 3 Total vaodludmede(smolLve).n..t 10 50 100 Approximate Solubility (pg/mL)... 1000 200 100 12.1.7 Icfotnhceensotrlautbioilnityesptiominattiiosnreaatcwhehdicahttohrepsruibosrttaonctheeiscosmolpulbelteesahdoduiltdiobneodfo1c0u0mmenLt,etdhe and shall be used as a starting point for the shake flask method (ETS-8-172.0). 12.1.8 If the 100 mL solvent level has been reached without complete dissolution of test sfluabsskt,agnrcaed,uwaeteigdhcoyluitnd1e0rm, ogr eq1uimvagletenstt. sDubilsuttaenctoe 1anLdwtriatnhstfeesrttosoalv1enLt.voTlhuemetric paa11pla77lrpo21trw.i.0o0ce)lx)edissm.htaoaaIrltfelsenibstcoeto1ilvun2lis-cso2eeib4dbnsltheteroraopvtudiaeorerdsntt,eitcortohmufelatailencltsoeeotswltsuhaumferboenssrootmeabllnusaucbexteiriilovmiitnesyadm.al,tdteh1itse0hsosopdhlguaw/tkmiieolLlnf..lbaeTsIkfuhttemhilefielztauehsndokdd(isEsh(sTEooSTulvl-Sd8e--d8b-e 13.0 Data Analysis and Calculations___________________________________________ 13.1 The solubility determination in this method is qualitative/semi-quantitative. 13.2 pTohientpoisinthtetorewfohriecha qthuealsiutabtsivtaendceetderismsionlavteisonin. solvent is confirmed visually. The solubility 13.3 Tcahlecucloantecdenbtyratthioenfoelsltoimwiantigoneqiusasteiomni:-quantitative in that the approximate concentration is cW=hear/eb: c= the semi-quantitative concentration pg/mL, ba== athmeoaupnptrooxf ismubastetaanmceowunetigohfesdolovuetn(tpagd)d,eadnd(mL). 14.0 Method Performance______________ ______________________________________ 14.1 Lmllaairrumggseetitbmaaentaidcrogovninanosryiofdifdneeragertrdiano.wrcrTdheuhemeenetarnoectpscthouoerrftaiwcsnoyaglytvtoheinnewtwchaoihrcneihccbhetehntiethnreagstosiaolodunldbveeieldsnitttiytmoisiasthatdideoednstee.odrlmuttoien,tehtdheiisssoeslruurtboejr.emcStaitnrogciean 14.2 Tquhaelidtaattiavoebetsatiinmedatitohnrooufgthhethsisolsutbuidlyityisoafnteessttismubatsitoanncoenilny aangdivsehnousoldlvbeentt.reated as a ETS-8-170.1 Solubility Determination: Screen Test Method Page 5 of 9 Page 22 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0T68 14.3 mFoerthaonda, cocrucroatleummneaesluurteiomnemnteothfotdhewsiullbbsteanusceeds.olubility concentration, the shake flask 15.0 P ollution P revention and W aste M anagem ent____________________________________ 15.1 bDrioskpeonsegolafsssacmopnlteaiwnearsstetobydipsplaocsiengofinglhaisgshpoipreltotews.BTU containers as appropriate. Use 16.0 R ecords________________________________________________________________________________ 16.1 Sign and date all observations and calculations. 17.0 A ttachm ents__________________________________________________________________________ 17.1 APrtetpacShhmeeetn. t A-Example of a Standardized Sample Preparation Sheet: Solubility Screen 18.0 R eferences_________________________________________________ __ 18.1 OChrgeamniiczaaltsi.onWfoarteErcSoonloumbiilcityC-oOopEeCraDtioGnuaidnedliDneev1e0l5o:ppmpe.n1t.-7O,EACdDopGteudid1e9l9in5e for Testing of 18.2 U(aGnndeitnTeedrraaSntotsafrtoeCrsmoElauntmivoinnroMTnemesttehnoGtdau)li.dPPerrloientveeecsnt.itoEionPnAA, Pg7ee1sn2tci-ycCi.d-O9e6sP-Pa0nT4dS2:T8op3xp0i..c718S-6u10b7s,Wta1na9tc9ee6rs:SoFlautbe,ilTitryansport 18.3 UCS1u-on1bli2utset,mad1nnS9cE9tea6sltu:etFsioaEntne,MvTirerotahnnomsdpe;onSrttahlaanPkderoFTtelracastniksofMnorAemtghaeotnidoc.nyP.TrOeevPsetPnGTtiuSoind8,e3lP0ine.7set8si.4ciE0dPeWAsaat7ne1dr2ST-oColx-u9ibc6il-i0ty4:1: pp. 18.4 D3MeteErmnviinraotniomneontfaTleLsatbSourbastotarnycMe ienthVoadriEoTuSs-S8o-1lv7e1n.0ts,.""Column Elution Method: Solubility 18.5 3M Environmental Laboratory Method ETS-8-172.0, "Shake Flask Method: Solubility Determination of Test Substance in Various Solvents." 19.0 Affected Documents_________ ;______________ ______________________________ 19.1 VETarSio-8u-s17S1o.l0v,e"nCtso."lumn Elution Method: Solubility Determination of Test Substance in 19.2 VETarSi-o8u-s17S2o.l0v,e"nStsh."ake Flask Method: Solubility Determination of Test Substance in ETS-8-170.1 Solubility Determination: Screen Test Method Page 6 of 9 Page 23 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 20.0 Revisions RNeuvmisbioenr ________________________________ Reason For Revision ReDvaisteion 1 rIet mwoasvidnegsirreafbelreentocems atokesptheecimficettheostdsmubosrteanucneivs.ersally applicable by 03/13/01 ETS-8-170.1 Solubility Determination: Screen Test Method Page 7 of 9 Page 24 of 171 Attachment A: Example Preparation Worksheet, page 1 of2 BACK TO MAIN GLP Study Number: F n virn n m e n ta l I ahnralarySQLURIUTY SCREEN _________________________ Sample preparation worksheet Test Substance: IDJfc------- -----Source: Date: Solvent: ID#: Source: Step 1 Weigh approximately 10 mg 1 mg o f test substance into a 2.5 mL-4 mL glass screw-top vial. Weight of test substance: -------------------mg Balance ID:--------------------- Date/lnitials: 2nd replicate optional:_ _mg Thermometer ID: 2 Add test solvent according to the table below. Following each addition of solvent, shake vlgorously/vortex, and sonicate the mixture and visually check for undissolved particles. Analyst Analyst Analyst Analyst volume added (mL)/ approx cone, after addition (ug/mL) Sample Prep D ateffim e- J- Step 2-1 Total volume solvent added (mL) Q.1 Approximate Solubility (ug/mL) 100,000 Flask vortex-mixed? Yes/No Room TempFlask sonicated? Yes/No Time-----------Flask allowed to settle? Yes/No Time-- OBSERVATIONS/NOTES Is there solute still presentTres-continue to step 2-2 NO- The solution is at 10%, and Is considered "Infinitely soluble." further solubility testing is required. Date/Time- -X- Step 2-2 Total volume solvent added (mL) Q.5 Approximate Solubility (ug/mD 20.000 Date/TIme- _Z_ Steo 2-3 Total volume solvent added (mL) 1 Approximate Solubility (uq/mU 1.0,000 Date/Time- -L - Step 2-4 Total volume solvent added (mL) 2 Approximate Solubility (uq/mU 5,000 Flask vortex-mixed? Yes/No Room Temp---------C Is there solute still present? Yes/No Flask sonicated? Yes/No Time----------- ------ min Flask allowed to settle? Yes/No Time--------- min Flask vortex-mixed? Yes/No Room TempFlask sonicated? Yes/No Time------------Flask allowed to settle? Yes/No Time-- -!C Is there solute still present? Yes/No Flask vortex-mixed? Yes/No Room Temp------!C Is there solute still present? Yes/No Flask sonicated? Yes/No Time---------------- min Flask allowed to settle? Yes/No Time--------- min Did the substance dissolve in 2 mL or less of solvent? Yes -Approximate concentration at which the test substance is soluble in solvent: The solubility of the test substance is to be determined via the shake flask method. or No Continue to page two for further testing. ng/ml Notes/ additional comments: 3M Environmental Laboratory Project # E01-0768 Page 25 of 171 Solubility DetermEinTaSt-i8o-n1:7S0.c1reen Test Method Page 8 of 9 3M Environmental Laboratory Project# E01-0768 Page 26 of 171 Attachment A Cont.: Example Preparation Worksheet, page 2 of2 BACK TO MAIN 3M Environmental Laboratory SOLUBILITY SCREEN GLP S tudy N u m b e r:_____________________________ Sample preparation worksheet Test Substance:_______________________ Irak_____________ Source:____________ Date:_____________________ Solvent: ID#: Source:____________ Step (continued from page 1) ***Did the te st substance dissolve in 2 m L? Yes/No If Y ES , the test is complete, and there is no need to continue with the screen test. If NO, continue to step 3 to determine the approximate solubility of the substance. 3 Weigh approximately 10 mg +1 mg of test substance into a 100 mL graduated stoppered cylinder/volumetric flask. Weight of test substance: ____________ m g Balance ID:________________t 2nd replicate o p tio n a l:_______ mg Thermometer ID:___________ t 4 Add test solvent according to the table below. Following each addition of solvent, shake vigorousiy/vortex, and sonicate the mixture and visually check for undissolved particles._________________________________________________________ Date/lnitials:. A n a ly s t volume added (mL)/ approx cone, after S olubilitv data addition (ug/mL) Date/Time / Step 4-1 Total vo lum e so lven t a dd ed (m L )... 10 A p p ro xim a te S olub ility ( u g /m l) ... 1,000 Sample Prep Flask vo rte x-m ixe d ? Y es/N o R oom T e m p Flask so nica ted ? Y e s/N o T im e Flask a llo w ed to se ttle ? Y e s/N o T im e OBSERVATIONS/NOTES Q min min Is there solute still present? Y es/N o A n a ly s t Date/Time / Step 4-2 Total vo lum e so lven t added ( m l) . . . 50 A p p ro xim a te S olub ility (u g /m L )... 200 Flask vo rte x-m ixe d ? Y e s/N o R oom T e m p Flask so nica ted ? Y e s/N o T im e Flask a llo w e d to settle? Y e s/N o T im e C Is there so lute still p resent? Y es/N o min min A n a ly s t D ate/Tim e / Step 4-3 Total vo lum e so lven t added (m L )... 100 A p p ro xim a te S olub ility (u g /m L )... 100 Flask vo rte x-m ixe d ? Y es/N o R oom T e m p Flask s o n ica te d ? Y e s/N o T im e Flask a llo w e d to settle? Y e s/N o T im e C min min Is there so lute still present? Y es/N o 5 Weigh approximately 10 mg 0.5 mg of test substance into a 1 L graduated stoppered cylinder/volumetric flask/or equivalent. Weight of test substance:______ mg__________________ Balance ID: . ____________________ Date/lnitials:. A n a ly s t Date/Tim e / Step 5-1 Total volum e solvent added (m L)... 1000 A pp ro xim a te S o lu b ility (u g /m L )... 10 Flask vo rte x-m ixe d ? Y es/N o R o om T e m p Flask so n ica te d ? Y e s/N o T im e Flask a llo w e d to settle ? Y es/N o T im e C Is there so lute still p resent? Y es/N o min min Conclusions: Did the substance dissolve in 1000 mL o r less o f solvent? Yes -Approximate concentration at which the test substance is soluble in solvent: ua/ml The solubility of the test substance is to be determined via the shake flask method. or No -The solubility of the test substance is to be determined via the column elution method. Notes/ additional comments: ETS-8-170.1 Solubility Determination: Screen Test Method Page 9 of 9 1 3M Environmental Laboratory BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Shake Flask M ethod: Solubility Determination of a Test Substance in Various Solvents Method Number: ETS-8-172.1 Adoption Date: 09/08/00 Effective Date: 03/27/01 Authors: Kristin L. Terrell, Mark L. Anderson, and Mark E. Ellefson Approved By: 1.0 Scope and Application__________________ ___________________________________ 1.1 PasonuldrupbOoirlsigetay.ndiAzeactetciroomrndinfinoagrtitothonetohEfecsoUunbnosimttaeindccSeCtsoattohepsaetErhanatvivoiernosnaonmludebDnitleaitvlieePslrooipntmeacetgnioitvn(eOAnEgteCesnDtcm)yga(utUrii.dxSe.(lieEn.gPe.sA,) wmmReaeefttteehhrroo/taddoci(eEsOtoTaEnSpCe-r/De8ml-i1Gem7tuhi0nia.d0naeroflylio)nrseocthrf1eeg0er5pne,raoeatlfneitmrdhteiOhnatPaenrPsytT10scSo0olGmujibupgiio/ldmiuetnyLlidnsmecforu8erse3tin0tbs.te7ea8spa4tnp0par)orl.yoxzciTmeehddaeutverpiearsseo.trhleueqbusihilsiatiykteeletfovlaetslh.kis' . ETS-8-172.1 Solubility Test: Shake Flask Method Page 1 of 11 Page 27 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 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 Method__________ ;_______________________________________ 2.1 vUosscuefsrbstiesenseetsgnaltsntsthceeoeesaltvcqi,ehnuwn-taostelaiigemtgraahaptcivhlvoeiemu,o/tdfsemeuttwrmpoicleriia-elcvqlalteuyhtea.as,ncnCttrrieftiaiawpvptlei-itvcchteaaiemtpdetp,eauestbadanethosdv,ebemssteaesasieatntllrisemitxdh(atebfhtrelcroadeanmepsksot)ti.lhwmuebAietplhdeprdeotcalioitpnmhnetesc,ineawanapnirtpdtryhrapotsfilopooarlcunuiearbottiefelistatetymstount hhrhhaoscsaaaaoualopconopoinigomcinpuparuqdthmiclcrrrruhzpyeoeosse(oeol.z,srTppntetnseetarwerstHAhitdmirindvaaaaeaiPatlevtttptralheelFisaeiyeyonsaeOpiiraetdncconnaipLreScostttnidr(nueeCaau)noeit)rrllrail.dx/rnnegtuMnirwdaiaaf.atami(bUeillinlnSa1nllduaggssldbe:ctttt1aeebowiueaatsg0od,uehlnnboiyandtidtdoaalairshvia2tnna2rdldoeruur0ds4ahddrndstts/iei.saehtisgao(dCuntlohfehsinigsoq-ua.t,testg2oarkurarra.6sbmeneoats,slsh1rndtaeaupteHeaCashmyidealerte),fycdanptb1iitsbfnnfalteHicoiieoalvltsrueyor:m,lse2m3vrttaldaivaHa0yipcteniuadei,la,ptamtu2ehLwlocCrltHaoyoeusvCiinoxtonlsipi/tlaoinilctMemonvla2blatsp/gieirelaa.SnnrantcsCi.apithetSonoeuwl,ydftrAaglyloovdsimi.ltlhnttlreeor2uhloaedpnaL4tebapkpl,teCseneiehrptteenseoa/roqroprMgfsloiauuyurlrtaruxerfisSllesslsoloiaiyiuemd.srcbrtar.dbhiohrniaalTsenaouapatStthntegctahlnpeaiyeltenodedrdymasocne,tniide4olepxsqsecuqe8.l)iuemaetsm,usDeinnihsuilardaatlideoelnraibktppbiudred1arefheerralu:nasyo1natgtten0ndoaee2diinddo4cbnd,rgeat72 33..10 3.2 3.3 rMDptiecSsShnearnooheaoasmemtlatgfitctvrrekheiepiueensnesolmsnessitnadttFasitemonemiblnbatgoapsltglp.tasnaalaraleknmnseeknTkeskeSdptho:rn:alaeeruerAmeAtaremhpatcnpmrgsareeoealdetaeeucpmhndnnagaoTteaptrrhddcrlalrayeioittbenipithnneoodldleat-infattnfcahs,mharnkaaeentrtamrioeaienselsulayspmaaygmu:tttltimieahsecToete-aternahdfrviln.lrerxolpeteta,olesr(_etuoetma_emdtm.cn_egpoee_des.esnc_stdsmus_taovi._nmpoufee_arrmtTst_eolhhps_ynhcaee_r(tteenlie_otsscc.o_rpmsgaoe_tlo.l.a,n_aerkpm_wtttTtmha_erihoaeom_onetnt_icdehsni_fesnrrta_bbd,,oaa_nlulotmse_aaoir_xrnonule_/tknaak.swr_enca_riidaedcs_esttt_seociriu_unoerans_/lnpree_ttar,irhd)_cine_eeaetgst_odntoeso_dfanwt_nrehmt_oaevahr_nmpato_isiacll_uvouelht_gyelha_uhtate_oitelci_tlfoha_tn_leh_)e_ 3.4 3.5 pIttScsohnaaraeomrttmrecheieereepnnddsltcaueiaortmrlehmreSerpsmopptluieaoelnignuacshsandoaunduatare(rrinesscddma):eel(oynRe(ItntefSeii.tcicpg)napa:l.tillreActopmeracesrtkaeostenntscv,ssoneea.awedsmdrusn.derpeelaldsecmsoitonon(uttwaaannlitolniosidonafergmanmtptceiolocseramtsela)pamntonaaaudklnynesntdnteearsnfa.irdnmoadmirldsaosar,lnivnadennradetn)pcaraaleynrsrtdeiicensadtelapttbhaievrrohaetuaeovglfiyhothre ETS-8-172.1 Solubility Test: Shake Flask Method Page 2 of 11 Page 28 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 3.6 CpaulricbhraasteiodnstSatnadnadrdartdo:aAchdieivluetisotannodfavrdarsiooluustiaomnsouinntas coofnacestnotcrakt,ioinnterramngeedioafteinotrerest. 4.0 Warnings and Cautions__________________________________ _________________ 4.1 4444....H1111....e1234althppNpHFWraraooaoocenrntckamdepdericolndoStettghuuiaeoareftnmehneltlp.tiayparsatotioleWppalrhevielaaaltertzlrntisnalintam,risgbndaeigsninasssd.to:taaif3rlhlMeeooawfocoEhderndcfav.ohlilreropmanalilrmctpsaealnoruttfsastelhodLef,satrehbeeopferrdaoretctsooecrdrymiu'bsraeetCdse.rhsieaaWmlmseipacalfareelgtpHylroeadvpzaeaatsarrdaastnhiRodeenevetsyie,ew. 4.2 44C..22a..u12tionAtmGosll:elatthstheesawsinrtoauvrlseeatsogisneere.lwsdhu(eicc.egh.tshcteeannptdoraisfrsudigbseialitrtueybpeorsfe)paacarcreeiddtoeanbrteaeltsocuobfnfeitcatirmeipnintlleaytriironinns.seeddwwitihthascoeltvoennet and prior 5.0 Interferences____________________________________________________________ 5.1 5.2 thbIsCemoaeoslrptunudustbswauerimiladbtiritsieetytnoasamsndmnccaerteasyemyesiconnhsanioiunsgsuosgtnlreldviapfiteribneocnetactteshnekr,afdtnelrtuyoertrewaheange.fncefreeena.ctnistsd,Ttnhghdoeleoacsisrnouostwlmueutrabeifrnnieelertieetaaydnnncdopaerfloyiutothshnrieedstroetoersfssatttlhmaaserbuptoicblneorsgatnpatdtornhoircteycieoep.mnsrsseTeiltnhoihmgefotpidohnurebararliaanytnynaakloylsyfssmitishsue. st 6.0 Equipment__________________________________________________________ _ _ 66666.....12345 ACIDVnenioclnaruuttltberyeixatfrit-u,comgHareliwaxbmceiaartilh.platanhobcenleaeMtsioneifcgnhr/socoitolliadvobielnintgog5100c5.a01mp.SmaLebgricil.eietsni,etsori.rfuegqeuitvuableesnto.r equivalent. 7.0 Supplies and M aterials______________________________________________________ 77777777........12385467 T5DDHPGC-ihriial2pssaiemm5eppsrt0smooiptlessbtmoaa-ocemmbbanLapllkaeeeGpentaeoggarusmrllsltya,atocaisspvagvsnsraphiouapgrataiplarboslaysl-udpetl1seseui.younp5asrreefitimzentrpcteedgoiLesaper.np,d.estiitcrpn(tiaepefgpsutrtsegaea,ctesnci,lsdrteiui1aomrbsumnetpbsLe1b,r5et,o1or%rabCn1eud-q0ol4ubfdm0istevh.LcaeC.alep.tonpttea.rl.volume), 5 pL to 1000 pL. ETS-8-172.1 Solubility Test: Shake Flask Method Page 3 of 11 Page 29 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E01 -0768 8.0 Supplies and Materials 888...132 AMWceaetttheoarn,neAo, lHS(TPMMLeCOT/HSyPp),eEHC1P./GLCC/gSrPaEdeC/fGroCmgEraMdeSfcrioemncEeMor Seqcuieinvcaele,notr. equivalent. 888...546 Tw0dC.ie0ealusi1lgtctihiMsnuiugnmbCgtsoCat1atC.hh4nlhecogemrsCioodalafrueCkktDLinwoionihintw,yhnadEMrwxpaiaueltlmierig-,ipQthAylebTM.p:opawrAtoaax0tnie.m0dr.1atrtMealnysCf9ea9rCr%iLnogsrttoobcekattse1orL,lufvtriooomlnumiSsiepgtrrmiecap.aflraesdkbaynd 9.0 Sample Handling 9.1 9.2 pRdaOurienletuccopotevaerridtdaahltstesiiaomusmnanepmstslihelpoesltfeehmtsienohaitrtiyaimlvaboleeegpbobkreoefeeopapnkantr.adialnityliuscoiotnsel.,dds,setttho-euryapg,meaan(yed.bgs.eamaapnppalreloyaxzlieimqduavotietailnyLgC1/a-/5nMaSlCy.)siiAsnlotcenrrinamasptai-vmceaplpylpe,etdhe 10.0 Quality Control__________________________________________________ 10.1 10.2 pmSSohaeimaankstp)uelrieFenRlomaefsuptkhlltieSicpapalmerteerpcse.ilpseilPoiTcrneraptioepanslriesc(2aaamtnoedprsl.maenopSarrleeeyt)pzuateopraapeltliraooscnvah.midtepeslteasvme(sefrsaoesmluirneeatorcifhptlhtieecsapttreveetcosisspeiolronfvooirdneeaacanhaltyimsise. 10.3 Q110u0..a33l..i12tyMbpvcdcfSCooorleeoaoresontnlnecstvpntthceaakeeottldmmonrssiaudsostiiwnrinnlcBbebyaaiBa.ltlltterihaaiilrnooannicstennnoekktdrksn..oautttcSfmSahAsctemurarhentobumneiuusenatptgpsdaalaiohllnqnetaltchuvcstsfhore.oe.ooen,ntuuTttoorsa(ghntasmfhhm)eltyoihtunesueensoastseolttdatvidhivomteleedenunspsutsttoislraoebesrimnnlulpbagbwprasnesloctiketphtklahvaeipgnsoerrrcsauneuoeatttpusimoiea(tnsiendrpd.saaelpttte.dioirnsdompoutdenercebdoereptsfpchdttreuahaaourmrnnrecraoenoceetusecislno)gseatt.nshdosa.oipTmntruhreyhoteeceacpttthlseomhyuessrserease,teiennhbaaatotlnileendyrdseyztteod 11.0 Calibration and Standarization ___________ ;____________________ 1111..12 AcTahllleibecrqoautmeipdpmopuernniotdrsutsooefdui,snestue(crdehasitalysm,tuhwseeteabknelaysly,tateintccda.al)rbdaasizlasepndeccaeicfacineoddrdaiinnugtiotstmosatltaaenbddoadraridltuootreypre,srpsahetiocniufglidcpabrtoieocneds.ure. ETS-8-172.1 Solubility Test: Shake Flask Method Page 4 of 11 Page 30 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 11.3 tAesltl ssuambsptalenscea,naanlydzaedfiwxeildl bame oruunntaogafiinnstteransatlasntdaanrddarcdu.rve containing varying amounts of 12.0 Calibration and Standarization ______________________________________________ 12.1 pP1111r2222re.e...1p111p...a.1234arraaPwtWbroVscAtioetceenroihidpreneeosnaeidaepiutncncegrawaahsthinohtrhftloioeualbteet1yohfrengtv2akuaetTsdecee.sitt1saoensshtaot(.ruutnse2eeEdltsbbfsduesiTiwpoeVstzttr(ite)lmSes(inoaev.ctuAd-nonshei8btsfcttpnhei-amsetecrta1a:ttlea.cot7twvlponhse0rtoRaacoehma.tls0rehlesuetave)treekcmit.enensiofntnoetitteraovotndAssrwsweuetas)ahitnbvhulliotallsmeeantrvtsboderdaeeseeetanisbedqstdocdleasmuireteogfieadfplvoolresonivaearstrrgdevenlsiveabndoidocendmoglebosptdvon.essnadekemtetrcedr.ltroeniiovc(nacnsreaatlite.etttlrigihilasnotey.ee.tsnets1u,dhsdIt5ntefeoshttnmnhuipnelsoabrrLittnetesh.hpytlfpee.aaiot)mhonrr.deteleciiRxyecnecstapleahoiemarcrrenosneyopcpddwarlseyderreovneleieolastgcupranllaolhburmeetrtwimidlsponieeetlneteyinheghtaedh,atestsd 12.1.5 12.1.6 12.1.7 tRPatPbsit(Shhneaadlrreeseeatfmeedapotnmppitlsprtsekaa3tmitiulusr"orh;neetbedaneiasspvmytattanitchrheloamdeau(sernwneppmespD.cs,eegedlteo)leatio.esthglsyaaewsu.hetasnscht3tsatidrpD.e,otivDeeb-tntaerhRreeasysdedsysoeslteo,epnsuRsv1llo(nucs,e1selrbdvs-,)paiRsiebe-sr4leRrnieee;ltdtdsp.ye1.eDpp)2isM1o,nAa.c,12ntyrhin.,-1si25xRbeida2,./beRnes.swl1dhpdToee.ar1lphi2-afvkn-4Reo,pe1es;r1ean2etttap2nht.eh1nt.dues1he3.dtt4..r-ci3sveRlDanaiAeepzwemaisenpltyswisedpete3os3h,lil,tet;toRaiiht,vnmDuonetecttdhpaeaeslteusyp4snthehedstea2al.eeuens,ltsroedstet-ahtnsRrcultecgeaoedosbdpmwtyunheabtlpien1yats,ou(hc"toa-umatmRttfnnhbbmeiedceenepte,tihriwnnt.2aoiiaaen,mdtledauunnrlmedathb)o-eefl 12.2 E1111122222q.....u22222.i....132l45ibPTATAac2tsTsrhupop6lahhhtfeabpentteeecaeiesrtsCoepaotrstdtoauencapxalan(scbtmuriblr/tceoomelmteopeinvsxfcooualiteiosleafxnrttmsaaeirsrtis2fbdemilhnauesya4eegttltgrpelvhsh3eheatbllieee0ydoaetsesnisrsiuhaot2"tbe.wpcrCanD4vlstnklyeueaashoeoesactcynownefslel2upeeedltttrrlaoe,hqmsResrCmieu,n.aeoaeidpnftlanyaeopiyesInbsuutlrfsbdtrh"fatrrmeaoaset,erttuburoie"aiinrroclbtsDddeeoaenstsdi)taillttvietdluaeayfneeednetotmslgiscf,r2ot(s(Rpoe2ah0nesarete0uol.bamrspa,bronaC0iSa2astudzc0u-tter"oto2ia0erse,onnna6eor"nRtsscle2aDeevieCmi4Cldncse)aieFtv,nohsyisiritovcnuoarl.fsene,obosutRanudpnlrrn1etc:eemapr2kcpoitspe.feht3pr3rpeutnbroie"drgeotfieo,,oteetdodahxara.ltcfneitnhfmooiaduensnapraiec"dtsdtptanuhDaederisbemolinayutoraxiyiprtnofsie1o1lmagnte,rhhmsRasateusoletepuefueshtpfltnultreii4yt)tcbgoi."ielh2e..0nt preparation. . ETS-8-172.1 Solubility Test: Shake Flask Method Page 5 of 11 Page 31 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 12.2.6 12.2.7 ApA"e1Dqu2ttul.aala2ieyppl.di33ppb-,rr(r1Roola2axext.bepii2dmme2.l5"aeaa.,sdttee"d"llDyyeDsa74acy82ry3i2bh,hR,eooReduuperrissp3n,"lo"t1,hf,2aei"n.n2Dfdc.i3uan"-yabD1l2a2at,sR.iye2o3te.n5p,oR.t2fiem"sp,ae4"m,"Dtp)halaeeyns2sd,eiRsceoepqpnuu3dlill"eisb,dearta(noltdaefbd"teeDalsesatdydv2e"es,DsRcsareeiylpbs34em,d"R)aieanypnbld"e, 12.3 S111111122a22222..m....33.33333..p.1...2.63547leAtlg11O1UUttTLmtssceoSaphhhl222uuoqlybpaaoasseeeer..i.biunss3e3mb2qiitteltnnsseaacaarha..e.uahp2t25prggbleppnlacaoyoeva..)lnltppanrn12tee.ttfpaepoerthbesaiftlhrrocsrhmtriysalioqooePdeSdhTatneealatpoeottwhl,hupplsn)irpeatiasihieflolsef.iociedtairroutamo-ilutooeloewtiiialscrctnlittuaaectlacnUrpsleyobelbpeeaeuutts)rotnbsattttlrpeesrlfm.stthbtiooauteanar,soaeitoecoottlesdaionvttluecrmisaialaeiyoafntocilebztieitcoolsllhdluthantalotuaa)einieeufuilnyueelsq/qtoancvluklrtsstriaisotytauulrauditoinit(afe)iahstyaolatantiosoa.ploo.untltveioeztselnaioyufcnrcattsri.sennudeosisoeisafrdasann1n.adb,iaar,iatlnmmimnntsmgo:ectlsnit.l1rva.Dteuautifeaafpadaoa0naasnditbkrattyunllaaetnodhereieenoeitpegwmrqecor,bhfLealyorieciutieetncateeippnCoa,utohohtodhde(ewlhtlrttosir/eeetomsdstteaMgdaaobo.thittoqgksuehtmh(caittfefhtsoiSfnu.oateeoekh.ofotopelitpisrahnnoaeeunrer.lavttlapoueeesehdurtegimcsesabipissdsntaierdeooadapqilds.ytrlapouriamnnte.iiouasinsliobplnustrn,souaxieoispusieav.ttlotribiltltaotltobtmmtaipuahnedtrNniatvvlmemniottyeieataniiiiooilsdnaoodtntyaueacpgottifeal.nnalretypotrstflr,bsignth:eyi,nodhbaoetbes(idlethcnnmeeyime3awfaarmcee.stgtkegtrcepednnuhendcpiio.ostanlrtselenngoheriatsfnttc1cnpa/gac:emriwstmcs.eueooitre5husufiesypcxrmintnoeuLebvnsntbaimtcselnagpsreesgrtsse/etacrereLetntoaotcnoayoacaraidtdrmntepttttfnnnpf3iireeiteaonaoidoopccov0amdnntsgonelncealt0.ptgeytiurot`rse0ostotoieseipthsnorupsneaosnfnttrnedycsedettlgotsagb,eiesirvtln,tnaslpiutlydne/yeeanedtkmmgyistpusnsgeteinrtltoearnstpLaaxaeneiobmbftl(nnpcoowefetitltdyeei.reaedtfhpenilhatston.leteroteiortdnog 13.0 Data Analysis and Calculations__________________________________________ 13.1 13.2 13.3 bAeMsSSaqyatcmaeumctnaahepnpdteslislaesoernwnsdwuiwwmidtllolelihblbvbclieceiaebrahlcetcoqiaiuofusallncaniabnsunatadeltlwsaiyifevstziiedtlieealddddnoubbdnaaveyaglitcrahaeadaiendanldctdsiciuentitainvldealagiiistabvs.etttrihdiadaoentuunidaois.nalinndrTedgcinhvutceeiriuditvbtirueehvua.seeilrl.