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

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 ofconversionCopyright British Standards Institution Provided by IHS under lice

2、nse with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-5:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 11357-5:2014. It is identical to ISO 11357-5:2013. It supersedes BS ISO

3、 11357-5:2013 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary p

4、rovisions 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 83.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was pub

5、lished under the authority of the Standards Policy and Strategy Committee on 30 April 2013.Amendments/corrigenda issued since publicationDate Text affected30 April 2014 This corrigendum renumbers BS ISO 11357-5:2013 as BS EN ISO 11357-5:2014Copyright British Standards Institution Provided by IHS und

6、er license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-5 March 2014 ICS 83.080.01 English Version Plastics - Differential scanning calorimetry (DSC) - Part 5: Determinat

7、ion of characteristic reaction-curve temperatures and times, enthalpy 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

8、du degr de transformation (ISO 11357-5:2013)Kunststoffe - Dynamische 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 ar

9、e bound to comply with the CEN/CENELEC Internal Regulations which 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

10、the CEN-CENELEC Management Centre or to any CEN member. This European 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 Ce

11、ntre has the same status as the official versions. CEN members are 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, Lithua

12、nia, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, 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-1

13、000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11357-5:2014 ECopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking perm

14、itted without license from IHS-,-,-BS 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 Standardization (ISO) and has been taken over as EN ISO

15、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 latest by September 2014, and conflicting national standard

16、s 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 all such patent rights. According to the CEN-CENELEC Int

17、ernal 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 Macedonia, France, Germany, Greece, Hungary, Iceland,

18、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 by CEN as EN ISO 11357-5:2014 without any modificatio

19、n. Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-5:2014ISO 11357-5:2013(E)BS ISO 11357-5:2013ISO 11357-5:2013(E) ISO 2013 All rights reserved iiiCon

20、tents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Apparatus and materials 26 Test specimens 27 Test conditions and specimen conditioning 28 Calibration 29 Procedure. 29.1 General . 29.2 Temperature-scanning method 29.3 Isothermal method 210 Determinati

21、on of results 410.1 Determination of characteristic temperatures 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 . 9Bibliog

22、raphy .10BS ISO 11357-5:2013ISO 11357-5:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 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 .

23、 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 Determination of characteristic times and enthalpy of reaction (isothermal method). 410.3 Determinat

24、ion of degree of conversion . 611 Precision . 912 Test report .Bibliography .10Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-This page deliberately left blankBS ISO

25、 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 observed when working with materials which cou

26、ld 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 calorimetry (DSC).The method applies to monomers, p

27、repolymers, 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

28、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 definitionsFor the purposes of this document, the t

29、erms 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 chains3.3degree of conversionquantity of reacted produ

30、ct 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 indicates the various stages of the reaction by me

31、ans of DSC curves. ISO 2013 All rights reserved 1Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 11357-5:2013INTERNATIONAL STANDARD ISO 11357-5:2013(E)Plastics

32、 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 runaway reaction or exhibit other dangerous behaviour

33、.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, and polymers in the solid or liquid state. The mate

34、rial 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, only the edition cited applies. For undated referen

35、ces, 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 definitions given in ISO 11357-1 and the following app

36、ly.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 obtained during a reaction compared with the maximum possibl

37、e 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 curves. ISO 2013 All rights reserved 1ISO 11357-5:20

38、13(E)BS EN ISO 11357-5:2014Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS ISO 11357-5:2013ISO 11357-5:2013(E)5 Apparatus and materialsThe apparatus and materials

39、are specified in ISO 11357-1.6 Test specimensThe test specimens are specified 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

40、and specimen conditioning are specified in ISO 11357-1.For specimens releasing 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 procedur

41、es shall be agreed between involved parties and included in the test report.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 Temp

42、erature-scanning methodThe temperature-scanning method is specified in ISO 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

43、 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 can be useful in defining the decomposition temperature.9.3 Isothermal method9.3.1 GeneralThe isothermal method can be carried out i

44、n two different ways once the specimen is loaded into the DSC sample holder: at constant temperature;2 ISO 2013 All rights reservedBS EN ISO 11357-5:2014ISO 11357-5:2013(E)Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction

45、 or networking permitted without license from IHS-,-,-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 otherwise, use a mass of 5 mg to 20 mg and ad

46、just 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 necessary to carry out conditioning and testi

47、ng 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 specified in ISO 11357-1.9 Procedure9.1 General

48、The 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, from ambient temperature to a temperature

49、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 onset of decomposition of the polymer.A preliminary