1、BRITISH STANDARD BS ISO 14848:1998 Plastics Unsaturated-polyester resins Determination of reactivity at 130C ICS 83.080.10BS ISO14848:1998 This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standar
2、ds Board and comes into effect on 15 August 1998 BSI 04-1999 ISBN 0 580 30005 6 National foreword This British Standard reproduces verbatim ISO 14848:1998 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinfor
3、ced thermosetting plastics and prepregs, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international
4、and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the B
5、SI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are respo
6、nsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the ISO title page, page ii, pages 1 to 5 and a back cover. This standard
7、 has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS ISO14848:1998 BSI 04-1999 i Contents Page National foreword Inside front cover Forewo
8、rd ii Introduction 1 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus 2 6 Procedure 2 7 Expression of results 2 8 Precision 5 9 Test report 5 Figure 1 Thermocouple 3 Figure 2 Example of centering device 3 Figure 3 Typical temperature-time curve 4 Table 1 Precision data 4ii b
9、lankBS ISO14848:1998 ii BSI 04-1999 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body i
10、nterested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechn
11、ical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75% of the member bodies casting a vote.
12、International Standard ISO14848 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. Descriptors: Plastics, moulding materials, thermosetting resins, polyester resins, tests, determination, chemical properties, polymerization.BS ISO14848:1998 BSI 04-1
13、999 1 Introduction The processing of unsaturated-polyester resins, as well as formulated products such as bulk moulding compound (BMC) and sheet moulding compound (SMC), depends on their reactivity, i.e.on their ability to polymerize under the action of a catalyst and under the effect of heat. The r
14、eactivity of such resins may be determined by different methods, such as this International Standard which makes use of the variation in temperature as a function of time. The use of the standardized conditions given in this International Standard make it possible to carry out comparisons between si
15、milar types of unsaturated-polyester resin. 1 Scope This International Standard specifies a method of measuring the time required for the temperature of a solution of unsaturated-polyester resin and a catalyst, heated in a thermostatically controlled bath at 130C, to rise from 80C to 140C, from 80C
16、to the maximum temperature reached; the maximum temperature reached; the speed of the reaction, determined by drawing a tangent at the point of inflection of the temperature/time curve. It applies in particular to unsaturated-polyester resins processed at a temperature higher than 100C. NOTEThe resu
17、lts are closely linked to the conditions. The aim of this International Standard is to define them as exactly as possible, particularly the following: a) The quantity and form of the resin sample being examined (test tube diameter, height of resin in the tube). b) The rate at which the sample is hea
18、ted in the bath. For example, the use of a liquid having a relatively low heat capacity (ethylene glycol, silicone oil) leads to slower heating. c) The type of thermometer used. Thermometers having a response slower than that of a thermocouple, and resistance probes having too large a heat-sensitive
19、 element, are unsuitable. d) The position of the heat-sensitive element in the resin, both heightwise and relative to the axis of the test tube containing the resin. e) The nature of the catalyst. 2 Normative references The following standards contain provisions which, through reference in this text
20、, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editi
21、ons of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 3219:1993, Plastics Polymers/resins in the liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate. ISO
22、 15038: 1) , Plastics Organic perester crosslinking agents for unsturated-polyester thermosetting materials Determination of active-oxygen content. EN 60584-2:1993, Thermocouples Part 2: Tolerances. 3 Principle Unsaturated-polyester resins are crosslinked by heating with a perester catalyst. A resin
23、/catalyst mixture (in the ratio 100g to 1g) is placed in a test tube kept in a thermostatically controlled bath at 130C and the rise in temperature recorded as a function of time for the entire duration of the reaction; the tangent drawn at the point of greatest slope of the recorded curve, thus giv
