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AR226-3113 Huntingdon d 1-. /"a ^casr ff> ^B^- V^->g- " E; PHYSICO-CHEMICAL PROPERTIES Sponsor DuPont Specialty Chemicals Jackson Laboratory Chambers Works Deepwater NJ 08023 USA Research Laboratory Huntingdon Life Sciences Ltd. Eye Suffolk IP237PX ENGLAND Draft: 29 October 1998 Final: 2 February 1999 Paee 1 of 32 Company Sanitized. Does not coniafn TSCA ("SI CONTENTS Page COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS .............................. 3 QUALITY ASSURANCE STATEMENT...................................................................................... 4 RESPONSIBLE PERSONNEL....................................................................................................... 5 6 SUMMARY..................................................................................................................................... INTRODUCTION........................................................................................................................... 7 TEST SUBSTANCE........................................................................................................................ 8 PHYSICAL PROPERTIES Freezing temperature.................................................................................................................. 9 Boiling temperature.................................................................................................................... 11 Relative density.......................................................................................................................... 13 Vapour pressure.......................................................................................................................... 15 Surface tension........................................................................................................................... 21 Water solubility...............................................................................;.......................................... 23 Explosive properties................................................................................................................... 30 Company Sanitized. Does not contain TSCA CBI Huntingdon Life Sciences COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS Physico-Chemical Properties The study described in this report was conducted in compliance with the following Good Laboratory Practice standards and I consider the data generated to be valid. The UK Good Laboratory Practice Regulations 1997 (Statutory Instrument No 654). EC Council Directive 87/18/EEC of 18 December 1986 (Official Journal No L 15/29). OECD Principles of Good Laboratory Practice (as revised in 1997), ENV/MC/CHEM(98)17. A. L. Comb, B.Sc., Ph.D. Study Director Huntingdon Life Sciences Ltd. IJA^..^.. Date Company Sanitized. Does r.oi contain TSCA CBf Huntingdon Life Sciences QUALITY ASSURANCE STATEMENT Physico-Chemical Properties The following have been inspected or audited in relation to this study Study Phases Inspected Protocol Date of Inspection 18 August 1998 Date of Reporting 18 August 1998 Process Based Inspections Relative density Freezing temperature Water solubility Surface tension Boiling temperature Vapour pressure Explosive properties 25 June 1998 29 June 1998 23 July 1998 21 August 1998 22 September 1998 29 September 1998 2 October 1998 25 June 1998 29 June 1998 28 July 1998 21 August 1998 22 September 1998 29 September 1998 2 October 1998 ^ Report 4 December 1998 4 December 1998 / Protocol: An audit of the protocol for this study was conducted and reported to the Study Director and Company Management as indicated above. Process based inspections: At or about the time this study was in progress inspections and audits of routine and repetitive procedures employed on this type of study were carried out. These were conducted and reported to appropriate Company Management as indicated above. Report Audit: This report has been audited by the Quality Assurance Department. This audit was conducted and reported to the Study Director and Company Management as indicated above. The methods, procedures and observations were found to be accurately described and the reported results to reflect the raw data. H^<X^ H. Comb, B.Sc. Principal Auditor, Department of Quality Assurance, Huntingdon Life Sciences Ltd. ^.