Document jGJd3D0Vozw8yq0RZ7wQ64wQ

AR226-3113 Huntingdon / PHYSICO-CHEMICAL PROPERTIES Sponsor DuPont Specialty Chemicals Jackson Laboratory Chambers Works Deepwater NJ 08023 USA Research Laboratory Huntingdon Life Sciences Ltd. Eye Suffolk IP23 7PX ENGLAND Draft: 29 October 1998 Final: 2 February 1999 Paee 1 o f 32 Company Sanitized. Does not contain TSCA CONTENTS COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS QUALITY ASSURANCE STATEMENT..................... RESPONSIBLE PERSONNEL............................. SUMMARY..................................... INTRODUCTION................................... TEST SUBSTANCE.................................................. PHYSICAL PROPERTIES Freezing temperature................................ Boiling temperature.............................. Relative density............................. Vapour pressure............................ Surface tension........................ Water solubility................................. Explosive properties................................. Page 3 4 5 6 7 8 9 11 13 15 21 23 30 Company Sanitized. Boss not contain TSCA CBI Huntingdon Life Sciences COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS Physico-Chemical Properties The sUiciyciescnbecl 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 Laboratoiy 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. ........ Date Company Sanitized. Does not contain TSCA CBf T 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 Jg 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 Report 25 June 1998 29 June 1998 23 July 1998 21 August 1998 22 September 1998 29 September 1998 2 October 1998 4 December 1998 25 June 1998 29 June 1998 28 July 1998 21 August 1998 22 September 1998 29 September 1998 2 October 1998 4 December 1998 Protocol: An audit of the protocol for this study and Company Management as indicated above. was conducted and reported to the Study Director r `^ r ^At r 6 time this Stady was " Progress inspections and audits of routme and repetitive procedures employed on this type of study were carried out. These were conducted and reported to appropriate Company Management as indicated above. R epo.- Audit. This report has been audited by the Quality Assurance Department. Th *ud;*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. Comb, B.Sc. Principal Auditor, Department o f Quality Assurance, Huntingdon Life Sciences Ltd. Date Company Sanitized. Doe-s not contain TSC CBI :4 : RESPONSIBLE PERSONNEL nunungaon 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.R.S.C. (Senior Scientist, Product Characterisation) P. Woods, H.N.C. (Scientist, Product Characterisation) . Company Sanitised. D ess no! contain TSCA CBl :5 : SUMMARY A study was performed to determine a series of physico-chemical properties offlH methods followed were amongst those described in the EEC Methods for tn^eterm ination 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 OECD method no. 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 A5 115 Surface tension (1 g/1 solution) A6 105 Water solubility A14 Explosive properties 2.34 x 10'4Paat25C 21.5 mN/m at 20C 200 g/1 at 10C 248 g/1 at 20C >284 g/1 at 30C Not explosive Company Sanitized- O' cj not contain TSCA f, INTRODUCTION TUs study was designed to determine a series of physico-chemical properties ^orm au o n on physjco-chemica1properties is important in the assessment of the p t o S S S a substance both at work and in the environment. The study was conducted in compliance with EEC Methods for the determination of physico chemical properties, Directive 92/69/EEC (OJ No. L383A, 29.12.92), Part A and the S S 1 ChemiCalS- The Physic{ ^ m ic a l properties investigated were: rek " Ve VaP0Ur ^ water 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 nndertaten between 24 August 1998 and 23 October 1998. Location of study : Huntingdon Life Sciences Ltd. Eye Suffolk IP23 7PX ENGLAND Primary data from the tests performed at Huntingdon stored in the archives of Huntingdon Life Sciences. Life Sciences, and a copy of the final report, are 7 Company Sanitised. Doe s i contain TSCA CB& Identity: Chemical name: Intended use: Appearance: Storage conditions: Lot number: Expiry date: Purity: Date received: TEST SUBSTANCE Pale yellow slurry Room temperature 3 2 years from date of receipt m 23 June 1998 - ,, ,___ J s a susPension at room temperature and separates into its component phases Henrp nsamphngthe test substance for use in each individual test, the material was warmed to 35 - 40C in order to