Document MGGBYaa0YVdj1jorZ5ZXVGzEx

AR U 6 '03% VAPOR PRESSURE TEST SUBSTANCE Identity: N-ethylperfluorooctane sulfonamidoethanol; may also be referred to as N-EtFOSE Alcohol or FM-3422. (1-Octanesulfonamide, N-ethylI.I^.S.S^AS.S.e.ejJ.S.S.S-heptadecafluoro-N-^-hydroxyethyl)-, CAS #1691-99-2) Remarks: Material is a white waxy solid. It is characterized as being stable at room temperature. The report indicates the sample was 99% pure. METHOD:_____________________________________ ________________________ Method followed: OECD Guideline 104, "Vapor Pressure Curve, Dynamic Method." GLP: Yes Year study was performed: 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). No note was made of any decomposition. RESULTS_________ The vapor pressures at 10C, 20C, 25C, and 30C were 0.194 Pa, 0.504 Pa, 0.792 Pa, and 1.227 Pa, respectively based on the decreasing pressure regression equation. Remarks: "The estimated vapor pressures for the increasing and decreasing pressure conditions differ by 42-50 percent." CONCLUSIONS______________________________________________________ The vapor pressure suggests this material would exist primarily in the gas phase in the atmosphere. DATA QUALITY______________________________ 006131 Reliability: 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). As described above, the vapor pressures calculated while pressure was increased vs. decreased differ by 42-50 percent. However, third party consultant review of the data concluded the study is valid. REFERENCES________________________________________ Determination of Vapor Pressure Curve by Dynamic Method for U1463 (ET FOSE), ASci Report# 044-VP.R3M, ASci Study ID #5030-044-01, November6, 1998. O T H E R _______________________________________________________________ Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 Last changed: 5/18/00 006132 STUDY TITLE AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 1 fc .^ 0 Determination of Vapor Pressure Curve by Dynamic Method for U1463 (ET FOSE) 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# 5030-044-018 3M Company Environmental Technology and Safety Services Sponsor Study ID# U1463 a This study report contains a total of 26 pages. The raw data package (33 pages) supporting this study is kept on file at AScI-DETD. Sponsor Study ID# U1463 006133 AScI Report #044-VP.R3M r AScI Study ID #5030-044-01 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). Sponsor Study ID# U1463 I / G0G134 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 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. I Type of Audit for AScI Study ID# 5030-044-01 Test Protocol In-Life Phase Raw Data and Draft Report Final Report Audit Date 3/26/98 4/3/98, 4/7/98 5/22/98, 5/27/98 11/4/98 Date Reported to Study Director and Management 3/27/98 4/6/98, 4/8/98 5/26/98, 5/27/98 11/5/98 AScI's Quality Assurance Unit Auditor Name (signed):______ Name (typed) :Alan Mozol .Bate. / / ./ i f ? ? Sponsor Study ID# U1463 006135 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 4 TABLE OF CONTENTS COVER P A G E .................................................................................................... CERTIFICATION OF GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT OF QUALITY ASSURANCE ................................................ TABLE OF CONTENTS.......................... ....................................................... STUDY SYNOPSIS........................................................................................... 1.0 INTRODUCTION ............................................................... .. ............. 2.0 TEST METHODS ......................................... ..................................... 3.0 TREATMENT OF RESULTS ............................................................. 4.0 RESULTS AND DISCUSSION .......................................................... 5.0 CONCLUSIONS ............................................................... : .............. 6.0 DEVIATION FROM APPROVED TEST PR O TO C O L .................... 7.0 REPORT SIG N A TU R E........................................................................ 8.0 REFERENCES ..................................................................................... 1 2. 3 4 6 8 8 10 10 11 12 12 12 TABLE 1. Toluene (Reference Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Increasing P re ssu 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# U 1463 00G136 Table of Contents (cont.) AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 5 TABLE 5. Range of Vapor Pressure Values for Toluene by the Dynamic Method from OECD and EEC-Laboratory Intercomparison Testing Program ( 4 ) ................................. .. . 17 TABLE 6. ET FOSE (Test Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Increasing Pressure ........................................................................... .......................... 18 TABLE 7. ET FOSE (Test Item): Boiling Points (T) and Corresponding Vapor Pressures (p) at Decreasing P re ssu re .......................................................................................................19 TABLE 8. ET FOSE (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 3 .................................... ................................................... 20 TABLE 9. ET FOSE (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 4 .........................................................................................21 TABLE 10. ET FOSE (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 Pre*ssure . 23 FIGURE 2. A Representative Plot of Log p (Pa) and 1/T (K) Toluene at Decreasing Pressure . 