^^^^ n^i^ Date Company Sanitized. Does not cantain TSCA CBI :4: RESPONSIBLE PERSONNEL nunimgaon Life Sciences Physico-Chemical Properties ! The following staff member has reviewed this report. T. C. Cowlyh, EurChem., C.Chem., M.R.S.C. (Scientific Manager, Product Characterisation, Eye) The following staff were responsible for the conduct of the work and reporting of the results. K. Niemtus, L.P-S.C. (Senior Scientist, Product Characterisation) P. Woods, H.N.C. (Scientist, Product Characterisation) Company Saniilssd. Cess not contain TSCA CBi SUMMARY A study was performed to determine a series of physico-chemical properties ofU^I|HBH_ybe methods followed were amongst those described in the EEC Methods for tnedetenmnadon of physico-chemical properties (A1-A17), specified in the Annex to Directive 92/69/EEC and the OECD Guidelines for the Testing of Chemicals. The physico-chemical properties which have been determined in this study are detailed below, together with the result obtained for each test. EEC . method no. OECD method no. Test Result Al 102 Freezing temperature -1C A2 103 Boiling temperature 101.5C A3 109 Relative density (D^) 1.14 ! A4 104 Vapour pressure 2.34xlO"4Paat250C A5 115 Surface tension (1 g/1 solution) 21.5mN/mat20C A6 105 Water solubility 200 g/1 at 10C 248 g/1 at 20C >284 g/1 at 30C A14 Explosive properties Not explosive Company Samilzed. Dose r:"ic3"fasn TSCA RSSt 6- INTRODUCTION _^^^^^^__ This study was designed to determine a series of physico-chemical properties Information on physico-chemical properties is important in the assessment of the potential effects of a substance both at work and in the environment. The study was conducted in compliance with EEC Methods for the determination of physicochemical properties. Directive 92/69/EEC (OJ No. L383A, 29.12.92), Part A and the OECD Guidelines for the Testing of Chemicals. The physico-chemical properties investigated were: freezing temperature, boiling temperature, relative density, vapour pressure, surface tension, water solubility, and explosive properties. The protocol was approved by Huntingdon Life Sciences Management on 7 July 1998, by the Sponsor on 17 July 1998 and by the Study Director on 13 August 1998. The experimental phase of the study was undertaken between 24 August 1998 and 23 October 1998. Location of study : Huntingdon Life Sciences Ltd. Eye Suffolk IP237PX ENGLAND Primal)' data from the tests performed at Huntingdon Life Sciences, and a copy of the final report, are stored in the archives of Huntingdon Life Sciences. .,. c.np^u^o------^73"091 Identity: Chemical name: j Intended use: i S Appearance: i i ! Storage conditions: Lot number: Date received: TEST SUBSTANCE Pale yellow slurry Room temperature 3 2 years from date of receipt M 23 June 1998 is a suspension at room temperature and separates into its component phases. Hence on sampling the test substance for use in each individual test, the material was warmed to 35 - 40C in order to yield a homogenous solution. Con^yS.nl.^.Dc^c^TSCACB, K) FREEZING TEMPERATURE (EEC Method Al, OECD Method 102) PRELIMINARY TEST A trial determination was conducted to determine the approximate freezing point and the nature of crystallisation. On cooling the active ingredient was observed to precipitate out of solution, however, at approximately 4C crystals of ice were observed to form. Consequently the definitive freezing point test was performed. METHOD The freezing point was determined by cooling------------|Ba ^coitntrolled rate and determination of a sample temperature plateau at the crystallisingpom^^^^ DEFINITIONS AND UNITS The freezing temperature of a substance is defined as the temperature (C) at which the phase transition from liquid to solid state at normal atmospheric pressure takes place. APPARATUS Seta Freezing Point Apparatus, Stanhope Seta Ltd. Calibration: The apparatus is regularly calibrated by means of reference compounds of known freezing point. PROCEDURE The Dewar flask was then filled with a freezing mixture of calcium chloride/ice and the sample tube filled to a suitable depth. The sample was stirred continuously and the temperature was measured at 30 second intervals until a plateau of five constant readings were