Document gDdBje6EVKO1zpXz3ozrxBLeJ

AKM-oJi VAPOR PRESSURE TEST SUBSTANCE Identity: N-Ethylperfluorooctanesulfonamide; may also be referred to as U1464, EtFOSA, EtPOSA, F-6309, or FX-12. (1Octanesulfonamide, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-N-ethyl-, CAS # 4151-50-2) Remarks: Material is a white solid. Report states that sample purity is 99% based on information supplied by Sponsor's representative. The lot number was not recorded. METHOD______________________________________ ' Method: OECD 104, Dynamic Method GLP (Y/N): Yes Year completed: 1998 Remarks: The following quote from the test report describes the only test deviation: "While testing test item, the air condenser was used in place of water condenser because of low melting point of the test item. To the best of our (AScI Corporation) current scientific knowledge and understanding, this deviation should have no effect on the outcome of this test." (Quote taken from the test report). RESULTS_________________________________________ ________ Vapor Pressure: The vapor pressures at 10, 20, 25, and 30C were 0.047, 0.142, 0.239, and 0.395 Pa, respectively based on the increasing pressure regression equation. Decomposition (yes/no/ambiguous): Not noted Remarks:. The estimated vapor pressures for the increasing and decreasing pressure conditions differ by 20 to 24%. CONCLUSIONS The vapor pressure as determined with the dynamic method was assumed to be 0.142 Pa at 20C based on the increasing pressure regression equation. DATA QUALITY________________________ 006007 R eliability: Klimisch ranking = 2. This study meets all the criteria for quality testing. However, the 99% purity may not be correct. The value was assigned by NMR which is incomplete. Possible non-linear plot (not enough data points). REFERENCES__________________________________________ Study conducted at the request of 3M Company by, AScI Corporation, Duluth, MN. OTHER___________________________________________________ Subm itter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 Last changed: 5/16/00 006008 AScI Report #045-VP.R3M AScl Study ID #5030-045-01 Page 1 STUDY TITLE F X -U Determination of Vapor Pressure Curve by Dynamic Method for U1464 (ET POSA) v DATA STANDARD OECD Guideline 104, "Vapor Pressure Curve, Dynamic Method" AUTHORS Mike Signorelli Linda Christensen Phillip Marquis STUDY COMPLETED November 6, 1998 TESTING FACILITY AScI Corporation/AScI-Duluth Environmental Testing Division 4444 Airpark Boulevard Duluth, MN 55811-5712 Tel. No. (218) 722-4040 STUDY IDENTIFICATION NUMBERS AScI Study ID# 5030-045-0l a 3M Company Environmental Technology and Safety Services Sponsor Study ID# U1464 a This study report contains total of 26 pages. The raw data package (34 pages) supporting this study is kept on file at AScI-DETD. Sponsor Study ID# U1464 006009 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 2 CERTIFICATION OF GOOD LABORATORY PRACTICE COMPLIANCE To the best of my knowledge, this study was conducted in accordance with OECD Good Laboratory Practice regulations (1). AScI Study Director Name (signed): J 2 . (O . Date: Name (typedV.l M a Christensen Sponsor Study ID# U1464 006010 AScI Report #045-VP.R3M AScl Study ID #5030-045-01 Page 3 STATEMENT OF QUALITY ASSURANCE The study data were reviewed by the AScI Quality Assurance Unit to assure that standard operating procedures and guidelines used to conduct this study were followed, and this report is an accurate reflection of the raw data. The types of audits performed for this study are listed in the following table. Type of Audit for AScI Study ID# 5030-045-01 Test Protocol In-Life Phase Raw Data and Draft Report Final Report Audit Date 3/26/98 4/3/98, 4/7/98 5/27/98 11/4/98 Date Reported to Study Director and Management 3/27/98 4/6/98, 4/8/98 5/27/98 11/5/98 AScTs Quality Assurance Unit Auditor Name (signed):.___ Name (typed'):Alan Mozol Date: Sponsor Study ID# U1464 006011 TABLE OF CONTENTS AScI Report #045-VP.R3M AScl Study ID #5030-045-01 Page 4 COVER P A G E ............................................................. ............................................................................ 1 CERTIFICATION OF GOOD LABORATORY PRACTICE C O M PL IA N C E................................. 2 STATEMENT OF QUALITY ASSURANCE ...................... ........................ ..................................... 3 TABLE OF C O N TEN TS............................................................ ................................................. .. 4' STUDY SY N O PSIS........................................................ .. . . .................................................. ............. 6 1.0 INTRODUCTION ........................... 8 2.0 TEST METHODS .......................................................................................................................... 8 3.0 TREATMENT OF RESULTS .....................................................................................................10 4.0 RESULTS AND DISCUSSION ........................................................................ 10 5.0 CONCLUSIONS ................................................................ 11 6.0 DEVIATIONS FROM APPROVED TEST P R O T O C O L ........................................................11 7i0 REPORT SIG N A T U R E ..................................................................................................................12 8.0 REFERENCES .............................. 12 TABLE 1. Toluene (Reference Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Increasing P re ss u re .............................................................................................. ' . . 13 TABLE 2. Toluene (Reference Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Decreasing Pressure .............. ..................................................................................14 TABLE 3. Toluene (Reference Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 1 .................................................................................15 TABLE 4. Toluene (Reference Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 2 ......................... ...................................................... 16 Sponsor Study ID# U1464 006012 AScl Report #045-VP.R3M AScI Study ID #5030-045-01 Page 5 Table of Contents (cont.) TABLE 5. Range of Vapor Pressure Values for Toluene by the Dynamic Method from OECD and EEC-Laboratory Intercomparison Testing Programs ( 4 ) .....................................17 TABLE 6. ET POSA (Test Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Rising Pressure ................................................... .............................................................18 TABLE 7. ET POSA (Test Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Decreasing P re ssu re ........................................................................................................ 19 TABLE 8. ET POSA (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 3 . .......................................................................................20 TABLE 9. ET POSA (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 4 .......................................................................................... 21 TABLE 10. ET POSA (Test Item): Responsibilities, Signatures, and Initials of Key Personnel Involved in the S tu d y ........... ..........................................................................................22 FIGURE 1. A Representative Plot of Log P (Pa) and 1/T (K) Toluene at Increasing Pressur FIGURE 2. A Representative Plot of Log P (Pa) and 1/T (K) Toluene at Decreasing Pressu FIGURE 3. A Representative Plot of Log P (Pa) and 1/T (K) P re ss u re .............................. ET POSA at Increasing . 25 FIGURE 4. A Representative Plot of Log P (Pa) and 1/T (K) ET POSA at Decreasing Pressure 26 RAW DATA PACKAGE APPENDIX A. Approved Study Protocol #045-VP.P3M and Amendments APPENDIX B. Test Item Information APPENDIX C. Test Item Receipt and Usage APPENDIX D. Raw Data Sheets Sponsor Study ID# U1464 006013 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 6 STUDY SYNOPSIS Title: X Determination of Vapor Pressure Curve by Dynamic Method for U1464 (ETPOSA) ' Test Method: Dynamic method as described in AScI Protocol# 045-VP.P3M Key Findings: 1) The estimated vapor pressures of the test item, ET POSA, are 0.142 and 0.176 Pa at 20C; and 0.239 Pa and 0.293 Pa at 25C. Study sponsor Company: 3M Environmental Technology & Safety Services 935 Bush Avenue Building 2-3E-09 St. Paul, Minnesota 55133-3331 Study Representative: Dr. Rich Purdy Ecotoxicologist Phone: (612) 778-5379 Fax: (612) 778-6176 Test item Trade Name: ET POSA. Lot/Batch Number: FC12 from John Eberlin 3/12/98. Sponsor Study Identification Number: U1464 Molecular Formula: C8F17S02NCH2CH3 Chemical Abstract Service Registry#/Code#: TradeSecret Physical Description: White waxy solid Percent Purity (% active ingredient): 99% Based on information supplied by Sponsor's Representative. Sponsor Study ID# U1464 006014 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 7 Stability Data: Stable at room temperature. Storage Conditions: Room temperature in