24 FIGURE 3. A Representative Plot of Log p (Pa) and 1/T (K) ET FOSE at Increasing P re s s u re ..........................................................................................................................25 FIGURE 4. A Representative Plot of Log P (Pa) and 1/T (K) ET FOSE at Decreasing Pressure 26 RAW DATA PACKAGE APPENDIX A. Approved Study Protocol #044-VP.P3M and Amendments APPENDIX B. Test Item Information APPENDIX C. Test Item Receipt and Usage APPENDIX D. Raw Data Sheets Sponsor Study ID# U1463 006137 AScI Report A044-VP.R3M AScI Study ID #5030-044-01 Page 6 STUDY SYNOPSIS Title: Determination of Vapor Pressure Curve by Dynamic Method for U1463 (ET FOSE) Test Method: Dynamic method as described in AScI Protocol# 044-VP.P3M Key Findings: 1) The estimated vapor pressures of the test item, ET FOSE, are 0.504 Pa at 20C and 0.792 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 Chemical Trade Name: ET FOSE. Lot/Batch Number. 61691-16 (Technical Laboratory Book, John Eberlin). Sponsor Study Identification Number: U1463 Molecular Formula: C8F 17S 0 2N(CH2CH3)CH2CH20H 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# U1463 006138 Stability Data: Stable at room temperature. I AScI Report #044-VP.R3M AScl Study ID #5030-044-01 Page 7 Storage Conditions: Room temperature in darkness. 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. Ia Study Initiation Date: 3/30/98. Experimental Dates Experiment Determination of Vapor Pressure Starting Date 4/3/98 Termination Date 4/8/98 / y 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# U1463 006139 AScl Report #044-VP.R3M AScI Study ID #5030-044-01 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% HN 03 acid bath and then rinsed with deionized water. 3) Rinsed three times each with acetone followed by hexane. J All glassware used were labeled with the relevant information required for proper identification. 2.2 Test Item. The test item, ET FOSE, 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, 14.21 g of test item was used. 2.3 Reference Item. Reagent-grade toluene was used as a reference item. All relevant information about the reference item is described earlier in this report. In this test, 35 ml of reference item 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# U1463 006140 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 9 2) Closed-tube mercury manometer to measure pressure. 3) 100-ml double-neck distillation flask. \ 4) 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 chemical 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 IDH U1463 006141 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 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 P) The two data sets are similar and have correlation coefficients greater than 0.990. 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# U1463 G0 6 1 4 2 AScI Report #044~VP.R3M AScI Study ID #5030-044-01 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 FOSE 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 = 11.09-3278 (1/T) r = -0.988, n = 5 (3) Decreasing pressure: log p = 11.42-3435 (1/T) r = -0.994, n = 5 (4) The regression line for decreasing pressure is more linear, than the increasing pressure regression line. 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 42-50 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. Two previous trials with the test item were performed prior to the test reported to determine the correct placement of the thermometer. 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 decreasing pressure regression equation, the vapor pressures at 10C, 20C, 25C, and 30C were 0.194 Pa, 0.504 Pa, 0.792 Pa, and 1.227 Pa, respectively. Sponsor Study ID# U1463 006143 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 12 6.0 DEVIATION 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 o f water condenser because of low melting point of the test item. To the best of our current scientific knowledge and understanding, this deviation should have no effect on the outcome of this test. 7.0 REPORT SIGNATURE 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# U1463 006144 TABLE 1. mmHg 47 64 77 100 124 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 13 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 1/T (K) 0.003245 0.003181 0.003138 0.003083 0.003034 Sponsor Study ID# U1463 006145 AScl Report #044-VP.R3M AScI Study ID #5030-044-01 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 0.003060 0.003143 0.003214 Sponsor Study ID# U1463 006146 AScl Report #044-VP.R3M AScI Study ID #5030-044-01 Page 15 TABLE 3. Toluene (Reference Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation l a T(C ) 10 20 25 30 Vapor Pressure (Pa) 1.7 X 103 2.9 X 103 3.8 X 13 4.9 X 103 Vapor Pressure (mmHg) 12.7 22.0 28.6 36.9 * Equation 1 --Log p = 10.27-1994 (1/T) > Sponsor Study ID# U1463 006147 4 ..