DIN EN ISO 11357-1-2017 Plastics - Differential scanning calorimetry (DSC) - Part 1 General principles (ISO 11357-1 2016) German version EN ISO 11357-1 2016《塑料 差示扫描量热法(DSC) 第1部分 通则.pdf

1、February 2017 English price group 17No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 83.080.01!%an“2627596www.din.de

2、DIN EN ISO 11357-1Plastics Differential scanning calorimetry (DSC) Part 1: General principles (ISO 113571:2016);English version EN ISO 113571:2016,English translation of DIN EN ISO 11357-1:2017-02Kunststoffe Dynamische DifferenzThermoanalyse (DSC) Teil 1: Allgemeine Grundlagen (ISO 113571:2016);Engl

3、ische Fassung EN ISO 113571:2016,Englische bersetzung von DIN EN ISO 11357-1:2017-02Plastiques Analyse calorimtrique diffrentielle (DSC) Partie 1: Principes gnraux (ISO 113571:2016);Version anglaise EN ISO 113571:2016,Traduction anglaise de DIN EN ISO 11357-1:2017-02SupersedesDIN EN ISO 113571:20100

4、3www.beuth.deDocument comprises 40 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.02.17 DIN EN ISO 11357-1:2017-02 2 A comma is used as the decimal marker. National foreword This document (EN ISO 11357-1:2016) has been prepare

5、d by Technical Committee ISO/TC 61 “Plastics” in collaboration with Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was DIN-Normenausschuss Kunststoffe (DIN Standards Committee Plastics), Working Committee NA 054-01-03 AA

6、 Physikalische, rheologische und analytische Prfungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 472 DIN EN ISO 472 ISO 80000-5 DIN EN ISO 80000-5 Amendments This standard differs from DIN EN ISO 11357-1:2010-03 as follows: a) nor

7、mative references have been updated; b) in subclause 3.7.2, Note 2 has been amended; c) the Bibliography has been updated; d) the standard has been editorially revised. Previous editions DIN EN ISO 11357-1: 1997-11, 2010-03 National Annex NA (informative) Bibliography DIN EN ISO 472, Plastics Vocabu

8、lary DIN EN ISO 80000-5, Quantities and units Part 5: Thermodynamics EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-1 October 2016 ICS 83.080.01 Supersedes EN ISO 11357-1:2009English Version Plastics - Differential scanning calorimetry (DSC) - Part 1: General principles (ISO 11357-1:

9、2016) Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 1: Principes gnraux (ISO 11357-1:2016) Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 1: Allgemeine Grundlagen(ISO 11357-1:2016) This European Standard was approved by CEN on 13 August 2016. CEN members are bound to

10、 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 the CEN-CE

11、NELEC 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 Centre has t

12、he 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, Lithuania, Luxem

13、bourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussel

14、s 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11357-1:2016 EEuropean foreword .4Introduction . 61 Scope . 72 Normative references 73 Terms and definitions . 74 Basic principles . 144.1 General 144.2 Heat-flux DSC . 144

15、.3 Power-compensation DSC 145 Apparatus and materials. 156 Specimen 167 Test conditions and specimen conditioning .177.1 Test conditions . 177.2 Conditioning of specimens 178 Calibration .178.1 General 178.2 Calibration materials 188.3 Temperature calibration 188.3.1 General. 188.3.2 Procedure 188.3

16、.3 Accuracy of calibration 198.4 Heat calibration . 198.4.1 General. 198.4.2 Procedure 208.4.3 Accuracy of calibration 208.5 Heat flow rate calibration . 218.5.1 General. 218.5.2 Procedure 219 Procedure239.1 Setting up the apparatus 239.1.1 Switching on .239.1.2 Purge gas 239.1.3 Experimental condit

17、ions 239.1.4 Baseline determination . 239.2 Loading the specimen into the crucible . 239.2.1 General. 239.2.2 Selection of crucibles 249.2.3 Weighing the specimen crucible 249.2.4 Loading the specimen .249.2.5 Determination of the mass of the specimen249.3 Insertion of crucibles into the instrument

18、. 249.4 Performing measurements 249.4.1 General. 249.4.2 Scanning mode .249.4.3 Isothermal mode .259.5 Post-run checks . 269.5.1 Check for loss in mass 269.5.2 Inspection of specimens . 269.5.3 Checking of crucibles and crucible holder 26Contents PageForeword 5DIN EN ISO 11357-1:2017-02 EN ISO 11357

19、-1:2016 (E) 2 Annex A (normative) Extended, high-precision, temperature calibration12.28Annex B (normative) Extended, high-precision, heat calibration 30Annex C (informative) Recommended calibration materials 32Annex D (informative) Interaction of calibration materials with different crucible materi