darkness. v Testing Facility Company: AScI Corporation/AScI-Duluth Environmental Testing Division (AScI) 4444 Airpark Blvd . Duluth, Minnesota 55811-5712 AScI Study Director: Linda Christensen Phone: (218) 722-4040 Fax: (218) 722-2592 Reference Item Trade Name: Toluene. Lot/Batch Number: 8608KTMH. CAS Registry#/Code#: 108-88-3. Percent Purity: 99.9%. Source: Mallinckrodt. Date Container Opened: 4/3/98. Study Initiation Date: 3/30/98. Experimental Dates Experiment Determination of Vapor Pressure Starting Date 4/3/98 Termination Date 4/8/98 / Location Raw Data and Final Report Certified copies will be archived at testing facility for five years from the date the study is completed, after which, the Sponsor will be contacted to determine further disposition of all records. Sponsor Study ID# U1464 006015 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 8 1.0 INTRODUCTION Chemical substances introduced into the environment present potential disposal and reentry hazards. The assessment of environmental fate and effect of these substances is required by various governmental agencies. Accordingly, one of the tests is to determine the vapor pressure of a substance. In this experiment, the test item boiling point is determined at a desired pressure and then vapor pressure and boiling point are correlated. The vapor pressure of a substance is an environmentally relevant property because (1) it indicates the probability of phase transition, volatilization (liquid/gas) or sublimation (solid/gas), of a chemical, (2) it helps substantiate predictions regarding the environmental behavior of chemicals, (3) chemical vapor pressure and water solubility allow for the calculation of chemical volatility from an aqueous solution, and (4) it is useful in deciding whether photochemically induced degradation can be determined in the homogenous gas phase or in an absorbed phase (OECD 1993). 2.0 TEST METHODS 2.1 Glassware. All glassware employed were cleaned before use by performing the following: 1) "Washed in hot detergent water and rinsed three times with warm tap water. 2) Immersed in 10% H N 03 acid bath and then rinsed with deionized water. 3) Rinsed three times each with acetone followed by hexane. All glassware used were labeled with the relevant information required for proper identification. 2.2 Test item. The test item, ET POSA, material safety data sheets, and certificate of analysis were received at AScI on March 27, 1998. The test item was in one glass bottle and was stored at room temperature in darkness as received. All relevant information about the test item is described earlier in this report. In this test, 13.39 g of test item was used. 2.3 Reference Item. Reagent grade toluene was used as a reference chemical. All relevant information about the reference item is described earlier in this report. In this test, 35 ml of reference chemical was used. 2.4 Test Apparatus. The test system consisted of: 1) 5-L Ballast bulb to vary pressure in double-neck distillation flask. Sponsor Study ID# U1464 006016 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 9 : 2) Closed-tube mercury manometer to measure pressure. 3) 100-ml double-neck distillation flask. 4) a Centigrade thermometer, 0.2C, with one hole rubber stopper to fit in the distillation flask. 5) Reflux condenser. 6) Heating element. 7) Vacuum pump. 8) Aspirator. 9) Boiling stones. 10) Nitrogen cylinder. 2.5 Determination of Vapor Pressure. The procedure to determine the vapor pressures of test and reference items was as follows: 1) Placed the item in double-neck distillation flask at a volume about onethird the flask volume, and added three to four boiling stones. 2) Flanged test system together and purged it with nitrogen. The pressure in the system was adjusted using vacuum. 3) Heated the item gradually until temperature equilibrium was reached, that is, when a constant boiling temperature was found. 4) At this point, recorded total pressure (in mm Hg) and boiling point T (in C). 5) For at least five different pressures, increased pressure and recorded new total pressures and boiling points when equilibria were reached. 6) To obtain the second set of data, recorded total pressure and boiling point as the pressure was lowered. Sponsor Study ID# U1464 006017 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 10 3.0 TREATMENT OF RESULTS For each data set with test and reference items, total pressure was converted to Pa unit by multiplying the observed millimeter mercury pressure with 133.3. Similarly, the boiling point (T) was converted to K by adding 273.15 to the observed C boiling point. The log of total pressure (Pa) vs. (1/T) from the individual data sets were regressed to develop the vapor pressure curves for each item. Vapor pressures for the test item and the reference item were determined at 10C, 20C, 25C, and 30C using appropriate linear regression equations. 