obtained. The test was performed in duplicate using a fresh test sample on each occasion. RESULTS A freezing point foi|ll|^Bl^Bjlpf-!C was determined (mean of-lC and-lC) as indicated by a plateau region in the cooling curve at this temperature (Figurel). CONCLUSION The freezing point of|^BHBBBfwas found to be -1C. . o . Company Sanitized. Does not contain TSCA CBi FIGURE 1 Freezing point curve foi J BOILING TEMPERATURE (EEC Method A2, OECD Method 103) METHOD The boiling temperature was determined by a modified Siwoloboff method. DEFINITION AND UNITS The normal boiling temperature is defined as the temperature (C) at which the vapour pressure of a liquid is the same as the Standard Pressure. APPARATUS Melting/boiling point apparatus: Model B-545, Buchi. Calibration: The apparatus is regularly calibrated by determination of boiling points of reference materials. PROCEDURE A boiling tilbe (3.2 mm diameter) was filled to a height of 5 - 10 mm with the sample and a boiling capillary was immersed, open end first. A trial, determination was made initially to estimate the boiling point of the substance. The boiling tube containing the sample and the boiling capillary was inserted into the sample holder and the temperature was raised at approximately 3C/min to about 10C below the anticipated boiling point. The temperature was then raised at approximately lC/min and the temperature noted at which a rapid continuous stream of bubbles was seen emerging from the inverted open end of the capillary. This temperature represents the boiling point. The determination was repeated until two measurements were obtained which agreed to within 1C of their mean (for boiling temperatures of up to 100C) and to within 2C (for boiling temperatures above 100C). RESULTS The results of duplicate boiling point determinations on|^^^^^^Hyvere as follows: Barometric pressure: 1014 mbar Observed value Boiling point (C) Pressure corrected value* Run I Run n 101.5 101.5 101.5 101.5 11- Company ,S.anstissAd. nDfo---- r'-"ti cl-o'n-'tain T-SCA CBE *Pressure correction Cb = 0.00009 (1013-Pb)(273 + Tb) where Pb and Tb is the ambient barometric pressure (mbar) is the observed boiling point (C) CONCLUSION of^----Rvaf The boiling temperature ,^^^^^^^^TM found to be 101.5C. 1? Company Sanitized. D"23 noi csr.t.a'n TSCA CBl ; RELATIVE DENSITY ! (EEC Method A3, OECD Method 109) METHOD ^^^"-"^ The relative density ojf^^^^^^--^--^j^^^^vl as determined relative to purified water using a pyknometer at 20C. DEFINITION AND UNITS The relative density (Dj) of solids and liquids is defined as the ratio of the mass of a volume of substance to be examined, determined at TC, and the mass of the same volume of water at 4C. APPARATUS Analytical balance: Pyknometer ModelRC 2TOP, Saitorius Instruments Glass, nominal 10 cm3 capacity at 20C, fitted with capillary stopper (BS 4699) REAGENTS Water: Purified by reverse osmosis and deionising; Elga Prima/Maxima PROCEDURE Sample pre-treatment: The test substance was heated to 36C in order to ensure that the material was homogenous. Test temperature 20C A clean, dry pyknometer was accurately weighed (wi) then filled to the limits of its capacity with pure water. It was then carefully stoppered without trapping air, dried and re-weighed (w2). The procedure was_then repeated with the same pyknometer using test substance. A Sub-sample of BHHHHB&vas transferred to the test pyknometer. The pyknometer was cooled to the test temperanu^irter which further material was added to ensure that the vessel was full to capacity. It was then carefully stoppered without trapping air, dried and re-weighed (w3). Two tests were performed concurrently using separate pyknometers. Parameters: mass of pyknometer empty (g) = Wi mass of pyknometer + water (g) = W2 mass of pyknometer + test substance (g) = W3 Company Sa^zed. Dc^ ^t contain TSCA CBi Calculations: mass of water to fill pyknometer (g) = w; - wi = Wi mass of test substance to fill pyknometer (g) = W3 - Wi = Wi relative density of test substance = Wz/Wi x p1 = Dj w where p is the density of water at the temperature of determination (0.998 g/ml) D^ RESULTS is the relative density of the test material at test temperature compared to water at4C Parameter Wl W2 W3 Wi Wz DJ xDj Determination 1 14.67987 24.26925 25.64580 9.58938 10.96593 1.14 1.14 Determination 2 . 