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1、BRITISH STANDARD BS ISO 11357-5:1999 Plastics Differential scanning calorimetry (DSC) Part 5: Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of conversion ICS 83.080.01; 17.200.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIG
2、HT LAW Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11357-5:1999 This British Standard, having been prepared under the direction of the Sector Policy and Strategy Committee for Materials and Chemicals, was published under the autho
3、rity of the Standards Policy and Strategy Committee on 30 August 2001 BSI 30 August 2001 ISBN 0 580 38436 5 National foreword This British Standard reproduces verbatim ISO 11357-5:1999 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical C
4、ommittee PRI/21, Plastics test methods, which has the responsibility to: 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 b
5、e found in the BSI 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 Sta
6、ndards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for
7、change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 10, an inside back cover and a back cover.
8、The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 11357-5:1999(E) OSI
9、 9991 INTERNATIONAL STANDARD ISO 11357-5 First edition 1999-12-01 Plastics Differential scanning calorimetry (DSC) Part 5: Determination of characteristic reaction- curve temperatures and times, enthalpy of reaction and degree of conversion Plastiques Analyse calorimtrique diffrentielle (DSC) Partie
10、 5: Dtermination des tempratures et temps caractristiques de la courbe de raction, de lenthalpie de raction et du degr de transformation Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO?11357-5:1999(E) ii? ? ? ? Licensed Copy: sheffieldun
11、 sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11357-5:1999(E) ISO 9991 All irhgts seredevriii ContentsPage Foreword.iv 1Scope 1 2Normative references1 3Definitions 1 4Principle2 5Apparatus and materials.2 6Test specimens2 7Test conditions and specimen condition
12、ing 2 8Calibration2 9Procedure.2 9.1General2 9.2Temperature-scanning method2 9.3Isothermal method.3 10Expression of results 4 10.1Determination of characteristic temperatures and enthalpy of reaction (temperature-scanning method).4 10.2Determination of characteristic times and enthalpy of reaction (
13、isothermal method).4 10.3Determination of degree of conversion.5 11Precision.8 12Test report8 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11357-5:1999(E) iv ISO 9991 All irhgts seredevr Foreword ISO (the International Organization fo
14、r 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 interested in a subject for which a technical committee has been established has the
15、 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 Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Internati
16、onal Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. 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
17、 bodies casting a vote. Attention is drawn to the possibility that some of the elements of this part of ISO 11357 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 11357-5 was prepared by Technical Committ
18、ee ISO/TC 61,Plastics, Subcommittee SC 5,Physical-chemical properties. ISO 11357 consists of the following parts, under the general titlePlastics Differential scanning calorimetry (DSC): ?Part 1: General principles ?Part 2: Determination of glass transition temperature ?Part 3: Determination of temp
19、erature and enthalpy of melting and crystallization ?Part 4: Determination of specific heat capacity ?Part 5: Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of conversion ?Part 6: Determination of oxidation induction time ?Part 7: Determination
20、 of crystallization kinetics ?Part 8: Determination of amount of water absorbed Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARDISO 11357-5:1999(E) ISO 9991 All irhgts seredevr1 Plastics Differential scanning calorimetr
21、y (DSC) Part 5: Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of conversion 1Scope This part of ISO 11357 specifies a method for the determination of reaction temperatures and times, enthalpies of reaction and degrees of conversion using diffe
22、rential scanning calorimetry (DSC). The method applies to monomers, prepolymers and polymers in the solid or liquid state. The material may contain fillers and/or initiators in the solid or liquid state. WARNING Caution should be observed when working with materials which could give a runaway reacti
23、on or exhibit other dangerous behaviour. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISO 11357. For dated references, subsequent amendments to, or revisions of, these publications do not apply
24、. However, parties to agreements based on this part of ISO 11357 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and
25、 IEC maintain registers of currently valid International Standards. ISO 11357-1:1997,Plastics Differential scanning calorimetry (DSC) Part 1: General principles. ISO 11357-3:1999,Plastics Differential scanning calorimetry (DSC) Part 3: Determination of temperature and enthalpy of melting and crystal
26、lization. 3Definitions 3.1 polymerization the process of converting a monomer or a mixture of monomers into a polymer 3.2 crosslinking the process of multiple intermolecular covalent or ionic bonding between polymer chains 3.3 degree of conversion the quantity of unreacted product remaining during a
27、 reaction compared to the initial quantity of the product NOTEThe degree of conversion will depend on both time and temperature. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11357-5:1999(E) 2 ISO 9991 All irhgts seredevr 4Principle Se
28、e ISO 11357-1:1997, clause 4. The test method described indicates the various stages of the reaction by means of DSC curves. 5Apparatus and materials See ISO 11357-1:1997, clause 5. 6Test specimens See ISO 11357-1:1997, clause 6. If the specimen is a liquid resin or a mixture, use a mass of 5 mg to
29、20 mg. In the case of thermosets, increase the specimen mass in order to have 5 mg to 20 mg of resin in the specimen. 7Test conditions and specimen conditioning For polymers, see ISO 11357-1:1997, clause 7. For monomers and prepolymers in the liquid phase, particularly those with volatile components