4.0 RESULTS AND DISCUSSION Reference Item: Toluene The observed data obtained for increasing and decreasing the pressure are shown in Tables 1 and 2, respectively for toluene. The calculated regression curves from the plotted curves, Figures 1 and 2, are: Increasing pressure: log p = 10.27-1994 (1/T) r = -0.999, n = 5 (1) Decreasing pressure: log p = 10.35-2023 (1/T) r = -0.998, n = 5 (2) The two data sets are similar and have correlation coefficients greater than 0.995. The estimated vapor pressures at 10, 20, 25, and 30C are listed in Tables 3 and 4 for the two toluene data sets. Table 5 lists the range of vapor pressure values determined by the dynamic method from interlaboratory comparisons (4). The toluene vapor pressures determined from equation 1 are within the ranges listed for the interlaboratory comparisons. The values determined from equation 2 are slightly lower at 10 and 20C. The vapor pressure for toluene at 20C (2.8 X 103 Pa) is lower than the criterion established in the protocol (2.9-3.1 X 103 Pa). The vapor pressure for toluene at 10C (1.6 X 10'3 Pa) is lower than the criterion stated in reference 4 (1.7-1.8 X 10"3 Pa). A problem occurred with the system as the pressure was decreased. To get the toluene to boil as the pressure was decreased, more boiling chips were added to the item. It is not clear whether this would have affected the temperature and pressure measurements. Sponsor Study ID# U1464 006018 AScI Report A045-VP.R3M AScI Study ID #5030-045-01 Page 11 The experimental design presented here for determining vapor pressure curves appears to provide data comparable to that reported in reference 4. The regression curves are linear for both increasing and decreasing pressures. Test Item: ET POSA The observed data obtained for increasing and decreasing the pressure are shown in Tables 6 and 7, respectively. The calculated regression curves from the plotted curves of log p vs (1/T), Figures 3 and 4 are: Increasing pressure: log p = 12.64-3954 (1/T) r = -0.999, n = 5 (3) Decreasing pressure: log p = 12.45-3871 (1/T) r = -0.997, n = 5 (4) The estimated vapor pressures at 10, 20, 25, and 30C are listed in Tables 8 and 9 for the test item. The estimated vapor pressures for the increasing and decreasing pressure conditions differ by 20 to 24 percent. 5.0 CONCLUSIONS The placement of the thermometer in the apparatus proved to be pivotal in establishing accurate, steady temperature measurements. The placement of the thermometer for the test item was different than that of the reference item. The thermometer was placed approximately one inch above the bubbling test item in the collection flask. The thermometer for the reference item was placed in the neck of the collection flask. Based on the increasing pressure regression equation, the vapor pressures at 10C, 20C, 25C, and 30C were 0.047 Pa, 0.142 Pa, 0.239 Pa, and 0.395 Pa, respectively. 6-0 DEVIATIONS FROM APPROVED TEST PROTOCOL The deviation which occurred while conducting this study is: 1) While testing test item, the air condenser was used in place of water condenser because of low melting point of the test item. Sponsor Study ID# U1464 006019 AScl Report #045-VP.R3M AScI Study ID #5030-045-01 Page 12 T the best of our current scientific knowledge and understanding, this deviation should have no effect on the outcome of this test. 7.0 REPORT STONATURE Responsibilities, signatures, initials, and names of key personnel involved in this study are in Table 10. 8.0 REFERENCES 1) Organization for Economic Cooperation and Development (OECD), 1993. OECD Guidelines for Testing of Chemicals. OECD Publication Information Center, Washington, DC. 2) Shoemaker, D.P. and C.W. Garland. 1962. Experiments in Physical chemistry. McGraw-Hill.Book Co., pp. 162-163. 