(TtenMnih)nteibictfaeiruemoinnsscogoatufinlotnednEst sdoxcitcfovhetniaeldtnsaitni3ngso0sur:tbthMhseetiarcfnerocsoluesloloitwnfatnitnthgesum ETS-8-172.1 Solubility Test: Shake Flask Method Page 6 of 11 Page 32 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 13.4 cSSawaalmmchuepprlllaeeet:eRpdrPeuDABcsi=i=swniogasitlnvaltehnwbredaeiaglflcoredablAloleocd/fuwBerselviaapinmXtaoegtrdpite1oleueq0ndssu0ioaan=sftgiao%SvtnaheR:merSapfDgoleelld(o%owsrRai%mnSgCDplVeeqs)u. aStioamn:ple precision will be where: BA|A==-ccBoonn|cc/e(e(nnAttrr+aaBttiioo)/nn2)oo=ffsSfiearcsmotnpredleprlReicpPalDitceate . 13.5 vwEqauxirtecihsalutb9isol0ienwo%a"nhbQceoloerofenbda:fsnaiRTGQedtroaoaaeavbunnbppestcge=oldlreeieiv.etn"=e1h(rdtse=tdICemofeadgtratQaiaitafyltapfoepbe/sebrroprlrasieeriraennnet1rgatcofveodbemetrehdboalReeoyf>twhtewbhQjieegeeftcohepadtrnbeaiooQruttrafhnlot.aleaortobemwqfudueOl,eeadtnsuthetdbteidyolnoinevuftarahttbliheVulleieezdasdilpan)uato.gaetiasnpD:stoeiaixtnn.otdnCmt'hsaaelQycnu-bTeleaaetrreseet.jstehtcTevthaeledue. oNbsuemrvbaetrioonfs Qtabulated 9R0a%ngCeonfidence 3 0.886 4 0.679 5 0.557 14.0 Data Analysis and Calculations 14.1 o(tPoahobnurerdvtelricqieioeinulsuraceisvotlsiutanovidloueueonteplfarieeeebdrrsxlacuseite.sladnttss.Tat,tohdSasefiaafptmmfQhoeeip-prnTellsteenet.acsadtteDvia)smetotaoricaacfmuyga<melubase1eatnn5nahat%dplatypp.hvsrleeiiNesencadowoipnstniieo-to-crhcnceootxemhimncselptpurlrfelideii-anaelcnanaaqttltliucdvrdeueaeasslttauatsaittlomeatosndnn.uadasbdatnlraebddtaedrdeaseeputvvaomairpalmtutoeiaiodantrnewtyds(.i%stfhhoIReorfeuSattnsD,) 14.1.1 14.1.2 mTrddcaafSeiovnaaahnepnedttmeataaorf,ltarip%pihadrtgsloepeeetRe>pihpnndrSoa1elcetaynrD5esptdtd,,%aetlahbidaetRdceaepxRaodP.tpctQweSaeDllsuty-Dea%tdne.fet,eohnosReTterttvsShtthmDhaoheDelaeeiuosk'xresaarueeotetmmtsentmlfhhilp'ateaoseahlirsueineQcnkdlifrdsint-arinhTtgtosbegurehmeersmsotiehwat<u.f.a,vu1olktdaIIr5helftvf%uheaattfngeehhll.asurreeteseIhdfkeqosfoeasuu.twrthdetaflaIisaeoitfcntethriaaanrooitlvonhcvnsueeueaatdr1tlllbatai5aumielgt%tmeearieao.ievdpyosnpaaoIsfrntloifeautnoaihjtentpntehes.tdocbisscstieTecanhacodaumatnrlsliicqwlpbtseueulebdiedrleteaiheiisatstnxtruec9iiicsoptsa0tlhenhrlu%ndiedaecdoebtaetodltdee ETS-8-172.1 Solubility Test: Shake Flask Method Page 7 of 11 Page 33 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 vtiima ethpeoiQnt-.TeInstc,luthdeenjuthsteifnicoant-icoonmfpolriadnrot psphiankge tfhlaesskhdakateafilsasnkot(et.og.beq-utessetdrefosur ltthse). 14.1.3 bdeffAlireaanrntsoanadklre.fscfmoioenrelsauptslhbaoloyirslyds,iti.tytbho.lIeefrIe%tofhpuRtiehtsalSritceeDrterhistbc.eeeoreTtinwanhsteierisreceeeunnttoaiettvhgsemetr,etteeoihtmar,rbereileetpe-moddtiaiianmlyyutssetbesdie/hnrooenten-uersoclvhdetaosbalossgeatrar<seyrae1emt5worep%irqlteehu-sfiieonrtveorad1tlc5huth%oeaets,rceehiktpathkfmoeoerartythe 14.2 hLstiiagmnhdeitasrtodQfuQusaueldaitnyintCifthiocenatctriaoollnibB.rlFaatoniorkn.thcisursvtuedcyo,ntthaeinLinOgQmwoirlel tbheaneqtuwailcteoththeealroewaecsotucnatlsiborfatthioen 14.3 b(Lc(QtpolOeaurnsonQattvkala.iiistndnIypafesrldbCiyigaottocnehrnkiatOftogtircrRtothoahlneuienBrtnetcbdleaaaarllnnrceiebkkavrlgsnea:rsoltsotiMaoouonntnefhddtsaeahtnrrlaoedainvdnladyednaatliesarncdlaodeytxcftoSeuiars)orsntvlsatviehhnleyaaanttltrhelte)eebB.icetilhlnealeieantrsinkast,hlttsemhhaaesmenatdmhpa5oltp0edal%se.mbsloTaaofynhrtkebthsheel,eebaavicruneectlsaetsorpucuftobemausdneenaqntlsutyetoenftthe 15.0 Pollution prevention and Waste Management 15.1 bDrioskpeonsegolafsssacmopnlteaiwnearsstetobydipsplaocsiengofinglhaisgshpoipreltotews.BTU containers as appropriate. Use 16.0 Records 1166..12 FSiilglnoauntdaldlaatpeparlolporbiasteervsaatmiopnlse apnredpcaaralctuiolantiwonosrk. sheets. 17.0 Attachments 17.1 Attachment A-Example Sample Preparation Worksheet. 18.0 References 18.1 18.2 UToO(GfrnrageCintnahesnedeprimozaSatriotttcairaaotelnCnssd.ofEloTWunrrmvaEainntrcseooMfrnnoSmoermotmehlnauoicttbdiaoi)Cll.niPotPyTroropee-tOvesetrecEanGttCitiouioDonindnAGe,alnPgiundeeiednsDsteci.lyceiE.ivndePeOelAosP1p0Pa7m5nT1:dSe2pn-Tp8Cto..3-xO019i.-6cE77-8CS0, 64uDA02bd:sGWotauppaniptdtec.edeer1lsiS:1-n19oFe79lau5f,toeb1r,i9lTi9tey6sting 18.3 UConliutemdnSEtaltuetsioEnnMvireothnomde;nStahlaPkeroFtelacstikonMAetgheondc.yP.rOevPePnTtiSon8,3P0e.7st8i4ci0deWsaatnedr SToolxuibcility: Solubility TEesTt:SS-8h-a1k7e2F.1lask Method Page 8 of 11 Page 34 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 18.4 18.5 18.6 NpBHESSC1pu9uTuoaa.6bbtrrmSrre3ss1ei-tpat;s-l8aaual,1Pnn-anD21acoc,y7g,eeMaf1:0senSi9:.sanNi0t9eFra,1Vely6an7SwCtda-Geo3ra.,lYii,ruobTdSaobubsrntrisaoalkdHnitnS,tissayTsop1.tn-li9SoT2vdc8rcs7ebht2.rn.oee;atoeQsnTpkn.dru7eT9aT0a1ner-t;sam7titUn1t:eas..AnftSiotpv.roepGmfrCooaOxvhtiueieomtrmnlniaeimTctreasee.slnStAtoEGnPlxuarupbilienydirlsteiiiitnlmsyi.gneDenO4sett.fhatfeEliercSdPmet.A:;aitnWi7Was1tt.iiHa2cos-s.nhC,Fio-nr9Nfeg6eaat-omt0Tino4ae,n1nsDa:tal.Cnd., 19.0 A ffected D ocum ents __________________ ___________ ;____________ 19.1 ESTubSs-t8a-n1c7e0i.n0,V"aSroioluubsilSitoylvSecnrtese."n Test: Approximate Solubility Determination of a Test 20.0 R evisions RNeuvmi1sbioenr FSSSSanieeeexdccccettttsiiiidooooonnnntlhv3e111e..4n26i2.n.t,,32cbrr,.o5elema,rfmnreaoekronrcesvetn.oenccpdleutesi"maoitrnnbolatyReeslrrepdihnnaeeiagscgfloiihnofsn-ietfcsadFpsntoeeetdhcresatetdRirodsaecuncvebbscnilsseat1tirpnao3itknf.na5u"cngetcfhasretorwiocmourenirgtdesehetrrefi1eoipnm4nwi.3tofi.avooserndams.deedctethidoo.nd. 0R3eD-v2ai7st-ie0o1n ETS-8-172.1 Solubility Test: Shake Flask Method Page 9 of 11 Page 35 of 171 BACK TO MAIN ATTACHMENTA: Example Sample Preparation Sheet (page 1 of2). Temperature of Study: c. 3 M E nvironm ental Laboratory S o lub ility Test: Shake F lask M ethod Sample preparation worksheet Studv # Analvstisl: Test Substance: Test Solvent: ID#: Source: ID#: Date: Test Vessel. 15m! centrifuge tube/Other(spedfy): solvenLctgnslly;____________ q/ml Source: W as the s o lu b ility scre e n te s t p e rfo rm e d p r io r to s ta rt? Y /N I f so, w h a t is the a p p ro x im a te c o n c e n tra tio n ? u/m l Balance ID: Thermometer ID: Room Temp: SFM vials ID#: "samDlelD" = Sample Description Total mass weight test substance (solute + solvent) added: added: internal Standard addition ________uL/ mis soin IS added to dilution factor samplelD-1.1.1 thru -1.1.4 Day1, Smp1 1 samplelD-1.2.1 thru -1.2.4 Day1,Smp2 1 sample ID-1.3.1 thru -1.3.4 Day1, Smp3 1 samplelD-1.4.1 th ru -1.4.4 Day1, Smp4 blank ' none added 1 samplelD-2.1.1 thru -2.1.4 Day2, Smp1 1 samplelD-2.2.1 thru -2.2.4 Day2, Smp2 1 samplelD-2.3.1 thru -2.3.4 Day2, Smp3 1 samplelD-2.4.1 thru -2.4.4 Day2, Smp4 blank none added 1 samplelD-3.1.1 thru -3.1.4 Day3, Smp1 1 samplelD-3.2.1 thru -3.2.4 Day3, Smp2 1 samplelD-3.3.1 thru -3.3.4 Day3, Smp3 1 samplelD-3.4.1 thru -3.4.4 Day3, Smp4 blank none added 1 Date/Time: Initials: Test Vessels sealed w/ tape? Y/N Test Vessels shaken/vortex-mixed? Y/N Test vessels placed on orbital incubator? Y/N Incubator ID: _ Speed: 11nternal Standard: Int. Std. Cone.: rpm Initial Temperature: __ C Date/Time/lnitlals: Observations/Comments: ID # :. jjg/ml C Day 1: Four "Day 1" samples are pulled and allowed to be placed in a temperature controlled environment for approx. 24 hours with no agitation. Date/Time/initiais: Location of samples:_______________________________________ Temperature of environment:________________!C Thermometer ID:________ . Visual observations: 3M Environmental Laboratory Project # E01-0768 Page 36 of 171 ETS-8-172.1 Solubility Test: Shake Flask Method Page 10 of 11 BACK TO MAIN ATTACHMENTA CONTINUED (page 2 of2). Day 2: Four "Day 2" samples are pulled and allowed to be placed in a temperature controlled environment for approx. 24 hours with no agitation. Location of samples: Visual observations: _ _ _ ^ Temperature of environment _ Thermometer ID: Date/Time/initiais: ______________ "Day 1" Test Vessels Centrifuged: Cent. ID: Visual observations: RPM or RCF readout: duration: min.__________________ Date/Time/inttiais: -Four aliquots from each of the four samples are to be made into glass/plastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution 1:______ with methanol. Methanol T N -A ______________________ Daterrime/initiais: Additional dilutions: Dilution factor (test solutlon:methanol): 1:___________ X's how many dilutions:_____________ =final dilution factor 1:________________ . f Diluter ID used:________________________ Amounts used:_________________ uL methanol,__________________________ ul samples -Store samples and extracts in a cooler at until time of analysis. Cooler ID :________________Cooler Temp:______________ ! Date/rime/initiais: 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:_______ _____ Visual observations: Temperature of environment Thermometer id : Date/Time/lnitials: ______________ "Day 2" Test Vessels Centrifuged: Cent. ID: Visual observations: RPM or RCF readout: duration: min. Date/Time/lnitials: -Four aliquots from each of the four replicates are to be made into glass/plastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution 1: with methanol. Methanol TN -A . Additional dilutions: Dilution factor ftest solution:methanol): 1: X's how manv dilutions: =final dilution factor: 1: ,, Diluter ID used: Amounts used: uL methanol. -Store samples and extracts in a cooler at until time of analysis. Cooler ID: Cooler Temp: C Date/Time/lnitials: . ul samoles Date/Time/iniiiais: Day 4: At approx. 24 hours of equilibration, the "Day 3" samples are to be aliquoted/extracted. Environment Temp.:______________ ! Therm. ID:__________________ Test Vessels Centrifuged: Cent. ID:____________________ RPM or RCF readout________ ,_______ duration:_______________ min. Date/Time/lnitials: Visual observations: . -Four aliquots from each of the four samples are to be made into glass/plastic autovials (also, check autovials for correct labeling). Yes/No -Immediately dilute the solution 1:______ with methanol. Methanol TN-A'______________________ Daterrime/initiais: Additional dilutions: Dilution factor (test solution:methanol): 1:___________ X's how many dilutions:_____________ =final dilution factor: 1:________________ . t Diluter ID used:________________________Amounts used:_________________ uL methanol.__________________________ ul samples -Store samples and extracts in a cooler at until time of analysis. Cooler ID :________________Cooler Temp:______________ DatarTime/iniiiais: 3M Environmental Laboratory Project # E01-0768 Page 37 of 171 ETS-8-172.1 Solubility Test: Shake Flask Method Page 11 of 11 3M Environmental Laboratory BACK TO MAIN 3M Environmental Laboratory Project #E01 -0768 Method Analysis of P otassium Perfluorooctanesulfonate or Other Fluorochemicals in W aste Stream or W ater Extracts Using H PLC-Electrospray/M ass Spectrometry Method Number: ETS-8-155.0 Adoption Date: ((jfofao Author: Mark L. Anderson, Mark E. Ellefson Revision Date: Approved By: UWAsnoianrldgys9Hi7sPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-l1u5o5r.o0chemicals in Waste Stream or Water ExtraPcatsge 1of 9 Page 38 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 1.0 Scope and Application_____________________________________________________ 1.1 eSlceocptreo:spTrahyis/mmaestshsopdecdtersocmriebtersy.the analysis ofwaste stream or water extracts using HPLC1.2 Applicable Compounds: Fluorochemicals or other electrospray ionizable compounds. 1.3 Matrices: Tap water, ground water, wastewater and other aqueous solutions. 2.0 Summary of M ethod________________________________________________________ 2.1 pTpEcoaeShrrmi/ftsMilpcumoSuoul)era.onthrodToccsdohteamedxneatporsnoaacautcrelntiybed(sdeP,issFfstriuOhsoceAmphea)aw,rnfsmaoalttryh/emzseri,e=spdueo4srbf1ifnylf3ulg.tuohoHreorPomoLccahtCsaes-nmeesliseeculcaeltlfcrsootionsorpantroeaotyhf(PeamrFsaOeisnlSsegc)slteparoneiosciopntrnroac,mhymaiero/tazrncyi=tze(aH4rbi9sPl9etLicoCro-fa 3.0 Definitions__________________________________________________________________ 3.1 uilTsoiynmhnsAdetiieerzttmemrmadtaoioaotsvsonnppa:drchbaEuoyeylutre,uhmicectetit)rrlcP.oi.czrsoiepTnmsrghasmeyuaeriIvoerocannIirioaiizzelnalatyiyttziioaooavnntfiasoi(ionElnauStbr(hIclAe)ee,sPsLeA,ICp)pt:mrr/MooTobchSseepesssh,sMyeeassrniticeodcrmcoPicnsmruteaerasslrsslfsoauawtcrPeealsaftcom.thfroeoTvmrshamperihcisLoeaeurlCiisIcnZomcpnslreuiiezntdshagestoliuebdorusneqtuo((aaiAf.rdeePr.,cunIpno)oo,tlte 3.2 pTrheesEsseulerdecr,torwpolhseeptsrreaabyryeIipoornnosidziuanctiesodonlbu(ytEiotShn,eaEarSpepIt)rl:iacnAastfimeornerteohdoftdaosotthfroieongngaizsealpetihcoatnrsiecpaevlrifafoietrilmnd.yedchaatragtemdodsrpohpelreitcs. 3.3 EseSle/MMctiSavsesslyysSdtpeimesccsrtiramoremineeaqtteuedrip(bpMyedmSw)a:siTsthhtoaecsPhilnaagtrfgloeerqmrautaLidoCru(Zmpao/nzle)damontahdsessruscbeoslemecqmtuiveeenrctdliyaeltdleyecttmeocra.tneudIo.fancstuarreed 3.4 ucpdsospyotainifsrnsllfatiyseeCezyirmewnaeocsgpnsinotea,tvthm,rhe"etttrsupZhncoiroe.m-teu)isn..omgpielnhrnaOIeaantrtaysthlhs"totvayheodnscserr.tsodteccuZnomocoof-fmonoussonvrspm(mpveirp.eeneaeaarnrty.tatic,ithotoiiZipoawnnolrn-a.nlaoslay,ypblTcmrcieocahlnoeanyeianmtfnchonsutoppereifnmmorarcagfncaopay,tetuuocniaeonrnetnmesnet:ddeniaTrittmEtrtsheeeiSaledsaen/irMcnMaofetrittrmeoScioccnmoderosamodeymnt.msphcdptaeeaeiTatrmsipethasbicrrosbloePteullmbelytgwaheawhtaeifyittoisthtshhtrhaohmeasmrevootcheneLmco.oeoCnsegniafHZmooeingontoisahuwlaytpaerhlseearrtetvrteofZritemeo,u-rtanrsb,htepuueZi,rsrt-aaeysft.er 3.5 Lv(MeCrasZMisosMnaLssay.ssnsLAxsylNplneTvxcetUrSrsoosimoefntrew'stseaaGrrr.eeu:CisdSiuemyrrosieltraenrMmt.lyisFcoMroofrtamwmssaaoLsrresyenPddxeleashttiafgaoinslrsemWdseiLfenoCdtrhoZtewhUemsssa9epn5re'ucsaainGlfidscupWiodepceiine)f.rdiacotwtioosntNhoeTfiM4n.s0itcrruommeansts AUnsianlgysHisPoLfCP-oEtalescstiruomspPraeyrf/lMuoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes2 of 9 Page 39 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 4.0 Warnings and Cautions_____________________________________________________ 4.1 Health and Safety Warnings: 4.1.1 Uemseplcoayustiaonvowltiatghethoefavpopltraogxeimcaabtleelsyf5o0r0t0heVporlotsb.e. When engaged, the probe 4.1.2 Wanhdeenyehwanedarl.ing samples or solvents wear appropriate protective clothing, gloves, 4.2 Cautions: 4.2.1 bOapcekrparteesssoulrveeenxtcpeuemdsp4s0b0elboawr,athbeacHkPp1re1s0s0urweilolfi4n0it0iabtearau(5to8m00atpicsi)s.huItfdtohwen. 4.2.2 Do not run solvent pumps to dryness. 5.0 Interferences________________________ ;______________________________ 5.1 Tstoormagineiomriazneyinptaerrfteorefnincsetsruwmheenntaantiaolnyztihnagt csaommpelsesin, Tcoefnltoanctshwoiuthldthneotsabme upsleedorfoerxstraamctp.le 66..10 EqmEuqoiudpiimpfimecanetntiot_n_lis_s_tie_nd_t_hb_ee_l_roa_ww__m_d_aa_yta_b_ae_s_mm__oe_dt_hi_foi_ed_d_d_ien_v_io_ar_tdi_oe_nr_st_.o__o_p_t_im__iz_e__t_h_e__sy_s_t_e_m__. _D__o_c_u_m__e_n_t any 6.1.1 MionicizroamtioansssPoularctfeo.rm LCZ Mass Spectrometer equipped with an electrospray 6.1.2 HanPd1a1u0t0osloamwppluerls.e solvent pumping system, solvent degasser, column compartment, 7.0 Supplies and M aterials_____________________________________________________ 7.1 Supplies 7.1.1 Hsyisgthempu.)r.ity grade nitrogen gas regulated to approximately 100 psi (or house air 7.1.2 HsizPeL)Coraneaqluyitviaclaelnct.olumn, such as a Betasil C18 column (50x2mm, 5 pm particle 7.1.3 Capped autovials or capped 15 mL centrifuge tubes. AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes3 of9 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 8.0 Reagents and Standards 8.1 Reagents ______ ,_______________________________________ 8.1.1 Methanol, HPLC grade or equivalent. 8.1.2 wMveainltldeir-oQro.TMr eqwuaivtearle(nAtS, TanMd tmypaeyIb)e, aplrlowviadteedr ubsyead Minitlhlii-sQmTeOthCodPlsuhsousyldstbeemMorilloit-hQeTMr 8.1.3 Ammonium acetate, reagent grade or equivalent. 8.1.3.1 When preparing different amounts than those listed, adjust accordingly. 8.1.3.2 2aaSpm.t0opmrrmeoopManrtiiuaraomtmeommvaocoeltnuetaimmutempe.eoraPfacoMteuutraireltlie.in-stQoolwauta2ito0en0r:,0WmLiexvigouhlnutamiplepatrlrolicxsoifmllaidasskte,alyared0dd.3its0hs0eolgved. 8.2 Calibration Standards 8.2.1 Tstyapnidcaarldlystawreopmreepthaoreddbdlaunrkinsg(Mthiellsi-aQmpwlaeteexr)t,ratwctoiomnaptrroixcebdluarnek.s, and solvent 9.0 Sample Handling__________________________________________________ 9.1 tSutbaensduarndtislaanndalysasims.ple extracts are stored in capped autovials or capped 15 mL centrifuge 9.2 Iafpapnroalxyismisatweliyll4beCdeulanytielda,nsatalynsdeasrdcasnanbde psaemrfoprlme eedx.tracts may be refrigerated at 10.0 Quality Control_________________________________________________ 10.1 Solvent Blanks, Method Blanks and Matrix Blanks 10.1.1 Seaoclvhensatmblpalneksse,tmtoetdheotedrbmlainneksc,oanntadmminaatrtiixonbloarnkcasraryreovperre.pared and analyzed with 10.1.2 Analyze a method blank and a matrix blank prior to each calibration curve. 10.2 Matrix Spikes 10.2.1 Meffaetcrtixonsptihkeesreacroevperreypeafrfeidcifeonrcyea.ch sample set and analyzed to determine the matrix 10.2.2 Massaotrciixatsepdikweitdhutphliecaatneaslyasries.prepared periodically to measure the precision 10.2.3 Athneaolyrizgeinthalesmamatprilex.spike and matrix spike duplicate (ifprepared) in the same run as 10.2.4 oMfathtreixinsiptiikalecaanldibmraatitorinxcsuprivkee odrupshliocautledcboenpcreenptraarteidonast s1h.5o-u5ldtifmalelsinthteheenmdiodg-ernanogues AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfoetnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes4 of9 Page 41 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 tchoencineinttiraaltcioanliborfatthioenacnuarlvyetei.feSxptirkeemceolnycleonwtrlaetvioenlssasrheoeuxldpefcatleldi.n the low-range of 10.3 Continuing Calibration Verifications 10.3.1 aCcocnutriancuyinogftchaelibcraalitbiornatvioenrifciucravteio.ns (CCV) are analyzed to verily the continued 10.3.2 oAfnoanlyezpeearmsaimd-pralengseet.calibration standard after everytenth sample, with a minimum 10.4 Internal Standard/Surrogate Standard 10.4.1 cwtAahoirnenlelcleianfexattntileroltrarnnwacsattiihiltoohisnpnitnaobpnterfhdottweahcreemedseasin(dnIaSa-tnrhl)aydemntebrgaaeeoytfifooobrifneeotthuafeensraeeancsdlaaytl.ltsyioibtTserq.haurteeaiosnIpnStiofcsnyuhsrtoevhueetlo.dtaITbSreghreesetpsIaSipknoesanhdlsyoeatuetalsadnbndbyeaaemaskdtonaduobenwlditsnathhfitanetgr 10.4.2 tAaqhnuedsauncartanirltoaiabgltyriaavsttieeislo.ysnteTacvnhuaderlavusreaud.tremrothagyeatbeenestuhirsoeeudaldnfaoblryetqsiucpaaikllieptdyrotccooenfdaturlolrelw.iintTchhliunedtsihunergrlosoagwmattpeoliemspuirdse-eprdaanrtaogteioonf 11.0 Calibration and Standardization__________________________________ 11.1 Afssihttano(nauyldly=adzrendaxotch2tueb+rvesbetfaxsonrm+dcaeacrdy)dutbhcseruiopnrvulgoegtMshtepadzrseisborLoyr.yltnoinxaeonarrdrofetoghlreleorswssuiinoitgnabe(ylaec=hsomsfetxwt +oarfebe.)xwtTraehciegtshc.taelTdibhr1ea/txai,ovonerrcaqugurevaedosrfattwico 11.2 pIfrethpearceaalibnreawtiosntacnudravreddcouersveno(itfmneeceetsascacreyp)taanndcerecarnitaelryizaep.erform routine maintenance or 11.3 uFpachtospoitgenebrhmstpthioucspetorti1plinnon0ocgw0gse0eontesoftpnrtopaqhdtbfueio)oaa.scnfntctatThsuinttheraadaintcsacedarywdaaliwsrpibdlprlfhsarrre.ootenimxodiqnum5ucceaaputnpierntvlbiyaetactro1tcai0unt1hrgp0aep0clrboyptwhopaatbfltnearrivnabteahtulhlestyeetfordeuf,tlthlaoganrealnaninlneytgehrteaaee.tr,efriuEtealxgmlcarraeamalsynipbsgbilroeeea:ntoniwowfenctehheiceesgunshcratuvriryenvgteoo(5f 12.0 Procedures________________________________________________________________ 12.1 Acquisition Set up . 12.1.1 Set up the sample list. 12.1.1.1 iaoeAnnnnssddttsrhitoughefmnetsheaadenmastylaei(ms(TdtT.paf0yloe0,r1ulTi0sseu1tc2fikinlfeceorrnr)ea,aOmtshcienetougybseleienartrgt1e(t2r0hs,0e2of0ffoi0trrhs0t2e).0lea0tlI0tpfe)hmr,aotbohfereetthmstehtaonarnnattimhnogen(e0wo4lfiittsfhhoteriAsAmaptratidhl)ee, AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OEtThSe-r8F-l1u5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes5 of 9 Page 42 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 111222...111...111...234 ATAysspssiieggnninaasnammHepPthlLeoCddep(sMrcorSgip)ratfimiolen.(sInalnedt vfiilael).position numbers. 12.1.2 ttDTsohpoAee4ccT9Str9rAIeRoaomtsAre.eCoatSetQhmarUevhereIetShaaapoIdcTpdiqnIr,uOogcipsslNiirctaiiakfnootdneornsmmaedmaledestecihsttteoihosSdo.n.IdaRAlSi.niefnSeutfhelotlethrsmeiAocMaanctnqiiziouciansirtso.iuiomtsinouanamslslcoyModnceatoraslosslelLacpyptaenpndxreoiGlnptUrhaiadIeDtndeiEmtainoTandsOstmoass 12.1.3 Tstyapnidcaarldlys.the analytical batch run sequence begins and ends with a set ofsolvent 12.1.4 peSvoaesmsryipbltleeesnaatnhreaslaaymnteaplcyleaz.rerdySowovlievtreh.nat bcolanntkinsusihnogucladlibberaatnioanlyvzeerdifpicearitoiodnic(aCllCyVto) minojencitteodr afoftrer 12.2 Using the Autosampler/Column Heater 12.2.1 PSleaccteiosnam12p.l1e.1v.ials into the sample tray according to the sample list prepared in 12.2.2 Aswttiatcchhinthgevparlovpee,rmaankaelystuicraeltchoaltutmhentiunbtihnegcisolruumnntohtehaetearpcpormopprairattme epnotr.ts.Ifusing the 12.3 Using the Inlet Editor 12.1.1 ciSnosenttsr-uiudmperteshneatplHopgProb1op1or0ik0a:tuesfionrgotphteimfoalllorewsipnogncseo.ndRiteioconrsdoarcattuacloncodnitdioitniosnthseinanthaelyst 12.1.1.1 Sample size = 10 |lL injection 12.1.1.2 Flow rate = 300 pL/min. 12.1.1.3 Cycle time = 10.0 minutes 12.1.1.4 MSSSoooolllvbvveeeilnnnetttpAGBh::raa2sdMe.0iecenmothtm:MapnooAnlme(T04881n1Mm...i..t005005mse.o0:00000OeniH(um)minA.)cetate 5%5959S.5..05t00o.0B.00p00%%%%% AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/lMuoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes6 of 9 Page 43 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 12.4 Instrument Set-up 12.4.1 R9E-le3efc6et,rr"otoOsptphreaeryaP/tMiloaatnfsosarnmSdpLMecCatrZionmtUeensteaernr'c"se.Goufidthee, tMheicMroamssaLssynPxlaNtfoTrmUsLeCr'Zs Guide or ETS- 12.4.2 Check the solvent level in reservoirs and refill ifnecessary. 