14.71513 24.69189 26.13326 9.97676 11.41813 1.14 CONCLUSION The relative density (D2^0)x o 'as found to be 1.14. Company Sanifzed. Dcss ^ co.tafn TSCA CBl ,. VAPOUR PRESSURE l (EEC Method A4, OECD Method 104) METHOD The vapour pressure onl^^----fwas determined using a vapour pressure balance. DEFINITION AND UNITS The vapour pressure of a substance is defined as the saturation pressure above a solid or liquid substance. At the thennodynamic equilibrium, the vapour pressure of a pure substance is a function of temperature only. The SI unit of pressure is the Pascal (Pa). APPARATUS The,vapour-pressure- balaace was constructed"by me Department of "Facilities Management at Huntingdon Lite Sciences. A furnace, containing test substance, is separated from one pan of the microbalance (1 g head, C.I. Electronics) by means of a moveable shutter. This entire assembly is housed in a bell-jar which can be evacuated to a vacuum of<10"5 Ton- by means of a diffusion pump and a rotary pump connected in series. The pressure within the system is measured by Pirani and ion gauges and the temperature of the furnace by a Type K thermocouple. The signals from the microbalance and thermocouple are sent to a chart recorder. PROCEDURE Prior to the determination of the vapour pressure ofB------^fthe water in the test substance was removed by evaporation under vacuum at 60C.Thetestwassubsequently performed on the dried active ingredient. A check on the stability of the test material at elevated temperatures under nitrogen was performed by differential scanning calorimetry. No evidence of decomposition occurred below 60C. The microbalance was calibrated with a NAMAS calibrated 1 mg weight. It was found mat 1 ug produced a deflection of 2.78 x lO^V. A quantity of test substance (0.39 g) was added to the furnace. The apparatus was men assembled and evacuated to a pressure of less than 1 x 10"5 Ton- (1.3 x 10"3 Pa). After stabilisation at a given temperature, the shutter was opened to allow a stream of vapour to impact upon one balance pan. The temperature and pan deflection were recorded on a chart recorder. .The trace obtained enabled the calculation of mass difference . The furnace temperature was then raised in steps of 1 to 2C and further measurements taken. A series of three runs were performed between temperatures of 29 to 52 C. The same sample was used for each test, with the pressure being kept at less than IxlO"5 Torr (1.3 x lO^Pa) throughout. Company San.SszedA . nD----^s nnoa.' ccQ- "'ia;ri T3CA CB6 CALCULATIONS No condensation occurred so the vapour pressure is related to the observed mass difference by the relationship: Ame Vapour pressure == --A--- The vapour pressure-temperature relationship is as follows: slope logmVp =------+ intercept Equation 1 Equation 2 Consequently, a plot of log Vp versus 1/T(K) should be linear and by extrapolation the vapour pressure at 298.15K (25C) can be calculated. Glossary of terms used in equations 1 and 2 A = g = Am = T = Vp = surface area of the aperture (5.952 x 10~6 m2) acceleration due to gravity (9.813 m/s2) mass difference (kg) temperature (K) vapour pressure (Pa) RESULTS The fall results are detailed in Tables 1 to 3 and a graphical representation in Figure 2. Correlation: Slope: Intercept: LogVpat25C: vapour pressure at 25-C: Run 1 -0.99744 -4470.6 11.284 -3.7100 1.95xl0-4 Run 2 -0.99428 -4155.4 10.391 -3.5461 2.84 x 10-4 Run 3 -0.99692 -4568.8 11.671 -3.6524 2.23 x 10" CONCLUSION The vapour pressure of----BBBBis 2.34 x 10-4 Pa at 25C. . ,. . Company Sanitized. Does r^t contafn TSCA CBl TABLE 1 Test results from run 1 TemperatureE CO Mass difference (Hg) Vapour pressure (Pa) I/Temperature (1/K) Log vapour pressure 52.0 51.0 49.5 48.5 47.0 46.5 45.0 44.0 43.0 41.5 39.5 38.0 36.0 35.0 33.5 32.5 30.0 2.16 1.94 1.68 1.46 1.28 1.20 1.02 0.88 0.78 0.72 0.64 0.48 0.40 0.36 0.28 0.30 0.22 0.00356 0.00320 0.00277 0.00241 0.00211 0.00198 Q:OOi6S 0.00145 0.00129 0.00119 0.00106 0.00079 0.00066 0.00059 0.00046 0.00049 0.00036 0.00308 0.00308 0.00310 0.00311 0.00312 0.00313 0:00314 0.00315 0.00316 0.00318 0.00320 0.00321 0.00323 0.00325 0.00326 0.00327 0.00330 -2.4484 -2.4951 -2.5576 -2.6185 -2.6757 -2.7037 -2.7743 -2.8384 -2.8908 -2.9255 -2.9767 -3.1016 -3.1808 -3.2266 -3.3357 -3.3057 -3.4404 Company Sanitized. Does not cwlasn TABLE 2 Test results from run 2 Temperature (C) Mass difference ("g) Vapour pressure (Pa) I/Temperature (1/K) Log vapour pressure 29.0 29.0 30.5 32.0 33.5 35.0 36.5 38.0 39.5 41.0 42.0 44.5 45.5 47.0 49.0 51.0 0.26 0.28 0.34 0.38 0.44 0.48 0.54 0.60 0.70 0.78 0.96 1.16 1.34 1.56 2.06 2.60 0.00043 0.00046 0.00056 0.00063 0.00073 0.00079 0.00089 0.00099 0.00115 0.00129 0.00158 0.00191 0.00221 0.00257 0.00340 0.00429 0.00331 - 0.00331 0.00329 0.00328 0.00326 0.00325 0:00323 0.00321 0.00320 0.00318 0.00317 0.00315 0.00314 0.00312 0.00310 0.00308 -3.3679 -3.3357 -3.2514 -3.2031 -3.1394 -3.1016 -3.0505 -3.0047 -2.9378 -2.8908 -2.8006 -2.7184 -2.6558 -2.5897 -2.4690 -2.3679 Comaanv Sanitized. Does not contain TSCA CS3 TABLE 3 Test results from run 3 Temperature (Q Mass difference (ug) Vapour pressure (Pa) I/Temperature (1/K) Log vapour pressnre 29.0 29.0 30.5 32.5 34.0 35.5 37.0 39.0 41.0 43.0 45.0 46.0 47.5 49.5 51.0 0.20 0.24 0.26 0.34 0.38 0.44 0.52 0.66 0.74 0.96 1.14 1.34 1.72 1.98 2.54 -0.00033 0.00040 0.00043 0.00056 0.00063 0.00073 0.00086 0.00109 0.00122 0.00158 0.00188 0.00221 0.00284 0.00326 0.00419 0.00331 0.00331 0.00329 0.00327 0.00326 0.00324 0.00322 0.00320 0.00318 0.00316 0.00314 0.00313 0.00312 0.00310 0.00308 -3.4818 -3.4026 -3.3679 -3.2514 -3.2031 -3.1394 -3.0669 -2.9633 -2.9136 -2.8006 -2.7260 -2.6558 -2.5473 -2.4862 -2.3780 . 10 . Company Sanitized. Doss not conta'n TSCA < ..--f -2.3 I -2.5 t0 => 0 a n *(P' OT 0) :3, N' (0 a. C3 ^ 0) 3 %, 0 u ^ 1 0 .3 -2.7- ^ - 60 9 -2.9- w -3.1 - ,, ,, -3-3 - 0'00305 FIGURE 2 Graphical representation of runs 1 to 3 , A" A " AB A. ' A 2 4 " A, H A" A A . ~ A ^ A 0-003'0 0'003'5 ^~^.--------^ 11'/1T SURFACE TENSION (EEC Method A5, OECD Method 115) METHOD The surface tension of an aqueous solution containing 1 g/1 of the active ingredient was determined with a surface tension torsion balance using the OECD harmonised ring method. DEFINITION AND UNITS Surface tension (a) is defined as the free surface enthalpy per unit of surface area and is reported in N/m (SI units) or mN/m (SI subunit). APPARATUS Surface tension torsion balance: Ring dimensions: White Electrical Instrument Co., Malvem Link, Worcs. Ring radius 6.37 mm Wire radius 0.150 mm Calibration: The calibration factor, 0b, by which all instrument readings shall be multiplied, was determined in accordance with: (T o - 0b=-------- 0" g where CTo = (7g = value cited in the literature for the surface tension of water (mN/m) at the test temperature measured value of the surface tension of water (mN/m) at that test temperature Literature value for the surface tension of water at 20C (do) = 72.7 mN/m. Measured surface tension of water at 20C (cfg)= 72.0 mN/m. Therefore, the calibration factor, 0b = 1.010 TEST SOLUTION PREPARATION Test substance (0.4 g) was dissolved in purified water (100 ml) to produce a 1 g/1 solution, with respect to the active ingedient. A second solution was prepared in a similar manner. PROCEDURE The test vessel was half rilled with liquid, put on the tensiometer test platform, and raised so that the 2-3 ring was mm below the liquid surface. The platform was lowered to draw a lamella from the liquid surface. The maximum force which arose just before the lamella was torn off is the surface tension and was recorded. Measurements were made at intervals until a constant value (to within 0.5 mN/m) was recorded. The room temperature was monitored throughout the test. .Tt. eanifized. Does -n^-^-an-t1a1'0-nTSCACB^ Company^"-" RESULTS Test temperature: 20C Solution concentration: 1 g/1 with respect to the active ingredient Initial values for the surface tension were obtained as soon as possible after transfer of the aqueous solution to the measurement vessel. Time (minutes) . Surface tension (mN/m) Measured Calibration corrected A B A B 0 23.0 24.5 23.0 24.5 10 23.0 24.5 23.0 24.5 20 23.0 25.0 23.0 25.0 30 23.5 25.0 23.5 25.0 From the results there was no apparent rime dependence of surface tension after transfer to the measuring vessel. Overall mean calibration corrected surface tension = 24.0 mN/m Harkins-Jordan* corrected value = 21.5 mN/m CONCLUSION The surface tensioi^gf a 1 g/1 solution ofjUHBIHlwas found to be 21.5 mN/m. As the results less than 60 mN/m.