yield a homogenous solution. UL . Q . Company Sanitized. Dc -,g contain SC CBI FREEZING TEMPERATURE (EEC Method A l, 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 a sample temperature plateau at the crystallising puun. DEFINITIONS AND UNITS it a controlled rate and determination of 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 f o r ^ g B H g f i ^ f - l C was determined (mean of -1C and -1C) as indicated by a plateau region in the cooling curve at this temperature (Figurel). CONCLUSION The freezing point of as found to be -1C. Q Company SSanitized. Does not contain TSCA CBI FIGURE 1 Freezing point curve fo z> oo 313 < (/) NQQ. ao<up> oo 3* HO) > o Si 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 tube (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 o f 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 o Barometric pressure: 1014 mbar rere as follows: Run I Run II Observed value Boiling point (C) Pressure corrected value* 101.5 101.5 101.5 101.5 1 1 - Company Sanitizsd. Do contain TSCA CBB *Pressure correction Cb = 0.00009 (1013-Pb)(273 + Tb) where Pb is the ambient barometric pressure (mbar) Tb is the observed boiling point (C) CONCLUSION The boiling temperature 01 'as found to be 101.5C. 1? Company Sanitized. Doss not contain TSCA CBl RELATIVE DENSITY (EEC Method A3, OECD Method 109) METHOD The relative density o at 20C. d e f in it io n a n d u n its " delem"" ed relaTC " pm fied water using a pyknometer mb'T r '" *!6.de" Si'y !D ` )o f ^ "'J" 1* * defined as the ratio of the mass of a volume of substance to be exanuued, detenuiued at r C, and the mass of the same volume of water at 4C. apparatus Analyticalbalance: Pyknometer REAGENTS Model RC 21OP, Sartorius Instruments Glass, nominal 10 cm3capacity at 20C, fitted with capillary stopper (BS 4699) py Water: S a a b L " TM * Sm0SiS md * * " * Ei<* procedure Sample pre-treatment: The test substance was heated tn w r hom ogenous. order to ensure that the material was Test temperature 20C pure water!7 ifw a s then^rafidty^^^^ ^ KmitS f itS caPacity with SET7 ^ Z l Z p^ z sn7y^reterwascooIed was then carefully stoppered without trapping air, dried S d m - w ^ ^ * Two tests were performed concunently using separate pyknometers. Parameters: mass of pyknometer empty (g) = Wj mass of pyknometer + water (g) = w2 mass of pyknometer + test substance (g) = w3 Company Sanitized. Dees not contain TSCA CBl Calculations: " of waIer "> pyJcnometer (g) = w, - w, = w, mass of test substance [o fig pyfcnometer (g) = w3- wj = w : relative density of test substance - Wj/W, x p T= D T W4 where D T 4 density of water at the temperature of determination (0.998 g/ml) is the relative density of the test material at at4C test temperature compared to water resulto The relative density (D^) oi ras found to be 1.14. . 1 A . Company Sanitized. Deas not contain TSCA CBI VAPOUR PRESSURE (EEC Method A4, OECD Method 104) METHOD The vapour pressure o: DEfTNITTON AND UNITS was determined using a vapour pressure balance. The vapour pressure o f a substance is defined as the saturation pressure above a solid or liouid substance. At the thermodynamic equilibrium, the vapour pressure of a pure substance is a function of temperature only. The SI unit of pressure is the Pascal (Pa). APPARATUS ^ _ y a p o u r .4>msaire- balance was constructed by the Department o f Facilities Management at Huntingdon Life Sciences. A furnace, contammg test substance, is separated from one pan of the 3 u , 8 EuleCtr0nics) by means of a moveabIe Gutter- This entire assembly is housed m a bell-jar which can be evacuated to a vacuum of <10s Torr by means o f a diffusion p u L and a rotary pump connected m senes. The pressure within the system is measured by Pirani and ion S r * * * * * * * * ^ the furnace by a Type K thermocouple. The s i g n a ^ f e " microbalance and thermocouple are sent to a chart recorder. PROCEDURE theJVap0"r PreSS"re " t o in the test substance " der * ^ S l S S u b s e p u p u U y performed on Ihe 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 microbaimice was calibrated with a NAMAS calibrated 1 m g weight. It was found that 1 uu produced a deflection o f 2.78 x 10'3V. 11121 1 ^ A quantity o f test substance (0.39 g) was added to the furnace. The apparatus was then assembled and evacuated to a pressure of less than 1x10 s Torr (1.3 x 10`3Pa). 