12.4.3 TCdihhseaesctskiepmthsbheloteuiptlhdoebfpethrfoelbasettawainnitdlhersnesopsljtaaecgeelgtechdaepeisdltlagaiernysl.eastIsfthsttheeeeeltnicpdapoisiflfltaohrueynp.drotobebwe uitnhsaatnisefyaecptoieryce,. 12.4.4 Turn on the nebulizing gas. 12.4.5 Open the tune page. Click on `Operate'to initiate the desolvation heaters. 12.4.6 Open the Inlet Editor. 111222...444...555...123 12.4.5.4 eRAOSSxeeeblpttlasoetdHewhlrjlPuevetsLdeostCodwtelhrqvipoetuehupnitmllinetipbotpfsrlooantcfotweoetbhm"tfueOooilnirpntzghr"aionet.obgludeetegaisoasfitsfrne1tlohed0aemfmkltiioiisnpnwtguoirtsafearosttohe.bu.esnepdrrvotehbdee..tipAoffintheempirsotbseh.ould be 12.4.6 Tchhaenignestirnumorednetrutoseosptthiemsiezpeatrhaemreesteprosnaste:the following settings. These settings may 12.4.6.1 Drying gas 250-425 liters/hour 12.4.6.2 ESI nebulizing gas 10-15 liters/hour 12.4.6.3 HPLC constant flowmode, flow rate 10 - 500 |lL/min 12.4.6.4 HPrPeLssCuries <o4p0er0abtianrg(cTohrirsecptalyra.)meter is not set, it is a guide to ensure the 12.4.6.5 Source Block temperature 150. 12.4.6.6 Desolvation temperature 250. 12.4.7 Picnorfiponirtemsthateatipotuendn,eiannptdaogatehllweoiittnhhsetirrtusampppaelrniactmarbueltneerilnso,fgotbhromeoakInt.iloent paangde,stsoarme pitleinlitshte, mstausdsysbpiencder with 12.4.7.1 All copies must be initialed and dated. 12.4.8 nCulimckbeorns isntacrlut dbeutatollnsaomn pthleesMtoabsseLaynnaxlytzoeodl.bar. Ensure start and end sample 13.0 Data Analysis and Calculations___________________________________ 13.1 Calculations: 13.1.1 Calculate matrix spike percent recoveries using the following equation: AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes7 of 9 Page 44 of 171 BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 % Recovery = Observed REexsupletc-teBdaRckegsuroltund Result x 100 t 13.1.2 Calculate percent difference using the following equation: % Difference = Expected CoEnxep.e-ctCeadlcCuolnaete.d Cone, x 100 13.1.3 Calculate actual concentration ofanalyte in matrix (pg/mL): On-Column Concentration (pg/mL) x Dilution Factors = Calculated Concentration 14.0 Method Pe r f o r m a n c e _________________________________________ 14.1 tTahnheaelcyLatleiimsb,riatthtoieofnLQOcuuaQrnvtceiot.antcioennt(rLatOioQn)iisssmeleetchtoedd,aasntahleytleo,waensdtmacacterpixtasbpleecnifoicn.-zFeoror mstaanndyard in 14.2 cSaollivbernattioanndcumrveteh.od blank values must be < Vi that ofthe lowest standard used in the 14.3 eTqhueaclotoef0fi.c9i8e0n.t ofdetermination (r2) value for the calibration curve must be greater than or 14.4 CstoanndtianrudincgonCcaelnibtrraattiioonn. Verification (CCV) percent recoveries must be 30% ofthe 14.5 Internal Standard recoveries should be within 50% ofthe spiked concentration. 14.6 paIfnecarflroyitrsemtr.ieaDdloioscnteudtmhieennsttyhasiltslemmacetatinhodnosdsaipnmertphfloeersmrarawenacndeaaltsyae.zcetdioonraorethneortamctieot,nms aasindteetnearnmcienmedabyybtehe 14.7 Ifofodtantoatiesdtoonbetarbelpeosratneddwdihsecnuspseerdfoinrmthaencteexctroitferthiaehraevpeornt.ot been met, the data must be 15.0 Pollution Prevention and Waste Management______________________ 15.1 pSiapmetptleewexastrtaecitswdaisspteosaenddifnlabmromkaebnleglsaoslsvceonnt tiasidniesrpsolsoecdaitendhiinghthBeTlaUbocroantotariyn.ers, and glass 16.0 Records_________________________________________________________ 16.1 Ehianneataaceldhgyersprata.toigorenhgamennedtehrwoatrdei,tdtseafnomropanlesthtnueadmpyaemg,eue:sxstttrhuaadcvytieootnrhpedrafotoejle,lcodtwinliuuntmgiobinneffroa,cramtcoqartu(iioisfniatiiponpnclliumcadebetldheo)e,dita,hnedr in the 16.2 Pataprpipneliticntahtboelettuhinenefionprsamtgruaetm,ioseannmttopruliennlcloilsugtd., eanind tahcequaipspitrioopnrmiateethsotuddfyrofmoldMera.ssCLoypnyxtahnesdeopthageres and 16.3 Plot the calibration curve then print these graphs and store in the study folder. AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfeotnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes8 of 9 Page 45 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 16.4 Panridntstdoarteaiinnttehgerasttuiodnysfuomldmer.ary, integration method, and chromatograms, from MassLynx, 16.5 Summarize data using suitable software and store in the study folder. 16.6 aBnadckloucpateiolenctorofbnaicckduaptaetloecatpropnroicprdiaattae.medium. Record in study notebook the file name 17.0 Attachments____________________________________________________ 17.1 None 18.0 References _____________________________________________________ 18.1 P5RlaZtf;oormr FLloCaZtsURsoeard's, WGuyitdhee,nMshiacwroemMas2s3U9KLZL;imUinteitde,dTKuidnogrdRomoa.d, Altrincham, WA14 18.2 M5RaZss;LoyrnFxloNatTs URoseadr',sWGuyitdhee,nMshiacwroemMas2s3U9KLZL;iUmnitietedd, TKuidnogrdoRmoa.d, Altrincham, WA14 18.3 AMltarsisnLcyhnamx N, WTAG1u4id5eRTZo; DoraFtaloAactsquRiosaitdio,nW, yMthicernosmhaawsseUMK23Li9mLiZte;dU, nTiuteddorKRinogaddo,m. 18.4 EElTeSct-r9o-s3p6r.a0y,/"MOapsesraStpiorencatrnodmMetaeirn"t.enance ofthe Micromass Platform LCZ 19.0 Affected Documents____________________________________________ 19.1 None 20.0 Revisions NReuvmisbieorn. Reason For Revision ReDvaistieon AUnsianlgysHisPoLfCP-oEtlaescstiruomspPraeyrf/MluoarsosoScptaencetrsoumlfoetnrayte or OETthSe-r8F-1lu5o5r.o0chemicals in Waste Stream or Water ExtPraacgtes9 of 9 Page 46 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Attachment B: Data Summary Tables Page 47 of 171 BACK TO MAIN Solubility Study Test Substance: PFOS. SD-018 (purity = 86.9%); and FOSA. SE-027 (purity TBD) Test Matrix: Male/Female Human Urine Test Temperature: 23-24 C Method(s) used: The solubility determination was performed according to United States Environmental Protection Agency OPPTS 830.7840, "Water Solubility: Column Elution Method; Shake Flask Method" and OECD 105, "Water Solubility" Guidelines, as implemented by 3M Laboratory in methods ETS-8-170.1 "Solubility Screen Test: Approximate Solubility Determination of a Test Substance in Various Solvents;" and ETS-8-172.1 "Shake Flask Method; Solubility Determination of a Test Substance in Various Solvents". All analyses were performed via LC/MS according to the method ETS-8-155.0 "Analysis of Perfluorooctane Sulfonate or Other Fluorochemicals in Waste Stream or Water Extracts Using HPLC-Electrospray/Mass Spectrometry",_____________________ Results: PFOS Averaae ua/mL Day 1 302 Day 2 325 Day 3 287 Total 305 Std Dev 12 40 30 14.2 Precision i%RSD) 4% 12% 10% 5% FOSA Averaae ua/mL Day 1 2.56 Day 2 2.88 Day 3 2.61 Total 2.68 Std Dev 0.38 0.12 0.047 0.2 Precision i%RSD) . 15% 4% 2% 7% Results for PFOS were corrected for standard purity. Purity for FOSA is unknown, therefore no corrections were made. Gxaet Copy f Original JM-- Initial Drii.e Results Summary 3M Confidential AVWWIIS V1V(J IN jWHO V liy io =?o| SsZmo*tI!3Oo--Sor3)'' 00 *< Page 1 Page BACK TO MAIN FOSA SE-027 Urine Solubility Results SamoType File _____ Corrected for Sample Name Sample Desc. Compound Name RT Area Amount fna/mLl 1:10 dilution ________________________________________________________________________________________________ pg/mL FOSA SAMPLE SAMPLE SAMPLE HILL0126.D HILL0127.D HILL0128.D SAMPLE SAMPLE SAMPLE HILL0130.D HILL0135.D HILL0136.D FOSA-1.1.1. FOSA-1.1.2 FOSA-1.1.3 FOSA-1.2.1 FOSA-1.2.2 FOSA-1.2.3 042301 -FOSA-1.1.1 Smp 042301 -FOSA-1.1.2 Dup 042301-FOSA-1.1.3 Trip 042301-FOSA-1.2.1 Smp 042301-FOSA-1.2.2 Dup 042301-FOSA-1.2.3 Trip FOSA FOSA FOSA FOSA FOSA &S0 8090670 5.89 6180725 5.886 5838914 5.889 8385467 5.885 8541720 5.888 8450504 346 223 213 309 313 312 3*43 2.23 2.13 3.09 3.13 3.12 SAMPLE SAMPLE SAMPLE HILL0138.D FOSA-1.3.1 042301-FOSA-1.3.1 Smp FOSA 5.882 6883587 HILL0139.D FOSA-1.3.2 042301-FOSA-1.3.2 Dup FOSA 5.886 6433005 HILL0141.D FOSA-1.3.3 042301-FOSA-1.3.3 Trip FOSA 5.886 6255010 from HPLC/MSD ''Hillary" analytical sequence H010426.S, reprocessed with Target Software by KLT 248 233 230 2.48 2.33 2.30 C a lc u la tio n s Average (pg/mL) Std Dev %RSD Spike % Recov. 2.60 0.7 28% 2.18 4.4% Rep2,3 ave&RPD 3.11 Day 1 results, pg/mL 0.0 average 2.56 1% std dev 0.38 2.37 0.1 4% %RSD: 15% SAMPLE SAMPLE SAMPLE HILL0152.D HILL0153.D HILL0154.D FOSA-2.1.1 FOSA-2.1.2 FOSA-2.1.3 042301 -FOSA-2.1.1 Smp 042301-FOSA-2.1.2 Dup 042301-FOSA-2.1.3 Trip FOSA FOSA FOSA 5.879 8103858 5.879 8151376 5.88 7853370 SAMPLE SAMPLE SAMPLE HILL0157.D HILL0158.D HILL0159.D FOSA-2.2.1 FOSA-2.2.2 FOSA-2.2.3 042301-FOSA-2.2.1 Smp 042301-FOSA-2.2.2 Dup 042301-FOSA-2.2.3 Trip FOSA FOSA FOSA 5.887 7993752 5.886 7697039 5.887 7443513 SAMPLE SAMPLE SAMPLE HILL0165.D FOSA-2.3.1 042301 -FOSA-2.3.1 Smp FOSA 5.879 7850050 HILL0166.D FOSA-2.3.2 042301-FOSA-2.3.2 Dup FOSA 5.882 7536620 HILL0167.D FOSA-2.3.3 042301-FOSA-2.3.3 Trip FOSA 5.88 7535404 from HPLC/MSD "Hillary" analytical sequence H010426.S, reprocessed with Target Software by KLT 317 296 291 298 280 269 289 279 275 3.17 2.96 2.91 2.98 2.80 2.69 2.89 2.79 2.75 3.02 0.1 5% 2.82 0.1 5% 2.81 0.1 ' 3% Day 2 results, pg/mL average 2.88 std dev 0.12 %RSD: 4% SAMPLE SAMPLE SAMPLE HILL0097.D HILL0099.D HILL0100.D FOSA-3.1.1 FOSA-3.1.2 FOSA-3.1.3 042301-FOSA-3.1.1, Smp 042301-FOSA-3.1.2, Dup 042301-FOSA-3.1.3, Trip FOSA FOSA FOSA 5.909 7201703 5.901 6731194 5.908 6998562 SAMPLE SAMPLE SAMPLE HILL0101.D HILL0102.D HILL0103.D FOSA-3.2.1 FOSA-3.2.2 FOSA-3.2.3 042301-FOSA-3.2.1, Smp 042301-FOSA-3.2.2, Dup 042301-FOSA-3.2.3, Trip FOSA FOSA FOSA 5.908 6990791 5.922 7009317 5.895 6836606 SAMPLE SAMPLE SAMPLE HILL0108.D FOSA-3.3.1 042301-FOSA-3.3.1, Smp FOSA 5.916 7065688 HILL0109.D FOSA-3.3.2 042301-FOSA-3.3.2, Dup FOSA 5.906 7377514 HILL0110.D FOSA-3.3.3 042301-FOSA-3.3.3, Trip FOSA 5.9 7030743 from HPLC/MSDi "Hillary" analytical sequence H010501 .s, reprocessed with Target Software by KLT 269 251 260 257 261 251 263 274 260 3M Confidential 5/14/01 2.69 2.51 2.60 2.57 2.61 2.51 2.63 2.74 2.60 o\ 2.60 0.1 3% 2.56 0.1 2% Day 3 results, pg/mL average 2.61 std dev 0.05 2.66 %RSD: 2% 0.1 3% Exact Copy of Original - KIT Initial Dale " Page 1 3M Environmental Laboratory Project # E 0 1 -0768 Page 4^ of 171 BACK TO MAIN PFOS SD-018 Urine Solubility Results Samole Name Mise Info Comoound Name corrected for 1:1,000 dilution Average pg/mL Corrected for std Std Dev R I Area Amt fna/mU DUritv na/mL %RSD SAMPLE SAMPLE SAMPLE HILL0037.D HILL0038.D HILL0039.D PFOS-1.1.1 PFOS-1.1.2 PFOS-1.1.3 042301 -PFOS-1.1.1 Smp PFOS 5.271 7570273 042301-PFOS-1.1.2 Dup PFOS 5.277 8619490 042301-PFOS-1.1.3 Trip PFOS 5.255 8589480 292.6 331.8 329.8 286 325 323 311 22.0 7% SAMPLE SAMPLE SAMPLE HILL0041.D HILL0046.D HILL0047.D PFOS-1.2.1 PFOS-1.2.2 PFOS-1.2.3 042301-PFOS-1.2.1 Smp PFOS 5.251 7600633 042301-PFOS-1.2.2 Dup PFOS 5.263 7571396 042301-PFOS-1.2.3 Trip PFOS 5.264 7594271 298.7 294.9 290.2 292 289 284 288 4.0 1% SAMPLE SAMPLE SAMPLE HILL0049.D PFOS-1.3.1 042301-PFOS-1.3.1 Smp PFOS 5.27 8267658 320.6 HILL0051.D PFOS-1.3.2 042301-PFOS-1.3.2 Dup PFOS 5.263 8045600 307.6 HILL0052.D PFOS-1.3.3 042301-PFOS-1.3.3 Trip PFOS 5.272 8019673 308.5 from HPLC/MSD "Hillary" analytical sequence H01 0426.S, reprocessed with Target Software by KLT 314 301 302 306 7.2 2% Day 1 results, jig/mL average 302 std dev %RSD: 12 4.0% SAMPLE SAMPLE SAMPLE HILL0037.D HILL0038.D HILL0039.D PFOS-2.1.1 PFOS-2.1.2 PFOS-2.1.3 042301 -PFOS-2.1.1 Smp PFOS 5.248 7420988 042301-PFOS-2.1.2 Dup PFOS 5.248 9885661 042301-PFOS-2.1.3 Trip PFOS 5.256 8832844 312 421 363 305 412 356 358 54 15% SAMPLE SAMPLE SAMPLE HILL0045.D HILL0046.D HILL0047.D PFOS-2.2.1 PFOS-2.2.2 PFOS-2.2.3 042301-PFOS-2.2.1 Smp PFOS 5.263 7021826 042301-PFOS-2.2.2 Dup PFOS 5.255 7094280 042301-PFOS-2.2.3 Trip PFOS 5.25 6410858 295 294 269 289 288 263 280 15 . 5% Day 2 results, pg/mL average 325 std dev 40 SAMPLE SAMPLE SAMPLE HILL0050.D PFOS-2.3.1 042301-PFOS-2.3.1 Smp PFOS 5.257 8177762 339 HILL0051.D PFOS-2.3.2 042301-PFOS-2.3.2 Dup PFOS 5.249 8319423 345 HILL0052.D PFOS-2.3.3 042301-PFOS-2.3.3 Trip PFOS 5.249 8547947 352 from HPLC/MSD "Hillary" analytical sequence H0105Q1.S, reprocessed with Target Software by KLT 332 338 345 338 7 2% %RSD: 12% SAMPLE SAMPLE SAMPLE HILL0064.D HILL0065.D HILL0066.D PFOS-3.1.1 PFOS-3.1.2 PFOS-3.1.3 042301 -PFOS-3.1.1 Smp PFOS 5.237 6815087 042301-PFOS-3.1.2 Dup PFOS 5.242 7544482 042301-PFOS-3.1.3 Trip PFOS 5.242 6794540 267.6 292.7 265.0 262 287 259 269 15.4 6% Day 3 results, pg average 287 std dev 30 SAMPLE SAMPLE SAMPLE HILL0072.D HILL0073.D HILL0074.D PFOS-3.2.1 PFOS-3.2.2 PFOS-3.2.3 042301-PFOS-3.2.1 Smp PFOS 5.245 8117378 042301-PFOS-3.2.2 Dup PFOS 5.249 8786445 042301-PFOS-3.2.3 Trip PFOS 5.251 9095599 308.4 359.3 319.1 302 352 312 322 26.5 8% %RSD: 10% SAMPLE SAMPLE SAMPLE HILL0077.D PFOS-3.3.1 042301-PFOS-3.3.1 Smp PFOS 5.238 7558687 292.4 286 271 HILL0078.D PFOS-3.3.2 042301-PFOS-3.3.2 Dup PFOS 5.243 6689145 262.7 257 14.5 0430.S,HILL0079.D PFOS-3.3.3 042301-PFOS-3.3.3 Trip PFOS 5.234 7103605 275.7 270 5% Exact Copy t originalfrom HPLC/MSD "Hillary" analytical sequence H01 reprocessed with Target Software by KLT_________________________________________________________ 3M Confidential initial Dat 5/14/01 Page 1 3M Environmental Laboratory Project # E01-0768 Page 50 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Pays 1 and 2 Analytical Instrument: HPLC/MSO "Hillary"; Analytical Sequence/Method: H0106.s/PFOS0425.m (ChemStatron); Reprocessing Method: H01042Gtm (T a rg e t) In i D ate B a tch Sam oTvoe R e S a m p le N am e S a m p le D ese. C om pound Name 4/26 /01 19:37 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0016.D 01003-07-01 0 ng/m L PFO S THPFOS 4/26 /01 19:48 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0Q 17.D 01003-07-02 2.5 ng/m L PFO S THPFOS 4/26 /01 19:59 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A L IB 1 H ILL0018.D 01003-07-03 5 ng/m L PFO S THPFOS 4/26/01 20 :1 0 D :\ch em \H tlIa fy.i\H 01 04 26 .b C A LIB 2 H ILL0019.D 01003-07-04 10 ng/m L PFO S THPFOS 4 /26 /01 20:21 D :\c h e m \H iila ry .i\H 0 1 0 4 2 6 .b C A LIB 3 H ILL0020.D 01003-07-05 25 ng/m L PFO S THPFOS 4/26/01 20:33 D :\c h e m \H illa ry .l\H 0 1 0 4 2 6 .b C A LIB 4 H ILL0021.D 01003-07-06 40 ng/m L PFO S THPFOS 4/26/01 20:44 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A U B 5 H ILL0022.D 0 1 0 0 3 -0 7 -0 7 50.1 ng /m L P F O S THPFOS 4/26/01 20:55 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 6 H ILL0023.D 01003-07-08 . 75.1 ng /m L PF O S THPFOS 4/26/01 21:06 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 7 H ILL0024.D 01003-07-09 100.2 ng/m L PFO S THPFOS 4/26/01 21:17 D :\ch em \H N Iary.i\H 01 04 26 .b C A L IB 8 H ILL0O 25.D 01003-07-10 250.5 ng/m L PFO S THPFOS 4/26/01 21:23 D :\ch em \H iH a ry.i\H 01 04 26.b C A L IB 9 H 1LL0026.D 01003-07-11 400.8 ng/m L PFO S THPFOS 4/26/01 21:40 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 10 H ILL0027.D 01003-07-12 , 501 ng/m L PFO S THPFOS 4/26 /01 21:51 D :\ch em \H illa ry.iA H 0 10 42 6.b SA M P LE H ILL0028.D 01003-07-13 1002 ng/m L PFO S THPFOS 4/27/01 0:28 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0042.D 01003-07-03 5 ng/m L PFO S THPFOS 4/27/01 0:39 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0043.D 01003-07-09 100.2 ng/m L PFO S THPFOS 4/27/01 3:05 D :\ch e m \H illa ry.i\H Q 1 0 4 2 6 .b S A M P LE H ILL0056.D 01003-07-03 5 ng/m L PFO S THPFOS 4/27/01 3:17 D :\c h e m \H illa ry .l\H 0 1 0 4 2 6 .b S A M P LE H ILL0057.D 01003-07-09 100.2 ng/m L PFO S THPFOS 4/27/01 5:53 D :\c h e m \H iila ry .l\H 0 1 0 4 2 6 .b S A M P LE H ILL0071.D 01003-07-03 5 ng/m L PFO S THPFOS 4/27/01 6:04 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0072.D 01003-07-09 100.2 ng/m L PFO S THPFOS 4/27 /01 7:34 D :\ch e m \H illa ry.t\H 0 1 0 4 2 6 .b S A M P LE H ILL 00 80 .D 01003-07-03 5 ng/m L PFO S THPFOS 4/27/01 7:45 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0081.D 01003-07-09 100.2 ng/m L PFO S THPFOS 4/27/01 8:19 D :\c h e m \H iila ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0084.D 0 1 0 0 3 -0 7 -0 1 0 ng/m L PFO S THPFOS 4/27/01 8:30 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0085.D 01003-07-02 2.5 ng/m L PFO S THPFOS 4/27 /01 8:41 D :\ch em \H N lH ry.i\H 01 04 26 .b C A U B 11 H IL L 0 0 8 6 .D 01003-07-03 5 ng/m L PFO S THPFOS 4/27/01 8:52 4/27/01 9:03 D :\ch em \K illary.i\H 01 04 26 .b D :\ch em \H N Iary.i\H 01 04 26 .b C A L IB 12 C A LIB 13 H ILL0087.D H ILL0088.D 01003-07-04 01003-07-05 10 ng/m L PFOS 25 ng /m L P FO S THPFOS THPFOS 4/27/01 9:15 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A U B 14 H ILL0089.D 01003-07-06 40 ng/m L PFO S THPFOS 4/27/01 9:26 D :\ch em \H illa ry.r1 H 0 10 42 6.b C A U B 15 H ILL0090.D 01003-07-07 50.1 ng /m L P F O S THPFOS 4/27 /01 9:37 D :\ch em \H ida ry.i\H 0 10 42 6.b C A L IB 16 H ILL0091.D 01003-07-08 75.1 ng /m L P F O S THPFOS 4/27 /01 9:48 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A L IB 17 H ILL0092.D 01003-07-09 100.2 n g /m L PFO S THPFOS 4/27 /01 9:59 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A L IB 18 H IL L 0 0 9 3 .D 01003-07-10 250.5 ng/m L PFO S THPFOS 4/27 /01 10:10 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A U B 19 H ILL0094.D 0 1 0 0 3 -0 7 -1 1 400.8 ng/m L PFO S THPFOS 4 /27 /01 10:22 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A U B 20 H ILL0095.D 01003-07-12 501 ng/m L PFO S THPFOS 4/27 /01 10:33 D :\ch em \H iH a fy.i\H 0 10 42 6.b S A M P LE H ILL0096.D 01003-07-13 1002 ng/mL PFOS THPFOS T w o c u r v e s w e r e a v e r a g e d u s in g T a r g e t s o ftw a r e to q u a n tify d a ta . A s ta n d a r d c u r v e ra n g e o f o n l y 10 le v e ls is a llo w e d . 5 - 5 0 0 n g /m L w a s th e ra n g e c h o s e n . 81 5.115 5.11 5.125 5.112 5 .0 9 7 5 .1 1 5 5.094 5.131 5 .0 9 7 5.117 5.11 5.11 5.109 5.111 5 .1 1 8 5.141 5.125 5.122 5.133 5.133 5.13 5.127 5.13 5.123 5.13 5 .1 2 3 5 .1 2 4 5.13 5.124 5.122 5.123 5.123 5.132 5 .1 2 3 A rea 1238088 1251680 1273626 1280488 1289080 1294694 1319187 1320686 1316830 1333532 1326197 1324859 1323984 1428715 1441029 1487926 1456794 1499176 1477095 1504963 1469125 1491338 1484350 1517040 1493288 1476860 1492539 1489446 1438972 1481229 1455720 1457008 1455144 1426062 1406375 88296 6.3% Am ount 254 254 254 254 -254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 C om pound Name PFBS PFBS PFBS PFBS PFBS PFBS PFBS . PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS RT 4 .3 7 3 4 .3 8 2 4 .3 8 3 4.39 4 .3 8 3 4.38 4.38 4 .3 6 7 4 .3 7 6 4 .3 7 5 4 .3 8 2 4 .3 8 9 4 .3 7 4 4 .3 9 7 4.401 4 .4 0 5 4 .3 9 7 4 .4 0 7 4.411 4.411 4 .4 0 8 4 .4 1 2 4 .4 0 9 4 .4 0 8 4 .4 0 9 4 .4 0 9 4.41 4 .4 1 6 4 .4 0 9 4 .4 0 7 4 .4 0 9 4 .4 0 2 4.41 4 .4 0 2 A rea 1933641 1933710 1932682 1943358 1949841 1941643 1930302 1953486 1971932 1956172 1987259 1977603 1983865 2021892 2000887 2033053 2045778 2055427 2044996 2044088 2044316 2052700 2038788 2035215 2007995 2020150 2027822 2029826 1952364 2023371 1982961 2031354 2025464 1994320 1997302 41289 2,1% In i D ate 4/26 /01 22:24 4/26 /01 22:36 4/26 /01 22:47 4/26 /01 22:58 4/26/01 23:09 4/26/01 23:32 4/26 /01 23:43 4/26 /01 23:54 4/27/01 0:05 4/27/01 0:16 4/27 /01 1:12 4 /27 /01 1:24 4/27/01 1:35 B a tch D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b O :\che m \H iliary.i\H 01 04 26 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :V ch em \H illa ry.i\H 0 10 42 6.b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\c h e m \H tlla ry.i\H 0 1 0426.b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b Sam oTvpe SA M P LE S A M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE F ile H ILL0031.D H ILL0032.D H ILL0033.D H ILL 00 34 .D H ILL0035.D H ILL0037.D H ILL0038.D H ILL0039.D H ILL0040.D H ILL0041.D H ILL0046.D H ILL0047.D H ILL0046.D S a m p le N am e 042301-PFO S-LCS P F O S -1 .4 .1b lk P F O S -1 .4 .2b lk PFOS-1.4.3 btk P FO S -1.4.4blkM S PFO S -1.1.1 PF O S -1.1.2 PF O S -1.1.3 P F O S -1.1.4M S PFO S -1.2.1 P F O S -1.2.2 P F O S -1.2.3 P F O S -U .4 M S S a m p le D esc. P F O S S o lve n t B la n k S pike 0 4 2 3 0 1-P F O S -1.4.1 M td Blk 0 4 2 3 0 1 -P F O S -1 .4.2 M td Blk 0 4 2 3 0 t - P F O S - 1 .4 .3 M td Blk 0 4 2 3 0 1 -P F O S -1 .4.4 M td Blk S pike 0 4 2 3 0 1-P F O S -1 .1.1 S m p 042301 -P F O S -1.12 Dup 04 23 01-P F O S -1 .1.3 T rip 0 4 2 3 0 1 -P F O S -1.1.4 S pike 0 4 2 3 0 1 -P F O S -1 .2.1 S m p 042301 -PFO S-12 2 Dup 0 4 2 3 0 1 -P F O S -1 .2 .3 T rip 0 4 2 3 0 1 -P F O S -1.2.4 S pike C om pound Name THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 81 5 .1 0 5 5 .1 1 2 5.111 5 .1 1 7 5.137 5.123 5.123 5.115 5.117 5.111 5.123 5.124 5 .1 1 5 A rea 1356608 1357667 1371641 1347413 1362229 1239933 1242749 1244758 1243279 1262274 1279599 1288849 1283560 Am ount 254 254 254 254 254 254 254 254 254 254 254 254 254 C om pound Name PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS BI 4 .3 7 7 4.37 4 .3 6 9 4 .3 7 4 4 .3 8 8 4 .3 8 8 4 .3 7 4 4 .3 9 3 4 .3 9 5 4 .3 9 7 4 .3 8 8 4 .3 9 5 4 .3 9 4 A rea 1932182 1900574 1910506 1921866 1925821 2179012 2222026 2225836 2165910 2148762 2164574 2202302 2190236 Ex^ct Copy of Qng'.fsl j ^ P _ W-lu-ni' u {mtsa Am ount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 2536492 1398111 Am ount 254 254 254 254 254 254 254 254 254 254 254 254 254 Page 1 of 5 3M Environmental Laboratory Project # E 0 1 -0768 Page 51 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/PFOS0425.m (ChemStation); Reprocessing Method: H010426tm (Target) 4/27/01 1:47 4/27/01 2:09 4/27/01 2:20 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch em \H iH a ry.i\H 01 04 26.b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE SA M P LE SA M P LE H ILL0049.D K 1 L L 0 0 5 1 .D H ILL0052.D P FO S -1.3.1 P F O S -1.3.2 P F O S -1.3.3 0423Q 1-P FO S-1.3.1 S m p 0 4 2 3 0 1 -P F O S -1.3.2 D up 04 23 Q 1 -P F O S -1.3.3 T rip THPFOS THPFOS THPFOS 5.13 5 .1 1 6 5.132 1269547 1282405 1283479 254 254 254 4/27/01 2:31 D :\ch em \H iIlary.i\H 01 04 26 .b S A M P LE H ILL0053.D PF O S -1.3.4M S 0 4 2 3 0 1-P F O S -1.3.4 S pike THPFOS 5.116 1277667 254 4/27/01 2:43 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0054.D 042301-P F O S -LC S P F O S S o lven t B lank S pike . THPFOS 5.123 1423859 254 4/27 /01 2:54 4/27 /01 3:50 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE SA M P LE H ILL0055.D H ILL0060.D P F O S -2 .4 .1b lk P F O S -2 .4 .2b lk 0 4 2 3 0 1-P FO S -2.4.1 M td Blk 0 4 2 3 0 1 -P F O S -2.4 .2 M id Blk THPFOS THPFOS S .1 3 5.131 1433506 1413614 254 254 4/27 /01 4:01 D :\c h e m \H illa fy .