^l--------^Rs considercdtobesurface active. *HARKINS, W.D. and JORDAN, H.R, J. Amer. Chem. Soc. 52,1751 (1930). . .. . Company Sanitized. ^ ^ obtain TSCA CB! WATER SOLUBILITY (EEC Method A6, OECD Method 105) DEFINITION AND UNITS The solubility in water is specified by the saturation mass concentration of the substance in water, and is a function of temperature. Solubility is specified in units of mass per volume of solution. The SI unit is kg/m3;g/1 may also be used. PROCEDURE HHHHB|s a suspension in water at room temperature, which forms a clear solution at elevated temperatures. Due to the apparent significant, temperature dependence of the solubility in water, the test was conducted at 10, 20 and 30C. The following modified procedure was employed at each temperature. |------------^20ml) was added to separate Wheaton vials, which were purged with nitrogen and ^Eue^^upucate samples were then stored in water baths at 10, 20 and 30C. After 4 days, the contents of each vial were centrifuged (2000 rpm for 5 minutes) and the supernatant solutions were separated and transferred to further Wheaton vials. These were then purged with nitrogen, sealed, returned to their respective water baths and stored for a farther 3 to 4 days. This equilibration and separation procedure was then repeated until no further solid material separated from solution. Sub-samples (2 ml) of each of the final supernatant solutions were diluted to volume (100 ml) with purified water, and these solutions were then diluted further (5 or 10 ml to 100 ml, depending on the anticipated level of active ingredient in the sample) with water. Aliquots (5 ml) of the resulting solutions were pipetted into separate 10 ml volumetric flasks, to which purified water (2 ml) and 0.2M aqueous sodium hydroxide (0.5 ml) were added before diluting to volume with acetonitrile. The final solutions were then diluted (5 to 10 ml) with mobile phase for analysis by ion chromatography. The pH of solutions were measured prior to and following the tests. 71 C.npanyS.nl.l"... 00^,31 con^TSCACBI ION CHROMATOGRAPHY CONDITIONS Instrument: Dionex GP40 Pump Dionex PED-2 Pulsed Electrochemical Detector Perkin-Elmer ISS 200 Autosampler Dionex ASRS-n Membrane Suppressor Column: PLRP-S (25 cm x 4.6 mm internal diameter) Column temperature: Ambient Mobile phase composition: ' ^ Regenerant solution Aqueous solution containing 2mM ammonium hydroxide and ImM sodium carbonate/acetonitrile (75:25 v/v) 50mN aqueous sulphuric acid Flow rate: & * '' fajection v o l u s-'m me:' lOml/min 100 ul Detector: Conductivity mode Retention time: Approximately 9 minutes The peak observed at 9 minutes corresponds to thp----^Bft------------|^--------fr^owm hich, mJBHfn information, supplied byjhe Sponsor, representsHHUm^HB^|pConsequently the levels of the water solubility test samples will be quantified relative to this component only. PREPARATION OF CALIBRATION A stock calibration solution of concentration 135.6 mg/1 of active ingredient was prepared by weighing test substance (108.4 mg) into a 100 ml volumetric flask and dissolving in and diluting to volume with purified water. A sub-sample (50 ml) of the stock solution was transferred to a 100 ml volumetric flask, to which 0.2M aqueous sodium hydroxide (5 ml) and purified water (20 ml) were added prior to diluting to volume with acetonitrile. Calibration solutions in the range 13.56 to 135.6 mg/1 were prepared by dilutions of the final solution with mobile phase. CALCULATIONS ofBHIUin The concentrations the analysed solutions (C^) were calculated from standards introduced before and after samples (bracketing standards) by the following equation: sample peak area x standard concentration (mg/1) CA(mg/l)= mean peak area of bracketing standards The concentrations of Zonyl FS-62 in the test solutions (Cg) were calculated from the following equation: CB (mg/1) = CA (mg/I) x dilution factor :24: Company Sanitized. Doss n=i cor.