EN ISO 11357-5-2014 en Plastics - Differential scanning calorimetry (DSC) - Part 5 Determination of characteristic reaction-curve temperatures and times enthalpy of reaction and de.pdf

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1、BSI Standards PublicationBS EN ISO 11357-5:2014BS ISO 11357-5:2013Plastics Differential scanningcalorimetry (DSC)Part 5: Determination of characteristicreaction-curve temperatures and times,enthalpy of reaction and degree ofconversionBS EN ISO 11357-5:2014 BRITISH STANDARDNational forewordThis Briti

2、sh Standard is the UK implementation of EN ISO 11357-5:2014. It is identical to ISO 11357-5:2013. It supersedes BS ISO 11357-5:2013 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this

3、committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014ISBN 978 0 580 83435 6ICS 8

4、3.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2013.Amendments/corrigenda issued since publicationDate Text affected30 April 2014 This corrigen

5、dum renumbers BS ISO 11357-5:2013 as BS EN ISO 11357-5:2014EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-5 March 2014 ICS 83.080.01 English Version Plastics - Differential scanning calorimetry (DSC) - Part 5: Determination of characteristic reaction-curve temperatures and times, ent

6、halpy of reaction and degree of conversion (ISO 11357-5:2013) Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 5: Dtermination des tempratures et temps caractristiques de la courbe de raction, de lenthalpie de raction et du degr de transformation (ISO 11357-5:2013)Kunststoffe - Dynami

7、sche Differenz-Thermoanalyse (DSC) -Teil 5: Bestimmung von charakteristischen Reaktionstemperaturen und -zeiten, Reaktionsenthalpie und Umsatz (ISO 11357-5:2013) This European Standard was approved by CEN on 6 March 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations whic

8、h stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This Eur

9、opean Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members a

10、re the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, R

11、omania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and

12、 by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11357-5:2014 EBS EN ISO 11357-5:2014EN ISO 11357-5:2014 (E)EN ISO 11357-5:2014 (E) 3 Foreword The text of ISO 11357-5:2013 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for St

13、andardization (ISO) and has been taken over as EN ISO 11357-5:2014 by Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the lates

14、t by September 2014, and conflicting national standards shall be withdrawn at the latest by September 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or al

15、l such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of

16、Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 11357-5:2013 has been approved

17、 by CEN as EN ISO 11357-5:2014 without any modification. BS EN ISO 11357-5:2014ISO 11357-5:2013(E)BS ISO 11357-5:2013ISO 11357-5:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Apparatus and materials 26 Tes

18、t specimens 27 Test conditions and specimen conditioning 28 Calibration 29 Procedure. 29.1 General . 29.2 Temperature-scanning method 29.3 Isothermal method 210 Determination of results 410.1 Determination of characteristic temperatures and enthalpy of reaction (temperature-scanning method) . 410.2

19、Determination of characteristic times and enthalpy of reaction (isothermal method). 410.3 Determination of degree of conversion . 611 Precision . 912 Test report . 9Bibliography .10BS ISO 11357-5:2013ISO 11357-5:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative r

20、eferences 3 Terms and definitions .4 Principle 5 Apparatus and materials 26 Test specimens7 est conditions and specimen conditioning 8 Calibration 9 Procedure.9.1 General . 29.2 Temperature-scanning method 29.3 Isothermal method 210 Determination of results 410.1 Determination of characteristic temp

21、eratures and enthalpy of reaction (temperature-scanning method) . 410.2 Determination of characteristic times and enthalpy of reaction (isothermal method). 410.3 Determination of degree of conversion . 611 Precision . 912 Test report .Bibliography .10This page deliberately left blankBS ISO 11357-5:2

22、013INTERNATIONAL STANDARD ISO 11357-5:2013(E)Plastics Differential scanning calorimetry (DSC) Part 5: Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of conversionWARNING Caution should be observed when working with materials which could give a

23、runaway reaction or exhibit other dangerous behaviour.1 ScopeThis part of ISO 11357 specifies a method for the determination of reaction temperatures and times, enthalpies of reaction, and degrees of conversion using differential scanning calorimetry (DSC).The method applies to monomers, prepolymers

24、, and polymers in the solid or liquid state. The material can contain fillers and/or initiators in the solid or liquid state.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references

25、, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principles3 Terms and definitionsFor the purposes of this document, the terms and d

26、efinitions given in ISO 11357-1 and the following apply.3.1polymerizationprocess of converting a monomer or a mixture of monomers into a polymer3.2crosslinkingprocess of multiple intermolecular covalent or ionic bonding between polymer chains3.3degree of conversionquantity of reacted product obtaine

27、d during a reaction compared with the maximum possible quantity of the productNote 1 to entry: The degree of conversion will depend on both time and temperature.4 PrincipleThe principle is specified in ISO 11357-1.The test method described indicates the various stages of the reaction by means of DSC

28、 curves. ISO 2013 All rights reserved 1BS ISO 11357-5:2013INTERNATIONAL STANDARD ISO 11357-5:2013(E)Plastics Differential scanning calorimetry (DSC) Part 5: Determination of characteristic reaction-curve temperatures and times, enthalpy of reaction and degree of conversionWARNING Caution should be o