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 o f 1 to 2C and further measurements taken. A series offeree runs were performed between temperatures of 29 to 52 C. The same samn'e -- c useo ror each test, wife fee pressure being kept at less than 1x10 s Torr (1.3 x 10^ Pa) throughout. Company Sanitised. D :s not contain T3CA CBl CALCULATIONS No condensation occuired relationship: SO the vapour pressure is related to the observed mass differenee by the Vapour pressure = A Equation 1 The vapour pressure-temperature relationship is as follows: v ,, slope . ioSiovp ~ + intercept Equation 2 Consequently, a plot of log Vp versus 1/T(K) should be pressure at 298.15K (25C) can be calculated. linear and by extrapolation the vapour Glossary of terms used in equations 1 and 2 A^ g14111 ~ r= = surface area of the aperture (5.952 x 1O'6m2) acceleration due to gravity (9.813 m/s2) mass difference (kg) temperature (K) vapour pressure (Pa) results The full results are detailed in Tables 1 to 3 and a graphical representation in Figure 2. Correlation: Slope: Intercept: Log Vp at 25C: Vapour pressure at 25C: Run 1 Run 2 Run 3 -0.99744 -0.99428 -0.99692 -4470.6 -4155.4 -4568.8 11.284 10.391 11.671 -3.7100 -3.5461 -3.6524 1.95 x 10"* 2.84 x 10-* 2.23 x 10-* CONCLUSION The vapour pressure of] is 2.34 x 10-4Pa at 25C. . 1C . Company Sanitized. Does not contain TSCA CBl TABLEI Test resnlts from inn 1 | Temperature I Mass I Vapour CQ I difference I pressure' 0) I (Pa) 1/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 'm m 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. Dces nof contain TABLE 2 Test results from run 2 Temperature Mass (C) difference (Mg) Vapour pressure (Pa) 1/Temperature Log (1/K) 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 . 1 0 . Company Sanitized. Does not contain TSCA CSl TABLE 3 Test results from run 3 Temperature Mass (C) difference G*g) Vapour pressure (Pa) 1/Temperature Log (1/K) vapour pressure 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. D lot contain TSCA CBJ FIGURE 2 Graphical representation of runs 1 to 3 NoJ oo u3n3> CtoO N(aD aoo 3trOj> oua B) 3' -CoOI > o53 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: White Electrical Instrument Co., Malvern T.inlr Worcs.. Ring dimensions: 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: where 0 0b = a g ct0 = value cited in the literature for the surface tension of water (mN/m) at the test temperature CJg = measured value of the surface tension of water (mN/m) at that test temperature Literature value for the surface tension of water at 20C (0O) = 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 filled with liquid, put on the tensiometer test platform, and raised so that the ring was 2 - 3 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 tom 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. 01 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. Overall mean calibration corrected surface tension = 24.0 mN/m Harkins-Jordan* corrected value = 21.5 mN/m CONCLUSION The surface tension f a i g/1 solution of less than 60 mN/m I :considered to ras found to be 21.5 mN/n As the resultis surface active. *HARKINS, W.D. and JORDAN, H.F., J. Amer. Chem. Soc. 52,1751 (1930). . .'">'1 Company Sanitized. Doss not contain i SCA C3! WATER SOLUBILITY (EEC Method A6, OECD Method 105) DEFINITION AND UNITS The solubility in water is specified by the saturation mass concentration o f the substance in water and ,s a function o f temperature. Solubility is specified in units o f mass per volume o f solution Th SI unit is kg/m 3; g/1 may also be used. PROCEDURE -, -------Xs 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 temperature " ^ 2 ^ ^ f UowinS mdified proCedure was employed attach ........ , E20 was added t0 separate Wheaton vials, which were purged with nitrogen and seated. Duplicate samples were then stored in water baths at 10, 20 and 30C. After 4 Z s Ae 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 seriarati!/0 water baths 311(1 stored for a father 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) 2 0.2M aqueous sodium hydroxide (0.5 ml) were added before diluting to volume with acetonitrile S e 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. 