3) Organization for Economic Cooperation and Development (OECD), 1997. Environment Directorate, Chemicals Group and Management Committee. OECD Series on Principles of Good Laboratory Practice and Compliance Monitoring. Number 1. OECD Principles on Good Laboratory Practice. Sponsor Study ID# U1464 006020 AScl Report #045-VP.R3M AScI Study ID #5030-045-01 Page 13 TABLE 1. mmHg 47 64 77 100 124 Toluene (Reference Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Increasing Pressure Measured Pressure P (Pa) 6265 8531 10264 13330 16529 Log p (Pa) 3.797 3.931 4.011 4.125 4.218 T (C) 35.0 41 2 45.5 51.2 56.5 Observed Temperature T (K) 308.15 314.35 318.65 324.35 329.65 irr(K ) 0.003245 0.003181 0.003138 0.003083 0.003034 Sponsor Study ID# U1464 006021 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 14 TABLE 2. mmHg 150 128 110 77 52 - Toluene (Reference Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Decreasing Pressure Measured Pressure P (Pa) 19995 17062 14663 10264 6932 Log P (Pa) 4.301 4.232 4.166 ' 4.011 3.841 T (C) 61.2 57.7 53.6 45.0 38.0 Observed Temperature T (K) 334.35 330.85 326.75 318.15 311.15 1/T (K) 0.002991 0,003023 0.00306 0.003143 0.003214 Sponsor Study ID# U1464 006022 AScI Report #045-VP.R3M AScI Study ID #5030-045-0] Page 15 TABLE 3. Toluene (Reference Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation i ' T (Q 10 20 25 30 Vapor Pressure (Pa) 1.7 X 13 2.9 X 103 3.8 X 103 4.9 X 103 Vapor Pressure (mmHg) 12.7 22.0 28.6 36.9 Sponsor Study ID# U1464 006023 AScl Report #045-VP.R3M AScI Study ID #5030-045-01 Page 16 TABLE 4. Toluene (Reference Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 2 T (C ) 10 20 25 30 Vapor Pressure (Pa) 1.6 X13 2.8 X 103 3.7 X 103 4.8 X 13 Vapor Pressure (mmHg) 12.0 21.1 27.5 35.6 Sponsor Study ID# U1464 006024 TABLE 5. ' AScI Report 045-VP.R3M AScI Study ID #5030-045-01 Page 17 Range of Vapor Pressure Values for Toluene by the Dynamic Method from OECD and EEC-Laboratory Intercomparison Testing Programs (4) Temperature (C) 10 20 30 Range of Vapor Pressure (Pa) (1.7-1.8) X 13 (2.9-3.1) X 13 (4.8-5.0) X 103 Sponsor Study ID# U1464 006025 AScl Report #045-VP.R3M AScI Study ID #5030-045-01 Page 18 TABLE 6. mmHg 42 58 68 83 94 ET POSA (Test item ): Boiling points (T) and Corresponding Vapor Pressures (p) at Rising Pressure Observed Pressure p (Pa) 5599 7331 9064 11064 12530 Log p (Pa) 3.748 3.888 3.957 4.044 4.098 T (Q 171.6 178.8 181.8 186.4 190.2 Observed Temperature T (K) 444.75 451.95 454.95 459.55 463.35 1/T (K) 0.002248 0.002213 0.002198 0.002176 0.002158 Sponsor Study ID# U 1464 006026 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 19 TABLE 7. mmHg 106 95 86 75 47 ET POSA (Test Item): Boiling points (T) and Corresponding Vapor Pressures (p) at Decreasing Pressure Observed Pressure P (Pa) 14130 12664 11464 9998 6265 Log p(Pa) 4.150 4.103 4.059 4.000 3.797 T(C ) 193.0 191.0 188.0 183.8 174.4 Observed Temperature T (K) 466.15 464.15 461.15 456.95 447.55 1/T (K) 0.002145 0.002154 0.002168 0.002188 0.002234 Sponsor Study ID# U1464 006027 AScl Report 0O45-VP.R3M AScl Study ID #5030-045-01 Page 20 TABLE 8. ET POSA (Test Item): Estimated Yapor Pressures (p) at Different Temperatures (T) Determined from Equation 3 ' T (0Q 10 20 25 30 , Vapor Pressure (Pa) 0.047 0.142 0.239 0.395 Vapor Pressure (mmHg) 0.36 X 10-3 1.06 X IO'3 1.79 X IO*3 2.97 X IO"3 Equation 3 --Log Pa = 12.64-3954 (1/T) Example Calculation Log Pa = 12.64-3954 (1/T) 10#C = 283.15K Log Pa = 12.64-3954 (1/283.15) Log Pa - 12.64-13.9643 Log Pa = 1.3243 Pa = Inv Log (-1.3243) Pa = 0.047 For mm Hg = 0.047 = 0.36 X 10'3 133.33 Sponsor Study ID# U1464 O06028 AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 21 TABLE 9. ET POSA (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 4 ' T ( Q 10 20 25 30 Vapor Pressure (Pa) 0.060 0.176 0.293 ' 0.479 Vapor Pressure (mmHg) 0.45 X IO*3 1.32X10-3 2.20 X IO"3 3.60 X IO-3 Equation 4 = Log Pa = 12.45-3871 (1/T) Sponsor Study ID# U1464 006029 AScI Report #045-VP.R3M AScl Study ID #5030-045-01 Page 22 TABLE 10. ET POSA (Test Item): Responsibilities, Signatures, and Initials of Key Personnel Involved in the Study | Personnel Linda Christensen | Mike Signorelli Alan Mozol Joe Amato Phillip Marquis Nancy Jordan Title/Responsibility Study Director Laboratory assistance Quality Assurance Auditor Project Manager Report Preparation Archivist Signature ^/al7fCj/J( -------. V ----- Initials tpt___ . \tf r\% % . Sponsor Study ID# U1464 006030 AScl Report #045-VP.R3M AScI Study ID #5030-045-01 Page 23 Figure 1. A Representative Plot of Log p (Pa) and 1/T (K) for Toluene at Increasing Pressure 006031 Sponsor Study ID# U 1464 1/T(K) AScI Report #045-VP.tt3M AScI Study ID #5030-045-01 Page 24 Sponsor Study ID# U1464 ZC0900 AScI Report #045-VP.g3M AScI Study ID #5030-045-01 Page 25 Figure 3. A Representative Plot of Log p (Pa) and 1/T (K) for ET POSA at Increasing Pressure 00603a Sponsor Study ID# UI464 1/T, K AScI Report #045-VP.R3M AScI Study ID #5030-045-01 Page 26 Figure 4. A Representative Plot of Log p (Pa) and 1/T (K) for ET POSA at Decreasing Pressure Sponsor Study ID# U1464 006034