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1、International Standard 584 0 d!l!l ,NTERNAT,ONAL ORGANIZATION FOR STANDARDlZATlON*MEYHAPDHAR DPTAHHSAWIR fl0 CTAHAAPT113AUHWORGANlSATlON INTERNATIONALE DE NORMALISATION Plastics - Unsaturated polyester resins - Determination of reactivity at 80 OC (conventional method) Plastiques - Rtkines de polyes
2、ters non saturks - D bj speed of heating the test portion placed in a temperature controlled bath. For example, the replacement of water in the bath by another fluid with a lower heat capacity (glycol, oil, etc.) leads to slower heating; c) type of temperature measuring element placed in the test po
3、rtion and its ability to respond to rapid changes in temperature. Thermometers with a slow response and thermocouples with large junctions between the resistance leads are unsatisfactory; d) accurate centring of the thermocouple in the test portion, both in height and in line with the axis. These co
4、nditions which are mandatory are specified in the text of this International Standard. 1 Scope and field of application This International Standard specifies a method for the deter- mination of the reactivity of unsaturated polyester resins as characterized by the maximum temperature reached by a so
5、lu- tion of unsaturated polyester resin and catalyst when heated in a water-bath at 80 OC, by the time taken for the temperature of the mixture to rise from 65 “C to this maximum temperature, and also, if the maximum temperature exceeds 90 “C, by the time taken for the temperature to rise from 65 to
6、 90 “C. These characteristics give an indication of the processing behaviour of unsaturated polyester resins and can be used to compare resins of similar type. As the test results depend very much on the conditions under which the test is carried out, these conditions are described in detail. NOTES
7、1 If the method is used to test commercial benzoyl peroxide catalyst, the results should be compared with those obtained for the same resin using pure benzoyl peroxide. 2 By agreement between the interested parties, certain test con- ditions can be modified : such as the test temperature (temperatur
8、e of the thermostatically controlled bath) and the quantity and type of catalyst system (mixtures of catalysts, combinations of catalysts and accelerators). 2 Principle Placing of a mixture of 100 parts of resin with 1 part of catalyst in a test-tube of defined size. Heating of the test-tube and its
9、 contents in a water-bath at 80 OC for the duration of the reaction, and noting (or recording) the rise in temperature with time. 3 Reagent During the analysis, use only reagents of recognized analytical grade. Benzoyl peroxide, catalyst. WARNING - Attention is drawn to the dangers involved in handl
10、ing pure benzoyl peroxide. A mixture of 50 % (m/m) of benzoyl peroxide catalyst in dibutyl phthalate having an active oxygen content between 3,25 and 333 % (m/m), as measured by known analytical methods. 1 Copyright International Organization for Standardization Provided by IHS under license with IS
11、O Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/28/2007 07:29:44 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 664-1962 (E) 4 Apparatus 4.1 Water-bath.11 maintained at 60 f 0,5 “C and provided with a thermostat and a circulation pump or stirrer. 4.
12、2 Test-tube, of borosilicate glass or any other glass giving the same results, of internal diameter 18 f 1 mm, length 210 f 5 mm and wall thickness 1 f 0.2 mm. 4.3 Iron-constantan thermocouple, consisting of wires of 1 f 0,05 mm thickness, with a welded junction of 2 mm diameter maximum and a meter
13、for measuring temperatures up to 250 OC, graduated in divisions of 2 OC. NOTE - It is desirable to use screened thermocouples that can be positioned centrally. 4.4 If available a recorder, permitting the readings of temperature on the graph paper to the nearest 1 OC and the time to the nearest 15 s.
14、 4.5 Device, for locating the thermocouple centrally in the test-tube (see the figure). 4.6 Balance, accurate to 0,Ol g. 4.7 Stop watch. 6 Procedure 5.1 Weigh 2 f 0,Ol g of the benzoyi peroxide-dibutyl phthalate mixture (clause 3) into a glass beaker of capacity 256 ml and add 100 f 1 g of resin at
15、a temperature between 15 and 30 OC. Continue stirring for 2 to 3 min. 5.2 Then immediately pour part of the mixture into the test- tube (4.2) to a height of 7 to 8 cm. Introduce the thermocouple into the mixture in a position on the axis of the tube and equidistant from the bottom and the surface of
16、 the mixture (see the figure). Then place the tube in the water-bath at 60 f 0,5 OC, so that the surface of the resin is well beneath the level of the surface of the water. 5.3 If a recorder is used, start and allow the recorder to run during the complete reaction. Alternatively, note the maximum te
17、mperature reached, as well as the time taken for the temperature of the mixture, determined by the thermocouple, to rise from 65 OC to the maximum temperature, and in the case where this temperature is greater than 90 OC, the time to rise from 65 to 90 OC. 5.4 Repeat the test, beginning at 5.1, unti
18、l two consecutive determinations do not differ by more than 5 OC in temperature and 10 % in time. 6 Test report The test report shall include the following information : a) a reference to this International Standard; b) a complete identification of the resin tested; c) the type of thermocouple used
19、and whether screened or unscreened; d) the individual values of the maximum temperature reached in the two tests and the average value; e) the individual values of the time taken for the tempera- ture to rise from 65 OC to the maximum temperature in the two tests and the average value; f) if the max
20、imum temperature is above 90 OC, the in- dividual values of the time taken for the temperature to rise from 65 to 90 OC in the two tests and the average value; g) if a recorder is used, the graphs giving the temperature plotted against time. h) any deviations from the standard test conditions speci-
21、 fied in this International Standard, for example type and temperature of the heating medium, catalyst system used, thermocouple system used, etc. (see note 2 to clause 1). 1) The water in the bath may be replaced by another fluid agreed upon by the interested parties. 2 Copyright International Orga
22、nization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/28/2007 07:29:44 MDTNo reproduction or networking permitted without license from IHS -,-,- 7 - A L- ISQ 584-1982 (E) Dimensions in millimetres int. 18 f I Section A-A
23、 Opening for thermocouple A .l Figure - Example of device for locating the thermocouple centrally in the test-tube 1) The levels for the test mixture and the thermocouple shall be in accordance with the instructions in 5.2. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/28/2007 07:29:44 MDTNo reproduction or networking permitted without license from IHS -,-,-