24、ing an indication of the speed of the reaction. 4 Reagents 4.1 Catalyst: tert-butyl perbenzoate, having a purity of over 96% (i.e.an active-oxygen content greater than 7,9% determined in accordance with ISO15038). NOTEIt is advisable not to store tert-butyl perbenzoate (m.pt. 8C) at a temperature lo
25、wer than 10C (to avoid crystallization); higher than 30C (to avoid deterioration in the quality of the product). 1) To be published.BS ISO14848:1998 2 BSI 04-1999 5 Apparatus 5.1 Thermostatically controlled bath, with a capacity between4litres and5litres, containing silicone oil having a viscosity b
26、etween100mPas and 500 mPas at 23C determined in accordance with ISO3219, maintained at a temperature of 130C 1C and equipped with a thermostat, a circulation pump and a stirrer located at a distance of10cm from the test tube (5.2). The stirring action shall be sufficient to maintain a uniform temper
27、ature in the bath. 5.2 Borosilicate-glass test tube, having an internal diameter of18mm, a length of at least180mm and a wall thickness of1,2mm 0,2mm, for use with the centering device (5.5). 5.3 Type J iron-constantan thermocouple, with a1,5mm wide protective sheath,0,25mm 0,01mm thick wires and a
28、welded junction of maximum diameter0,54mm (reaction time 28/100 s), inserted in a1,6mm diameter metal guide fitted with a stop17cm from the end, and connected to a temperature recorder equipped with an automatic cold-source compensator (seeFigure 1). 5.4 Chart recorder, allowing the temperature to b
29、e read off the trace to within1C and having a chart speed of60mm/min, or a computer-based data-acquisition system. 5.5 Centering device, with a diameter of (18)mm, made of PTFE for instance, for centering the thermocouple in the middle of the test tube (seeFigure 2). 5.6 Balance, accurate to 0,01 g.
30、 5.7 Stopwatch. 5.8 Beaker, capacity 150 ml. 5.9 Watchglass. 5.10 Glass rod. 6 Procedure 6.1 Weigh the glass beaker (5.8) and then weigh into it100g 0,1g of resin at a temperature of23C 2 C. 6.2 Add a quantity of catalyst (4.1) such that the ratio of catalyst to resin is1:100 by mass. Stir with the
31、glass rod (5.10) to homogenize. 6.3 Cover the beaker with a watchglass (5.9) and allow to stand for45min5min. Fill the test tube (5.2) to a height of7,5cm 0,2cm. Fit the centering device (5.5) in place and insert the thermocouple (5.3). Immerse the test tube in the bath (5.1), maintained at130C, ens
32、uring that the surface of the resin is2cm below the level of the silicone oil in the bath. To ensure the reproducibility of the determination, the centering device shall be checked every six months to confirm that its dimensions are still within the specified tolerances. If they are not, the device
33、shall be replaced. 6.4 Record the temperature as a function of time throughout the duration of the reaction (seeFigure 3). 6.5 Remove the thermocouple-guide/thermocouple assembly immediately after the determination, when the recorder has stopped (seeFigure 3), to avoid resin adhering to the thermoco
34、uple. 6.6 Carry out at least two determinations. 7 Expression of results The reactivity of the resin is characterized by the following parameters: the maximum temperature T, in degrees Celsius, reached during the reaction; the time t 1 , in seconds, taken for the temperature to rise from 80C to 140C
35、; the time t 2 , in seconds, taken for the temperature to rise from 80C to the maximum temperature. In addition, the gradient (tan ) of the tangent drawn at the point of inflection of the curve provides an indication of the rate of the reaction, in degrees Celsius per second (seeFigure 3). Measure t
36、he values of these parameters for each determination and calculate the arithmetic mean in each case. 0004 , BS ISO14848:1998 BSI 04-1999 3 Figure 1 Thermocouple Figure 2 Example of centering deviceBS ISO14848:1998 4 BSI 04-1999 Table 1 Precision data Figure 3 Typical temperature-time curve t 1 60 s
37、60 s t 1 120 s T t 1 t 2 T t 1 t 2 r 2% 14% 12% 2% 8% 7,5% R 3% 16% 19% 4% 11% 15% r = repeatability R = reproducibility Confidence level 95%BS ISO14848:1998 BSI 04-1999 5 8 Precision Following a round robin organized in France in1996, the precision of this method has been calculated to be as shown
38、inTable 1. 9 Test report The test report shall contain the following information: a) a reference to this International Standard; b) all details necessary to identify the sample tested; c) the temperature at which the determination was carried out, if different from 130C; d) the type of thermocouple
39、used; e) the results, expressed in accordance with clause7; f) details of any operation not specified in this International Standard, and details of any incident which may have affected the results; g) the date and location of the test.BS ISO 14848:1998 BSI 389 Chiswick High Road London W4 4AL BSIBr
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