^n T3CA CS8 RESULTS The detector calibration was found to be linear over the range 0 to 135.6 mg/I of standard solutions in mobile phase with a regression coefficient of 0.9986 (Table 4, Figure 3). Table 5 presents a summary of the results of the tests at 10 and 20C and shows that the water solubility ofllBBHf5 200 ^ at looc and 248 g^ at 200C- Table 6 presents the primary data for these tests. Samples from the test at 30C were not analysed by the chromatography system, since on leaving aliquots of the test substance to stand for 4 days clear solutions were obtained. Consequently the solubility o^HBBIBlfat 30C will be reported as greater than 284 g/l - the concentration of the i active ingredient in the neat test substance. [ No peaks were observed in the chromatograms of the blank solutions indicating that the analytical I method was free from interference. CONCLUSION The water solubility of| than 284 g/1 at 30C. [wasfound to be 200 g/1 at 10C, 248 g/1 at 20C and greater ..,<;. Company Sanitized. Doss not contain TSCA CBi TABLE 4 Standard calibration fo; iy ion chromatography Standard concentration (mg/1) 13.56 27.11 54.22 81.33 108.4 135.6 Linear regression (including x = 0, y = 0) x = concentration y = peak area y = 598x + 1320 r= 0.9986 Peak area 8431 17756 35827 52060 65912 80589 9ft Company Sanitized. Doss not contain TSfA rof FIGURE 3 Standard calibration ^fl^^Him^ion chromatography 60 80 Concentration (mg/1) TABLES Measurements of water solubility at 10 and 20C Test temperature (C) Concentration (g/I) Mean concentration (g/I) pHof final saturated solution 10 200,200 200 0.6,0.7 20 248, 249 248 0.7,0.7 Initial pH of test substance = 0.7 (0 28: Company Sanitized. Doss not contain TSCA CB( TABLE 6 : Ion chromatographic analysis of samples from the water solubility test fo; Sample 54.22 mg/1 std 10C sample A 10C sample B 54.22 mg/1 std 54.22 mg/1 std 20C sample A 20C sample B 54.22 mg/1 std Peak area 34623 61064 61069 31719 34989 39772 39960 34623 CA (mg/1) 99.81 99.82 l 61.96 62.25 Dilution factor 2000 2000 4000 4000 EXPLOSIVE PROPERTIES (EEC Method A14) METHOD A Koenen test apparatus was used for determination of sensitivity to heat (flame), a fall hammer for determination of sensitivity to shock and a friction test apparatus for determination of sensitivity to fricdon. DEFINITION The material is said to possess explosive properties, if a positive result is recorded on any one or all of the tests, which is defined as follows: Thermal sensitivity (effect of flame): ^ An audible explosion, with the steel tube blown into three or more fragments. Mechanical sensitivity (shock): An audible explosion or if the material ignites. Mechanical sensitivity (friction): An audible explosion, crepitation or bursting into flame. :30: Company Sanitized. C-oas net contain TSCA CBf' THERMAL TEST APPARATUS Koenen apparatus made according to BAM 785-0004 with propane gas supply through calibrated flow meter. The four burners consume 3-4 litres/min of propane gas. PROCEDURE OF THERMAL TEST ^^^^^^Hvas poured into new drawn steel tubes 75 mm x 24 mm i.d.. The tubes were closed with an orifice plate (6 mm or 2 nnn orifice) and heated at the specified rate on the Koenen apparatus for 5 minutes or until an explosion occurred; Tests were conducted using 6 mm orifice plates followed by three using 2 mm orifice plates. THERMAL TEST RESULTS Duplicate tests were performed with the 6 mm orifice plate and on each occasion the liquid boiled and extinguished the burners. This was considered to occur due to the large content of water-in the test substance. j Tl (seconds) T2 (seconds) Observations 2 mm orifice Test 1 67 Test 2 63 Test 3 53 300 Orange flame which turned yellow, tube recovered intact 300 Orange flame which turned yellow, tube recovered intact 300 Orange flame which turned yellow, tube recovered intact Where Tl = time from start of test to flame from nozzle T2 = time from start of test to explosion, or end of test (300 seconds) 31- Company Sanitised. Dcss net csntain TSCA CBi MECHANICAL SENSITIVITY (SHOCK) TEST APPARATUS Impact hammer apparatus made according to BAM 782-0005 with 10 kg weight and specified sample dies. PROCEDURE OF SHOCK TEST 40 mm3 of|fl|HlBlBvas put in the die assembly and placed on the anvil in the drop hammer apparatus. A 10 kgweignt was released from a height of 0.4 m. The test was performed six times using a different sample and die assembly on each occasion. SHOCK TEST RESULTS 1 2 3 4 5 6 Replicate Result N N N N N N Where N = no evidence of explosion or decomposition. CONCLUSION ; not explosive. 32 Comaanv SanEti^d. Doss no? cori'aip TRCA CBl