(I AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 16 TABLE 4. Toluene (Reference Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 2a T (C) 10 20 25 30 Vapor Pressure (Pa) 1.6 X 13 2.8 X 103 3.7 X 13 4.8 X 103 Vapor Pressure (mmHg) 12.0 21.1 27.5 35.6 * Equation 2 --Log p = 10.35-2023 (1/T) Sponsor Study ID# U1463 006148 TABLE 5. I AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 17 Range of Vapor Pressure Values for Toluene by the Dynamic Method from OECD and EEC-Laboratory Intercomparison Testing Program (4) Temperature (C) 10 20 30 Range of Vapor Pressure (Pa) (1.7-1.8) X 103 (2.9-3.1) X 103 (4.8-5.0) X 103 Sponsor Study ID# U1463 00S149 * . I * TABLE 6. mmHg 42 55 67 81 96 AScI Report #044-VP.R3M AScI Study ID 030-044-01 Page 18 ET FOSE (Test Item): Boiling points (T) and Corresponding Vapor Pressures (p) at Increasing Pressure Observed Pressure P (Pa) 5599 7332 8931 10797 12797 Log p (Pa) 3.748 3.865 3.951 4.033 4.107 T (Q 174.6 179.0 187.2 190.2 197.0 Observed Temperature T (K ) 447.75 452.15 460.35 463.35 470.15 1/T (K) 0.002233 0.002212 0.002172 0.002158 0.002127 > Sponsor Study ID# U1463 006150 TABLE 7. mmHg 93 83 68 48 37 AScI Report 044-VP.R3M AScI Study ID #5030-044-01 Page 19 ET FOSE (Test Item): Boiling points (D and Corresponding Vapor Pressures (p) at Decreasing Pressure Observed Pressure P (Pa) 12397 11064 9064 6398 4932 Log p (Pa) 4.093 4.044 3.957 3.806 3.693 T(C ) 195.8 191.6 188.2 176.4 172.2 Observed Temperature T(K) 468.95 464.75 461.35 449.55 445.35 1/T (K) 0.002132 0.002152 0.002168 0.002224 0.002245 4r Sponsor Study ID# U1463 006151 AScl Report #044-VP.R3M AScl Study ID #5030-044-01 Page 20 TABLE 8. ET FOSE (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 3 T (Q 10 20 25 30 Vapor Pressure (Pa) 0.326 0.809 1.246 1.892 Vapor Pressure (mmHg) 2.44 X 10-3 6.07 X 10-3 9.35 X 10-3 14.2 X IQ"3 Equation 3 - Log Pa = 11.09-3278 (1/T) Example Calculation Log Pa = 11.09-3278 (1/T) 10C = 283.15K Log Pa = 11.09-3278 (1/283.15) Log Pa = 11.09-11.5769 Log Pa = 0.4869 Pa = Inv Log (-0.4869) Pa = 0.326 For mm Hg = 0.326 = 2.44 X 10r3 133.33 Sponsor Study ID# U 1463 006152 ASci Report #044-VP.R3M AScI Study ID #5030-044-01 Page 21 TABLE 9. ET FOSE (Test Item): Estimated Vapor Pressures (p) at Different Temperatures (T) Determined from Equation 4 ` T (Q 10 20 25 30 Vapor Pressure (Pa) 0.194 0.504 0.792 1.227 Vapor Pressure (mmHg) 1.46 X 10-3 3.78 X IO-3 5.94 X IO-3 9.21 X IO-3 Equation 4 --Log Pa = 11.42-3435 (1/T) Sponsor Study ID# U1463 00G153 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 Page 22 TABLE 10. ET FOSE (Test Item): Responsibilities, Signatures, and Initials of Key Personnel Involved in the Study Personnel Linda Christensen Mike Signorelli Alan Mozol Joe Amato Phil Marquis Nancy Jordan Title/Responsibility Study Director Laboratory Assistance Quality Assurance Auditor Project Manager Report Preparation Archivist Signature Initials A I Sponsor Study ID# U1463 006154 AScl Report #044-VP.R3M AScI Study ID #5030-044-01 Page 23 Sponsor Study ID# U1463 AScI Report #044-VP.R3M AScI Study ID #5030-04141 Sponsor Study ID# U1463 006156 AScI Report #044-VP.R3M AScl Study ID #5030-044^01 Page 25 Figure 3. A Representative Plot of Log p (Pa) and 1/T(K) for ET FOSE at Increasing Pressure 00G157 Sponsor Study ID# UI463 1/T(K) . AScl Report *044-VP.R3M AScl Study ID *5030-04101 Page 26 Figure 4. A Representative Plot of Log p (Pa) and 1/T(K) for ET FOSE at Decreasing Pressure 0.00212 0.00214 0.0021 Q ^ 0 .00218 0.00220 0.00222 0.00224 0.00226 o 0 (ft 1/T(K) K* 01 00 Sponsor Study 1D0 UI463 .> AScI Report #044-VP.R3M AScl Study ID #5030-044-01 RAW DATA PACKAGE APPENDIX A. Approved Study Protocol #044-V P .P 3M and Amendments APPENDIX B. Test Item Information APPENDIX C. Test Item Receipt and Usage APPENDIX D. Raw Data Sheets Sponsor Study ID# U1463 006159 -- AScl Corporation 4444Airpark Boulevard, Duluth, Minnesota 5581/ November 4, 1 9 9 8 <218) 722-4040 Fax (2 181 722-2592 To: Study File 5030-044-01 From: Alan E. Mozol, QAU Manager RE: Raw data package deficiencies The following deficiencies were noted by the Sponsor when editing DRAFT report and raw data for this study: 1. The chain of custody provided by the Sponsor was not signed by AScI-Environmental Testing Division (ETD) personnel. Test item ET FOSE (3M Company Lab Reguest Number U1463) was received at AScI-ETD on March 27, 1998. The sample was received by Michael Signorelli, whom is no longer employed at AScI-ETD. The test item was properly logged in following AScI-ETD SOP SUB-01-R. The "Test Item Receipt and Shipping Form" was properly completed noting March 27, 1998 as the dated received. The completed form is contained in the raw data on page 28. The Chain-of-Custody was not signed as an oversight by Mr. Signorelli. 2. On page 31 in the raw data, an entry was crossed out and not properly error coded by the technician. The initial value was 3.39101 and the 39 after the decimal were crossed out and replaced by 93 which provides a correct value. The correct value is a calculated value and not a raw data point. The lack of proper error coding was a technician error. f The following explanation is also provided for clarity: On page 33, some entries are blacked-out to make them unreadable. These entries do not pertain to the vapor pressure study, but do apply to other studies conducted on the test item. G0G1G0 AScI Report #044-VP.R3M AScl Study ID #5030-044-01 APPENDIX A. Approved Study Protocol #044-V P .P 3M and Amendments Sponsor Study ID# U1463 Pag of 006161 AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Page 1 o f 12 R \# V co i' AScI CORPORATION/AScI-DULUTH ENVIRONMENTAL TESTING DIVISION Determination of Vapor Pressure Curve by Dynamic Method AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Test Item: ET FOSE Sponsor Study ID# U1463 Paqe GGG162 AScI Protocol# 044-VP.P3M ASci Study ID# 5030-044-01 Final Version Page 2 of 12 The following information and signatures are necessary to be in compliance with Good Laboratory Practice regulations (GLP) and/or AScI's Policy. TO BE COMPLETED BY AScI BASED ON INFORMATION PROVIDED BY STUDY SPONSOR Study Sppn$Qr Company: Site Address: Mailing Address: Phone: Fax#: 3M Company 3M Center St. Paul, MN 55144-1000 Dr. Rich Purdy 3M Company Environmental Technology & Safety Services 935 Bush Avenue Bldg. 2-3E-09, P.O. Box 33331 . St. Paul, MN 55133-3331 612/778-5379 FAX 612/778-6176 Sponsor Study Identification Number Number: U1463. Lot/Batch Number: 61691-16 (Technical Laboratory Book No., John Eberlin). Chemical Abstract Service RegistryVCode#: TradeSecret. Molecular Formula: CgF 17S 0 2N (CH2CH3) CH2CH2OH. Physical Description: White waxy solid. Sponsor Study ID# U 1463 006163 AScl Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Page 3 of 12 Percent Purity (% active ingredient!: 99% Based on information supplied by Sponsor's Representative. Stability Data: Stable at room temperature. Melting Point: Not determined. Boiling Point: Expected to be less than 350C. Storage Conditions: Room temperature in darkness. Reference Item: Toluene Note: The sponsor will provide the Material Safety Data Sheets and other relevant information for test chemical. Authorization to Return Test Chemical and Samplers'): Sponsor's authorized agent to receive samples and any remaining test chemical. Name: Dr. Rich Purdy Title: Shipping Address: Ecotoxicologist 3M Company Environmental Technology & Safety Services 935 Bush Avenue Building 2-3E-09 St. Paul, Minnesota 55133-3331 + Phone: 612-778-5379 Fax: 612-778-6176 Sponsor Study ID# U1463 0G164 AScI Protocol# 044-VP.P3M AScl Study ID# 5030-044-01 Final Version Page 4 of 12 Protocol Approval (The following is to be signed by the appropriate study personnel.) Sponsor's Study Representative: Name (signed): _______ Date: *X~? / a r A Name (typed): ___________Dr. Rich Purdv ^ _______ (_______________________________ \ Title: ___________________Ecotoxicologist_____________________________________________ Sponsor Study ID# U1463 Pago 6 006165 AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Rage 5 of 12 TO BE COMPLETED BY AScI Study Conducted By Address: AScI Corporation/AScI-Duluth Environmental Testing Division (AScI) 4444 Airpark Boulevard Duluth, MN 55811 Phone: (218) 722-4040 Fax#: (218) 722-2592 The study director is located at this facility. Data Standard OECD Guideline 104, "Vapor Pressure Curve, Dynamic Method." Proposed Experimental Dates Experiment: Vapor Pressure Curve Determination Starting Date: April 3, 1998 Termination Date: April 3, 1998 Sponsor Study ID# U1463 -Ipih 006166 AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Page 6 of 12 Protocol Approval (The following is to be signed by the appropriate study personnel.) Sponsor Study ID# U1463 &CS167 AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Page 7 o f 12 1.0. 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). k 2.0. 0 QUALIFYING STATEMENT The dynamic method is restricted to test items that do not undergo chemical reaction, for example, autoxidation, rearrangement or degradation, at temperatures below the boiling points. In this study, if the test item boiling point is greater than 350C or if the test item froths, then the test substance vapor pressure will be not be determined via the Dynamic Method. Sponsor Study ID# U1463 Pag of 006168 AScI Protocol# 044-VP.P3M AScl Study ID# 5030-044-01 Final Version Page 8 of 12 3.0. 0 OBJECTIVE The objective of the present study is to develop if possible, the vapor pressure curve for the test item using the Dynamic Method. With the test objective, and GLP regulations in mind, AScI has prepared the following protocol. 4.0.0 TEST METHODS 4 .L 0 Test Apparatus. The test apparatus (Figure 1, Shoemaker and Garland 1962) will consist of: (1) 5-L Ballast bulb to vary pressure in double-neck distillation flask; (2) Closed-tube mercury manometer to measure pressure; (3) Double-neck distillation flask; (4) Centigrade thermometer (accuracy 0 .1 C) with one hole rubber stopper ^ to fit the distillation flask; (5) Reflux condenser; (6) Heating element; (7) Vacuum pump; (8) Nitrogen cylinder; and (9) Boiling stones to avoid bumping in boiling liquid. Sponsor Study ID# U1463 006169 AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Page 9 of 12 4.2.0 Determination of Vapor Pressure . The procedure to determine the vapor pressure curves for ' test and reference substances will be as follows: (1) Place test substance in double-neck distillation flask at a volume not exceeding one-third the flask volume, and add two or three boiling stones; (2) Flange the apparatus together and vacuum it; (3) Adjust the pressure in the apparatus to 103 Pa using nitrogen; (4) Heat the test substance gradually until equilibrium is reached, that is, when a constant boiling temperature is found; (5) At this point, record the total pressure (Pa) and boiling point (T); (6) Increase pressure and record the new pressure and boiling point when equilibrium is reached; (7) Continue this procedure for at least at 5 different pressures for up to 105 Pa pressure; (8) To obtain a second set of data, record pressures and boiling points as pressure is lowered to 103 Pa. * 5.0.0 Treatment of Results. For each data set, log of total pressure (Pa) will be calculated and boiling point (T) transformed to Kelvin (K). The log Pa and i/T (in K) will be then used to develop two vapor pressure curves. From each vapor pressure curve, the test substance vapor pressure at three temperatures in the range of 0-50 C, and at 25C will be determined by data interpolation or extrapolation and reported. Sponsor Study ID# U1463 .j 006170 AScI Protocol# 044-VP.P3M AScI Study ID# 5030-044-01 Final Version Page 10 of 12 6.0.0 REPORT PREPARATION v The final report will be prepared according to instructions presented in OECD Series on Principles of GLP and Compliance Monitoring, Number 1, OECD Principles on GLP 1997. The report will include (1) Cover and descriptive title, (2) Test and reference item identifications (3) Characterization of test item including purity, stability, and homogeneity, (4) Information describing the test sponsor, test facility, and contributors (5) duly signed statements regarding GLP Compliance and Quality Assurance, (6) Study Synopsis, (7) Introduction and Objectives, (8) Materials and Methods, (9) Results and Discussion, (10) Conclusions, (11) any Deviations from the Approved Study Plan, (12) Study Director's Report Signature, (13) a list of personnel involved in the Study and their Functions, (14) Literature References, (15) Raw Test Data, including the plot of log P versus 1/T, and (16) Appendices. 