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0061.D P F O S -2 .4 .3b lk 0 4 2 3 0 1-P F O S -2.4.3 M td Blk THPFOS 5.119 1421004 254 4/27/01 4:13 4(27(OX 4:24 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b O :\c h e m \H iffa ry .f\H O 104 2 6 .b SA M P LE S A M P LE H ILL0062.D H ILL0063.D P F O S -2 .4 .4b lkM S P F O S -2 .1 .1 0 4 2 3 0 1 -P F O S -2 .4.4 M td B lk S pike 042301 -P F O S -2 .1.1 Sm p THPFOS THPFOS 5.13 5.122 1403989 1287849 254 254 4/27/01 4:35 D :\ch e m \H illa ry.i\H 0 1 04 26 .b SA M P LE H ILL0064.D PF O S -2.1.2 042301-P F O S -2.1.2 D up THPFOS 5.136 1278367 254 4/27/01 4:57 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H 1LL0066.D PF O S -2.1.3 04 23 01 -P F O S -2 .1.3 T rip THPFOS 5.123 1294319 254 4/27/01 5:08 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0067.D PF O S -2.1.4M S 0 4 2 3 0 1 -P F O S -2 .1.4 Spike THPFOS 5.13 1272974 254 4/27 /01 5:20 D :\e he m \H illary.i\H 01 04 26 .b SA M P LE H ILL0068.D P FO S -2.2.1 04 23 01-P F O S -2.2.1 S m p THPFOS 5.136 1434509 254 4/27 /01 5:31 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0069.D P F O S -2.2.2 042301-P F O S -2.2.2 D up THPFOS 5 .1 3 7 1421082 254 4/27/01 5:42 4/27/01 6:38 D :\ch e m \H ilIa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.A H 0 1 0 4 2 6 .b SA M P LE SA M P LE H ILL0070.D H ILL0075.D PF O S -2.2.3 PF O S -2.2.4M S 0 4 2 3 0 1 -P F O S -2 .2 .3 T rip 0 4 2 3 0 1-P FO S -2.2.4 S pike THPFOS THPFOS 5.131 5 .1 3 7 1441500 1430472 254 254 4/27/01 6:49 4/27/01 7:00 D :\ch em \H iJla ry.A H 01 04 26 .b D :\c h e m \H illa ry .l\H 0 1 0 4 2 6 .b SA M P LE SA M P LE H ILL0076.D H ILL0077.D P FO S -2.3.1 PF O S -2.3.2 04 23 01-P F O S -2.3.1 S m p 042301-P F O S -2.32 Dup THPFOS THPFOS 5.129 5 .1 2 3 1423581 1417186 254 254 4/27 /01 7:11 4/27/01 7:23 D :\c h e m \H iila ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 04 26 .b SA M P LE SA M P LE H ILL0078.D H ILL0079.D PF O S -2.3.3 PFO S -2.3.4M S 0 4 2 3 0 1 -P F O S -2 .3 .3 T rip 04 23 01-P F O S -2 .3.4 S pike THPFOS THPFOS 5 .1 3 3 5 .1 3 7 1411658 1451012 254 254 In i D ate 4 /26 /01 19:14 4/26 /01 19:26 4/26/01 22:02 4/26/01 22:13 4/26/01 23:20 4/27/01 0:50 4 /2 7 /0 1 1:01 4/27/01 1:58 4/27/01 3:28 4/27/01 3:39 4/27/01 4:46 4/27/01 6:15 4/27/01 6:27 4/27/01 7:56 4/27/01 8:08 4/27 /01 10:44 4/27 /01 10:55 B a tch O :\che m \H iIla ry.i\H 0 10 42 6.b D :\c h e m \H ilia ry .i\H 0 1 042B .b D :\c h e m \H illa ry .A H 0 1 04 26 .b D :\ch em \H N Iary.i\H 01 04 26 .b D :\ch em \H iH a ry.i\H 01 04 26.b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H iila ry .i\H 0 1 0 4 2 5 .b D :\c h e m \H illa ry .l\H 0 1 0 4 2 6 .b D :\ch em \H itlary.i\H 01 04 26 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H Q 10 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch em \H N Iafy.i\H 01 04 26 .b D :\c h e m \H ilfa ry .i\H 0 t0 4 2 6 .b Sem pTyps SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE S A M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE E H ILL0014.D H ILL0015.D H ILLD 029.D H ILL0030.D H 1L L 0 0 3 6 .D H JLL0044.D H ILL0045.D H ILL0050.D H ILL0058.D H 1L L 0 0 5 9 .D H ILL0065.D H ILL0073.D H ILL0074.D H ILL0082.D H ILL0083.D H ILL0097.D H ILL0093.D S a m o te N am e T N -A 4802 MeOH TN -A 4802 M eO H TN -A 4802 M eO H TN -A 4802 M eO H TN -A 4802 M eOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 M eOH TN -A 48 02 M eO H TN -A 4802 M eOH TN -A 4802 M eO H TN -A 4802 M eOH T N -A 4802 M eOH T N -A 4802 M eO H T N -A 4802 M eO H T N -A 4802 M eOH T N -A 4 8 02 MeOH S a m p le D esc. S o lven t Blank S o lve n t B lank S o lve n t B lank S o lve n t B lank S o lve n t B lank S o lve n t B lank S o lven t Blank S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t B lank S o lve n t B lank S o lve n t B lank S o lve n t Blank S o lven t Blank S o lven t Blank Solvent Blank C om pound Name THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RI 0 0 0 0 0 5.255 0 0 0 0 5 .2 5 6 0 0 0 0 0 0 1342769 73849 5.5% A rea 0 0 0 0 0 7825 0 0 0 0 7710 0 0 0 0 0 0 Am ount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4 .3 9 4 4 .3 9 4 4 .3 9 6 4 .3 9 4 4 .3 9 4 4 .3 9 5 4 .4 0 9 4 .3 9 8 4 .4 0 8 4.4 4 .4 1 5 4 .4 0 9 4 .4 0 9 4.401 4 .4 0 9 4.41 4 .4 2 3 4 .4 1 5 4 .4 1 6 4 .4 1 9 4 .4 0 8 2195975 2216090 2203291 2220887 1977507 1931697 1944188 1913426 1898991 2201997 2231938 2202521 2203090 1973173 1956138 1940430 1930607 1936770 1899523 1917144 1951546 C orppound N am e PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS El 4 .3 8 7 0 4.39 0 4.402 4 .4 0 7 0 4 .4 0 8 4 .4 2 3 0 4 .4 2 3 4 .4 2 9 0 4 .4 3 6 0 4.431 0 2056957 137331 6.7% A rea 6824 0 9125 0 8664 8480 0 8742 8244 0 9199 8487 0 8442 0 9918 0 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 2674044 1439870 Am ount 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page 2 of 5 3M Environmental Laboratory Project # E01-0768 Page 52 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Tlmepoint(s): Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/PFOS0425.m (ChemStation); Reprocessing Method: H010426Lm (Target) In i D ate B a tch Sam pTvpe F ile S a m p le N am e . S a m p le D esc. C om pound Nam e 4/26/01 19:37 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0016.D 01003-07-01 0 ng/m L PFO S PFOS 4/26/01 19:48 D :\ch em \H iIiary.i\H 01 04 26 .b S A M P LE H ILL0017.D 0 1 0 0 3 -0 7 -0 2 2.5 ng/m L PFO S PFOS 4 /26 /01 19:59 D :\ch em \H iH a ry.i\H 01 04 26.b C A LIB 1 H ILL0018.D 0 1 0 0 3 -0 7 -0 3 5 ng/m L PFO S PFOS 4/26/01 20:10 D :\ch e m \H illa ry.A H 0 1 0 4 2 6 .b C A LIB 2 H ILL0019.D 0 1 0 0 3 -0 7 -0 4 10 ng/m L PFO S PFOS 4 /26 /01 20:21 D :\ch em \H N Iary.i\H 01 04 26 .b C A LIB 3 H ILL0020.D 0 1 0 0 3 -0 7 -0 5 25 ng/m L PFO S PFOS 4/26/01 20:33 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 4 H ILL0021.D 01003-07-08 40 ng/m L PFO S PFOS 4/26/01 20:44 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 5 H ILL0022.D 0 1 0 0 3 -0 7 -0 7 50.1 ng /m L PFO S PFOS 4/26/01 20:55 D :\ch e m \H itla ry.i\H 0 1 0426.b C A LIB 6 H ILL0023.D 01003-07-08 75.1 ng /m L PF O S PFOS 4/26/01 21:06 D :\ch e m \H illa ry.f\H O 1 O 4 2 0 .b C A LIB 7 H ILL0024.D 0 1 0 0 3 -0 7 -0 9 100.2 ng/m L PFO S PFOS 4/26/01 21:17 D :\ch e m \H illa ry.f\H 0 1 0 4 2 6 .b C A LIB 8 H ILL0025.D 0 1 0 0 3 -0 7 -1 0 250.5 ng/m L PFO S PFOS 4/26/01 21:28 4/26/01 21:40 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 9 C A LIB 10 H ILL0026.D H ILL0027.D 01003-07-11 . 0 1 0 0 3 -0 7 -1 2 400.8 ng/m L PFO S 501 ng/m L PFO S PFOS PFOS 4/26 /01 21:51 D :\ch em \H iH a ry.i\H 01 04 26.b SA M P LE H ILL0028.D 0 1 0 0 3 -0 7 -1 3 1002 ng/m L PFO S PFOS 4/27/01 0:28 D :\c h e m \H ilia r y .i\H 0 1 0 4 2 6.b S A M P LE H ILL0042.D 0 1 0 0 3 -0 7 -0 3 5 ng/m L PFO S PFOS 4/27/01 0:39 D :\ch em \H iIlary.i\H 01 04 26 .b SA M P LE H ILL0043.D 0 1 0 0 3 -0 7 -0 9 100.2 ng/m L PFO S PFOS 4/27/01 3:05 4/27/01 3:17 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE S A M P LE H ILL0056.D H ILL0057.D 0 1 0 0 3 -0 7 -0 3 0 1 0 0 3 -0 7 -0 9 5 ng/m L PFO S 100.2 ng/m L PFO S PFOS PFOS 4/27/01 5:53 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0071.D 0 1 0 0 3 -0 7 -0 3 5 ng/m L PFO S PFOS 4/27/01 6:04 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0072.D 0 1 0 0 3 -0 7 -0 9 100.2 ng/m L PFO S PFOS 4/27/01 7:34 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b S A M P LE H ILL0080.D 0 1 0 0 3 -0 7 -0 3 5 ng/m L PFO S PFOS 4/27/01 7:45 4/27/01 8:19 D :\ch e m \H ilIa ry.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 042S.b SA M P LE SA M P LE H ILL0081.D H ILL0084.D 0 1 0 0 3 -0 7 -0 9 01003-07-01 100.2 ng/m L PFO S 0 ng/m L P F O S PFOS PFOS 4/27/01 8:30 D :\ch e m \H illa ry.i\H 0 1 0426.b SA M P LE H ILL0085.D 0 1 0 0 3 -0 7 -0 2 2.5 ng/m L PFO S PFOS 4/27/01 8:41 D :\ch e m \H illa ry.i\H 0 1 0 4 2 B .b C A L IB 11 H IL L 0 0 8 6 .D 0 1 0 0 3 -0 7 -0 3 5 ng/m L PFO S PFOS 4/27/01 8:52 D :\ch em \H i1lary.i\H 0 10 426 .b C A L IB 12 H ILLO O 07.D 0 1 0 0 3 -0 7 -0 4 10 ng/m L PFO S PFOS 4/27/01 9:03 D :\ch em \H N Iary.i\H 01 04 26 .b C A L IB 13 H IL L 0 0 8 8 .D 0 1 0 0 3 -0 7 -0 5 25 ng/m L PFO S PFOS 4/27/01 9:15 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A L IB R I 4 H ILL0089.D 0 1 0 0 3 -0 7 -0 6 40 ng/m L P F O S PFOS 4/27/01 9:26 D :V ch em \H illa ry.i\H 0 10 42 6.b C A L IB 15 H ILL0090.D 0 1 0 0 3 -0 7 -0 7 50.1 ng/m L PF O S PFOS 4/27/01 9:37 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A L IB 16 H IL L 0 0 9 1 .D 0 1 0 0 3 -0 7 -0 8 75.1 ng/m L PF O S PFOS 4/27/01 9:48 D :\ch e m \H illa ry.t\H 0 1 0426.b C A L IB 17 H IL L 0 0 9 2 .D 0 1 0 0 3 -0 7 -0 9 100.2 ng/m L PFO S PFOS 4/27/01 9:59 D :\ch e m \H illa ry.i\H 0 1 0426.b C A L IB 18 H IL L 0 0 9 3 .D 0 1 0 0 3 -0 7 -1 0 250.5 ng/m L PFO S PFOS 4/27/01 10:10 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 19 H ILL0094.D 01003-07-11 . 400.8 ng/m L PFO S PFOS 4 /27 /01 10:22 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b C A LIB 20 H ILL0095.D 01003-07-12 501 ng/m L PFO S PFOS 4/27/01 10:33 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE H ILL0096.D 01003-07-13 1002 ng/m L PFO S PFOS T w o c u r v e s w e r e a v e r a g e d u s in g T a r g e t s o ftw a r e to q u a n tify d a ta . A s ta n d a r d c u r v e r a n g e o f o n ly 10 le v e ls is a llo w e d . 5 - 5 0 0 n g /m L w a s th e r a n g e c h o s e n . EI 0 5.32 5 .3 3 5 5.329 5 .3 1 5 5.332 5 .3 1 8 5 .3 4 8 5.322 5 .3 3 5 5 .3 2 7 5.328 5.326 5 .3 2 9 5.333 5.351 5.335 5 .3 2 5 5 .3 3 6 5 .3 3 6 5 .3 3 3 0 5 .3 3 3 5 .3 3 3 5 .3 3 3 5 .3 3 4 5 .3 2 7 5.34 5 .3 2 7 5 .3 3 2 5 .3 3 4 5 .3 2 6 5 .3 3 5 5 .3 2 6 A rea 0 512B9 138659 254205 660047 1055533 1291097 1939424 2537734 6004211 8957654 10985845 18864507 176475 2586427 150106 2627085 151691 2666281 148867 2633934 0 83665 142999 254810 607053 1065908 1360299 1965188 2630530 6077465 9143568 11226796 19703670 Am ount 0 2.8 5.0 9.3 24.9 40.5 50.1 75.6 99.3 254.6 394.8 504.8 983.7 6.1 99.7 5.1 99.0 5.1 100.6 5.1 99.4 0.0 2.7 4.9 9.1 2 5 .0 39.1 50.2 76.7 100.3 254.1 393.9 503.5 1 0 3 3 .7 % T he ore t!ca | - 9 9 .5 % 9 3 .4 % 9 9 .5 % 101.2% 100.1% 100.7% 9 9 .1 % 101.6% 9 8 .4 % 100.8% 122.5% 9 9 .5 % 102.6% 9 8 .8 % 9 9 .5 % 100.4% 101.1% 9 9 .2 % 9 7 .4 % 9 0 .5 % 100.0% 9 7 .8 % 100.3% 102.1% 100.1% 101.5% 9 8 .3 % 100.5% - Page 3 of 5 3M Environmental Laboratory Project # E01-0768 Page 53 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Tlmepolnt{s}: Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/PFOS0425.m (ChemStalion); Reprocessing Method: HO10426tm (Target) In i D ate 4/26/01 22 :2 4 4/26/01 22:36 4/26/01 22:47 4/26/01 22:58 4/26/01 23:09 B a tch D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.l\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b Sam pTvpe SA M P LE S A M P LE SA M P LE SA M P LE SA M P LE E i!S H ILL0031.D H ILLD 032.D H ILL0033.D H ILL0034.D S a m le N am e 042301-PFO S-LCS P F O S -1 .4.1 blk P F O S -1 .4 .2b lk P F O S -1.4.3b!k H ILL0035.D P FO S -1.4.4blkM S S a m p le D esc. P F O S S o lve n t B lank Spike 0 4 2 3 0 1 -P F O S -1.4.1 M td B Ik 0 4 2 3 0 1 -P F O S -1 .4 2 M td Blk 0 4 2 3 0 1 -P F O S -1 .4 .3 M td Blk 0 4 2 3 0 1-P F O S -1.4.4 M td Blk Spike Com DOund Name PFOS PFOS PFOS PFOS . PFOS SI 5.322 0 0 0 5.354 A rea 2260230 0 0 0 2520637 Am ount 8 9 .8 0.0 0.0 0.0 101.1 S a m p le P u rity A ve ra ge jigfrnL S td D ev % RSD c o rre c te d n a /m L Spike R ecovery 88 90% 99 101% 4/26/01 23:32 4/26/01 23:43 4/26/01 23:54 4/27/01 0:05 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :1chem \H if(ary.t\H 010426.b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE S A M P LE SA M P LE SA M P LE H 1LL0037.D H K .L003 .D H ILL0039.D H ILL0040.D P FO S -1.1.1 P F O S -i.f.2 P F O S -1.1.3 PFO S -1.1.4M S 0 4 2 3 0 1 -P F O S -1.1.1 S m p 042301-PFOS-1.1.2 Dup 0 4 2 3 0 1 -P F O S -1 .1.3 T rip 04 2 3 0 1 -P F O S -1 .1 .4 Spike PFOS PFOS PFOS PFOS 5.271 5 .2 7 7 5 .2 5 5 5.264 7570273 8619490 8589480 9810483 2 9 2 .6 3 3 1 .8 329.8 3 9 6 .8 286 325 323 388 311 22.0 7% 78% 4/27/01 0:16 4/27/01 1:12 4/27 /01 1:24 4/27/01 1:35 D :\c h e fn \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 26 .b D :\c b e m \H iila ry .f\H 0 1 0 4 2 6 .b D :\ch e m \H illa fy.i\H 0 1 0 4 2 6 .b SA M P LE SA M P LE SA M P LE SA M P LE H ILL0041.D H ILL0046.D H JLL0047.D H IL L D 0 4 .8 .D P FO S -1.2.1 P F O S -1.2.2 PFO S -1.2 .3 P F O S -1.2.4M S 042301-P F O S -1.2.1 Sm p 0 4 2 3 0 1 -P F O S -1.2.2 D up 0 4 2 3 0 1 -P F O S -1 .2 .3 T rip 04 2 3 0 1 -P F O S -1 .2 .4 Spike PFOS PFOS PFOS PFOS 5.251 5.263 5.264 5.256 7600633 7571398 7594271 9667899 2 9 8 .7 2 9 4 .9 2902 385.1 292 289 284 377 288 4.0 1% 90% 4/27/01 1:47 4/27/01 2:09 4/27/01 2:20 4/27/01 2:31 4/27/01 2:43 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch em \H illa ry.iU H 0104 26 .b D :\c h e m \H illa ry .t\H 0 1 0 4 2 6 .b D :\ch e m \H illa T y.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE H ILL0049.D H 1L L 0 0 5 1 .D H ILL0052.D P F O S -1.3.1 P F O S -1.3 .2 P F O S -1.3 .3 H ILL0053.D P F O S -1.3.4M S H ILL0054.D 042301-P FO S -LC S 04 2301-P F O S -1.3.1 Sm p 0 4 2 3 0 1-P F O S -1.3.2 D up 0 4 2 3 0 1 -P F O S -1 .3.3 T rip 0 4 2 3 0 1 -P F O S -1 .3.4 Spike P F O S S o lve n t B lank Spike PFOS PFOS PFOS PFOS PFOS 5.27 5.263 5.272 5 .2 6 3 5 .3 3 3 8267658 8045600 8019673 10242365 2342701 3 2 0 .6 3 0 7 .6 308.5 4 0 5 .2 9 1 .0 314 301 302 397 89 306 7.2 2% 93% 91% 4/27/01 2:54 4/27/01 3:50 4/27/01 4:01 4/27/01 4:13 D :\ch e m \H illa ry.i\H 0 1 0 4 26 b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H ilta ry.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b SA M P LE SA M P LE SA M P LE SA M P LE H ILL0055.D H ILL0060.D H ILL0061.D H ILL0062.D P F O S -2 .4 .1b lk P FO S -2.4.2W k P F O S -2 .4 .3b lk P F O S -2 .4 .4b lkM S 0 4 2 3 0 1-P FO S -2.4.1 M td Bik 0 4 2 3 0 1 -P F O S -2.4 .2 M td Blk 0 4 2 3 0 1 -P F O S -2.4 .3 M td Blk 0 4 2 3 0 1 -P F O S -2 .4 .4 M td B lk S pike PFOS PFOS PFOS PFOS 0 0 0 5.333 0 0 0 2571930 0.0 0.0 0.0 104.8 103 105% 4/27/01 4:24 4/27/01 4:35 4/27/01 4:57 4/27/01 5:08 4/27/0 f 5:20 4/27/01 5:31 4/27/01 5:42 4/27/01 6:38 D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch em \H iIlary.i\H 01 04 26 .b D :\ch em \H iflary.t\H 0 10 42 6.b D :\ch etn \H itlary.i\H 010426.b D :\ch e m \H illa ry.i\H 0 1 .0 4 2 6 .b D :\ch e m \H illa fy.i\H 0 1 0 4 2 6 .b SA M P LE SA M P LE SA M P LE SA M P LE H 1L L 0 0 6 3 .D H ILL0064.D H ILL0066.D H ILL0067.D SAMPLE SA M P LE SA M P LE SA M P LE H ILL0068.D H ILL0069.D H ILL0070.D H ILL0075.D P FO S -2.1.1 PF O S -2.1.2 PF O S -2.1.3 P F O S -2.1.4M S PFOS-2.2.1 PF O S -2.2.2 PF O S -2.2.3 P F O S -2.2.4M S 04 23 01-P F O S -2.1.1 Sm p 042301-P F O S -2.1.2 Dup 0 4 2 3 0 1 -P F O S -2 .1 .3 T rip 0 4 2 3 0 1 -P F O S -2 .1.4 S pike 042301-PFOS-22.1 S m p 0 4 2 3 0 1-PFO S-2.2J2 Dup 0 4 2 3 0 1 -P F O S -2 .2 .3 T rip 0 4 2 3 0 1 -P F O S -2 .2 .4 Spike PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS . 5 .2 6 2 5 .2 7 6 5 .2 5 7 527 7822147 8758474 6011616 10379987 5.36 0 0 5.34 46170 0 0 2618661 300.1 335.2 3 0 8 .3 4 1 5 .5 1.4 0.0 0.0 104.9 294 329 302 407 103 308 18.3 6% 101% 105% 4/27/01 6:49 4/27/01 7:00 4/27/01 7:11 4/27/01 7:23 D :\c h e m \H illa ry .l\H 0 1 0 4 2 6 .b D :\cbem \H jJJary.A H 010 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 04 26 .b SA M P LE SA M P LE S A M P LE SA M P LE H ILL0076.D H ILL0077.D H ILL0078.D H ILL0079.D P FO S -2.3.1 PF O S -2.3.2 P F O S -2.3.3 P F O S -2.3.4M S 0 4 2 3 0 1-PFO S-2.3.1 S m p 042301-P F O S -2.3.2 Dup 0 4 2 3 0 1 -P F O S -2 .3 .3 T rip 0 4 2 3 0 1 -P F O S -2.3 .4 S pike PFOS PFOS PFOS PFOS 0 0 0 5.34 0 0 0 2483685 0.0 0.0 0.0 98.1 96 98% a v e ra g e std d e v % RSD: D a y 1 re s u lts 302 12 4.0% 3M Environmental Laboratory Project# E01-0768 Page 54 of 171 Page 4 of 5 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Tlmepoint(s): Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/PFOS0425.m (ChemStatlon); Reprocessing Method: H010426tm (Target) In i D ate 4/26/01 19:14 4/26/01 19:26 4/26/01 22:02 4/26/01 22:13 4/26/01 23 :2 0 4/27/01 0:50 4/27 /01 1:01 4/27/01 1:58 4/27/01 3:28 4/27/01 3:39 4/27/01 4:46 4/27/01 6:15 4/27/01 6:27 4/27/01 7:56 4/27/01 8:08 4/27/01 10:44 4/27/01 10:55 B a tch D :\cb e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa fy.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa fy.j\H 0 1 0 4 2 6 .b D :\ch ern\H iIla ry.i\H 0 10 42 6.b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 26 .b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 26 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H D 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\ch e m \H illa ry.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b D :\ch e m \H illa fy.i\H 0 1 0 4 2 6 .b D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b Sam pTvpe SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE SA M P LE S a H ILL0014.D H ILL0015.D HILLOO S.D H ILL0030.D H ILL0036.D H ILL0044.D H ILL0045.D H ILL0050.D H ILL0058.D H ILL0059.D H 1LL0065.D H ILL0073.D H ILL 00 74 .0 H ILL0082.D H ILL0083.D H 1LL0097.D H ILL0098.D Sam D le N am e T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4 8 0 2 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH T N -A 4802 MeOH S a m p le D esc. S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t B lank S o lve n t B lank S o lve n t B lank S o lve n t B lank S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t Blank S o lve n t B lank S o lve n t B lank S o lve n t B lank Com DOund Name PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 51 5 .4 2 4 0 5 .4 1 9 5.431 0 0 0 5 .3 6 7 0 0 5.34 0 0 0 0 5.433 5.431 A re a 36585 0 65012 22312 0 0 0 31709 0 0 33691 0 O 0 0 50495 14767 Am ount B e low L O Q 0 B e lo w LO Q B e low LO Q 0 0 0 B e low LO Q 0 0 B e low LO Q 0 O 0 0 B e low LO Q 0 Page 5 of 5 3M Environmental Laboratory Project# E01 -0768 Page 55 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Day 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/PFOS0425.m (ChemStation); Reprocessing Method: H010S01t.m (Target) Quant range; 10-501 ng/mL Day 2 samples were re-aliquotted from the initial centrifuge tube on 05-01-01 Into 1.5 mL centrifuge tubes, centrifuged, and then diluted 1:100 and 1:10 for a final dilution factor of 1:1,000 prior to analysis. SampType File Sample Name Mise Info SAMPLE HILL0016.D 01003-07-01 0 ng/mL PFOS SAMPLE HILL0017.D 01003-07-02 2.5 ng/mL PFOS CALIB_1 Disabled HILL0018.D 01003-07-03 5 ng/mL PFOS CALIB_2 HILL0019.D 01003-07-04 10 ng/mL PFOS CALIB_3 HILL0020.D 01003-07-05 25 ng/mL PFOS CALIB_4 HILL0021.D 01003-07-06 40 ng/mL PFOS CALIB^S HILL0022.D 01003-07-07 50.1 ng/mL PFOS CALIB_6 HILL0023.D 01003-07-08 75.1 ng/mL PFOS CALIB~7 HILL0024.D 01003-07-09 100.2 ng/mL PFOS CALIB~8 HILL0025.D 01003-07-10 250.5 ng/mL PFOS CALIB~9 HILL0026.D 01003-07-11 400.8 ng/mL PFOS CALIB_10 HILL0027.D 01003-07-12 501 ng/mL PFOS SAMPLE HILL0028.D 01003-07-13 1002 ng/mL PFOS SAMPLE HILL0041.D 01003-07-03 5 ng/mL PFOS SAMPLE HILL0042.D 01003-07-09 100.2 ng/mL PFOS SAMPLE HILL0054.D 01003-07-03 5 ng/mL PFOS SAMPLE HILL0055.D 01003-07-09 ' 100.2 ng/mL PFOS SAMPLE HILL0058.D 01003-07-01 0 ng/mL PFOS SAMPLE HILL0059.D 01003-07-02 2.5 ng/mL PFOS CALIB_11 Disabled HILL0060.D 01003-07-03 5 ng/mL PFOS CALIB_12 HILL0061.D 01003-07-04 10 ng/mL PFOS CALIB.J3 HILL0062.D 01003-07-05 25 ng/mL PFOS CALIB~14 HILL0063.D 01003-07-06 40 ng/mL PFOS CALIBJ5 HILL0064.D 01003-07-07 50.1 ng/mL PFOS CALIB~16 HILL0065.D 01003-07-08 75.1 ng/mL PFOS CALI B--17 HILL0066.D 01003-07-09 100.2 ng/mL PFOS CALIB~18 HILL0067.D 01003-07-10 250.5 ng/mL PFOS CALI B--19 HILL0068.D 01003-07-11 400.8 ng/mL PFOS CALIB_20 HILL0069.D 01003-07-12 501 ng/mL PFOS SAMPLE HILL0070.D 01003-07-13 1002 ng/mL PFOS Compound Name RT THPFOS 5.119 THPFOS 5.116 THPFOS 5.123 THPFOS 5.122 THPFOS 5.117 THPFOS 5.117 THPFOS 5.124 THPFOS 5.118 THPFOS 5.125 THPFOS 5.124 THPFOS 5.119 THPFOS 5.115 THPFOS 5.116 THPFOS 5.129 THPFOS 5.117 THPFOS 5.122 THPFOS 5.117 THPFOS 5.131 THPFOS 5.108 THPFOS 5.115 THPFOS 5.117 THPFOS 5.117 THPFOS 5.131 THPFOS 5.111 THPFOS 5.115 THPFOS 5.122 THPFOS 5.117 THPFOS 5.103 THPFOS 5.11 THPFOS 5.115 Area 1282312 1300843 1310415 1318634 1324328 1329731 1346360 1335866 1352724 1343468 1338624 1349352 1311155 1385797 1376301 1375001 1372102 1373368 1387395 1396556 1407101 1388273 1399058 1399532 1382061 1384218 1375930 1364296 1378457 1357091 Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Compound Name PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS RT 4.39 4.388 4.409 4.408 4.41 4.409 4.416 4.411 4.404 4.417 4.411 4.408 4.408 4.408 4.41 4.401 4.402 4.409 4.407 4.401 4.417 4.416 4.416 4.411 4.401 4.415 4.402 4.403 4.402 4.407 Area Amount 1737872 254 1742704 254 1726536 254 