20、als .35Annex E (informative) General recommendations .37Bibliography .3810 Test report 26DIN EN ISO 11357-1:2017-02 EN ISO 11357-1:2016 (E) 3 European foreword This document (EN ISO 11357-1:2016) has been prepared by Technical Committee ISO/TC 61 “Plastics” in collaboration with Technical Committee

21、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 April 2017, and conflicting national standards shall be withdrawn at the latest by Ap

22、ril 2017. 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. This document supersedes EN ISO 11357-1:2009. According to the CEN-CENELEC I

23、nternal 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

24、, 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 11357-1:2016 has been approved by CEN as EN ISO 11357-1:2016 without any modificat

25、ion. DIN EN ISO 11357-1:2017-02 EN ISO 11357-1:2016 (E) 4 ForewordISO (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 committee

26、s. Each member body interested 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 Inter

27、national Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the diff

28、erent types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shal

29、l not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is

30、 information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT)

31、see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical propertiesThis third edition cancels and replaces the second edition (ISO 11357-1:2009), 3.7.2 of which has been technically revised.ISO

32、 11357 consists of the following parts, under the general title Plastics Differential scanning calorimetry (DSC): Part 1: General principles Part 2: Determination of glass transition temperature and glass transition step height Part 3: Determination of temperature and enthalpy of melting and crystal

33、lisation 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 (isothermal OIT) and oxidation induction temperature (dynamic OIT) P

34、art 7: Determination of crystallization kineticsDIN EN ISO 11357-1:2017-02 EN ISO 11357-1:2016 (E) 5 IntroductionISO 11357 describes thermoanalytical DSC test methods which can be used for quality assurance purposes, for routine checks of raw materials and finished products or for the determination

35、of comparable data needed for data sheets or databases. The procedures given in ISO 11357 apply as long as product standards or standards describing special atmospheres for conditioning of specimens do not specify otherwise.DIN EN ISO 11357-1:2017-02 EN ISO 11357-1:2016 (E) 6 SAFETY STATEMENT Person

36、s using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure comp

37、liance with any regulatory requirements.1 ScopeISO 11357 specifies several differential scanning calorimetry (DSC) methods for the thermal analysis of polymers and polymer blends, such as thermoplastics (polymers, moulding compounds and other moulding materials, with or without fillers, fibres or re

38、inforcements), thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements), and elastomers (with or without fillers, fibres or reinforcements).ISO 11357 is intended for the observation and measurement of various properties of, and phenomena associated with, the above-m

39、entioned materials, such as physical transitions (glass transition, phase transitions such as melting and crystallization, polymorphic transitions, etc.), chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.), the stability to oxidation, and the heat capacit

40、y.This part of ISO 11357 specifies a number of general aspects of differential scanning calorimetry, such as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report common to all following parts.Details on performing specific methods are given in s

41、ubsequent parts of ISO 11357 (see Foreword).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 references, the latest edition of t

42、he referenced document (including any amendments) applies.ISO 472, Plastics VocabularyISO 80000-5, Quantities and units Part 5: Thermodynamics3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 and ISO 80000-5 and the following apply.DIN EN ISO 11357-

43、1:2017-02 EN ISO 11357-1:2016 (E) 7 3.1differential scanning calorimetryDSCtechnique in which the difference between the rate of flow of heat into a specimen crucible containing the specimen and that into a reference crucible (3.3) is derived as a function of temperature and/or time while the specim

44、en and reference are subjected to the same controlled temperature programme in a specified atmosphere using a symmetrical measurement systemNote 1 to entry: It is common practice to record, for each measurement run, a curve in which temperature or time is plotted as the abscissa and heat flow rate (

45、3.4) difference as the ordinate. The endothermic and/or exothermic direction is indicated on the DSC curve.Note 2 to entry: According to the principles of thermodynamics, energy absorbed by a system is considered positive while energy released is negative. This approach implies that the endothermic

46、direction points upwards in the ordinate and the exothermic direction downwards (see Figures 1 and 2). It also has the advantage that the direction of thermal effects in plots of heat flow rate (3.4) and specific heat is consistent.3.2calibration materialmaterial for which one or more of the thermal

47、 properties are sufficiently homogeneous and well established to be used for the calibration of a DSC instrument or for the assessment of a measurement method3.3reference cruciblecrucible used on the reference side of the symmetrical crucible holder assemblyNote 1 to entry: Normally, the reference crucible is empty.Note 2 to entry: In special cases, such as the measurement of highly filled or reinforced polymers or specimens having a heat capacity comparable to that of the crucible, a suitable material can be used inside the reference crucible. This reference material shou