7-0.0 QUALITY ASSURANCE Test procedures, documentation, records and reports will conform to GLP Standards as promulgated under the OECD Chemicals Group and Management Committee, Environment Directorate, 1997. The AScI Quality Assurance Unit will perform one in-life phase audit during the test, and will also audit the study plan, test data and report. .The test will be unacceptable if vapor pressures of reference item (toluene) are not in the following ranges: 1.7 + 0.1 x 103 at 10C; 3.0 0.1 x 103 at 20C; and 4.9 0.1 x 103 at 30C. During the study, if AScI realizes a need to amend the approved study plan, we will document reasons for such changes and contact the Sponsor for approval. The changes will also be signed and dated by the Study Director and maintained with the study plan. After acceptance of the final report by the Sponsor, AScI will return the a portion of the remaining test substance to the Sponsor, and a portion will be retained for archiving. Sponsor Study ID# U1463 006171 Paga AScJ Protocol# 044-VP.P3M AScl Study ID# 5030-044-01 Final Version Page 11 o f 12 Raw data from this study, study protocol, pertinent written and telephone communications, and final report will be archived for five years at AScl. Dining the fifth year, AScl will contact the Sponsor regarding further storage of all records. 8.0.0 REFERENCES Organization for Economic Cooperation and Development (OECD), 1993. OECD Guidelines for Testing of Chemicals. OECD Publication Information Center, Washington, DC. Shoemaker, D.P. and C.W. Garland. 1962. Experiments in Physical chemistry. McGraw-Hill Book Co., pp. 162-163. 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# U1463 006172 AScl Protocol# 044-VP.PRO AScl Study ID# 5030-044-01 Final Version Page 12 of 12 FIGURE 1. APPARATUS FOR VAPOR PRESSURE DETERMINATION Sponsor Study ID# U 1463 Paga 006173 ASCI Protocol# 044-VP.P3M ASCI Study IDI 5030-044-01 Amendment - 4/2/98 AMENDMENTS (AScI Protocol# 044-VP.P3M) e following amendments have been instituted for Protocol# 044-VP.P3M, Sponsor Study ID# U1463. 1. The centigrade thermometer used for the study will have gradations of 0.2C and not 0.1 C. ' This is due to the commercial availability of thermometers in the expected test range of 0C-200C. 2. The distillation flask will be 100 ml instead of 500 ml to accommodate the smaller sample size. 3. The distillation flask will be insulated with foil during the experiments to minimize heat loss. Amendment Approval Sonsor's Study ReureSentive: ^ Name isienedh/ l - ^ ' ' * i^ T ^ Name ftvpedV. Dr. Rich^Pdrdv7 Title: Ecotoxicoloeist Date: / ) p H P 1' ! 9 ? f f Sponsor Study ID# U1463 006174 AScI Report #044-VP.R3M AScI Study ID #5030-044-01 APPENDIX B. Test Item Information 9 Sponsor Study ID# U1463 pag _ i^ o f ^ 006175 * ^ * MATERIAL'SAFETY d a t a SHEET (intermediate) 3M 3M Center St. Paul, Minnesota 55144-1000 1-800-364-3577 or (612) 737-6501 (24 hours) Copyright, 1997, Minnesota Mining and Manufacturing Company. All rights reserved. Copying and/or downloading of this information for the purpose of properly utilizing 3M products is allowed provided that: 1) the information is copied in full with no changes unless prior agreement is obtained from 3M, and 2) neither the copy nor the original is resold or otherwise distributed with the intention of earning a profit thereon. DIVISION: SPECIALTY MATERIALS DIVISION MATERIAL: FLUOROCHEMICAL ALCOHOL FM-3923 FM-3924 FM-4084 FM-4120 FM-4121 F-8904 F-8905 F-8960 ID NUMBER: 41-2600-8904-4 41-2600-8905-1 41-2600-8960-6 41-2700-3923-7 41-2700-3924-5 41-2700-4084-7 41-2700-4120-9 41-2700-4121-7 ISSUED: October 30, 1997 SUPERSEDES: May 03, 1996 DOCUMENT: 04-1162-9 U l4 (u 3 1. INGREDIENT C.A.S. NO. PERCENT N -ETHYLPERFLUOROOCTANESULFONAMIDOETHYL ALCOHOL.............................. 1691-99-2 100 2. PHYSICAL DATA BOILING POINT:..... VAPOR PRESSURE:.... VAPOR DENSITY:..... EVAPORATION RATE:... SOLUBILITY IN WATER: SPECIFIC GRAVITY:... PERCENT VOLATILE:... pH: ...................................... VISCOSITY:.......... MELTING POINT:..___ APPEARANCE AND ODOR: Amber, waxy solid. N/A < 27 psia 6131F N/D N/D neglig. ca. 1.6 Water=1 0% N/A N/A N/D AScI Study ID# 5030-044-01 006176 Abbreviations: N/D - Not Determined N/A - Not Applicable CA - Approximately Pagj3T = f-2? * > ' HSDS: FLUOROCHEMICAL ALCOHOL FM-3923 FM-3924 FM-4084 FM-4120 FM-4121 F-8904 F-8905 F-8960 October 30, 1997 PAGE 2 3. FIRE AND EXPLOSION HAZARD DATA FLASH POINT:.................. > 300 F PMCC FLAMMABLE LIMITS - LEL:....... N/A FLAMMABLE LIMITS - UEL:....... N/A AUTOIGNITION TEMPERATURE:..... N/D AScI Study ID# 5030-044-01 EXTINGUISHING MEDIA: Mater spray, Carbon dioxide, Dry chemical, Foam SPECIAL FIRE FIGHTING PROCEDURES: Hear full protective clothing, including helmet, self-contained, positive pressure or pressure demand breathing apparatus, bunker coat and pants, bands around arms, waist and legs, face mask, and protective covering for exposed areas of the head. UNUSUAL FIRE AND EXPLOSION HAZARDS: See Hazardous Decomposition section for products of combustion. NFPA HAZARD CODES: HEALTH: 2 FIRE: 1 REACTIVITY: 0 UNUSUAL REACTION HAZARD: none 4. REACTIVITY DATA STABILITY: Stable INCOMPATIBILITY - MATERIALS/CONDITIONS TO AVOID: None known. HAZARDOUS POLYMERIZATION: Hazardous polymerization will not occur. HAZARDOUS DECOMPOSITION PRODUCTS: Carbon Monoxide and Carbon Dioxide, Hydrogen Fluoride. 