1720895 254 1770020 254 1787802 254 1786195 254 1789034 254 1791645 254 1774591 254 1789155 254 1796642 254 1764193 254 1769946 254 1764551 254 1783815 254 1769874 254 1780686 254 1788657 254 1769985 254 1750426 254 1770162 254 1793510 254 1763775 254 1748667 254 1777945 254 1745338 254 1751400 254 1799585 254 1769921 254 3M Environmental Laboratory Project # E 0 1 -0768 Page 56 of 171 Page 1 of 4 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: MaJe/Female Normal Human Urine; Timepoint(s): Day 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/PFOS0425.m (ChemStation); Reprocessing Method: H010501t.m (Target) Quant range: 10-501 ng/mL Day 2 samples were re-aliquotted from the initial centrifuge tube on 05-01-01 into 1.5 mL centrifuge tubes, centrifuged, and then diluted 1:100 and 1:10 for a final dilution factor of 1:1,000 prior to analysis. SAMPLE HILL0031.D 042301-PFOS-LCS PFOS Solvent Blank Spike SAMPLE HILL0032.D PFOS-2.4.1blk 042301-PFOS-2.4.1 Mtd Blk SAMPLE HILL0033.D PFOS-2.4.2blk 042301-PFOS-2.4.2 Mtd Blk SAMPLE HILL0034.D PFOS~2.4.3blk 042301-PFOS-2.4,3 Mtd Blk SAMPLE HILL0035.D PFOS-2.4.4blkMS 042301-PFOS-2.4.4 Mtd Blk Spike SAMPLE HILL0037.D PFOS-2.1.1 042301-PFOS-2.1.1 Smp SAMPLE HILL0036.D PFOS-2.1.2 042301-PFOS-2.1.2 Dup SAMPLE HILL0039.D PFOS-2.1.3 042301-PFOS-2.1.3 Trip SAMPLE HILL0040.D PFOS-2.1.4MS 042301-PFOS-2.1.4 Spike SAMPLE HILL0045.D PFOS-2.2.1 042301-PFOS-2.2.1 Smp SAMPLE H1LL0046.D PFOS-2.2.2 042301-PFOS-2.2.2 Dup SAMPLE HILL0047.D PFOS-2.2.3 042301-PFOS-2.2.3 Trip SAMPLE H1LL0048.D PFOS-2.2.4MS 042301-PFOS-2.2.4 Spike SAMPLE HILL0050.D PFOS-2.3.1 042301-PFOS-2.3.1 Smp SAMPLE HILL0051.D PFOS-2.3.2 042301-PFOS-2.3.2 Dup SAMPLE HILL0052.D PFOS-2.3.3 042301-PFOS-2.3.3 Trip SAMPLE HILL0053.D PFOS-2.3.4MS 042301-PFOS-2.3.4 Spike THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.122 5.115 5.109 5.122 5.111 5.115 5.108 5.116 5.116 5.123 5.122 5.11 5.117 5.117 5.116 5.116 5.111 1322947 1317272 1319308 1316462 1318338 1215865 1161890 1218774 1224336 1256724 1246843 1245602 1219461 1211070 1227470 1222931 1223446 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4.414 4.407 4.408 4.394 4.403 4.408 4.401 4.409 4.402 4.408 4.401 4.409 4.402 4.41 4.408 4.409 4.397 1715710 1718184 1695951 1698236 1686696 1912250 1969789 1995209 1951822 1900616 1926427 1881971 1935761 1958520 1962518 1984447 1937135 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Average: 1319470 Std Deviation: 65017 %RSD: 4.9% 1806527 86617 4.8% SAMPLE SAMPLE SAM PLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0014.D TN-A 4802 MeOH HILL0015.D TN-A 4802 MeOH HILL0029.D TN-A 4802 MeOH HILL0030.D TN-A 4802 MeOH HILL0036.D TN-A 4802 MeOH HILL0043.D TN-A 4802 MeOH HILL0044.D TN-A 4802 MeOH HILL0049.D TN-A 4802 MeOH HILL0056.D TN-A 4802 MeOH HILL0057.D TN-A 4802 MeOH HILL0071.D TN-A 4802 MeOH HILL0072.D TN-A 4802 MeOH Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank ' Solvent Blank THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.189 0 5.195 0 0 0 0 0 0 0 0 0 7753 0 6699 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4.418 0 0 0 0 0 0 0 0 0 0 0 7561 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 3M Environmental Laboratory Project# E01-0768 Page 57 of 171 Page 2 of 4 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Day 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/PFOS0425.m (ChemStation); Reprocessing Method: H010501t.m (Target) Quant range: 10-501 ng/mL. Day 2 samples were re-allquotted from the initial centrifuge tube on 05-01-01 Into 1.5 mL centrifuge tubes, centrifuged, and then diluted 1:100 and 1:10 for a final dilution factor of 1:1,000 prior to analysis. SampType File Sample Name Mise Info Compound Name RT Area Amount SAMPLE HILL0016.D 01003-07-01 0 ng/mL PFOS PFOS 00 0 SAMPLE HILL0017.D 01003-07-02 2.5 ng/mL PFOS PFOS 5.326 71773 4 CALIB_1 Disabled HILL0018.D 01003-07-03 5 ng/mL PFOS PFOS 5.326 129494 6 CALIB_2 HILL0019.D 01003-07-04 10 ng/mL PFOS PFOS 5.318 230148 10 CALIB_3 HILL0020.D 01003-07-05 25 ng/mL PFOS PFOS 5.32 628525 26 CALIB_4 HILL0021.D 01003-07-06 40 ng/mL PFOS PFOS 5.32 994126 40 CALIB_5 HILL0022.D 01003-07-07 50.1 ng/mL PFOS PFOS 5.32 1255424 50 CALIB 6 HILL0023.D 01003-07-08 75.1 ng/mL PFOS PFOS . 5.321 1866886 75 CALIB 7 HILL0024.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.342 2434000 99 CALIB 8 HILL0025.D 01003-07-10 250.5 ng/mL PFOS PFOS 5.32 5704519 252 CALIB 9 HILL0026.D 01003-07-11 400.8 ng/mL PFOS PFOS 5.322 8544962 397 CALIB_10 HILL0027.D 01003-07-12 501 ng/mL PFOS PFOS 5.318 10504197 506 SAMPLE HILL0028.D 01003-07-13 1002 ng/mL PFOS PFOS 5.319 18199294 1041 SAMPLE HILL0041.D 01003-07-03 5 ng/mL PFOS PFOS 5.332 152981 7 SAMPLE HILL0042.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.32 2399378 99 SAMPLE HILL0054.D 01003-07-03 5 ng/mL PFOS PFOS 5.326 158654 7 SAMPLE HILL0055.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.32 2404840 99 SAMPLE HILL0058.D 01003-07-01 0 ng/mL PFOS PFOS 00 0 SAMPLE HILL0059.D 01003-07-02 2.5 ng/mL PFOS PFOS 5.311 72552 4 CALIB 11 Disabled HILL0060.D 01003-07-03 5 ng/mL PFOS PFOS 5.326 130239 6 CALI B--12 HILL0061.D 01003-07-04 10 ng/mL PFOS PFOS 5.32 233273 10 CALIB_13 HILL0062.D 01003-07-05 25 ng/mL PFOS PFOS 5.32 621213 25 CALIB_14 HILL0063.D 01003-07-06 40 ng/mL PFOS PFOS 5.334 994794 40 CALIB 15 HILL0064.D 01003-07-07 50.1 ng/mL PFOS PFOS 5.314 1220007 50 CALIB 16 HILL0065.D 01003-07-08 75.1 ng/mL PFOS PFOS 5.325 1796101 74 CALIB 17 HILL0066.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.325 2409666 99 CALIB 18 HILL0067.D 01003-07-10 250.5 ng/mL PFOS PFOS 5.327 5602770 251 CALIB 19 HILL0068.D 01003-07-11 400.8 ng/mL PFOS PFOS 5.313 8515207 406 CALIB 20 HILL0069.D 01003-07-12 501 ng/mL PFOS PFOS 5.313 10313769 494 SAMPLE HILL0070.D 01003-07-13 1002 ng/mL PFOS PFOS 5.325 17653606 995 % Recovery - - 105% 103% 100% 101% 100% 99% 100% 99% 101% - - 99% - 99% - - - 104% 102% 100% 99% 99% 99% 100% 101% 99% - T w o c u rv e s w e re a v e ra g e d u s in g T a r g e t s o ftw a re to q u a n tify d a ta . A s ta n d a rd c u rv e ra n g e of o n ly 1 0 le v e ls is a llo w e d . 5 -5 0 0 n g /m L w a s th e in itia l ra n g e c h o s e n . H o w e v e r, th e 5 n g /m L std d id n o t m e e t a c c e p ta n c e c rite ria , th e re fo re th e 5 n g /m L s td w a s disabled a n d th e d a ta w a s re -q u a n tifie d u s in g th e std c u rv e ra n g e 1 0 -5 0 1 n g /m L 3M Environmental Laboratory Project# E01-0768 Page 58 of 171 Page 3 of 4 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Day 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/PFOS0425.m (ChemStation); Reprocessing Method: H010501t.m (Target) Quant range: 10-501 ng/mL Day 2 samples were re-aliquotted from the Initial centrifuge tube on 05-01-01 into 1.5 mL centrifuge tubes, centrifuged, and then diluted 1:100 and 1:10 for a final dilution factor of 1:1,000 prior to analysis. Average pg/mL, dil factor corrected Sample Std Dev Purity %RSD SampTvbe SAMPLE FMe Samole Name HILL0031.D 042301-PFOS-LCS Mlsc Info PFOS Solvent Blank Spike Comoound Name S I Area Amt fna/mLI PFOS 5.325 2110116 89 corrected na/mL Spike Recovery 87 89% SAMPLE SAMPLE SAMPLE SAMPLE HILL0032.D HILL0033.D H1LL0034.D PFOS-2.4.1blk PFOS-2.4.2blk PFOS-2.4.3blk HILL0035.D PFOS-2.4.4blkMS 042301-PFOS-2.4.1 Mtd Blk 042301-PFOS-2.4.2 Mtd Blk 042301-PFOS-2.4.3 Mtd Blk 042301-PFOS-2.4.4 Mtd Blk Spike PFOS PFOS PFOS PFOS 0 0 .0 0 0 0 5.314 2188222 0 0 0 94 92 94% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0037.D HILL0038.D HILL0039.D H1LL0040.D PFOS-2.1.1 PFOS-2.1.2 PFOS-2.1.3 PFOS-2.1.4MS HILL0045.D HILL0046.D HILL0047.D HILL0048.D PFOS-2.2.1 PFOS-2.2.2 . PFOS-2.2.3 PFOS-2.2.4MS 042301-PFOS-2.1.1 Smp 042301-PFOS-2.1.2 Dup 042301-PFOS-2.1.3 Trip 042301-PFOS-2.1.4 Spike 0423O1-PFOS-2.2.1 Smp 0423O1-PFOS-2.2.2 Dup 042301-PFOS-2.2.3 Trip 042301-PFOS-2.2.4 Spike PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.248 7420988 5.248 9885661 5.256 8832844 5.249 9719956 5.263 5.255 5.25 5.257 7021826 7094280 6410858 9712496 312 421 363 417 295 294 269 421 305 358 412 54 356 15% 409 52% 289 280 288 15 263 5% 412 135% Day 2 results, ftg/mL average std dev 325 40 %RSD: 12% SAMPLE SAMPLE SAMPLE SAMPLE HILL0050.D HILL0051.D HILL0052.D HILL0053.D PFOS-2.3.1 PFOS-2.3.2 PFOS-2.3.3 PFOS-2.3.4MS 042301-PFOS-2.3.1 Smp 042301-PFOS-2.3.2 Dup 042301-PFOS-2.3.3 Trip 042301-PFOS-2.3.4 Spike PFOS PFOS PFOS PFOS 5.257 5.249 5.249 5.251 8177762 8319423 8547947 9269162 339 345 352 398 332 338 338 7 345 2% 390 53% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0014.D HILL0015.D HILL0029.D HILL0030.D HILL0036.D HILL0043.D HILL0044.D HILL0049.D HILL0056.D HILL0057.D HILL0071.D HILL0072.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.413 0 5.419 5.403 0 0 0 5.34 0 0 5.412 5.404 24002 0 40197 16788 0 0 0 23584 0 0 38878 14734 below LOQ 0 below LOQ below LOQ 0 0 0 below LOQ 0 0 below LOQ below LOQ 3M Environmental Laboratory Project# E01-0768 Page 59 of 171 Page 4 of 4 Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 2 and 3; Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010430.s/PFOS0425.m (ChemStation); Reprocessing Method: H010430tm (Target) SamoTvoe File Samle Name SAMPLE HILL0016.D 01003-07-01 Mlse Info 0 ng/mL PFOS Comoound Name THPFOS 5 1 Area 5.105 1240800 Amount 254 SAMPLE HILL0017.D 01003-07-02 2.5 ng/mL PFOS THPFOS 5.101 1259512 254 CALIB 1 HILL0018.D 01003-07-03 5 ng/mL PFOS THPFOS 5.096 1268358 254 CALIB 2 HILL0019.D 01003-07-04 10 ng/mL PFOS THPFOS 5.104 1273859 254 CALIB 3 HILL0020.D 01003-07-05 25 ng/mL PFOS THPFOS 5.103 1287880 254 CALIB 4 HILL0021.D 01003-07-06 40 ng/mL PFOS THPFOS 5.104 1293445 254 CALfB 5 HILL0022.0 01003-07-07 50.1 ng/mL PFOS THPFOS 5.105 1299052 254 CALIB 6 HILL0023.D 01003-07-08 75.1 ng/mL PFOS THPFOS 5.101 1297549 254 CALIB 7 HILL0024.D 01003-07-09 100.2 ng/mL PFOS THPFOS 5.105 1310823 254 CALIB 8 HILL0025.D 01003-07-10 250.5 ng/mL PFOS THPFOS 5.103 1305549 254 CALIB 9 HILL0026.D 01003-07-11 400.8 ng/mL PFOS THPFOS 5.103 1299241 254 CALIB 10 HILL0027.0 01003-07-12 501 ng/mL PFOS THPFOS 5.095 1306826 254 SAMPLE HILL0028.D 01003-07-13 1002 ng/mL PFOS THPFOS 5.109 1302797 254 SAMPLE HILL0041.D 01003-07-03 5 ng/mL PFOS THPFOS 5.1 1390044 254 SAMPLE HILL0042.D 01003-07-09 100.2 ng/mL PFOS THPFOS 5.103 1386912 254 SAMPLE HILL0054.D 01003-07-03 5 ng/mL PFOS THPFOS 5.103 1417554 254 SAMPLE HILL0055.D 01003-07-09 100.2 ng/mL PFOS THPFOS 5.101 1416339 254 SAMPLE HILL0068.D 01003-07-03 5 ng/mL PFOS THPFOS 5.11 1463633 254 SAMPLE HILL0069.D 01003-07-09 100.2 ng/mL PFOS THPFOS 5.103 1453681 254 SAMPLE HILL0081.D 01003-07-03 5 ng/mL PFOS THPFOS 5.098 1482897 254 SAMPLE HILL0082.D 01003-07-09 100.2 ng/mL PFOS THPFOS 5.101 1463161 254 SAMPLE HILL0085.D 01003-07-01 0 ng/mL PFOS THPFOS 5.101 1470609 254 SAMPLE HILL0086.D 01003-07-02 2.5 ng/mL PFOS THPFOS 5.095 1481303 254 CALIB 11 HILL0087.D 01003-07-03 5 ng/mL PFOS THPFOS 5.097 1492012 254 CALIB 12 HILL0088.D 01003-07-04 10 ng/mL PFOS THPFOS 5.095 1477732 254 CALI8 13 HILL0089.D 01003-07-05 25 ng/mL PFOS THPFOS 5.112 1481121 254 CALIB 14 HLL0090.D 01003-07-06 40 n g /m l PFOS THPFOS 5.095 1479643 254 CALIB 15 HILL0091.D 01003-07-07 50.1 ng/mL PFOS THPFOS 5.095 1475404 254 CALIB 16 HILL0092.D 01003-07-08 75.1 ng/mL PFOS THPFOS 5.094 1469508 254 CALIB 17 HILL0093.D 01003-07-09 100.2 ng/mL PFOS THPFOS 5.096 1496019 254 CALIB 18 HILL0094.D 01003-07-10 250.5 ng/mL PFOS THPFOS 5.109 1476250 254 CALIB 19 HILL0095.D 01003-07-11 400.8 ng/mL PFOS THPFOS 5.097 1466888 254 CALIB 20 HILL0096.D 01003-07-12 501 ng/mL PFOS THPFOS 5.109 1475286 254 SAMPLE HILL0097.D 01003-07-13 1002 ng/mL PFOS THPFOS 5.103 1440061 254 SAMPLE HILL0031.D 042301-PFOS-LCS SAMPLE HILL0032.D PFOS-2.4.1blk SAMPLE HILL0033.D PFOS-2.4.2blk SAMPLE HILL0034.D PFOS-2.4.3blk SAMPLE HILL0035.D PFOS-2.4.4blkMS SAMPLE HILL0037.D PFOS-2.1.1 SAMPLE HILL0038.D PFOS-2.1.2 SAMPLE HILL0039.D PFOS-2.1.3 SAMPLE HILL0040.D PFOS-2.1.4MS SAMPLE HILL0045.D PFOS-2.2.1 SAMPLE HILL0046.D PFOS-2.2.2 SAMPLE HILL0047.D PFOS-2.2.3 SAMPLE HILL0048.D PFOS-2.2.4MS SAMPLE HILL0050.D PFOS-2.3.1 SAMPLE HILL0051.D PFOS-2.3.2 SAMPLE HILL0052.D PFOS-2.3.3 SAMPLE HILL0053.D PFOS-2.3.4MS PFOS Solvent Blank Spike 042301 -PFOS-2.4.1 MtdBIk 042301-PFOS-2.4.2 Mtd BIk 042301-PFOS-2.4.3 Mtd BIk 042301-PFOS-2.4.4 Mtd BIk Spike 042301-PFOS-2.1.1 Smp 042301-PFOS-2.1.2 Dup 042301-PFOS-2.1.3 Trip 042301-PFOS-2.1.4 Spike 042301-PFOS-2.2.1 Smp 042301-PFOS-2.2.2 Dup 042301-PFOS-2.2.3 Trip 042301-PFOS-2.2.4 Spike 042301-PFOS-2.3.1 Smp 042301-PFOS-2.3.2 Dup 042301-PFOS-2.3.3 Trip 042301-PFOS-2.3.4 Spike THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.095 5.096 5.101 5.103 5.095 5.101 5.102 5.102 5.104 5.101 5.096 5.102 5.102 5.103 5.097 5.096 5.096 1325456 1344481 1347423 1347097 1324124. 1163460 1199081 1228695 1219919 1364440 1385823 1392690 1376257 1367578 1373402 1382100 1373073 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Page 60 of 171 Page 1 of 5 BACK TO MAIN Comoound Name PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS RI 4.384 4.38 4.382 4.382 4.382 4 .3 7 6 4.376 4.38 4.376 4.375 4.375 4.374 4.381 4.386 4.381 4.381 4.373 4.381 4.382 4.391 4.401 4.394 4.394 4.396 4.394 4.397 4.394 4.388 4.394 4.395 4.395 4.396 4.38 4.382 4.381 4.375 4.379 4.389 4.38 4.387 4.388 4.387 4.383 4.387 4.382 4.381 4.374 4.374 4.376 4.374 4.374 A re a 1897371 1883485 1898698 1894001 1891481 1895316 1887750 1894332 1899388 1877817 1884885 1906259 1898513 1873917 1895596 1870203 1863988 1941991 1934618 1898558 1912978 1882104 1898530 1905370 1894008 1892338 1891942 1897650 1911398 1928086 1869148 1898244 1911397 1902178 A m ount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 1823070 1834828 1867721 1835565 1847790 1968845 2112105 2098049 2057424 1826163 1818895 1022627 1820132 1841611 1797985 1016031 1843565 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 3M Environmental Laboratory Project# E01-0768 Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 2 and 3; Analytical Instrument: HPLC/MSD "Hillary"; SAMPLE HILL0058.D 042301-PFOS-LCS PFOS Solvent Blank Spike THPFOS SAMPLE HILL0059.D PFOS-3.4.1blk 042301-PFOS-3.4.1 Mtd Blk THPFOS SAMPLE HILL0060.D PFOS-3.4.2blk 042301-PFOS-3.4.2 Mtd Blk THPFOS SAMPLE HILL0061.D PFOS-3.4.3blk 042301-PPOS-3.4.3 Mtd Blk THPFOS SAMPLE HILL0062.D PFOS-3.4.4blkMS 042301-PFOS-3.4.4 Mtd Blk Spike THPFOS SAMPLE HILL0064.D PFOS-3.1.1 042301-PFOS-3.1.1 Smp THPFOS SAMPLE HILL0065.D PFOS-3.1.2 042301-PFOS-3.1.2 Dup THPFOS SAMPLE HILL0066.D PFOS-3.1.3 042301-PFOS-3.1.3 Trip THPFOS SAMPLE HILL0067.D PFOS-3.1.4MS 042301-PFOS-3.1.4 Spike THPFOS SAMPLE HILL0072.D PFOS-3.2.1 042301-PFOS-3.2.1 Smp THPFOS SAMPLE HILL0073.D PFOS-3.2.2 042301-PFOS-3.2.2 Dup THPFOS SAMPLE H ILL0074.D PFOS-3.2.3 042301-PFOS-3.2.3 Trip THPFOS SAMPLE HILL0075.D PFOS-3.2.4MS 042301-PFOS-3.2.4 Spike THPFOS SAMPLE HILL0077.D PFOS-3.3.1 042301-PFOS-3.3.1 Smp THPFOS SAMPLE HILL0078.D PFOS-3.3.2 042301-PFOS-3.3.2 Dup THPFOS SAMPLE HILL0079.D PFOS-3.3.3 042301-PFOS-3.3.3 Trip THPFOS SAMPLE HILL0080.D PFOS-3.3.4MS 042301-PFOS-3.3.4 Spike THPFOS 5.095 5.098 5.096 5.098 5.103 5.097 5.109 5.102 5.107 5.105 5.109 5.111 5.104 5.104 5.11 5.101 5.098 1394750 1419875 1420804 1433374 1406537 1310521 1294952 1296261 1334559 1305210 1308424 1312470 1289916 1325618 '1332228 1339789 1327428 254 ' 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Average: 1364258.28 Std Deviation: 82080 %RSD: 6.0% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0014.D HILL0015.D HILL0029.D HILL0030.D HILL0036.D HILL0043.D HILL0044.D HILL0049.D HILL0056.D HILL0057.D HILL0063.D HILL0070.D HILL0071.D HILL0076.D HILL0083.D HILL0084.D HILL0098.D HILL0099.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4002 MeOH TN-A 4802 MeOH TN-A 4002 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 0 0 0 0 0 0 0 5.178 0 0 0 0 0 0 5.172 0 5.2 0 0 0 0 0 0 0 0 7634 0 0 0 0 0 0 8030 0 7970 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page 61 of 171 Page 2 o f5 BACK TO MAIN PFE3S PFBS PFBS PFBS PFBS PFBS PFBS PFBSPFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4.367 4.363 4.368 4.369 4.375 4.376 4.38 4.38 4.379 4.384 4.388 4.39 4.397 4.397 4.389 4.386 4.383 0 0 0 0 0 4.409 0 0 0 0 0 0 0 4.423 0 0 0 0 1828732 1870275 1875725 1883710 1858704 2034585 2079222 2046016 2057849 2128725 2170045 2160742 2146697 2084860 2030571 2064866 2068536 1925085.4 95672 5.0% 0 0 0 0 0 7786 0 0 0 0 0 0 0 7887 0 0 0 0 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 3M Environmental Laboratory Project # E 0 1 -0768 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 2 and 3; Analytical Instrument: HPLC/MSD "Hillary"; SampTvpe File SAMPLE HILL0016.D Sample Name 01003-07-01 Mise Info 0 ng/mL PFOS Compound Name PFOS El 0 Area 0 Amt fna/mU 0.0 SAMPLE HILL0017.D 01003-07-02 2.5 ng/mL PFOS PFOS 5.311 77068 3.4 CALIB 1 HILL0018.D 01003-07-03 5 ng/mL PFOS PFOS 5.306 140922 5.7 CALIB 2 HILL0019.D 01003-07-04 10 ng/mL PFOS PFOS 5.314 250842 9.8 C ALIB 3 HILL0020.D 01003-07-05 25 ng/mL PFOS PFOS 5.313 644213 24.7 CALIB 4 HILL0021.D 01003-07-06 40 ng/mL PFOS PFOS 5.307 1035507 39.7 CALIB 5 HILL0022.D 01003-07-07 50.1 ng/mL PFOS PFOS 5.308 1297981 50.1 CALIB 6 HILL0023.D 01003-07-08 75.1 ng/mL PFOS PFOS 5.311 1923999 74.8 CALIB 7 HILL0024.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.308 2507092 98.2 CALIB 8 HILL0025.D 01003-07-10 250.5 ng/mL PFOS PFOS 5.306 5879693 248.2 CALIB 9 HILL0026.D 01003-07-11 400.8 ng/mL PFOS PFOS 5.306 8875074 394.1 O> t-- |03 O HILL0027.D SAMPLE HILL0028.D 01003-07-12 01003-07-13 501 ng/mL PFOS 1002 ng/mL PFOS ' PFOS PFOS 5.305 5.312 10870332 18717748 493.2 968.5 SAMPLE HILL0041.D 01003-07-03 5 ng/mL PFOS PFOS 5.31 163873 6.7 SAMPLE HILL0042.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.306 2519548 98.9 SAMPLE HILL0054.D 01003-07-03 5 ng/mL PFOS PFOS 5.313 136445 5.6 SAMPLE HILL0055.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.312 2484938 99.2 SAMPLE HILL0068.D 01003-07-03 5 ng/mL PFOS PFOS 5.32 166490 6.5 SAMPLE HILL0069.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.306 2588211 99.5 SAMPLE HILL0081.D 01003-07-03 5 ng/mL PFOS PFOS 5.301 162640 6.5 SAMPLE HILL0082.D 01003-07-09 100.2 ng/mL PFOS PFOS 5.304 2575229 100.2 SAMPLE H1LL0085.D 01003-07-01 0 ng/mL PFOS PFOS 00 0.0 SAMPLE HILL0086.D 01003-07-02 2.5 ng/mL PFOS PFOS . 5.298 74899 3.3 C A LIB 11 H IL L0 08 7 .D 0 1003-07-03 5 ng/mL PFOS PFOS 5.3 138171 5.8 C A LIB 12 H IL L0 08 8 .D 01003-07-04 10 ng/mL PFOS PFOS 5.298 248359 9.7 C A LIB 13 H IL L0 08 9 .D 01003-07-05 25 ng/mL PFOS PFOS 5.322 648497 24.9 C A LIB 14 H IL L0 09 0 .D 0 1003-07-06 40 ng/mL PFOS PFOS 5.298 1030084 39.6 C A LIB 15 H IL L0 09 1 .D 01003-07-07 50.1 ng/mL PFOS PFOS 5.298 1323882 50.9 CA LIB 16 H IL L0 09 2 .D 01003-07-08 75.1 ng/mL PFOS PFOS 5.304 1963056 75.6 CA LIB 17 H IL L0 09 3 .D 01003-07-09 100.2 ng/mL PFOS PFOS 5.299 2594831 100.2 CA LIB 18 H1LL0094.D 01003-07-10 250.5 ng/mL PFOS PFOS 5.312 6013719 255.9 CA LIB 19 H IL L0 09 5 .D 01003-07-11 400.8 ng/mL PFOS PFOS 5.3 9177063 406.4 CALIB 20 HILL0096.D 01003-07-12 501 ng/mL PFOS PFOS 5.319 11174689 508.1 SAMPLE HILL0097.D 01003-07-13 1002 ng/mL PFOS PFOS 5.313 18959651 982.2 Two curves w e re averaged using Ta rg et software to quantify data. A standard curve range o f o n ly 10 levels Is allowed. 5-500 ng/m L was the range chosen. %Recovery 114% 98% 99% 99% 100% 100% 98% 99% 98% 98% 133% 99% 113% 99% 100% 99% 130% 100% - 112% 97% 100% 99% 102% 101% 100% 102% 101% 101% - 3M Environmental Laboratory Project # E01-0768 Page 62 of 171 Page 3 of 5 Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepointfs): Days 2 and 3; Analytical Instrument: HPLC/MSD "Hillary"; SampTypeI nie Samle Name SAMPLE SAMPLE SAMPLE SAMPLE HILL0031.D 042301-PFOS-LCS HILL0032.D PFOS-2.4.1blk HILL0033.D PFOS-2.4.2bIk HILL0034.D PFOS-2.4.3blk SAMPLE HILL0035.D PFOS-2.4.4blkMS Misc Info 042301-PFOS-2.4.1 Mtd Blk 042301-PFOS-2.4.2 Mtd Blk 042301-PFOS-2.4.3 Mtd Blk 042301-PFOS-2.4.4 Mtd Blk Spike SAMPLE SAMPLE SAMPLE SAMPLE HILL0037.D HILL0038.D HILL0039.D HILL0040.D PFOS-2.1.1 PFOS-2.1.2 PFOS-2.1.3 PFOS-2.1.4MS 042301-PFOS-2.1.1 Smp 042301-PFOS-2.1.2 Dup 042301-PFOS-2.1.3 Trip 042301-PFOS-2.1.4 Spike SAMPLE SAMPLE SAMPLE SAMPLE HILL0045.D HILL0046.D HILL0047.D HILL0Q48.D PFOS-2.2.1 PFOS-2.2.2 PFOS-2.2.3 PFOS-2.2.4MS 042301-PFOS-2.2.1 Smp 042301-PFOS-2.2.2 Dup 042301-PFOS-2.2.3 Trip 042301-PFOS-2.2.4 Spike SAMPLE HILL0050.D SAMPLE HILL0051.D SAMPLE HILL0052.D PFOS-2.3.1 PFOS-2.3.2 PFOS-2.3.3 SAMPLE HILL0053.D PFOS-2.3.4MS SAMPLE HILL0058.D 042301-PFOS-LCS 042301-PFOS-2.3.1 Smp 042301-PFOS-2.3.2 Dup 042301-PFOS-2.3.3 Trip 042301-PFOS-2.3.4 Spike PFOS Solvent Blank Spike SAMPLE HILL0059.D SAMPLE HILL0Q60.D SAMPLE HILL0061.D PFOS-3.4.1bIk PFOS-3.4.2blk PFOS-3.4.3b!k SAMPLE HILL0062.D PFOS-3.4.4b!kMS 042301-PFOS-3.4.1 Mtd Blk 042301-PFOS-3.4.2 Mtd Blk 042301-PFOS-3.4.3 Mtd Blk 042301-PFOS-3.4.4 Mtd Blk Spike SAMPLE SAMPLE SAMPLE SAMPLE HILL0064.D HILL0065.D HILL0066.D HILL0Q67.D PFOS-3.1,1 PFOS-3.1.2 PFOS-3.1.3 PFOS-3.1.4MS 042301-PFOS-3.1.1 Smp 042301-PFOS-3.1.2 Dup 042301-PFOS-3.1.3 Trip 042301-PFOS-3.1.4 Spike SAMPLE SAMPLE SAMPLE SAMPLE HILL0072.D HILL0073.D HILL0074.D HILL0075.D PFOS-3.2.1 PFOS-3.2.2 PFOS-3.2.3 PFOS-3.2.4MS 042301-PFOS-3.2.1 Smp 042301-PFOS-3.2.2 Dup 042301-PFOS-3.2.3 Trip 042301-PFOS-3.2.4 Spike SAMPLE HILL0077.D SAMPLE HILL0078.0 SAMPLE HJLL0079.D SAMPLE HILL0080.D PFOS-3.3.1 PFOS-3.3.2 PFOS-3.3.3 PFOS-3.3.4MS 042301-PFOS-3.3.1 Smp 042301-PFOS-3.3.2 Dup 042301-PFOS-3.3.3 Trip 042301-PFOS-3.3.4 Spike Comeound Name PFOS PFOS PFOS PFOS PFOS SI 5.305 0 0 0 5.305 Area 2196915 0 0 0 2461943 PFOS PFOS PFOS PFOS 5.235 5.242 5.242 5.237 7481346 9178901 8215875 9849022 PFOS PFOS PFOS PFOS 0 0 0 5.305 0 0 0 2441252 PFOS PFOS PFOS PFOS PFOS 0 0 0 5.306 5.305 0 0 0 2368154 2208565 PFOS PFOS PFOS PFOS 0 0 0. 