93 Company Sanitised. Do 3 not contain TSCA CBS ION CHROMATOGRAPHY CONDITIONS Instrument: Column: Column temperature: Dionex GP40 Pump Dionex PED-2 Pulsed Electrochemical Detector Perkin-Elmer ISS 200 Autosampler Dionex ASRS-II Membrane Suppressor PLRP-S (25 cm x 4.6 mm internal diameter) Ambient Mobile phase composition: * g? Aqueous solution containing 2mM ammonium hydroxide and ImM sodium carbonate/acetonitrile (75:25 v/v) Regenerant solution 50mN aqueous sulphuric acid Flow rate: 10 ml/min Injection volume:' 100 pi Detector: Conductivity mode Retention time: Approximately 9 minutes The peak observed at 9 minutes corresponds to thel tv/hich, from SPnSOr' representSl H H H H H i H P c S q u e n t l y the c o m p o n e n tS T 11TM 1* * * Water S,UbiIity teSt SampIes wil1 be quantified relative to this PREPARATION OF CALIBRATION A stock calibration solution o f concentration 135.6 mg/1 of active ingredient was prepared by ghing test substance (108.4 mg) into a 100 ml volumetric flask and dissolving in and diluting to vo ume with purified water. A sub-sample (50 ml) of the stock solution was transferred to a 100 ml I hhT WhlCh '2M aqUeOUS S0dium hydroxide <5 mI) 311(1 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 ^ nc1f i ions Hie analysed solutions ( C J were calculated from standards introduced before and after samples (bracketing standards) by the following equation: C fmg/l) - sampIe Peak 31-63x standard concentration (mg/1) mean peak area of bracketing standards The concentrations of Zonyl FS-62 in the test solutions (CB) were calculated from the following equation: 6 CB(mg/l) - CA(mg/I) x dilution factor Company Sanitized. Does nzi contain TSCA C38 : 24 : RESULTS The detector calibration was found to be linear over the range 0 to 135.6 mg/1 of standard solutions in mobile phase with a regression coefficient of 0.9986 (Table 4, Figure 3). Table 5 presents a sui solubility of for these tests- y of the results of the tests at 10 and 20C and shows that the water is 200 g/1 at 10C and 248 g/1 at 20C. Table 6 presents the primary daia Samples from the test at 30C were not analysed by the chromatography system, since on leaving aliquots o fjjy e stsu b sta n c e to stand for 4 days clear solutions were obtained. Consequently the solubility f m ^ m ^ t 30C will be reported as greater than 284 g/1 - the concentration of the .1 active ingredient in the neat test substance. No peaks were observed in the chromatograms of the blank solutions indicating that the analytical method was free from interference. 3 CONCLUSION ] The water solubility than 284 g/1 at 30C. of^B M j^fllw as found to be 200 g/1 at 10C, 248 g/1 at 20C & and u greater 1 ! OS Company Sanitized. Does net contain TSC CBi TABLE 4 Standard calibration foi y ion chromatography Standard concentration (mg/1) ( 13.56 1 27.11 ] 54.22 . 81.33 j 108.4 135.6 I } Linear regression y = 598x+1320 i (including x = 0, y = 0) r = 0.9986 j x = concentration 1 y = peak area l I Peak area 8431 17756 35827 52060 65912 80589 # Company Sanitized. Boos not contain TSC m s FIGURE 3 Standard calibration fo: [by ion chromatography Peak Height M TABLE 5 Measurements of water solubility at 10 and 20C Test temperature Concentration (C) 1 (g/I) 10 200,200 | 20 248, 249 I Initial pH of test substance = 0.7 Mean concentration (g/I) 200 248 pH of final saturated solution 0.6,0.7 0.7,0.7 ii : 28 : Company Sanitized. Doss not contain TSCA CBf giSvJ v i s i U!C)UW fui! a s u y f j o u i i u c a a u e M iw rj TABLE 6 Ion chrom atographic analysis of samples from the w ater 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 i 61 96 62 25 Dilution factor 2000 2000 " 4000 4000 CB(g/1) 199.6 199.6 247.8 249.0 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 friction. 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. Company Sanitized. Coos net contain TSCA CBI1 : 30 : 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 /as poured into new drawn steel tubes 75 mm x 24 mm i.d.. The tubes were closed with an orificeplate (6 mm or 2 mm 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. T1 (seconds) T2 (seconds) Observations 2 mm orifice Test 1 Test 2 Test 3 67 63 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 T1 = time from start of test to flame from nozzle T2 = time from start of test to explosion, or end of test (300 seconds) 3 1 - Company Sanitized. Dc-ss net certain i SCA CB MECHANICAL SENSITIVITY (SHOCK) TEST APPARATUS M pact hammer apparatus made according to BAM 782-0005 with 10 kg weight and specified sample PROCEDURE OF SHOCK TEST M D ^tL0fW ^ f VaS PUt,iD ^ die assembly and placed on the anvil in the drop hammer apparatus. A 10 kg weight was released from a height of 0.4 m The test was nerfhmviH usmg a different sample and die assembly on each occasion. ' P a n n e d six times SHOCK TST RESULTS Replicate 1 2 3 4 5 6 Result N N N N N N Where N - no evidence of explosion or decomposition. CONCLUSION ...... not explosive. : 32 : Comasnv Sanitized. Does no? contain TSCA CBl