5. ENVIRONMENTAL INFORMATION SPILL RESPONSE: Observe precautions from other sections. Collect spilled material. Place in a closed container. RECOMMENDED DISPOSAL: Incinerate in an industrial or commercial facility. Combustion products will include HF. Disposal alternative: Dispose of waste product in a facility permitted to accept chemical waste. 006177 Abbreviations: N/D - Not Determined N/A - Not Applicable CA - Approximately Page > ISDS: FLUQROCHEMICAL ALCO H O L FM-3923 FH-3924 FH-4084 FH-4120 FM-4121 F-8904 F-8905 F-8960 October 30, 1997 PAGE 3 5. ENVIRONMENTAL INFORMATION (continued) ENVIRONMENTAL DATA: Not determined. REGULATORY INFORMATION: Volatile Organic Compounds: N/D. VOC Less H20 & Exempt Solvents: N/D. AScI Study ID# 5030-044-01 Since regulations vary, consult applicable regulations or authorities before disposal. U.S. EPA Hazardous Waste Number = None (Not U.S. EPA Hazardous). EPCRA HAZARD CLASS: FIRE HAZARD: No PRESSURE: No REACTIVITY: No ACUTE: No CHRONIC: No 6. SUGGESTED FIRST AID EYE CONTACT: No need for first aid is anticipated. SKIN CONTACT: Wash affected area with soap and water. INHALATION: If signs/symptoms occur, remove person to fresh air. If signs/symptoms continue, call a physician. IF SWALLOWED: No need for first aid is anticipated. 7. PRECAUTIONARY INFORMATION EYE PROTECTION: Avoid eye contact. Wear safety glasses with side shields. Wear full faceshield when handling molten material. SKIN PROTECTION: Avoid skin contact. Wear appropriate gloves when handling this material. Wear appropriate gloves, such as Nomex, when handling this material to prevent thermal burns. RECOMMENDED VENTILATION: Provide appropriate local exhaust when product is heated. Provide sufficient ventilation to maintain emissions below recommended exposure limits. If exhaust ventilation is not adequate, use 006178 "abbreviations: N/D - Not Determined N/A - Not Applicable CA - Approximately SDS*: FLUOflOCHEHICAL ALCOHOL FM-3923 FM-3924 FM-4084 FM-4120 FH-4121 F-8904 F-8905 F-8960 Ictbber 30, 1997 PAGE 4 7. PRECAUTIONARY INFORMATION (continued) appropriate respiratory protection. RESPIRATORY PROTECTION: Avoid breathing of vapors. Avoid breathing of airborne material. Select one of the following NIOSH approved respirators based on airborne concentration of contaminants and in accordance with OSHA regulations: half-mask organic vapor respirator, full-face organic vapor respirator, full-face supplied air respirator. PREVENTION OF ACCIDENTAL INGESTION: Nash hands after handling and before eating. Do not ingest. RECOMMENDED STORAGE: Keep container closed when not in use. FIRE AND EXPLOSION AVOIDANCE: Not applicable. AScI Study ID# 5030-044-01 EXPOSURE LIMITS INGREDIENT VALUE UNIT TYPE AUTH SKIN* N -ETHYLPERFLUOROOCTANESULFONAMIDOETHY L ALCOHOL.......................... 0.1 MG/M3 TWA 3M Y * SKIN NOTATION: Listed substances indicated with 'Y' under SKIN refer to the potential contribution to the overall exposure by the cutaneous route including mucous membrane and eye, either by airborne or, more particularly, by direct contact with the substance. Vehicles can alter skin absorption. .* g SOURCE OF EXPOSURE LIMIT DATA: - 3M: 3M Recommended Exposure Guidelines > 8. HEALTH HAZARD DATA EYE CONTACT: No adverse health effects are expected from eye contact. SKIN CONTACT: Product is not expected to be irritating to the skin. May be absorbed through the skin and persist in the body for an extended time. Abbreviations: N/D - Not Determined N/A - Not Applicable CA - Approximately 006179 MS&S: FLUOROCHEHICAL ALCOHOL FM-3923 FM-3924 FM-4084 FH-4120 FH-4121 F-8904 F-8905 F-8960 Octbber 30, 1997 PAGE 5 8. HEALTH HAZARD DATA (continued) INHALATION: May be absorbed by inhalation and persist in the body for an extended time. IF SWALLOWED: Ingestion is not a likely route of exposure to this product. Illness may occur after a single swallowing of relatively large quantities of this material. OTHER HEALTH HAZARD INFORMATION: This product is not known to contain any substances regulated under California Proposition 65. SECTION CHANGE DATES HEALTH HAZARD DATA SECTION CHANGED SINCE May 03, 1996 ISSUE ASci Study ID# 5030-044-01 Abbreviations: N/D - Not Determined N/A - Not Applicable CA - Approximately The information in this Material Safety Data Sheet (MSDS) is believed to be correct as of the date issued. 3M MAKES NO WARRANTIES, EXPRESSED OR IMPLIED, INCLUDING, BUT NOT LIMITED TO, ANY IMPLIED WARRANTY OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE OR COURSE OF PERFORMANCE OR USAGE OF TRADE. User is responsible for determining whether the 3M product is fit for a particular purpose and suitable for user's method of use or application. Given the variety of factors that can affect the use and application of a 3M product, some of which are uniquely within the user's knowledge and control, it is essential that the user evaluate the 3M product to determine whether it is fit for a particular purpose and suitable for user's method of use or application. 