5.313 0 0 0 2459314 PFOS PFOS PFOS PFOS 5.237 5.242 5.242 5.247 6815087 7544482 6794540 8532934 PFOS PFOS PFOS PFOS 5.245 5.249 5.251 5.237 8117378 8786445 9095599 11117925 PFOS PFOS PFOS PFOS 5.238 5.243 5.234 5.238 7558687 6689145 7103605 9203477 Amt fnafmU 89.3 0.0 0.0 0.0 99.1 308.4 359.3 319.1 401.7 0.0 0.0 0.0 99.8 0.0 0.0 0.0 95.4 89.5 0.0 0.0 0.0 98.4 267.6 292.7 265.0 340.5 308.4 359.3 319.1 401.7 292.4 262.7 275.7 369.2 Page 63 of 171 Pago 4 of 5 BACK TO MAIN Sample Purity corrected no/mL 87 Average pg/mL Std Dev %RSD Spike Recovery 89% 97 99% 302 322 352 26.5 312 8% 393 72% 100% 93 95% 88 90% 96 262 287 ' 259 333 302 352 312 393 286 257 270 361 98% 269 15.4 6% 65%. 322 26.5 8% 72% 271 14.5 5% 92% average std dev %RSD: Day 3 results 287 30 10.4% 3M Environmental Laboratory Project # E01-0768 Solubility Study, Shake Flask Method; Test Compound: PFOS; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 2 and 3; Analytical Instrument: HPLC/MSD "Hillary"; SAMPLE HILL0014.D TN-A 4802 MeOH SAMPLE HILL0015.D TN-A 4802 MeOH SAMPLE HILL0029.D TN-A 4802 MeOH SAMPLE HILL0030.D TN-A 4802 MeOH SAMPLE HILL0036.D TN-A 4802 MeOH SAMPLE HILL0043.D TN-A 4802 MeOH SAMPLE H1LL0044.D TN-A 4802 MeOH SAMPLE HILL0049.D TN-A 4802 MeOH SAMPLE HILL0056.D TN-A 4802 MeOH SAMPLE HILL0057.D TN-A 4802 MeOH SAMPLE HILL0063.D TN-A 4802 MeOH SAMPLE HILL0070.D TN-A 4802 MeOH SAMPLE HILL0071.D TN-A 4802 MeOH SAMPLE HILL0076.D TN-A 4802 MeOH SAMPLE HILL0083.D TN-A 4802 MeOH SAMPLE HILL0084.D TN-A 4802 MeOH SAMPLE HILL0098.D TN-A 4802 MeOH SAMPLE HILL0099.D TN-A 4802 MeOH Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank Solvent Blank PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS 5.398 0 0 0 0 0 0 0 0 0 0 0 0 5.333 0 0 5.424 5.404 27635 0 0 0 0 0 0 0 0 0 0 0 0 30130 0 0 47439 15154 Below LOQ 0 0 0 0 0 0 0 0 0 0 0 0 Below LOQ 0 0 Below LOQ Below LOQ Page 64 of 171 Page 5 of 5 3M Environmental Laboratory Project # E01-0768 BACK TO MAIN BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/FOSA0425.m (ChemStation); Reprocessing Method: H010426a.m (Target) SampType Pile Sample Name Mise Info Compound Name RT Area ' Amount Compound Name RT SAMPLE SAMPLE CALIB_1 XX CALIB_2 CALIB_3 CALIB_4 CALIB_5 CALIB_6 CALIB_7 CALIB_8 CALIB_9 CALIB_10 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE CALIB_11 XX CALIBJ2 CALIBJ3 CALIB_14 CALIB_15 CALIB_16 CALIB_17 CALIB_18 CALIB_19 CAUB_20 SAMPLE SAMPLE HILL0105.D H1LL0106.D HILL0107.D HILL0108.D HILL0109.D HILL0110.D HILL0111.D HILL0112.D H1LL0113.D HILL0114.D HILL0115.D HILL0116.D HILL0117.D HILL0131.D HILL0132.D H1LL0146.D HILL0147.D HILL0161.D HILL0162.D HILL0171.D HILL0172.D HILL0173.D HH.L0174.D HILL0175.D HILL0176.D HILL177.D HILL0178.D HILL0179.D HILL0180.D HILL0181.D HILL0182.D HILL0183.D HILL0120.D SAMPLE SAMPLE SAMPLE SAMPLE HILL0121.D HILL0122.D HILL0123.D ' HILL0124.D 01003-25-01 01003-25-02 01003-25-03 01003-25-04 01003-25-05 01003-25-06 01003-25-07 01003-25-08 01003-25-09 01003-25-10 01003-25-11 01003-25-12 01003-25-13 01003-25-03 01003-25-09 01003-25-03 01003-25-09 01003-25-03 01003-25-09 01003-25-01 01003-25-02 01003-25-03 01003-25-04 01003-25-05 01003-25-06 01003-25-07 01003-25-08 01003-25-09 01003-25-10 01003-25-11 01003-25-12 01003-25-13 042301-FOSA-LCS FOSA-1.4.1blk FOSA-1.4.2blk FOSA-1.4.3blk FOSA-1.4.4blkMS ' 0 Std 2.5 ng/mL FOSA 5.3 ng/mL FOSA 10.1 ng/mL FOSA 25 ng/mL FOSA 40.3 ng/mL FOSA 49.9 ng/mL FOSA 74.9 ng/mL FOSA 100.8 ng/mL FOSA 249.6 ng/mL FOSA 403.2 ng/mL FOSA 499.2 ng/mL FOSA 1008 ng/mL FOSA 5.3 ng/mL FOSA 100.8 ng/mL FOSA ' 5.3 ng/mL FOSA 100.8 ng/mL FOSA 5.3 ng/mL FOSA 100.8 ng/mL FOSA 0 Std 2.5 ng/mL FOSA 5.3 ng/mL FOSA 10.1 ng/mL FOSA 25 ng/mL FOSA 40.3 ng/mL FOSA 49.9 ng/mL FOSA 74.9 ng/mL FOSA 100.8 ng/mL FOSA 249.6 ng/mL FOSA 403.2 ng/mL FOSA 499.2 ng/mL FOSA 1008 ng/mL FOSA THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.123 5.111 5.116 5.116 5.109 5.118 5.115 5.116 5.112 ' 5.115 5.116 5.112 5.116 5.11 5.119 5.11 5.111 5.111 5.115 5.115 5.116 5.118 5.109 5.115 5.11 5.109 5.107 5.112 5.124 5.117 5.123 5.119 5.109 5.108 5.115 5.117 5.116 1465515 1447576 1439545 1445222 1441747 1427400 1441987 1447199 1441812 1459549 1432834 1428416 1447369 1265387 1298469 1170043 1177767 1145578 1120490 1122982 1107259 1096459 1125849 1101993 1104242 1111672 1107520 1113145 1124167 1114186 1126570 1146487 1387790 1379938 1385495 1413232 13887B7 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4.394 4.39 4.395 4.401 4.387 4.389 4.386 4.395 4.39 4.394 4.395 4.39 4.387 4.381 4.39 4.382 4.389 4.389 4.393 4.394 4.388 4.383 4.388 4.387 4.389 4.388 4.386 4.391 4.395 4.389 4.387 4.383 4.381 4.38 4.387 4.381 4.387 SAMPLE SAMPLE SAMPLE SAMPLE HILL0126.D HILL0127.D HILL0128.D HILL0129.D FOSA-1.1.1 FOSA-1.1.2 FOSA-1.1.3 FOSA-1.1.4MS THPFOS THPFOS THPFOS THPFOS 5.112 5.112 5.115 5.11 1223896 1207970 1198241 1184556 254 254 254 254 PFBS PFBS PFBS PFBS 4.391 4.384 4.387 4.381 SAMPLE SAMPLE SAMPLE SAMPLE HILL0130.D HILL0135.D HILL0136.D HILL0137.D FOSA-1.2.1 FOSA-1.2.2 FOSA-1.2.3 FOSA-1.2.4MS THPFOS THPFOS THPFOS THPFOS 5.118 5.108 5.11 5.11 1223960 1227152 1210108 1202734 254 254 254 254 PFBS PFBS PFBS PFBS 4.383 4.379 4.375 4.382 Area 2007446 2027800 2026487 2021996 2015250 2007486 2028225 2012838 1997221 1999512 2008100 1999395 1988333 1993211 1945472 1974246 1924449 1984007 1933728 1989610 1975741 1962904 1986462 1965181 1958152 1969738 1941113 1940454 1955186 1940675 1933249 1964405 1875014 1893699 1872319 1876934 1861408 1863247 1889163 1858991 1860013 1887871 1901597 1890574 1875132 Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 3M Environmental Laboratory Project# E01-0768 Page 65 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepolnt(s): Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/FOSA0425.m (ChemStation); Reprocessing Method: H010426a.m (Target) SAMPLE SAMPLE SAMPLE SAMPLE HILL0138.D HILL0139.D HILL0141.D HILL0142.D FOSA-1.3.1 FOSA-1.3.2 FOSA-1.3.3 FOSA-1.3.4MS THPFOS THPFOS THPFOS THPFOS 5.112 5.109 5.116 5.116 1177514 1188089 1173989 1179158 254 254 254 254 PFBS PFBS PFBS PFBS 4.39 4.381 4.381 4.388 SAMPLE HILL0143.D 042301-FOSA-LCS THPFOS 5.116 1152061 254 PFBS 4.395 SAMPLE SAMPLE SAMPLE SAMPLE HILL0144.D HILL0145.D HILL0150.D HILL0151.D FOSA-2.4.1blk FOSA-2.4.2blk FOSA-2.4.3blk FOSA-2.4.4blkMS THPFOS THPFOS THPFOS THPFOS 5.112 5.115 5.109 5.116 1308838 1332634 1307643 1312788 254 254 254 254 PFBS PFBS PFBS PFBS 4.383 4.386 4.38 4.387 SAMPLE SAMPLE SAMPLE SAMPLE HILL0152.D HILL0153.D HILL0154.D HILL0156.D FOSA-2.1.1 FOSA-2.1.2 FOSA-2.1.3 FOSA-2.1.4MS THPFOS THPFOS THPFOS THPFOS 5.116 5.109 5.116 5.116 1110585 1194990 1181747 1165222 254 254 254 254 PFBS PFBS PFBS PFBS 4.387 4.388 4.388 4.388 SAMPLE SAMPLE SAMPLE SAMPLE HILL0157.D HILL0158.D HILL0159.D HILL0160.D FOSA-2.2.1 FOSA-2.2.2 FOSA-2.2.3 FOSA-2.2.4MS THPFOS THPFOS THPFOS THPFOS 5.116 5.115 5.109 5.11 1202436 1233448 1228256 1224603 254 254 254 254 PFBS PFBS PFBS PFBS 4.388 4.387 4.388 4.389 SAMPLE SAMPLE SAMPLE SAMPLE HILL0165.D HILL0166.D HILL0167.D HILL0168.D FOSA-2.3.1 FOSA-2.3.2 FOSA-2.3.3 FOSA-2.3.4MS THPFOS THPFOS THPFOS THPFOS 5.116 5.111 5.117 5.116 1158902 1162327 1177491 1181915 254 254 254 254 PFBS PFBS PFBS PFBS 4.395 4.39 4.388 4.387 Average: Std Deviation: %RSD: 1249014 125832 10.1% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0103.D HILL0104.D HILL0118.D HILL0119.D HILL0125.D HILL0133.D HILL0134.D HILL0140.D HILL0148.D HILL0149.D HILL0155.D HILL0163.D HILL0164.D HILL0169.D HILL0170.D HILL0184.D HILL0185.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 0 0 5,187 0 0 0 0 0 0 0 0 0 0 0 0 0 0 O 0 8097 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4.426 0 4.403 0 4.41 4.409 4.408 4.403 4.41 0 4.41 4.417 0 4.403 0 4.415 0 1900215 1882956 1853824 1873732 1836551 1875879 1889627 1868213 1876885 1783250 1910331 1870518 1853384 1863768 1900272 1907383 1899528 1883593 1866181 1891600 1875392 1926471 60064 3.1% 10752 0 9817 0 10811 10138 7466 11533 10126 0 10883 9378 0 9038 0 9491 0 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Page 2 of 5 3M Environmental Laboratory Project# E01-0768 Page 6 6 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days la n d 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/FOSA0425.m (ChemStation); Reprocessing Method: H010426a.m (Target) SampType File Sample Name Mise Info Compound ame RT Area Amount SAMPLE SAMPLE HILL0105.D HILL0106.D 01003-25-01 01003-25-02 0 Std 2.5 ng/mL FOSA FOSA FOSA 0 5.973 0 92513 0.0 1.8 % Recovery Excluded Excluded CALIB 1 XX CALIB_2 CALIB_3 HILL0107.D HILL0108.D HILL0109.D 01003-25-03 01003-25-04 01003-25-05 5.3 ng/mL FOSA 10.1 ng/mL FOSA 25 ng/mL FOSA FOSA FOSA FOSA 5.977 5.977 5.977 175825 333744 832878 4.5 9.5 25.6 Excluded 94.1% 102.4% CALIB_4 CALIB_5 HILL0110.D HILL0111.D 01003-25-06 01003-25-07 40.3 ng/mL FOSA 49.9 ng/mL FOSA FOSA FOSA 5.979 5.976 1346447 1622197 42.5 51.0 105.4% 102.2% CALIB_6 CALIB_7 CALIB_8 CALIB_9 CALIB_10 SAMPLE HILL0112.D HILL0113.D HILL0114.D HILL0115.D HILL0116.D HILL0117.D 01003-25-08 01003-25-09 01003-25-10 01003-25-11 01003-25-12 01003-25-13 74.9 ng/mL FOSA 100.8 ng/mL FOSA 249.6 ng/mL FOSA 403.2 ng/mL FOSA 499.2 ng/mL FOSA 1008 ng/mL FOSA FOSA FOSA FOSA FOSA FOSA FOSA 5.978 5.98 5.976 5.978 5.973 5.977 2412994 3249134 7439185 11510014 13881086 24702641 77.6 106.6 255.5 409.4 507.2 998.1 103.6% 105.8% 102.4% 101.5% 101.6% Excluded SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0131.D HILL0132.D HILL0146.D HILL0147.D HILL0161.D HILL0162.D HILL0171.D 01003-25-03 01003-25-09 01003-25-03 01003-25-09 01003-25-03 01003-25-09 01003-25-01 5.3 ng/mL FOSA 100.8 ng/mL FOSA 5.3 ng/mL FOSA 100.8 ng/mL FOSA 5.3 ng/mL FOSA 100.8 ng/mL FOSA 0 Std FOSA FOSA FOSA FOSA FOSA FOSA FOSA 5.971 5.973 5.965 5.965 5.972 5.969 0 200577 3024244 157381 2919745 190625 2792405 0 5.3 101.7 4.0 99.1 5.1 94.2 0.0 Excluded 100.9% Excluded 98.4% Excluded 93.4% Excluded SAMPLE CALIB 11 XX CALIBJ2 CALIBJ 3 CALIB_14 CALIB_15 CALIBJ6 CALIBJ 7 HILL0172.D HILL0173.D HILL0174.D HILL0175.D HILL0176.D HILL0177.D HILL0178.D HILL0179.D 01003-25-02 01003-25-03 01003-25-04 01003-25-05 01003-25-06 01003-25-07 01003-25-08 01003-25-09 2.5 ng/mL FOSA 5.3 ng/mL FOSA 10.1 ng/mL FOSA 25 ng/mL FOSA 40.3 ng/mL FOSA 49.9 ng/mL FOSA 74.9 ng/mL FOSA 100.8 ng/mL FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA 5.964 5.973 5.971 5.969 5.958 5,964 5.969 5.966 75933 152433 297834 743034 1216120 1485755 2183173 2971186 1.4 3.9 8.5 23.3 39.2 48.0 72.6 100.1 Excluded Excluded 84.4% 93.2% 97.3% 96.1% 97.0% 99.3% CALIB_18 CALIB_19 CALIB_20 SAMPLE HILL0180.D HILL0181.D HILL0182.D HILL0183.D 01003-25-10 01003-25-11 01003-25-12 01003-25-13 249.6 ng/mL FOSA 403.2 ng/mL FOSA 499.2 ng/mL FOSA 1008 ng/mL FOSA FOSA FOSA FOSA FOSA 5.971 5.972 5.977 5.973 6959290 10720207 13077641 23820299 243.7 393.0 492.6 969.4 97.6% 97.5% 98.7% Excluded " Only 10 levels may be quantified due to software limitations, therefore 5-500 ng/mL was chosen. However, since not all blank samples had a FOSA response of less than half the 5 ng/mL response, the 5 ng/mL standard was disabled and the LOQ becam Page 3 of 5 3M Environmental Laboratory Project # E 0 1 -0768 Page 67 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days 1 and 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/FOSA0425.m (ChemStation); Reprocessing Method: H010426a.m (Target) .' Calculations Average (pg/mL) Std Dev on-column dll factor corrected % RSD SampType File Sample Name Misc Info Compound ame RT Area Amount ng/mL FOSA Spike % Recov. SAMPLE SAMPLE SAMPLE SAMPLE HILL0120.D HILL0121.D HILL0122.D HILL0123.D 042301-FOSA-LCS FOSA-1.4.1blk FOSA-1.4.2b!k FOSA-1.4.3blk FOSA Solvent Blank Spike 042301-FOSA-1.4.1 Mtd Blk 042301-FOSA-1.4.2 Mtd Blk 042301-FOSA-1.4.3 Mtd Blk FOSA FOSA FOSA FOSA 5.971 5.893 0 5.894 3056177 106755 0 135380 107 3 0 4 0.00 0.00 0.04 111% SAMPLE HILL0124.D FOSA-1,4.4b!kMS 42301-FOSA-1.4.4 Mtd Blk Spike FOSA 5.977 2921968 103 107% SAMPLE SAMPLE SAMPLE SAMPLE HILL0126.D HILL0127.D HILL0128.D HILL0129.D FOSA-1.1.1 FOSA-1.1.2 FOSA-1.1.3 FOSA-1.1.4MS 042301-FOSA-1.1.1 Smp 042301 -FOSA-1.1.2 Dup 042301-F0SA-1.1.3 Trip 042301-FOSA-1.1.4 Spike PQ3A FOSA FOSA FOSA M9 5.89 5.88S 5.887 9090670 6180725 5838914 8313598 343 223 213 312 3.43 2.60 2.18 2.23 0.7 4.4% Rep2,3 RPD 2.13 .. 28% ; 3.12 98% -based on reps 2&3 only SAMPLE SAMPLE SAMPLE SAMPLE HILL0130.D HILL0135.D HILL0136.D HILL0137.D FOSA-1.2.1 FOSA-1.2.2 FOSA-1.2.3 FOSA-1.2.4MS 042301-FOSA-1.2.1 Smp ' 042301-FOSA-1.2.2 Dup 042301-FOSA-1.2.3 Trip 042301-FOSA-1.2.4 Spike FOSA FOSA FOSA FOSA 5.889 5.8B5 5.888 5.887 8385467 8541720 8450504 10811323 309 313 312 412 3.09 3.11 3.13 0.0 3.12 1% 4.12 105% Day 1 results, pg/mL average 2.56 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0138.D HILL0139.D HILL0141.D HILL0142.D HILL0143.D FOSA-1.3.1 FOSA-1.3.2 FOSA-1.3.3 FOSA-1.3.4MS 042301-FOSA-LCS 042301-FOSA-1.3.1 Smp 042301-FOSA-1.3.2 Dup 042301-FOSA-1,3.3 Trip 042301-FOSA-1.3.4 Spike FOSA Solvent Blank Spike FOSA FOSA FOSA FOSA FOSA 5.882 5.886 5.886 5.886 5.97 6883587 6433005 6255010 9067750 2756837 248 233 230 340 98 2.48 2.37 2.33 0.1 2.30 4% 3.40 107% 102% std dev %RSD: 0.38 15% SAMPLE SAMPLE SAMPLE SAMPLE HILL0144.D HILL0145.D HILL0150.D HILL0151.D FOSA-2.4.1blk FOSA-2.4.2blk FOSA-2.4.3blk FOSA-2.4.4blkMS 042301-FOSA-2.4.1 Mtd Blk 042301-FOSA-2.4.2 Mtd Blk 042301-FOSA-2.4.3 Mtd Blk 42301-FOSA-2.4.4 Mtd Blk Spike FOSA FOSA FOSA FOSA 00 00 00 5.97 2811726 0 0 0 98 102% SAMPLE SAMPLE SAMPLE SAMPLE HILL0152.D HILL0153.D HILL0154.D HILL0156.D FOSA-2.1.1 FOSA-2.1.2 FOSA-2.1.3 FOSA-2.1.4MS 042301-F0SA-2.1.1 Smp 042301-FOSA-2.1.2 Dup 042301-F0SA-2.1.3 Trip 042301-FOSA-2.1.4 Spike FOSA FOSA FOSA FOSA 5.879 5.879 5.88 5.887 8103858 8151376 7853370 10247004 317 . 296 291 393 3.17 2.96 2.91 3.93 3.02 0.1 5% 96% SAMPLE SAMPLE SAMPLE SAMPLE HILL0157.D HILL01S8.D HILL0159.D HILL0160.D FOSA-2.2.1 FOSA-2.2.2 FOSA-2.2.3 FOSA-2.2.4MS 042301-FOSA-2.2.1 Smp 042301-FOSA-2.2.2 Dup 042301-FOSA-2.2.3 Trip 042301-FOSA-2.2.4 Spike FOSA FOSA FOSA FOSA 5.887 5.886 5.887 5.888 7993752 7697039 7443513 9662387 298 280 269 359 2.98 2.82 2.80 0.1 2.69 5% 3.59 80% Day 2 results, pg/mL average 2 .8 8 SAMPLE SAMPLE SAMPLE SAMPLE HILL0165.D HILL0166.D HILL0167.D HILL0168.D FOSA-2.3.1 FOSA-2.3.2 FOSA-2.3.3 FOSA-2.3.4MS 042301-FOSA-2.3.1 Smp 042301-FOSA-2.3.2 Dup 042301-FOSA-2.3.3 Trip 042301-FOSA-2.3.4 Spike FOSA FOSA FOSA FOSA 5.879 5.882 5.88 5.886 7850050 7536620 7535404 9615944 289 279 275 362 2.89 2.79 2.75 3.62 2.81 0.1 3% 84% std dev %RSD: 0.12 4% Page 4 of 5 3M Environmental Laboratory Project# E01-0768 Page 6 8 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Days la n d 2 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010426.s/FOSA0425.m (ChemStation); Reprocessing Method: H010426a.m (Target) SampType File Sample Name SAMPLE HILL0103.D TN-A 4802 MeOH SAMPLE SAMPLE HILL0104.D TN-A 4802 MeOH HILL0118.D TN-A 4802 MeOH SAMPLE HILL0119.D TN-A 4802 MeOH SAMPLE HILL0125.D TN-A 4802 MeOH SAMPLE HILL0133.D TN-A 4802 MeOH SAMPLE HILL0134.D TN-A 4802 MeOH SAMPLE HILL0140.D TN-A 4802 MeOH SAMPLE SAMPLE HILL0148.D TN-A 4802 MeOH HILL0149.D TN-A 4802 MeOH SAMPLE HILL0155.D TN-A 4802 MeOH SAMPLE SAMPLE SAMPLE HILL0163.D HILL0164.D HILL0169.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH SAMPLE HILL0170.D TN-A 4802 MeOH SAMPLE HILL0184.D TN-A 4802 MeOH SAMPLE HILL0185.D TN-A 4802 MeOH Mise Info Compound ame FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA RT 5.981 5.976 5.979 5.978 0 5.978 0 5.972 0 0 5.972 0 0 5.986 5.984 5.977 5.971 Area 143948 47424 129092 53533 0 24760 0 40478 0 0 38428 0 0 48316 17972 136896 49865 Amount <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp <1/2 LOQ resp Page 5 of 5 3M Environmental Laboratory Project# E01-0768 Page 69 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Tim epoint(s): Day 3 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/FOSA0425.m (ChemStation); Reprocessing Method: H010501a.m (Target) SampType File Sample Name Mise Info SAMPLE HILL0078.D 01003-25-01 . 0 Std SAMPLE HILL0079.D 01003-25-02 2.5 ng/mL FOSA C A LIB J HILL0080.D 01003-25-03 5.3 ng/mL FOSA CALIB_2 HILL0081.D 01003-25-04 10.1 ng/mL FOSA CALIB_3 HILL0082.D 01003-25-05 25 ng/mL FOSA CALIB_4 HILL0083.D 01003-25-06 40.3 ng/mL FOSA CALIB_5 HILL0084.D 01003-25-07 49.9 ng/mL FOSA CALIB_6 HILL0085.D 01003-25-08 74.9 ng/mL FOSA CALIB_7 HILL0086.D 01003-25-09 . 100.8 ng/mL FOSA CALIB_8 HILL0087.D 01003-25-10 249.6 ng/mL FOSA CALIB_9 HILL0088.D CALIBJO HILL0089.D 01003-25-11 01003-25-12 403.2 ng/mL FOSA 499.2 ng/mL FOSA SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE CALIBJ 1 CALIBJ 2 HILL0090.D HILL0104.D HILL0116.D HILL0119.D HILL0120.D HILL0121.D HILL0122.D 01003-25-13 01003-25-09 01003-25-09 01003-25-01 01003-25-02 01003-25-03 01003-25-04 1008 ng/mL FOSA 100.8 ng/mL FOSA 100.8 ng/mL FOSA 0 Std 2.5 ng/mL FOSA 5.3 ng/mL FOSA 10.1 ng/mL FOSA C A LIB J 3 HILL0123.D 01003-25-05 25 ng/mL FOSA C A LIB J 4 HILL0124.D 01003-25-06 40.3 ng/mL FOSA C A LIB J 5 HILL0125.D 01003-25-07 49.9 ng/mL FOSA C A LIB J 6 HILL0126.D 01003-25-08 74.9 ng/mL FOSA CALIBJ 7 CALIBJ 8 CALIBJ 9 HILL0127.D HILL0128.D HILL0129.D 01003-25-09 01003-25-10 01003-25-11 100.8 ng/mL FOSA 249.6 ng/mL FOSA 403.2 ng/mL FOSA CALIBJO HILL0130.D 01003-25-12 499.2 ng/mL FOSA SAMPLE HILL0131.D 01003-25-13 1008 ng/mL FOSA Compound Name THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS RT 5.115 5.116 5.117 5.117 5.113 5.116 5.129 5.11 5.123 5.111 5.115 5.115 5.122 5.117 5.125 5.115 5.123 5.126 5.114 5.122 5.115 5.131 5.124 5.12 5.119 5.117 5.118 5.115 Area 1381461 1374933 1393833 1385169 1380163 1376007 1374674 1374202 1380970 1382975 1394460 1388280 1389397 1244044 1247230 1266027 1262927 1263723 1282166 1280362 1275643 1276350 1274208 1269909 1287101 1292619 1288469 1293221 Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Compound Name PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS RT 4.408 4.401 4.41 4.416 4.42 4.408 4.407 4.41 4.423 4.411 4.401 4.414 4.414 4.402 4.41 4.415 4.415 4.418 4.421 4.414 4.415 4.416 4.424 4.419 4.412 4.416 4.411 4.422 Area 1798374 1777751 1801694 1810322 1800005 1780106 1812881 1766585 1798232 1773614 1805937 1776350 1788258 1778858 1778060 1789621 1775266 1808173 1804070 1774497 1778220 1785753 1775648 1757613 1767480 1778677 1776855 1781355 Amount 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Page 1 of 5 In itia i L 3M Environmental Laboratory Project # E 0 1 -0768 Page 70 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Day 3 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/FOSA0425.m (ChemStation); SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0093.D FOSA-3.4.1blk HILL0094.D FOSA-3.4.2blk HILL0095.D FOSA-3.4.3blk HILL0096.D FOSA-3.4.4blkMS HILL0097.D FOSA-3.1.1 HILL0099.D FOSA-3.1.2 HILL0100.D FOSA-3.1.3 HILL0101.D FOSA-3.2.1 HILL0102.D FOSA-3.2.2 HILL0103.D FOSA-3.2.3 HILL0107.D FOSA-3.2.4MS HILL0108.D FOSA-3.3.1 HILL0109.D FOSA-3.3.2 HILL0110.D FOSA-3.3.3 HILL0112.D FOSA-3.3.4MS HILL0113.D 042301 -FOSA-LCS HILL0114.D Diluter Blk HILL0115.D MeOH blk w /IS 042301 -FOSA-3.4.1, Mtd Blk 042301-FOSA-3.4.2, Mtd Blk 042301-FOSA-3.4.3, Mtd Blk 042301-FOSA-3.4.4. Mtd Blk Spike 042301-FOSA-3.1.1, Smp 042301-FOSA-3.1.2, Dup 042301-FOSA-3.1.3, Trip 042301-FOSA-3.2.1, Smp 042301-FOSA-3.2.2, Dup 042301-FOSA-3.2.3, Trip 042301-FOSA-3.2.4, Spike 042301-FOSA-3.3.1, Smp 042301-FOSA-3.3.2, Dup 042301-FOSA-3.3.3, Trip 042301-FOSA-3.3.4, Spike FOSA Solvent Blank Spike Diluter blank with IS mix Methanol with IS mix THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 5.118 5.123 5.124 5.123 5.118 5.117 5.124 5.117 5.117 5.118 5.116 5.124 5.128 5.123 5.111 5.13 5.122 5.115 1236810 1299549 1331679 1313977 . 1186398 1180945 1174802 1170460 1157352 1169370 1142996 1120852 1115271 1120639 1102414 1168358 1184946 809160 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS PFBS 4.396 4.402 4.41 4.416 4.403 4.41 4.409 4.409 4.402 4.418 4.408 4.403 4.407 4.415 4.404 4.415 4.415 4.414 1629186 1708821 1727981 1714291 1735419 1725206 1738131 1757667 1733154 1755402 1710176 1739019 1748703 1743829 1709063 1691538 1645960 1075206 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 254 Average: Std Deviation: %RSD: 1262315 112912 8.9% 1745413 108834 6.2% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0077.D HILL0091.D HILL0092.D HILL0098.D HILL0105.D HILL0106.D HILL0111.D HILL0117.D HILL0118.D HILL0132.D HILL0133.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS THPFOS 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 0 00 PFBS 00 0 Page 2 of 5 3M Environmental Laboratory Project# E01-0768 Page 71 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Day 3 Analytical instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/FOSA0425.m (ChemStation); SampType File SAMPLE HILL0078.D Sample Name 01003-25-01 Mise Info 0 Std Compound ame FOSA RT 0 Area 0 Amount 0 % Recovery - SAMPLE CALIB_1 CALIBJ2 CALIB_3 CALIB_4 CALIB_5 CALIB_6 CALIB_7 CALIB_B CALIB_9 CALIB_10 SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE C A LIB J1 CALIBJ 2 CALIB_13 CALIBJ 4 CALIBJ 5 CALIBJ 6 CALIBJ 7 CALIBJ 8 CALIB 19 CALIB 20 SAMPLE HILL0079.D HILL0080.D HILL0081.D HILL0082.D HILL0083.D HILL0084.D HILL0085.D HILL0086.D HILL0087.D HILL0088.D HILL0089.D HILL0090.D HILL0104.D HILL0116.D HILL0119.D HILL0120.D HILL0121.D HILL0122.D HILL0123.D HILL0124.D HILL0125.D HILL0126.D HILL0127.D HILL0128.D HILL0129.D HILL0130.D HILL0131.D 01003-25-02 01003-25-03 01003-25-04 01003-25-05 01003-25-06 01003-25-07 01003-25-08 01003-25-09 01003-25-10 01003-25-11 01003-25-12 01003-25-13 01003-25-09 01003-25-09 01003-25-01 01003-25-02 01003-25-03 01003-25-04 01003-25-05 01003-25-06 01003-25-07 01003-25-08 01003-25-09 01003-25-10 01003-25-11 01003-25-12 01003-25-13 2.5 ng/mL FOSA 5.3 ng/mL FOSA 10.1 ng/mL FOSA 25 ng/mL FOSA 40.3 ng/mL FOSA 49.9 ng/mL FOSA 74.9 ng/mL FOSA 100.8 ng/mL FOSA . 249.6 ng/mL FOSA 403.2 ng/mL FOSA 499.2 ng/mL FOSA 1008 ng/mL FOSA 100.8 ng/mL FOSA 100.8 ng/mL FOSA OStd 2.5 ng/mL FOSA 5.3 ng/mL FOSA 10.1 ng/mL FOSA . 