29、bserved when working with materials which could give a runaway reaction or exhibit other dangerous behaviour.1 ScopeThis part of ISO 11357 specifies a method for the determination of reaction temperatures and times, enthalpies of reaction, and degrees of conversion using differential scanning calori

30、metry (DSC).The method applies to monomers, prepolymers, and polymers in the solid or liquid state. The material can contain fillers and/or initiators in the solid or liquid state.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are

31、indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principles3 Terms and defini

32、tionsFor the purposes of this document, the terms and definitions given in ISO 11357-1 and the following apply.3.1polymerizationprocess of converting a monomer or a mixture of monomers into a polymer3.2crosslinkingprocess of multiple intermolecular covalent or ionic bonding between polymer chains3.3

33、degree of conversionquantity of reacted product obtained during a reaction compared with the maximum possible quantity of the productNote 1 to entry: The degree of conversion will depend on both time and temperature.4 PrincipleThe principle is specified in ISO 11357-1.The test method described indic

34、ates the various stages of the reaction by means of DSC curves. ISO 2013 All rights reserved 1ISO 11357-5:2013(E)BS EN ISO 11357-5:2014BS ISO 11357-5:2013ISO 11357-5:2013(E)5 Apparatus and materialsThe apparatus and materials are specified in ISO 11357-1.6 Test specimensThe test specimens are specif

35、ied in ISO 11357-1.If not specified otherwise, use a mass of 5 mg to 20 mg and adjust the specimen mass if the thermal effect is too high or too low.7 Test conditions and specimen conditioningFor polymers, the test conditions and specimen conditioning are specified in ISO 11357-1.For specimens relea

36、sing volatile components, it may be necessary to carry out conditioning and testing with the specimen enclosed in a gas-tight specimen crucible which is resistant to high temperature and pressure.Suitable conditioning procedures shall be agreed between involved parties and included in the test repor

37、t.8 CalibrationThe calibration is specified in ISO 11357-1.9 Procedure9.1 GeneralThe test may use one of two different methods, depending on what information is required: temperature-scanning method; isothermal method.9.2 Temperature-scanning methodThe temperature-scanning method is specified in ISO

38、 11357-1.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 K/min to 20 K/min. Use the same scan rate for all tests which are intended to be comparative.The final temperature shall be lower than

39、the temperature corresponding to the onset of decomposition of the polymer.A preliminary test can be useful in defining the decomposition temperature.9.3 Isothermal method9.3.1 GeneralThe isothermal method can be carried out in two different ways once the specimen is loaded into the DSC sample holde

40、r: at constant temperature;2 ISO 2013 All rights reservedBS EN ISO 11357-5:2014ISO 11357-5:2013(E)BS ISO 11357-5:2013ISO 11357-5:2013(E)5 Apparatus and materialsThe apparatus and materials are specified in ISO 11357-1.6 Test specimensThe test specimens are specified in ISO 11357-1.If not specified o

41、therwise, use a mass of 5 mg to 20 mg and adjust the specimen mass if the thermal effect is too high or too low.7 Test conditions and specimen conditioningFor polymers, the test conditions and specimen conditioning are specified in ISO 11357-1.For specimens releasing volatile components, it may be n

42、ecessary to carry out conditioning and testing with the specimen enclosed in a gas-tight specimen crucible which is resistant to high temperature and pressure.Suitable conditioning procedures shall be agreed between involved parties and included in the test report.8 CalibrationThe calibration is spe

43、cified in ISO 11357-1.9 Procedure9.1 GeneralThe test may use one of two different methods, depending on what information is required: temperature-scanning method; isothermal method.9.2 Temperature-scanning methodThe temperature-scanning method is specified in ISO 11357-1.Carry out a temperature scan

44、, from ambient temperature to a temperature high enough to record the whole of the reaction peak, at a scan rate in the range 5 K/min to 20 K/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

45、onset of decomposition of the polymer.A preliminary test can be useful in defining the decomposition temperature.9.3 Isothermal method9.3.1 GeneralThe isothermal method can be carried out in two different ways once the specimen is loaded into the DSC sample holder: at constant temperature;2 ISO 2013

46、 All rights reservedBS ISO 11357-5:2013ISO 11357-5:2013(E) starting at ambient temperature and heating as quickly as possible to reach the constant measurement temperature.NOTE The choice of procedure will depend on the model of calorimeter used for the test. The measurement temperature is selected

47、on the basis of a trial run in the temperature-scanning mode. The temperature is intended to be in the vicinity of the temperature at which the peak obtained in the scanning mode begins.9.3.2 Constant-temperature methoda) Place the reference crucible in the calorimeter.b) Set the instrument to the d

48、esired measurement temperature.c) Let the calorimeter stabilize at the selected temperature for 5 min.d) Place the crucible containing the specimen in the calorimeter.e) Record the DSC curve.f) Remove the crucible containing the specimen and let it cool down to ambient temperature.g) Place the cruci

49、ble containing the specimen back in the calorimeter.h) Record the DSC curve again (the second curve will be subtracted from the first to correct for the calorimeter perturbation caused by the introduction of the crucible).NOTE When using this procedure, it is difficult to ensure that the manual operation by which the crucible is introduced into the calorimeter is carried out repeatedly for the determination and the blank run. Also, changes to the state of the specimen can have occurred during the reaction. Subtraction of the tw