3M provides information in electronic form as a service to its customers. Due to the remote possibility that electronic transfer may have resulted in errors, omissions or alterations in this information, 3M makes no representations as to its completeness or accuracy. In addition, information obtained from a database may not be as current as the information in the MSDS available directly from 3M. 006180 MATERIAL INFORMATION TRANSPORTATION DOCUMENT Division: BE - SPECIALTY MATERIALS DIVISION Issued: 07/22/97 Supersedes: 05/03/96 MITS Document: 04-3216-1 Status: Complete M storisli FLUOROCHEMICAL AMIDE FM-4220 F-7604 F-7605 F-8005 F-8903 F-8929 F-8947F-8961 F-9391 AUTHOR SECTION Status: Complete Date : 03/16/95 Div. Author: COOPER WIGGINTON Div. Contact: TAMMY JOHNSON Requester: KELLY BOELKE Phone: 520-6108 Phone : 737-4152 Phone : 736-4830 Comment: FX-12 (41-2600-8903-6) will be charged to the tank truck at elevated temperature (e.g., 95-105C) and will be maintained at this temperature to keep it molten and facilitate easy drainage. FX-12 essentially has no flashpoint (e.g., it is >>250F). Specific Use: FX-12 MATERIAL TYPE:........................ Type of Solid:... .................... Specific Gravity:.................... pH:................................... Tested for Flammable Solid:.......... SOLID WAXY 1.7 N/A No PROTECTIVE SERVICE REQUIREMENTS: Protect from Freezing:............... Protect from Heat:................... Requires Dry Ice:.................... No No No STORAGE REQUIREMENTS: Store:................................ Inside; Outside Water Reactive:...................... No Light Sensitive:..................... No CHEMICAL COMPATIBILITY WITH PACKAGING MATERIALS: Polyethylene:......................... No Plain Steel:....................... Yes Glass:................................ Yes Epon Lined Steel:.................... Yes Stainless Steel:....................... Yes REPORTABLE QUANTITY OF HAZARDOUS SUBSTANCE: Reportable:...........................No MARINE POLLUTANT HAZARDOUS SUBSTANCE: Pollutant:........................... No AScI Study ID# 5030-044-01 HAZARD DEFINITIONS: Abbreviations: N/D - Not Determined N/A - Not Applicable - 3M INTERNAL USE ONLY - 006181 Paqe 2 2 * 2 2 * * 64-3216-1 MATERIAL INFORMATION TRANSPORTATION DOCUMENT ____ AUTHOR SECTION (continued) Page 2 * DOT HAZARD CLASSES (SOLID) * MEETS NONE OF THE HAZARD DEFINITIONS HAZARDOUS MATERIAL: Ingredient's No Ingredients Selected... C.A.S. No. Percent TOXICOLOGY SECTION Status: Complete Name: LARA ANDERSEN HAZARD DEFINITIONS: * TOXICOLOGY * MEETS NONE OF THE HAZARD DEFINITIONS Date: 03/24/95 Phone: 612-737-0 TRANSPORTATION SECTION Status: Complete ID/Sample Package Description FCS A/C.FCC PSC Flash Pt 41-2600-8961-4 55 GAL/220 LITER METAL DRUM Classifier: RAYMOND DUZYNSKI 05/03/96 4 A53 A 41-2600-9391-3 55 GAL/220 LITER METAL DRUM Classifier: RAYMOND DUZYNSKI 07/22/97 4 A53 A 41-2600-8947-3 55 GAL/220 LITER METAL DRUM Classifier: RAYMOND DUZYNSKI 04/24/96 4 A53 A 41-2700-4220-7 55 GAL/220 LITER METAL DRUM Classifier: RAYMOND DUZYNSKI 03/29/95 4 A53 A 41-2600-8903-6 CARGO TANK TRUCK Classifier: RAYMOND DUZYNSKI 04/09/96 3 A53 A 41-2600-8929-1 55 GAL/220 LITER METAL DRUM Classifier: RAYMOND DUZYNSKI 09/18/95 4 A53 A AScI Study ID# 5030-044-01 Abbreviations: N/D - Not Determined N/A - Not Applicable - 3M INTERNAL USE ONLY - P^esi 006182 03/26/1993 3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY SAMPLE 1 LAB REQUEST NO. U1463 REQUESTOR NAME: RE PURDY DEPARTMENT: 0211 PROJECT NO: 06 DATE RECEIVED: 03/26/1993 DESC: ET-FOSE BP and VP Determinations CONTRACT LAB(S): ASCI EXP COMP DATE: 05/*T/199a DATE COMPLETED: ^ PROJECT LEAD: RE PURDY PHONE NO: 3M FAX NO: 612-778-6176 Bottle labeled: REX N.R. ETFOSE Alcohol 61691-16 See FM-3923 MSDS Tare - 97g J. Eberlin 53-6S-02 Do vapor pressure under GLP, determine boiling point as part of VP study. SAMPLE DATE CODE DESCRIPTION RESULT MDL or (95% C.I.) 1 03/12/98 ET-FOSE ~ ASCI BOIL-PT-E EQUILIBRIUM BOILING POINT * ASCI VAP-PRESS VAPOR PRESSURE * = CONTRACT LAB DATA 4 = UPDATED DATA Pag AScI Study ID# 5030-044-01 006183 DATE: 03/26/1998 3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY PARAMETER LAB REQUEST NO. U1463 CONTRACT LAB ASCI PROJECT NUMBER 06 SHIP DATE PROJECT LEAD: RE PURDY TELEPHONE : FAX : 612-778-6176 Computer Test Name Code Sample Numbers Sample Available Date Result Due Date BOIL-PT-E EQUILIBRIUM BOILING POINTI VAP-PRESS VAPOR PRESSURE 1 03/27/1993 05/27/1993 03/27/1998 05/27/1999 *r i AScI Study ID# 5030-044-01 006184 Chain of Custody Record 3M Environmental Laboratory Form35178-PWO 3MFacility Laub Addr* 3-3-01 CJ^Stai,j'jgCode b+TXulj el 3 S '& v s . \ n Av/e m a ; r/vv SampledBy(Print) Contractor A. SamplerSignature Sj /\ A ^ ~ a . ! p x ^ J ^ \ Item Sample # Description 1 U ) i; 3 2 u)H U H -1 3 lu Date Time 2 '.Ifp J !*p 07041 3MPro|ectTill T-?oSr 4. T-YS>fr SMFacllltyContact V f pur 3MTelephoneNumber ^ /v k i a ) ~>7X- S Z 7<7 Matrix Number Containers of each Preservatives s zo n OZz 8zN zo 5 8> 1 \ 1 1 4 5 6 .-Qool 7 8 P o 9M 10 11 12 13 Item # I e L Relinquished By/Affiliation ^ A ^ O & a d l A t/ Time Date /PM-y"' ' 3 J z W Shipped Via W/ V Total Containers of Each Item 3MRaquealer (?. 1P u r d l / 3MProteiLo^j (?.' 1 f 3MProjectNumber - Xv 'VT , * ' 3MDepartmentNumber OI) LabRequest^empiateNumber LLU f a Z . J u f W l . O Samples Split See Attachment C om m ents AScI Stud y ID# 5030-0414-01 Received By/Affiliation Time Date o-- * y? H* AScI Report #044-VP.R3M AScI Study ID #5030-044-01 APPENDIX C. Test Item Receipt and Usage Sponsor Study ID# U1463 Pag 006186 AScI Corporation/AScI-Dulutf Environmental Testing Oivisior SOP No.: Sl/B-Ol-R Reviewer: ^^ TEST SUBSTANCE RECEIPT AND SHIPPING FORM Instructions: F ile copy o f com pleted form (both Parts l & II) in th e stu d y file . PART I- Test Substance Receipt est Substance: -asoc. Study ID#: (Write for our study #): ' 7ate*Test Substance Received: "S,/? -/? 