25 ng/mL FOSA 40.3 ng/mL FOSA 49.9 ng/mL FOSA , 74.9 ng/mL FOSA 10.8 ng/mL FOSA 249.6 ng/mL FOSA 403.2 ng/mL FOSA 499.2 ng/mL FOSA 1008 ng/mL FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA 5.991 5.993 5.985 5.982 5.984 5.997 5.985 5.985 5.98 6.004 5.983 5.983 5.999 6 0 5.984 5.987 5.983 5.99 5.984 5.999 5.986 5.988 5.988 5.985 5.994 5.984 84044 160849 307301 768189 1231657 1519482 2227975 3036314 6971036 10819514 12885941 23137645 2915113 2902871 0 72740 152363 298779 736231 1203821 1473022 2181078 2931206 6818287 10436918 12664603 22575515 3 5 10 25 41 50 76 103 253 405 505 1018 100 99 0 2 5 10 24 40 49 74 101 248 396 495 992 - - 97% 100% 102% 100% 101% 102% 101% 101% 101% - 102% 102% . - - 95% 97% 99% 98% 99% 101% 99% 98% 99% - 3M Environmental Laboratory Project# E01-0768 Page 72 of 171 Page 3 of 5 BACK TO MAIN Solubility Study, Shake Flask Method; T est Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Tim epoint(s): Day 3 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/FOSA0425.m (ChemStation); on-column Caluculations Average (pg/mL) Std Dev dil factor corrected % RSD SampType File Sample Name Mise Info Compound Name RT Area Amount ug/mL FOSA S p ik e % R e c o v . SAMPLE HILL0097.D FOSA-3.1.1 042301-FOSA-3.1.1, Smp FOSA 5.909 7201703 269 2.69 SAMPLE HILL0099.D FOSA-3.1.2 042301-FOSA-3.1.2, Dup FOSA 5.901 6731194 251 2.51 SAMPLE HILL0100.D FOSA-3.1.3 042301-FOSA-3.1.3, Trip FOSA 5.908 6998562 260 2.60 Not enough sample was available to prepare the spike replicate for sample #1. Spike results from samples two and three shall suffice to demonstrate spike recoveries. 2.60 0.1 3% SAMPLE SAMPLE SAMPLE SAMPLE HILL0101.D HILL0102.D HILL0103.D HILL0107.D FOSA-3.2.1 FOSA-3.2.2 FOSA-3.2.3 FOSA-3.2.4MS 042301-FOSA-3.2.1, Smp 042301-FOSA-3.2.2, Dup 042301-FOSA-3.2.3, Trip 042301-FOSA-3.2.4, Spike FOSA FOSA FOSA FOSA 5.908 5.922 5.895 5.9 6990791 7009317 6836606 9016954 257 261 251 351 2.57 2.61 2.51 3.51 2.56 0.1 2% 99% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0108.D HILL0109.D HILL0110.D FOSA-3.3.1 FOSA-3.3.2 FOSA-3.3.3 HILL0112.D FOSA-3.3.4MS HILL0113.D 042301-FOSA-LCS 042301-FOSA-3.3.1, Smp 042301-FOSA-3.3.2, Dup 042301-FOSA-3.3.3, Trip 042301 -FOSA-3.3.4, Spike FOSA Solvent Blank Spike FOSA FOSA FOSA FOSA FOSA 5.916 5.906 5.9 5.909 5.991 7065688 7377514 7030743 9073879 2750436 263 274 260 354 99 2.63 2.74 2.60 3.54 2.66 0.1 3% 92% 103% Day 3 results , pg/mL average 2.61 std dev 0.05 %RSD: 2% Page 4 of 5 3M Environmental Laboratory Project # E 0 1 -0768 Page 73 of 171 BACK TO MAIN Solubility Study, Shake Flask Method; Test Compound: FOSA; Test Matrix: Male/Female Normal Human Urine; Timepoint(s): Day 3 Analytical Instrument: HPLC/MSD "Hillary"; Analytical Sequence/Method: H010501.s/FOSA0425.m (ChemStation); dil factor corrected SampType SAMPLE SAMPLE SAMPLE File HILL0093.D HILL0094.D HILL0095.D SAMPLE HILL0096.D SAMPLE HILL0114.D SAMPLE HILL0115.D Sample Name FOSA-3.4.1blk FOSA-3.4.2blk FOSA-3.4.3blk FOSA-3.4.4blkMS Diluter Blk MeOH blk w/ IS Mlsc Info 042301-FOSA-3,4.1, Mtd Blk 042301-FOSA-3.4.2, Mtd Blk 042301-FOSA-3.4.3, Mtd Blk 042301-FOSA-3.4.4, Mtd Blk Spike Diluter blank with IS mix Methanol with IS mix Compound ame FOSA FOSA FOSA FOSA FOSA FOSA RT 6.007 5.992 5.986 5.984 0 0 Area 553440 523878 450065 3129563 0 0 Amt 20 18 15 111 0 0 fig/mL FOSA 0.20 0.18 0.15 ** 116% SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE HILL0077.D HILL0091.D HILL0092.D HILL0098.D HILL0105.D HILL0106.D HILL0111.D HILL0117.D HILL0118.D HILL0132.D HILL0133.D TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH TN-A 4802 MeOH FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA FOSA 5.988 5.991 5.992 5.99 5.992 5.991 5.916 0 0 5.984 5.986 79511 166363 63070 40614 30961 18624 46114 0 0 150108 56599 0 0 0 0 0 0 0 0 0 0 0 Day 3 samples were initially diluted on 04-25-01 and analyzed for FOSA in sequence H010430.S Method blank samples demonstrated a significant amount of FOSA. The Day 3 samples were again diluted 10X with methanol along with a diluter blank to check for FOSA background in the diiuter, and a methanol blank spiked with IS mix to check for FOSA background/contamination in the internal standard mix. Method blank samples analyzed in seq H010501 ,s still had a background of FOSA, but it was determined that the FOSA was somehow introduced to the urine during the prep procedure prior to dilution since the diluter blank and IS blank came out "clean." Days 1 and 2 method blank samples demonstrate that the urine used for the study had no initial background of FOSA, and so the level of FOSA in Day 3 mtd blks was due to a small amt of FOSA introduced to the test system during sample preparation. This background of FOSA in the Day 3 mtd blks may be disregarded since it was only incurred on the day of test analyte In addition, and was a random, inadvertent error that does not affect the solubility results for the other three Day 3 samples. Page 5 of 5 3IVI Environmental Laboratory Project # E01-0768 Page 74 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Attachment C: Sample Chromatograms Chromatograms included for both PFOS and FOSA: -3 Solvent Blank Chromatograms -3 Method Blank Chromatograms -9 Sample Chromatograms (3 chrom per day) Page 75 of 171 BACK TO MAIN Data File: D:\chem\Hillary.i\H010426.b\HILL0029.D 3M Environmental Laboratopa g e 1 Report Date: 01-May-2001 11:16 Project#E0 1 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D :\chem\Hillary.i\H010426.b\HILL0029.D Lab Smp Id TN-A 4802 MeOH Inj Date 26-APR-2001 22:02 Operator KLT Inst ID: hillary. Smp Info TN-A 4802 MeOH Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010426.S Method D:\chem\Hillary.i\H010426.b\H0100426t.m Meth Date- 01-May-2001 11:12 terrell Quant Type: ISTD Cal Date 26-APR-2001 21:40 Cal File: HILL0027.D Als bottle 92 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) Compound Not Detected. 4.389 4.410 (1.000) 5.419 5.334 (1.000) 9125 65012 JJjjj iQg-fr P Cd-ICo-Oi Sxsot C o p y o f O rig in a l Ja Initial Page 76 of 171 Data File: D:\chem\Hillary.iSH010426.bSHILL0029.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Pase 2 Exact Copy f Origina' _M l S itia l V rtO rot . Date Page 77 of 171 Data File: D:\chem\Hillary.i\H010426.b\HILL0029.D BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Pa?e 3 Exact Copy f Original .....Date Page 78 of 171 RD ea pt ao r Ft i le: D at e D : : 0\ c3h- Me ma y\ H-2i0l l0a1r y 0. i9\:H1 70 1 0 5 0 1 . b \ H I L L 0 0 3 6 . D BACK TO MAIN 13 M Environmental L a b o ra to lja g e Project#E01 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010501.b\HILL0036.D Lab Smp Id TN-A 4802 MeOH Inj Date 01-MAY-2001 22:59 Operator KLT Inst ID: hillary.i Smp Info TN-A 4802 MeOH Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010501 s Method D:\chem\Hillary.i\H010501.b\H010501t.m Meth Date 03-May-2001 08:17 terrell Quant Type: ISTD Cal Date 01-MAY-2001 21:19 Cal File: HILL0027.D Als bottle 93 ' Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) Compound Not Detected. Compound Not Detected. Compound Not Detected. ifu 91( fiExact Copy of Origiri! initial __ _ Date Page 79 of 171 Data F ile : D:\chem\Hi 1lary.i\H010501.b\HILL0036.D BACK TO MAIN 3M Environmental Laboratory p _ Project# E01-0768 s M 2 PFBS <U n d e te c te d ) initial f Originan Dat Page 80 of 171 Data File: D:\chern\Hi 1l a r y , i\H010501.b\HILL0036.D 3 PFOS (U n d e te c te d ) BACK TO MAIN 3M Environmental Laboratory page 3 Project# E01-0768 Page 81 of 171 DR ea tpao r Ft i le: D at e D : : \0c1h- Me ma y\ H-2i0l l0a1r y 1. i3\ :H2 90 1 0 4 3 0 . b \ H I L L 0 0 5 7 . D BACK TO MAIN 3M Environmental L a b o ra to ^ a g e 1 Project#E01 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D :\chem\Hillary.i\H010430.b\HILL0057.D Lab Smp Id TN-A 4802 MeOH Inj Date Operator 30-APR-2001 18:57 KLT Inst ID: hillary.i Smp Info TN-A 4802 MeOH Mise Info Comment Method Meth Date Cal Date Samples analyzed on HPLC1100 LC/MSD "Hillary1', H010430.S D:\chem\Hillary.i\H010430.b\H0100430t.m 01-May-2001 12:59 terrell Quant Type: ISTD 30-APR-2001 13:21 Cal File: HILL0027.D Als bottle 93 ' Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1 THPFOS 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT RBL RT RESPONSE (ng/mL) <ng/raL) Compound Not Detected Compound Not Detected Compound Not Detected Exact Copy of Original! $ 7 ____ _ W H L astiai Date Page 82 of 171 Data F ile ; D;\chem\Hi 11a ry . i \H010430.b\HILL0057, D BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 Pa^e 2 Page 83 of 171 Bata File: B:\chemSHillary.i\H010430.bSHILL0057.B 2 PFOS (U n d e te c te d ) BACK TO MAIN 3M Environmental Laboratory Project # E 0 1-0768 PaSe 3 fj, C _ tftr - in itia l :,* O A !k L Date Page 84 of 171 DR ea pt ao rFt iDl ea:t e D: : 0\ c1h-eMma y\ H-2i0l l0a1r y1. i1\:H1 60 1 0 4 2 6 . b \ H I L L 0 0 3 2 . D BACK TO MAIN 3M Environmental L a b o ra to ^a g e 1 Project#E01 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0032.D Lab Smp Id PF0S-1.4.1blk Inj Date 26-APR-2001 22:36 Operator KLT Inst ID: hillary.i Smp Info 1,OOOX dil 042301-PFOS-l Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010426.S Method D:\chem\Hillary.i\H010426.b\H0100426t.m Meth Date 01-May-2001 11:12 terrell Quant Type: ISTD Cal Date 26-APR-2001 21:40 Cal File: HILL0027.D Als bottle 22 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.111 5.131 (1.000) 1357667 4.369 4.410 (1.000) 1900574 Compound Not Detected 254.000 254.000 L , I'. r -B a r Page 85 of 171 Data File: L:\chem\Hillary.iSH010426.bSHILL0032.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 PaSe 2 Page 86 of 171 Data File: DjSchemSHillarg.iSH010426.bSHILL0C'32.D 2 PFOS (U n d e te c te d ) BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 Exact Copy of Original InIitita!. - & Patet il Page 87 of 171 BACK TO MAIN RD ea pt ao rFt iDl ea:t e :D :0\ c3h-eMma y\ H-2i0l l0a1r y0. i9\:H1 60 1 0 5 0 1 . b \ H I L L 0 0 3 2 . D 3MEnvironmental Laboratori Project# E01 -0768 e 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D :\chem\Hillary.i\H010501.b\HILL0032.D Lab Smp Id PFOS-2.4.lblk Inj Date 01-MAY-2001 22:15 Operator KLT Inst ID: hillary.i Smp Info 1,000X dii 042301-PFOS-2 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010501 s Method D :\chem\Hillary.i\H010501.b\H010501t.m Meth Date 03-May-2001 08:17 terrell Quant Type: ISTD Cal Date 01-MAY-2001 21:19 Cal File: HILL0027.D Als bottle 22 ' Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 PFOS ' QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.114 5.109 (1.000) 1317272 4.407 4.402 (1.000) 1718184 Compound Not Detected. 254.000 254.000 Page 88 of 171 Data F ile ? D :\chem \H i1la r y . i\H 010501.b\H ILL0032.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 Page 2 Exact Copy oi ontj'.js Page 89 of 171 Data File: D:\chem\Hillary.i\H010501,b\HILL0032.D 3 PFOS (U n d e te c te d ) BACK TO MAIN 3M Environmental Laboratory Project # E01 -0768 PaSe 3 Exact Copy of Or- na1 -- ..... O a ts f & W y y O ] Page-^Pof 1/1 BACK TO MAIN DR ea tpao rFt iDl ea:t e D: :0\ c1h-eMma y\ H-2i0l l0a1r y1. i3\:H2 90 1 0 4 3 0 . b \ H I L L 0 0 5 9 . D 3M Environmental Laboratorpa g e x Project#E01 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file : D:\chem\Hillary.i\H010430.b\HILL0059.D Lab Smp Id: PFOS-3.4.lblk Inj Date : 30-APR-2001 19:19 Operator : KLT Inst ID: hillary.i Smp Info : 1,000X dil 042301-PFOS-3 Mise Info : Comment : Samples analyzed on HPLC1100 LC/MSD "Hillary", H010430.S Method : D:\chem\Hillary.i\H010430.b\H0100430t.m Meth Date : 01-May-2001 12:59 terrell Quant Type: ISTD Cal Date : 30-APR-2001 13:21 Cal File: HILL0027.D Als bottle: 22 Dil Factor: 1 . 0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS . QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.098 5.108 (1.000) 1419875 4.363 4.380 (1.000) 1870275 Compound Not Detected. 254.000 254.000 Page 91 of 171 Data File: D:\chern\Hi 1lary.i\H010430,b\HILL0059.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 "fcpy n f ?-: Page 92 of 171 D ata F i le : D :\chem SHilla ry .i\H 0 1 0 4 3 0 ,b \H IL L 0 0 5 9 ,D 2 PFOS (U n d e te c te d ) BACK TO MAIN 3M Environmental Laboratory Project #E 01-0768 Page 3 BACK TO MAIN DR ea pt ao rFt iDl ea:t e :D :0\ c1h-Me ma y\ H-2i0l 0l a1r y1. i1\:H1 60 1 0 4 2 6 . b \ H I L L 0 0 3 7 . D 3M Environmental LaboratoiM^ -, Project # E01-076Bd y e 1 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file : D:\chem\Hillary.i\H010426.b\HILL0037.D Lab Smp Id: PFOS-1.1.1 Inj Date : 26-APR-2001 23:32 Operator : KLT Inst ID: hillary.i Smp Info : 1,000X dil 042301-PFOS-l Mise Info : Comment : Samples analyzed on HPLC1100 LC/MSD "Hillary", H010426.S Method : D :\chem\Hillary.i\H010426.b\H0100426t.m Meth Date- : 01-May-2001 11:12 terrell Quant Type: ISTD Cal Date : 26-APR-2001 21:40 Cal File: HILL0027.D Als bottle: 26 ' Dii Factor: 1 . 0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.123 4.388 5.270 5.131 (1.000) 4.410 (1.000) 5.334 (1.029) 1239933 2179012 7570273 254.000 254.000 292.634 293 Exae! Copy of Ordinal Jiy___ _ initiai l w 5" Page 94 of 171 Data Files DsSehenSHillary.i\H010426.b\HILL0037.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 2 Page 95 of 171 Data Filet D;\chemSHillary.i\H010426.b\HILL0037.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 Exact Copy of Origina! W J Z -iit- a Date Page 96 of 171 RD ea pt ao rFt iDl ea:t e :D : \0c1h- Me ma y\ -H2i0l l0a1r y. 1 i\H 1 :1 0 6 1 0 4 2 6 . b \ H I L L 0 0 4 1 . D BACK TO MAIN 3M Env ir o n TM ^ l Uboratow projectWE01-0768 1 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file : D:\chem\Hillary.i\H010426.b\HILL0041.D Lab Smp Id: PFOS-1.2.1 Inj Date : 27-APR-2001 00:16 Operator ' : KLT Inst ID: hillary.i Smp Info : 1,000X dil 042301-PFOS-1 Mise Info : Comment : Samples analyzed on HPLC1100 LC/MSD "Hillary", H010426.S Method : D:\chem\Hillary.i\H010426.b\H0100426t.m Meth Date : 01-May-2001 11:12 terrell Quant Type: ISTD Cal Date : 26-APR-2001 21:40 Cal File: HILL0027.D Al s bottle: 30 Dil Factor: 1 . 0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS ' QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.110 4.396 5.251 5.131 (1.000) 4.410 (1.000) 5.334 (1.027) 1262274 2148762 7600633 254.000 254.000 298.657 299 Hxscf Copy of -- -M -- initial ____ Dale Page 97 of 171 Data File} D:\chem\Hillary.i\H010426.b\HILL0041.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Exact Copy of Original Enitial ..... auDlairtee ( Page 98 of 171 Data File! D:\chem\Hillary.i\H010426.b\HILL0041.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 Exact Copy of Original lir initial 05 fa-o I Dato ' Page 99 of 171 DR ea pt ao rFt iDl ea:t e :D : 0\ c1h- Me ma y\ H-2i0l l0a1r y1. i1\:H1 60 1 0 4 2 6 . b \ H I L L 0 0 4 9 . D BACK TO MAIN 3Mfwironmental lJbora^a g e 1 project # e o i-076b 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0049.D Lab Smp Id PFOS-1.3.1 Inj Date 27-APR-2001 01:47 Operator KLT Inst ID: hillary.i Smp Info 1,000X dil 042301-PFOS-1 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010426.S Method D :\chem\Hillary.i\H010426.b\H0100426t.m Meth Date 01-May-2001 11:12 terrell Quant Type: ISTD Cal Date . 26-APR-2001 21:40 Cal File: HILL0027.D Als bottle 34 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.129 4.394 5.269 5.131 (1.000) 4.410 (1.000) 5.334 (1.027) 1269547 2195975 0267658 254.000 254.000 320.624 321 Exact Copy of Original Kl/ Initial ( fr lM Datf* Page 100 of 171 Data File: D:\chem\Hillary.i\H010426.b\HILL0049.D BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Page 2 Page 101 of 171 Data File: D:\chem\Hillar9.iSH010426.bSHILL0049.D 2 PFOS BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 initial ' 'J ' ' - . C0-te0> - Page 102 of 171 BACK TO MAIN DR ea pt ao rFt iDl ea:t e D: : 0\ c3h-eMma y\ H-2i0l l0a1r y0. i9\:H1 70 1 0 5 0 1 . b \ H I L L 0 0 3 7 . D 3MEnviro"mentf'i-^r^ a g e 1 Project#E01-076S a 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file : D:\chem\Hillary.i\H010501.b\HILL0037.D Lab Smp Id: PFOS-2.1.1 Inj Date : 01-MAY-2001 23:11 Operator : KLT Inst ID: hillary, Smp Info : 1;000X dil 042301-PFOS-2 Mise Info : Comment : Samples analyzed on HPLC1100 LC/MSD "Hillary", H010501.s Method : D :\chem\Hillary.i\H010501.b\H010501t.m Meth Date : 03-May-2001 08 17 terrell Quant Type: ISTD Cal Date : 01-MAY-2001 21: 19 Cal File: HILL0027 .D Als bottle: 26 Dii Factor: 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.115 4.407 5.248 5.109 (1.000) 4.402 (1.000) 5.312 (1.191) 1215865 1912250 7420988 254.000 254.000 311.873 312 Page 103 of 171 Data File D:\chem\HiHary.iSH010501.b\HILL0037.D BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Page 2 Page 104 of 171 Data F ile: D:\chem\Hi1lary.i\H010501.b\HILL0037.D 3 PFOS BACK TO MAIN Page 33M Environmental Laboratory Project# E01-0768 Efxaet Copi Page 105 of 171 DR ea pt ao rFt i Dl ea:t e :D : \0c3h- Me ma y\-H2 0i l l0a1r y 0. i9\ H: 1071 0 5 0 1 . b \ H I L L 0 0 4 5 . D BACK TO MAIN a g e 13M Environmental Laborato Project#E01 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010501.b\HILL0045.D Lab Smp Id PFOS-2.2.1 Inj Date 02- MAY-2001 00:40 Operator KLT Inst ID: hillary.i Smp Info 1,000X dil 042301-PFOS-2 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010501.S Method D:\chem\Hillary.i\H010501.b\H010501t.m Meth Date 03- May-2001 08:17 terrell Quant Type: ISTD Cal Date 01-MAY-2001 21:19 Cal File: HILL0027.D Als bottle 30 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/raL) (ng/mL) 5.122 4*408 5.262 5.109 (1.000) 4.402 (1.000) 5.312 (1.194) 1256724 1900616 7021826 254.000 254.000 294.754 295 Page 106 of 171 Data File; D:\chem\Hi11ary*iSH010501.bSHILL0045,D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Page 107 of 171 Data File: D:\ohem\Hi 1lary,i\H010501.b\HILL0045.D 3 PFOS BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 Page 108 of 171 BACK TO MAIN DR ea pt ao r Ft i lDe a. :t e D: : \0c3h-eMma \yH- 2i0l l0a1r y0. i9\:H1 70 1 0 5 0 1 . b \ H I L L 0 0 5 0 . D 3M EnvironPmroejenctatl#LEab0o1-r0a7to65 ?age 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010501.b\HILL0050.D Lab Smp Id PFOS-2.3.1 Inj Date 02- MAY-2001 01:36 Operator KLT Inst ID: hillary.i Smp Info 1,000X dil 042301-PFOS-2 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010501.S Method D:\chem\Hillary.i\H010501.b\H010501t.m Meth Date 03- May-2001 08:17 terrell Quant Type: ISTD Cal Date 01-MAY-2001 21:19 Cal File: HILL0027.D Al s bottle 34 ' Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Vers ion: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1 THPFOS * 2 PFBS 3 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.116 4.409 5.257 5.109 (1.000) 4.402 (1.000) 5.312 (1.192) 1211070 1958520 8177762 254.000 254.000 339.416 339 & f O rig in ,^ Page 109 of 171 BACK TO MAIN Data File: D:\chemSHillary,i\H010501.bSHILL0050.D D:NchemSHilla r y . SH010501, bSHILL0050. D 1.1- 3M Environmental Laboratory Project #E01-0768 Page 2 1. 0- 0.9- 0. 8- 0.7- ~SO 0.6-. <. o S 0,5-' 0.4- _o_l_____i_l______il______2_I_0____2__I 5_____3 _I_0____3_I_5____4__I 0_____4_I_5Mins_i_o_____5_I_5_____l_o_____e_l_s____?_l_____7_1_0____s_l_o_____s_i_s_____l_o l Page 110 of 171 Data File: D:SchemSHillaryti\H010501.bNHILL0050.D 3 PFOS BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 Page 111 of 171 DR ea pt ao rFt iDl ea:t e :D :0\ c1h- Me ma y\ H-2i0l l0a1r y1. i3\:H2 90 1 0 4 3 0 . b \ H I L L 0 0 6 4 . D BACK TO MAIN 13M Environmental Laboratoj&age P roject#e o i-0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010430.b\HILL0064.D Lab Smp Id PFOS-3.1.1 Inj Date 30-APR-2001 20:15 Operator KLT Inst ID: hillary.i Smp Info 1,000X dil 042301-PFOS-3 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010430.S Method D:\chem\Hillary.i\H010430.b\H0100430t.m Meth Date 01-May-2001 12:59 terrell Quant Type: ISTD Cal Date 30-APR-2001 13:21 Cal File: HILL0027.D Als bottle 26 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.097 4.375 5.237 5.108 (1.000) 4.380 (1.000) 5.318 (1.197) 1310521 2034585 6815087 254.000 254.000 267.605 268 P a g e 112 o f 171 Data File} D:\chem\Hillary.i\H010430.b\HILL0064.D BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Page 2 Page 113 of 171 Data F ile} D:\chem\Hi1lary,i\H010430.b\HILL0064,D 2 PFOS BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 Page 114 of 171 DR ea pt ao rFt iDl ea:t e :D : 0\ c1h-eMma\yH-2i0l l0a1r y1. i3\:H3 00 1 0 4 3 0 . b \ H I L L 0 0 7 2 . D BACK TO MAIN 3MEnvironmental Laboratog Project#E01-076B 1 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file : D:\chem\Hillary.i \H010430.b\HILL0072.D Lab Smp Id: PFOS-3.2.1 Inj Date : 30-APR-2001 21:45 Operator : KLT Inst ID: hillary.i Smp Info : 1,000X dii 042301-PFOS-3 Misc Info : Comment : Samples analyzed on HPLC1100 LC/MSD "Hillary", H010430.s Method : D :\chem\Hillary.i\H010430.b\H0100430t.m Meth Date : 01-May-2001 12:59 terrell Quant Type: ISTD Cal Date : 30-APR-2001 13:21 Cal File: HILL0027 .D Als bottle: 30 Dil Factor: 1 . 0 0 0 0 0 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.104 4.383 5.245 5.108 (1.000) 4.380 (1.000) 5.318 (1.197) 1305210 2128725 8117378 254.000 254.000 309.586 310 Page 115 of 171 Data F ile : D:\chero\Hillara.i\H010430,bSHILL0072.D BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 PaSe 2 Page 116 of 171 Data File: D:\chem\Hillary.i\H010430.b\HILL0072.D 2 PFOS BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Page 3 Ixaet Copy of $ri(H )\ Page 117 of 171 DR ea pt ao rFt iDl ea:t e :D : 0\ c1h- Me ma y\ H-2i0l 0l a1r y1. i3\:H3 00 1 0 4 3 0 . b \ H I L L 0 0 7 7 . D BACK TO MAIN 3MEnvironmental Laboratopa g e x Project#E01 -0768 3M Environmental Laboratory PFOS, SD-018, Solubility in Urine Data file D:\chem\Hillary.i\H010430.b\HILL0077.D Lab Smp Id PFOS-3.3.1 Inj Date 30-APR-2001 22:41 Operator KLT Inst ID: hillary.i Smp Info 1,000X dil 042301-PFOS-3 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary", H010430.S Method D:\chem\Hillary.i\H010430.b\H0100430t.m Meth Date- 01-May-2001 12:59 terrell Quant Type: ISTD Cal Date 30-APR-2001 13:21 Cal File: HILL0027.D Als bottle 34 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Vers ion: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 PFOS QUANT SIG MASS 427 299 499 CONCENTRATIONS ON-COLUMN PINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.104 4.397 5.237 5.108 (1.000) 4.380 (1.000) 5.318 (1.191) 1325618 2084860 7558687 254.000 254.000 292.440 292 O f O f i0 ; m h -n tw - Page 118 of 171 Data File: D:\ohemSHillara.iSH010430.bSHILL0077.D BACK TO MAIN 3M Environmental Laboratory Project # E 0 1-0768 PaSe 2 Page 119 of 171 Data F ile: D:\cheroSHillary.iSH010430.bSHILL0077.D 2 PFOS BACK TO MAIN 3M Environmental Laboratory Project # E01 -0768 Page <xl0~6> Page 120 of 171 RD ea pt ao rFt iDl ea:t e :D :3\ c0h-eAmp r\ -H2i0l0l a1r y1. i4\:H0 70 1 0 4 2 6 . b \ H I L L 0 1 1 9 . D BACK TO MAIN 13M Environmental LaboratcR&ge Project#E01 -0768 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0119.D Lab Smp Id TN-A 4802 MeOH Inj Date 27-APR-2001 14:51 Operator KLT Inst ID: hillary.i Smp Info TN-A 4802 MeOH Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:05 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 91 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS 7 PFBS QUANT SIG MASS 427 299 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) Compound Not Detected. Compound Not Detected. ti kl ~ & J ijr O _ D a te " Page 121 of 171 Data Filet D:\chero\Hillary.i\H010426.bSHILL0119.