30、, it may be necessary to carrying out conditioning and testing with the specimen enclosed in a gas-tight specimen pan which is resistant to high temperature and pressure. 8Calibration See ISO 11357-1:1997, clause 8. 9Procedure 9.1General The test can use one of two different methods, depending what
31、information is required: ?temperature-scanning method; ?isothermal method. 9.2Temperature-scanning method See ISO 11357-1:1997, subclause 9.4. Carry out a temperature scan, from ambient temperature to a temperature high enough to record the whole of the reaction peak, at a scan rate in the range 5 C
32、/min to 20 C/min. Use the same scan rate for all tests which are intended to be comparative. The final temperature shall be lower than the temperature corresponding to the onset of decomposition of the polymer. A preliminary test will be useful in defining the decomposition temperature. Licensed Cop
33、y: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11357-5:1999(E) ISO 9991 All irhgts seredevr3 9.3Isothermal method 9.3.1General The isothermal method can be carried out in two different ways once the specimen is inside the calorimeter cell: ?at cons
34、tant temperature; ?starting at ambient temperature and heating as quickly as possible to reach the constant measurement temperature. NOTEThe choice of procedure will depend on the model of calorimeter used for the test. The measurement temperature is selected on the basis of a trial run in the tempe
35、rature-scanning mode. The temperature has to be in the vicinity of the temperature at which the peak obtained in the scanning mode begins. 9.3.2Constant-temperature procedure a)place the reference pan in the calorimeter; b)set the instrument to the desired measurement temperature; c)let the calorime
36、ter stabilize at the selected temperature for 5 min; d)place the pan containing the specimen in the calorimeter; e)record the DSC curve; f)remove the pan containing the specimen and let it cool down to ambient temperature; g)place the pan containing the specimen back in the calorimeter; h)record the
37、 DSC curve again (the second curve will be subtracted from the first to allow for the calorimeter perturbation caused by the introduction of the pan). NOTEWhen using this procedure, it is difficult to ensure that the manual operation by which the pan is introduced into the calorimeter is carried out
38、 repeatably for the determination and the blank run. Subtraction of the two curves may therefore introduce a small error. 9.3.3Procedure starting at ambient temperature a)place both pans (reference and specimen) in the calorimeter at ambient temperature; b)increase the calorimeter temperature, at th
39、e highest possible rate, to the selected measurement temperature; c)record the DSC curve; d)allow the calorimeter to cool down to ambient temperature; e)repeat the process without removing the pans, and record the DSC curve again (the second curve will be subtracted from the first to allow for the c
40、alorimeter perturbation caused by the rapid heating process). 9.3.4Residual enthalpy At the end of an isothermal run (e.g. a polymerization reaction), allow the instrument to cool to ambient temperature with the specimen still inside it. Then heat up the specimen at the same rate as in a temperature
41、 scan in order to determine whether there is any residual enthalpy (i.e. whether any additional polymerization occurs). Add this enthalpy to the isothermal value to give the total enthalpy of reaction. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy,
42、 (c) BSI ISO 11357-5:1999(E) 4 ISO 9991 All irhgts seredevr 10 Expression of results 10.1 Determination of characteristic temperatures and enthalpy of reaction (temperature- scanning method) See also ISO 11357-3. Figure 1 DSC curve with exothermic peak (temperature-scanning method) The temperatures
43、shown in Figure 1 are: Tionset of reaction, corresponding to the point at which the DSC curve departs from the initial baseline; Teiextrapolated onset temperature, corresponding to the point at which the extrapolated baseline on the low- temperature side of the curve is intersected by the tangent to
44、 the curve at the point of inflection; Tpmaximum reaction rate, corresponding to the top of the peak; Tefextrapolated end temperature, corresponding to the point at which the extrapolated baseline on the high- temperature side of the curve is intersected by the tangent to the curve at the point of i
45、nflection; Tfend of reaction, corresponding to the return of the DSC curve to the final baseline. The enthalpy of reaction ?HR, in joules per gram, is obtained by integrating the area between the reaction peak and the baseline from Tito Tf. 10.2 Determination of characteristic times and enthalpy of
46、reaction (isothermal method) Each procedure (9.3.2 and 9.3.3) will require a different length of time for the reaction to begin. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 04:22:37 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11357-5:1999(E) ISO 9991 All irhgts seredevr5 Note the time
47、t0when the specimen reaches temperature equilibrium. Measure the following times from this point (see Figure 2): tionset of reaction, corresponding to the departure of the DSC curve from the initial baseline; teiextrapolated onset time, corresponding to the point at which the extrapolated baseline o
48、n the low- temperature side of the curve is intersected by the tangent to the curve at the point of inflection; tpmaximum reaction rate, corresponding to the top of the peak; tfend of reaction, corresponding to the return of the DSC curve to the baseline. Figure 2 DSC curve with exothermic peak (iso
49、thermal method) The enthalpy of reaction during the isothermal stage is obtained by integrating the area between the reaction peak and the baseline from tito tf. NOTEIt is necessary to select the temperature of the test in order to get the record of the peak as described on Figure 2. If needed, the temperature of the test may be lowered. If the reaction starts instantaneously, use Figure 3. When the reaction starts immediately, the curve will look like Figure 3. In such cases, tiand teicannot be measured. Time tiis take
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