'and Number of Containers Received: jss Weight of Container and Test Substance: Dated Initials of Receiver I /l CeJ < et Weight of Test Substance (if provided): ' s is cy `ode of Transportation (check one): a^n->w* Aufine UPS Fed.Exp, escription of Label and Other Information That Came With Test Substance: U IMU3 Other 7r * .< est Substance Lot No., Batch No., etc.: is ( io 4 I ~~ clivity/Purity: Density: Solubility in Water: Color rm (check one): Liquid : Pellet Paste: Other "rage Location and Temperature: (Z~T ] -C ''h ' C-*nlotvO f-- rigmal MSDS and Mailing Receipts Filed in Notebook: Yes c/ltyh . Pjg_ofMSDS and Mailing Receipts Filed in the StudyJFile: Yes rh U 5oW V fifJ L . t Substance Containers are Re-labeled: Yes ffectiye: 1/1998 ID* 5030-044-01 AScl Study 00G187 P a g a 2 t : Pa9 Page 4 of 5 J .s I AScI Coiporation/AScI-Duiuth Environmental Testing Division SOP No.: SJJB-02-U Reviewer: .j 4 - f l TEST SUBSTANCE USAG E FORM I Instructions: A copy of this form must be filed in the Study File. AScI Study ID# 5030-044-01 j PART I- Test Substance j______________________ Test Substance: I'M t # 3 Sponsor *3 pate Test Substance Received: Type and Number of . ,, pmtainet<s) Opened: 1 a,4 !* ', ! 3 C ontainer: 3 /~l C ,, ? AScI Study ID#: S t ? 3 0 ~ O H ^ { - 0 \ Dated Initials of Person A / Opening Containers): *aA / \ ^ , Gross W ^tV ' ' V. : Net W m gl^pf Test Substance (tfivaHablft) ' Y 1 0 ( I f u sR -h c*X > OV 5 /z ? /rj/ v /rA r * Test Substance Lot N o., Batch N o., etc.: ART - Test Substance Usage Log 1 - Date a^ U j^ 3-Li l ? l ct 7 I 5. I. V- 5 8. Amount (/tl, m l, mg, g) of Test Substance Removed Total Removed to Date 'Z-3* -------- 1r.'n& v W ----i--q----.---z---i....X........ ^ L .M ?- Effective: 1/1998 f Pag* J z l o f 2 Purpose ^Lt/Wrve i/P</r P rC & '*'U v .p . k P* t'aga Staff's Dated Initials (a/o5t 3 f r y ' j v Mjf n/uh 'y < M ~ ^ tVj y f/d -v /rh r 006188 Page 4 of 5 * AScI Report #044-VP.R3M AScI Study ID #50304)44-01 APPENDIX D. Raw Data Sheets Sponsor Study ID# U1463 006189 0 AScI Corporation/AScI-DuIuth Environmental Testing Division Date: / A A mAnalyst:. VAPOR PRESSURE DATA SHEET __________ Study Test Item: -----*--x*>n--v-n----i--- I l l l p I l i P i l S T -3 M> Cs~LUS',J v _ I I U H iI to o I3TZo Us>S-Z>7 LOgPpa H < im t *V| IT v t 3 tA t l yzsT - Temp. CO 0 H l,'zys", r 157, Z , Sh>S' Temp. <K)b 3 d TifS" 3 | 4 v3 r 3 !^<U5" 3 f2 4 .? r 3~ zt> ^r I Temp. (K) <2/ O o '5'45<?i o o 3 tX l 17031 7/ O030ST3 O t &> 3o~$<-j in ' lo t Mk `M Of Ml T5-/7^ 5~/<? */<?-<> 7_ 3 7 ,0 *WWri*firsj cLxp ^iWvw4^iu^wt^ n% no >7 Notes: l'f'ZH r r H WU-3 T UL i H iS ooctZ j 4.7.3 tH H .lkU T j 4< 1|3^ 3iSrHo*33 b i'T ^ 7 ,7 - M5",o ~5>Y,0 31H*3szzo^r 371/t^f" 3 i? \ir 3i Ulst #1 0~L<ci( lOOlTZ i9 iOoy>h> (7. 0Ul)H2> 0> O Z ^ H * -ArivW kvui- ce.i^i-v. 4 ISKPcrr- C W fL v /iw ' r W L u j&Aa^ +"1^ U ditive TUX"9 (/ J g C o L r , ^orvyo<^-________ * - --- ------ W i r M n K ^ k r H-fc-<4 3 0 ^ 0 r~ 'TCXfc. - c Z ^ ^ J - Pp. = 133.3 (P ^ ) p w "0. O i 0 OS'lie - 0 lOOOSDM b Temp. (K) = 273.15 + Temp. (C) 1P M ----------------------------a t ^ Zu- J- 'u f<- ............. .... a 0 .0 0 ^ 1 ' 3'5~ zi-?---2-3*? ---------------- iiiUTL- 3 "AS- - * " >*^ 0 0 6 1 9 0 P * 9 .2 _ f-l? V-' I Date:. Analyst:. I X *mm Ut l 5"5" u n t/f 1? flwi^Ur DECT n n n v m ix ii a bi r AScI comot*on/ASci-Duiuth I l l l l f ' l A V A IL A O L t Environment*! Testing Division VAPOR PRESSURE DATA SHEET __________ __________ Study ID#: S TT$ Q - O H H ^ } Test Item: ( / _______ V ? " 5 s i,r T arsia /0-7-< i7,3 (1 0 ( ^ 4 ^ <X*4,4 Ca s h s ', 4 \ Log V . ^)i T3.5IS" H .leT ^/l 4,0^313 04340? 3 14 $-7334 tro iso + i 3 ,U ^ " 5 o3-2~ Temp. <C) m .o IW , 2. ftl.b 1n r ,- ? iy -0 'i l'~ 7 ,'Z -- Temp. (K)b W T -.l 5" H s ~ i 1iSH b0i3s~ q y-O tir 4 (< 9 '.`5S" U tils' /W 5135- 1 Temp. CK) tfz 0<?Z2-/ ^ OiOO-ZlTZ. <9, O~KS~f iOO 2/3-2, OiO(fl.l$~L. & tOOT-ils? tOO'lT-T'i O iO o^ H r r ~<9id)^4 >>00331 la -OiOOTJm- k -Q ftli iOOZZS' -0>oooZ^% Notes: ` Pp. = 133.3 (P,TM) b Temp. (K) = 273.15 + Temp. (C) 006191 Page v-w 3? P(mm) P(Pa) Log P(Pa) Toluene 47 6265.1 3.796928 64 8531.2 3.93101 77 10264.1 4.011321 100 13330 4.12483 124 16529.2 4.218252 12.6 1685 ^ . 3.2266 .^22:g4D<<293>^ 3.468 - ^ 2 5 ^ 4 3817.8 , 3.582 36.88 4915.6^ 3.692 150 19995 4.300921 128 17062.4 4.23204 110 14663 4.166223 77 10264.1 4.011321 52 6931.6 3.840833 ^27.7 35.8 1607.2 3.206 '"S8287f>, 3.4515 ` uPoU. i 3.567 f4771jD 3.679 U1463 42 5598.6 3.748079 55 7331.5 3.865193 67 8931.1 3.950905 81 10797.3 4.033315 96 12796.8 4.107101 0.00188 0.000479 0.00745 0.0114 0.2506 0.6392 0.9936 1.521 -0.6009 -0.1943 -0.0028 0.182 93 12396.9 4.093313 83 11063.9 4.043908 68 9064.4 3.957339 48 6398.4 3.806071 37 4932.1 3.693032 0.00127 0.00335 0.00528 0.00821 0.1692 0.4461 0.7043 1.094 -0.7717 -0.3506 -0.1522 0.0392 BEST COPY AVAILABLE ; T(C) T(K) 1/T(K) 35 41.2 45.5 51.2 56.5 308.15 314.35 318.65 324.35 329.65 0.003245 0.003181 0.003138 0.003083 0.003034 10 283.15 0.003532 20 293.15 0.003411 25 298.15 0.003354 30 303.15 0.003299 61.2 57.7 53.6 45 38 334.35 330.85 326.75 318.15 311.15 0.002991 0.03023 0.00306 0.003143 0,003214 10 283.15 0.003532 20 293.15 0.003411 25 298.15 0.003354 30 303.15 0.003299 r=0.999 a=0.00515 b=-0.000501 r=0.998 a=0.00512 b-- 0.000496 174.6 179 187.2 190.2 197 10 20 25 30 195.8 191.6 188.2 176.4 172.2 10 20 25 30 447.75 452.15 4(30.35 463.35 470.15 0.002233 0.002212 0.002172 0.002158 0.002127 283.15 293.15 298.15 303.15 0.003532 0.003411 0.003354 0.003299 468.95 464.75 461.35 449.55 445.35 0.002132 0.002152 0.002168 0.002224 0.002245 283.15 293.15 298.15 303.15 0.003532 0.003411 0.003354 0.003299 r=0.988 a=0.00335 b=-0.000298 r=0.994 a=0.00331 b=-0.000287 Page 22of^? AScI Study ID# 5030-044-01 006192