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 Page 2 * 1 THPFOS (Undetected) * 7 PFBS (Undetected) Exact Copy of O r i g l i _ f o ____ _ D5-I(Q\ njia! Date Page 122 of 171 Data File; D:\chemSHillary.i\H010426.bSHILL0119.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Page 3 Y (xlO^) Exact Copy of Origina] initial '. _ 6 6 -f(n O ) Page 123 of 171 BACK TO MAIN DR ea pt ao rFt i Dl ea:t e :D : 3\ c0h- eAmp r\ -H2i0l0l a1r y1. i4\:H0 80 1 0 4 2 6 . b \ H I L L 0 1 4 8 . D 3MEnvironmentalI Labora to |,a g e 1 #Project E01-076B 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0148.D Lab Smp Id TN-A 4802 MeOH Inj Date 27-APR-2001 20:15 Operator KLT Inst ID: hillary.i Smp Info TN-A 4802 MeOH Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D :\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:08 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 92 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 49 8 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) Compound Not Detected. 4.409 4.387 (1.000) Compound Not Detected. 10126 254.000 Page 124 o f 171 Data Fi lei DiSchemSHillary,i\H010426.b\HILL0148.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 Pag 2 Ion _4_^_0_____4_^_2Hin_4_^_4____________4_^_8_ Of Original ... D a t e Page 125 of 171  Data F ile : D:\chemSHillara.iSH010426.bSHILL0148.D BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 PaSe 3 Y <xl<y-3) Page 126 of 171 DR ea pt ao rFt i Dl ea:t e D: : 0\ c3h-eMma y\ H-2i0l l0a1r y1. i3\:H0 01 1 0 5 0 1 . b \ H I L L 0 0 9 2 . D BACK TO MAIN 3MEnvironmental Laboratorv,a g e Project#E01 -0768 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010501.b\HILL0092.D Lab Smp Id TN-A 4802 MeOH Inj Date 02- MAY-2001 09:26 Operator KLT Inst ID: hillary.i Smp Info TN-A 4802 MeOH Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" H010501.S Method D :\chem\Hillary.i\H010501.b\H010501a.m Meth Date 03- May-2001 11:02 terrell Quant Type: ISTD Cal Date 02-MAY-2001 08:53 Cal File: HILL0089.D Als bottle 93 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS QUANT SIG MASS 427 299 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) Compound Not Detected. Compound Not Detected. Page 127 of 171 Data F ile; D;\chem\Hillary.i\H010501.b\HILL0092,D BACK TO MAIN JMInvfwrVmQip|(lfWtiClbOfIr4tr^to6N8 Page 2 Ion _4_._4_____4_.M8 in__5_,_2_____5_._6_____6_._0_ x 2 PFBS (U ndetected) Exact Copy of Originai irtU ia l Stte-L L- ..i a5 / Page 1 2 / of 171 I I Data F i l e D :\chem \H i 1la r y . i\H 01050 1.b \H IL L 0 092 .D 3 FOSA BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Page 3 4 9 ` o ! O r *9 t C o p 'V Page 129 of 171 DR ea pt ao rFt iDl ea:t e D: :3\ c0h- eAmp r\ -H2i0l0l a1r y1. i4\:H0 70 1 0 4 2 6 . b \ H I L L 0 1 2 1 . D BACK TO MAIN 13M Environmental Laboratd^age Project#E01 -0768 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0121.D Lab Smp Id FOSA-1.4.lblk Inj Date 27-APR-2001 15:13 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-1 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:05 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 55 ' Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.108 4.379 5.892 5.122 (1.000) 4.387 (1.000) 5.977 (1.345) 1379938 1893699 106755 254.000 254.000 2.50445 2.50 V i'i P a g e 130 o f 171 Data F i le : D :\c h e m \H illa ry .i\H 0 1 0 4 2 6 .b \H IL L 0 1 2 1 .D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Page 131 of 171 Data F ile : DlSchemSHi 11ary.iSH010426.bSHILL0121.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 PaSe 3 /? *Y ' P V r * - MM it lb T & k L - - S JfitfQ Page 132 o f 171 BACK TO MAIN Data File: D:\chem\Hillary.i\H010426.b\HILL0144.D 3M Environmental Laboratorpa g e 1 Report Date: 30-Apr-2001 14:08 Project#E01 -0768 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0144.D Lab Smp Id FOSA-2.4.lblk Inj Date 27-APR-2001 19:30 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-2 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date. 30-Apr-2001 14:08 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 71 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Vers ion: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.111 5.122 (1.000) 130S838 4.383 4.387 (1.000) 1875879 Compound Not Detected. 254.000 254.000 c*et CoPV ....Ha.......... Originai j! Page 133 of 171 Data F ile : B :\ch e m \H illary.i\H010426*bSHILL0144,B BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 PaSe 2 Page 134 of 171 Data File} D:\chem\Hillary.i\H010426.b\HILL0144.D 2 FOSA (Undetected) BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Page 3 o f Origf, J& kL Page 135 of 171 BACK TO MAIN RD eapt ao rFt iDl ea:t e :D :0\ c3h- Me ma y\ H-2i0l 0l a1r y1. i3\:H0 10 1 0 5 0 1 . b \ H I L L 0 0 9 3 . D 13M Environmental LaboratorP age Project# E01 -0768 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D :\chem\Hillary.i\H010501.b\HILL0093.D Lab Smp Id FOSA-3.4.lblk Inj Date 02- MAY-2001 09:38 Operator KLT Inst ID: hillary.i Smp Info FOSA Urine Solub Day 3 Re-diluted samples 5-01-01 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" H010501.S Method D:\chem\Hillary.i\H010501.b\H010501a.m Meth Date 03- May-2001 11:02 terrell Quant Type: ISTD Cal Date 02-MAY-2001 08:53 Cal File: HILL0089.D Als bottle 71 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 FOSA QUANT SIG 'MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.117 4.396 6.007 5.118 (1.000) 4.410 (1.000) 5.993 (1.366) 1236810 1629186 553440 254.000 254.000 19.8742 19.9 Exact Copy of Original _ 4Pmi t_ial_ .....M. DdateL , Page 136 of 171 Data File} D}\chem\Hi1lary.i\H010501.b\HILL0093.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 Page 2 x 2 PFBS Page 137 of 171 Data F ile t D:\chem\Hi 1lary.i\H 010501.b\H ILL0093.D 3 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E01 -0768 Page 3 O 'm Via__ ?-* Page 138 of 171 BACK TO MAIN RD ea pt ao rFt i Dl ea:t e D: : 3\ c0h- eAmp r\ -H2i0l 0l a1r y1. i4\:H0 70 1 0 4 2 6 . b \ H I L L 0 1 2 6 . D 3MEnviroPnrmoejnetcatl#'^Eo0r1a-0t7o6-8pa 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine U d L d l i i e D :\chem\Hillary.i\H010426.b\HILL0126.D Lab Smp Id Inj Date FOSA-1.1.1 27-APR-2001 16:09 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-1 Misc Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:05 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 59 Dil Factor 1 . 0 0 0 0 0 Inte_grator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1 THPFOS 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.112 4.390 5.889 5.122 (1.000) 4.387 (1.000) 5.977 (1.341) 1223896 1863247 9090670 254.000 254.000 342.874 343 Page 139 of 171 Data File: D:\chem\Hillary.i\H010426.b\HILL0126.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Page 140 of 171 Data File: D :SchemSH i11ary .iSH010426.b\HILL0126.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E 0 1-0768 Page 3 ..fe . in itia l m OrU*<- MM Date Page 141 of 171 BACK TO MAIN DR ea pt ao rFt iDl ea:t e D: : 3\ c0h-eAmp r\ H- 2i0l 0l a1r y1. i4\:H0 70 1 0 4 2 6 . b \ H I L L 0 1 3 0 . D S h a re 13M Environmental Laboratoi Project# E01-076i 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0130.D Lab Smp Id FOSA-1.2.1 Inj Date 27-APR-2001 16:54 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-1 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D :\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:05 terrell Quant Type: ISTD Cal Date 27-APR 2001 14:17 Cal File: HILL0116.D Als bottle 63 Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 493 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.118 4.382 5.888 5.122 (1.000) 4.387 (1.000) 5.977 (1.344) 1223960 1887871 8385467 254.000 254.000 309.497 309 C o p y b l O rig in s ] Kt Page 142 of 171 Data File; D:\chem\Hillary.iSH010426.b\HILL0130.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Page 143 of 171 Data F ile : D:\chem\Hillary.iSH010426.bSHILL0130.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Page 3 Page 144 of 171 DR ea pt ao rFt iDl ea:t e :D :3\ c0h-eAmp\rH- 2i0l l0a1r y1. i4\:H0 80 1 0 4 2 6 . b \ H I L L 0 1 3 8 . D BACK TO MAIN 3M Environmental Laboratorpage 1 Project#E01 -0768 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D :\chem\Hillary.i\H010426.b\HILL0138.D Lab Smp Id FOSA-1.3.1 Inj Date 27-APR-2001 18:23 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-1 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:05 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 67 ' Dii Factor 1.00000 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.111 4.390 5.881 5.122 (1.000) 4.387 (1.000) 5.977 (1.340) 1177514 1900215 6883587 254.000 254.000 248.307 248 .. tri w v p y f O r i g i n a l ' , , O a tt> Page 145 of 171 Data F ile : D:\chem\Hi 11ary.i\H010426.bSHILL0138.D BACK TO MAIN 3M Environmental Laboratory Project # E01 -0768 Pae 2 4.4 4.8 5.2 5.6 6.0 ________ Hin__________________ * 7 PFBS Page 146 of 171 Data File; D:\chem\Hi 1lary.i\H010426.b\HILL0138.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E01 -0768 3 - ..fftr ^ ititi f Page 147 of 171 BACK TO MAIN D a t a F i l e : D : \ c h e m \ H i l l a r y . i \ H 0 1 0 4 2 6 . b \ H I L L 0 1 5 2 . D 3MEnvirnment^ Report Date: 30-Apr-2001 14:08 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file : D:\chem\Hillary.i\H010426.b\HILL0152.D Lab Smp Id: FOSA-2.1.1 Inj Date : 27-APR-2001 21:00 Operator : KLT Inst ID: hillary.i Smp Info : 10X dil 042301-FOSA-2 Mise Info : Comment : Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method : D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date : 30-Apr-2001 14:08 terrell Quant Type: ISTD Cal Date : 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle: 75 Dil Factor: 1.00000 Integrator: Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.115 4.387 5.879 5.122 (1.000) 4.387 (1.000) 5.977 (1.340) 1110585 1783250 8103858 254.000 254.000 317.291 317 iiXdct Copy of W: 1j*'7 : i * tf-lir c i Page 148 o f 171 Data File} D:\chemSHillar9.iSH010426.bSHILL0152.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 PaSe 2 Eicaet Copy of Page 149 of 171 Data F ile : D:\chem\Hillary.i\H010426.b\HILL0152.D 2 FOSA BACK TO MAIN Page 33M Environmental Laboratory Project # E01 -0768 D rl^O ] DR aeptao rFt iDl ea:te :D :3\c0h-Ae mp r\H-2i0l0la1r y1.i4\:H0 80 1 0 4 2 6 .b \H I L L 0 1 5 7 .D BACK TO MAIN 3MEnviroHnmreonjteacltU#tbooi-r0a7t6o8ga g e 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0157.D Lab Smp Id FOSA-2.2.1 Inj Date 27-APR-2001 21:56 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-2 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method > D :\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:08 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 79 ' Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Vers ion: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.116 4.387 5.886 5.122 (1.000) 4.387 (1.000) 5.977 (1.342) 1202436 1863768 7993752 254.000 254.000 297.956 298 O *** Page 151 of 171 Data File: D:\chem\Hillary.i\H010426.b\HILL0157.D BACK TO MAIN 3M Environmental Laboratory Project #E01-0768 Pag 2 Efxaet froew fV ; . : Ka fW & i: It .................. & Page 152 of 171 Data F ile : D :\c h e m \H illa rg .iS H 0 104 26.b \H IL L 015 7.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E 01-0 768 Page 3 05H H ) Page 153 of 171 BACK TO MAIN DR ea pt ao rFt iDl ea:t e :D :3\ c0h- eAmp r\ -H2i0l0l a1r y1. i4\:H0 80 1 0 4 2 6 . b \ H I L L 0 1 6 5 . D 3M Environmental Laboratory _ Project # E01-0768 a ^ e 1 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D :\chem\Hillary.i\H010426.b\HILL0165.D Lab Smp Id FOSA-2.3.1 Inj Date 27-APR-2001 23:25 Operator KLT Inst ID: hillary.i Smp Info 10X dil 042301-FOSA-2 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:08 terrell Quant Type: ISTD Cal Date 27-APR-2001 14:17 Cal File: HILL0116.D Als bottle 83 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.116 4.394 5.879 5.122 (1.000) 4.387 (1.000) 5.977 (1.338) 1158902 1883593 7850050 254.000 254.000 288.823 289 ixaet Copy of Ongut*: -- i't--. a Hfiiife! .... Date Page 154 of 171 Data File D:\chem\Hi1lary.i\H010426.b\HILL0165.D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Ion _4_._4_____4_,8Hin__5_._2_____5_._6_____6_._0_ Page 155 of 171 Data File; D:\chem\Hi 1lary.i\H010426.b\HILL0165.D 2 FOSPl BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 D a tg Page 156 of 171 BACK TO MAIN DR ea pt ao rFt i Dl ea:t e D: : \0c3h-eMma y\ H-2i0l l0a1r y1. i3\:H0 10 1 0 5 0 1 . b \ H I L L 0 0 9 7 . D 3MEnVir0proef#Loi-07 ^ a g e 1 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file. D:\chem\Hillary.i\H010501.b\HILL0097.D Lab Smp Id FOSA-3.1.1 Inj Date 02- MAY-2001 10:22 Operator KLT Inst ID: hillary.i Smp Info FOSA Urine Solub Day 3 Re-diluted samples 5-01-01 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" H010501.S Method D :\chem\Hillary.i\H010501.b\H010501a.m Meth Date 03- May-2001 11:02 terrell Quant Type: ISTD Cal Date 02-MAY-2001 08:53 Cal File: HILL0089.D Als bottle 75 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.117 4.403 5.909 5.118 (1.000) 4.410 (1.000) 5.993 (1.342) 1186398 1735419 7201703 254.000 254.000 268.781 269 Page 157 o f 171 Data File: D;\chem\Hi1lary*i\H010501.b\HILL0097,D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 PaSe 2 x 2 PFBS E x act C o p y t ony- ** 1in11P_t_l_a__l_____ Ds!p Page 158 of 171 Data F ile } D:\chem\Hillar-a.i\H010501.b\HILL0097.D 3 FOSO BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 3 fixsef Copy f _ Kit Unitisi * S d t l Date Page 159 of 171 BACK TO MAIN DR ea pt ao rFt iDl ea:t e :D : 0\ c3h-eMma y\ H-2i0l l0a1r y1. i3\:H0 20 1 0 5 0 1 . b \ H I L L 0 1 0 1 . D 3MEnvir0T n r ^ Project#E0i-076f a 1 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010501.b\HILL0101.D Lab Smp Id FOSA-3.2.1 Inj Date 02-MAY-2001 11:07 Operator KLT Inst ID: hillary.i Smp Info FOSA Urine Solub Day 3 Re-diluted samples 5-01-01 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" H010501.S Method D:\chem\Hillary.i\H010501.b\H010501a.m Meth Date 03-May-2001 11:02 terrell Quant Type: ISTD Cal Date 02-MAY-2001 08:53 Cal File: HILL0089.D Als bottle 78 Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host: W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds . * 1 THPFOS * 2 PFBS 3 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.116 4.409 5.907 5.118 (1.000) 4.410 (1.000) 5.993 (1.340) 1170460 1757667 6990791 254.000 254.000 256.520 256 ix set Copy of Origins'* lfo _ .i f r h - a f ilia l ..^ Date Page 160 of 171 Data File{ D:\chem\Hillary.i\H010501.bSHILL0101.B BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 x 1 THPFOS rii as C 5 -J fc 0 l _ Bate Page 161 of 171 Data File: D:\chem\Hi 1lary.i\H010501,b\HILL0101,D 3 FOSA BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 PaSe 3 Her Jn im .......i b a t e Page 162 of 171 BACK TO MAIN DR ea pt ao rFt iDl ea:t e D: : \0c3h-Me ma y\ H-2i0l l0a1r y1. i3\:H0 20 1 0 5 0 1 . b \ H I L L 0 1 0 8 . D 3M Environmental Laboratow n Project# E01-0768a 9 e 1 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D :\chem\Hillary.i\H010501.b\HILL0108.D Lab Smp Id FOSA-3.3.1 Inj Date 02-MAY-2001 12:25 Operator KLT Inst ID: hillary.i Smp Info FOSA Urine Solub Day 3 Re-diluted samples 5-01-01 Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" H010501.S Method D:\chem\Hillary.i\H010501.b\H010501a.m Meth Date 03-May-2001 11:02 terrell Quant Type: ISTD Cal Date 02-MAY-2001 08:53 Cal File: HILL0089.D Als bottle 82 ' Dil Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Version: 4.10 Processing Host W19401 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 2 PFBS 3 FOSA QUANT SIG MASS 427 299 498 CONCENTRATIONS ON-COLUMN FINAL RT EXP RT REL RT RESPONSE (ng/mL) (ng/mL) 5.124 4.403 5.915 5.118 (1.000) 4.410 (1.000) 5.993 (1.344) 1120852 1739019 7065688 254.000 254.000 262.600 263 D e lir 1 Page 163 of 171 Data F ile: D:\chem\Hillary.i\H010501,bSHILL0108,D BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Page 2 Page 164 of 171 Data F ile; D:\chem\Hi 1lary.i\H010501.b\HILL0108,D 3 FOSA BACK TO MAIN Page 33M Environmental Laboratory Project # E01 -0768 Page 165 of 171 BACK TO MAIN DR ea pt ao rFt iDl ea:t e :D :3\ c0h- eAmp r\ -H2i0l0l a1r y1. i4\:H0 70 1 0 4 2 6 . b \ H I L L 0 1 1 4 . D 3MEnvironmental Laboratoa Project#E01-07<& x 3M Environmental Laboratory FOSA, SE-027, Solubility in Urine Data file D:\chem\Hillary.i\H010426.b\HILL0114.D Lab Smp Id 01003-25-10 Inj Date 27-APR-2001 13:55 Operator KLT Inst ID: hillary.i Smp Info 249.6 ng/mL FOSA in MeOH Mise Info Comment Samples analyzed on HPLC1100 LC/MSD "Hillary" 04-26-01 Method D:\chem\Hillary.i\H010426.b\H0100426a.m Meth Date 30-Apr-2001 14:05 terrell Quant Type: ISTD Cal Date 27-APR-2001 13:55 Cal File: HILL0114.D Als bottle 10 Calibration Sample, Level: Dii Factor 1 . 0 0 0 0 0 Integrator Falcon Compound Sublist: all.sub Target Vers ion: 4.10 Processing Host: W19401 8 Concentration Formula: Amt * DF * CpndVariable Cpnd Variable Local Compound Variable Compounds * 1 THPFOS * 7 PFBS 2 FOSA QUANT SIG MASS 427 299 498 RT EXP RT REL RT RESPONSE 5.114 4.393 5.976 5.122 (1.000) 4.387 (1.000) 5.977 (1.360) 1459549 1999512 7439185 AMOUNTS CAL-AMT ON-COL (ng/mL) (ng/mL) 254.000 254.000 249.600 256 Page 166 of 171 Data File? D:\chem\Hillarg.i\H010426.bSHILL0114.D BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Page 2 1 THPFOS Ion 4 .0 4 .2 4 ,4 4 .6 4.8 ___________ H in ___________________ Page 167 of 171 Data F ile ; D:\chem SHillary.i\H010426.b\HILL0114.D 2 FOSA BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Page 3 r Page 168 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01 -0768 Attachment D: Sample Calculations Page 169 of 171 BACK TO MAIN 3M Environmental Laboratory Project# E01-0768 Purity and dilution correction factors. PFOS, SD-018 10 pL sample was diluted with 990 pl_ methanol fo ra 1:100 dilution, followed by a second dilution to 1:1,000. 100 pL of 1:100 diluted sample was diluted with 900pL methanol. Therefore the on-column concentration was multiplied by a factor of 1,000 for the final reported value. Then, the samples were corrected for the purity of the standards used to analyze the samples. The standard purity was 97.9%. The solubility reported is the amount of PFOS in standard material id# SD-018 that dissolves in water at 23-24 C. FOSA, SE-027: 10 pL sample was diluted with 990 pL methanol for a 1:100 dilution. Therefore the on-column concentration was multiplied by a factor of 100 for the final reported value. The standard purity was unknown, therefore no purity correction was done. The solubility reported is the amount of FOSA in standard material id# SE-027 that dissolves in water at 23-24 C. Mean and standard deviation were calculated using functions provided in Microsoft Excel software. Standard deviation was used to measure the scatter about the mean of a data set; thus, it can be used to estimate the precision of a method. Relative standard deviation presents a measure of the magnitude of the standard deviation and is calculated by dividing the standard deviation by the mean. Means are calculated by adding individual entities and dividing the resultant sum by the number of individual entities. Standard deviation was calculated using the following equation: -Where n is the number of observations, and x is sample concentration. Average/Standard Deviation /%RSD example calculations: Sample Concentration Calculations ID pg/mL Rep1 302 Average (302+325+287)/3= 305 Rep 2 325 Std Dev (see above equation)= 19 Rep 3 287 %RSD (19/305)= 6% Rep 3 146.7 %RSD (19.0/143)= 13.3% For calculating the precision of two numbers, Relative Percent Difference was used to report the precision of the datum using the following equation: RPD=(A-B)/((A+B)/2) Example: Rep1= 2.23, Rep 2=2.13; RPD=(2.23-2.13)/((2.23+2.13)/2) = 28% Criteria and equations for rejecting suspected outlier values: Data that did not meet acceptance criteria as described in the OPPTS and OECD guidelines was excluded using statistical justification provided by Dixon's Q-test. A data point may be excluded if " Q observed" is greater than " Q tabuiated" with 90% confidence. Qobserved = gap/range where "gap" is the difference between the questionable data point and the closest value of the data set, and "range" is the difference between the highest and lowest value of the data set. Q-tabulated (90% confidence) for 3 observations (or data points) is 0.886, and 4 observations is 0.679. Page 170 of 171 BACK TO MAIN 3M Environmental Laboratory Project # E01-0768 Q-Test Example (S haded n u m ber represents the su spected outlier): Description Sample Conc., Rep1 u3a./4m3L Sample Conc., Rep2 2.23 Sample Conc., Rep3 2.13 Range (Rep1-Rep3): 1.3 Gap (Rep1-Rep2): Qobserved (Gap/Range): No. observations: 1.2 0.923 3 Retain? No Q-Test example conclusion: Since Q obServed. 0.923, was greater than Q ,abuiated, 0.886, rep 1 may be excluded. Page 171 of 171