EN ISO 11357-3-2018 en Plastics - Differential scanning calorimetry (DSC) - Part 3 Determination of temperature and enthalpy of melting and crystallization.pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Plastics - Differential scanning calorimetry (DSC)Part 3: Determination of temperature and enthalpy of melting and crystallizationBS EN ISO 113573:2018National forewordThis British Standard is the UK implementation of E

2、N ISO 113573:2018. It is identical to ISO 113573:2018. It supersedes BS EN ISO 113573:2013, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this committee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

3、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 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 96206 6ICS 83.080.01Compliance with a British Standar

4、d cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN ISO 113573:2018EUROPEAN STANDARDNORME EUROPENNEE

5、UROPISCHE NORMEN ISO 11357-3May 2018ICS 83.080.01 Supersedes EN ISO 113573:2013EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN Ref. No. EN ISO 113573:2018: EAll rights of explo

6、itation in any form and by any means reserved worldwide for CEN national MembersPlastics Differential scanning calorimetry (DSC) Part 3: Determination of temperature and enthalpy of melting and crystallization (ISO 113573:2018)Plastiques Analyse calorimtrique diffrentielle (DSC) Partie 3: Dterminati

7、on de la temprature et de lenthalpie de fusion et de cristallisation (ISO 113573:2018)Kunststoffe Dynamische DifferenzThermoanalyse (DSC) Teil 3: Bestimmung der Schmelz und Kristallisationstemperatur und der Schmelz und Kristallisationsenthalpie (ISO 113573:2018)This European Standard was approved b

8、y CEN on 24 February 2018.CEN members are 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. Uptodate lists and bibliographical references concerning such national standa

9、rds may be obtained on application to the CENCENELEC 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 notif

10、ied to the CEN-CENELEC Management Centre 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, Icel

11、and, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English VersionEN ISO 11357-3:2018 (E)European forewordThis document (EN ISO 113573:2018) has been prepared by

12、Technical Committee ISO/TC 61 “Plastics” in collaboration with 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 Nov

13、ember 2018, and conflicting national standards shall be withdrawn at the latest by November 2018.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights.This

14、document supersedes EN ISO 113573:2013.According to the CENCENELEC 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 Yugos

15、lav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.Endorsement noticeThe text of ISO 113573:2

16、018 has been approved by CEN as EN ISO 113573:2018 without any modification.2BS EN ISO 113573:2018ISO 11357-3:2018Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Apparatus and materials 26 Test specimen 27 Test conditions and specimen conditioning 28 Calibrati

17、on 29 Procedure. 29.1 Setting up the apparatus. 29.2 Loading the test specimen into the crucible 29.3 Insertion of crucibles . 29.4 Temperature scan . 210 Expression of results 310.1 Determination of transition temperatures . 310.2 Determination of enthalpies . 411 Precision . 512 Test report . 5Bib

18、liography 6 ISO 2018 All rights reserved iiiContents PageBS EN ISO 113573:2018ISO 11357-3:2018ForewordISO (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

19、 out through ISO technical committees. 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 nongovernmental, in liaison with ISO, also take part in the work. ISO

20、collaborates closely with the International 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 a

21、pproval criteria needed for the different 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 th

22、e subject of patent rights. ISO shall 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

23、 trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs a

24、dherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties.This third edition cancels an

25、d replaces the second edition (ISO 113573:2011), which has been technically revised. The main changes compared to the previous edition are as follows: the normative references in Clause 2 have been updated; the sample mass is referring to polymer matrix; the procedure has been extended to cover mate

26、rials with wider crystallisation ranges; the calculation of heats of transition has been clarified to include computer aided methods.A list of all parts in the ISO 11357 series can be found on the ISO website.iv ISO 2018 All rights reservedBS EN ISO 113573:2018Plastics - Differential scanning calori

27、metry (DSC) Part 3: Determination of temperature and enthalpy of melting and crystallization1 ScopeThis document specifies a method for the determination of the temperatures and enthalpies of melting and crystallization of crystalline or partially crystalline plastics.2 Normative referencesThe follo

28、wing documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 472

29、, Plastics VocabularyISO 113571, Plastics Differential scanning calorimetry (DSC) Part 1: General principles3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 and ISO 11357-1 and the following apply.ISO and IEC maintain terminological databases for u

30、se in standardization at the following addresses: IEC Electropedia: available at https:/www.electropedia.org/ ISO Online browsing platform: available at https:/www.iso.org/obp3.1meltingtransition stage between a fully crystalline or partially crystalline solid state and an amorphous liquid of variab

31、le viscosityNote 1 to entry: The transition, also referred to as “fusion”, is characterized by an endothermic peak in the DSC curve. An exception to this definition is the case of liquid crystals, where the term “amorphous liquid” is replaced by “ordered liquid”.3.2crystallizationtransition stage be

32、tween an amorphous liquid state and a fully crystalline or partially crystalline solid stateNote 1 to entry: The transition is characterized by an exothermic peak in the DSC curve. An exception to this definition is the case of liquid crystals, where the term “amorphous liquid” is replaced by “order

33、ed liquid”.3.3enthalpy of fusionheat required to melt a material at constant pressureNote 1 to entry: It is expressed in kilojoules per kilogram (kJ/kg) or joules per gram (J/g).INTERNATIONAL STANDARD ISO 11357-3:2018 ISO 2018 All rights reserved 1BS EN ISO 113573:2018ISO 11357-3:20183.4enthalpy of

34、crystallizationheat released by the crystallization of a material at constant pressureNote 1 to entry: It is expressed in kilojoules per kilogram (kJ/kg) or joules per gram (J/g).4 PrincipleSee ISO 113571.5 Apparatus and materialsApparatus and materials shall be in accordance with ISO 113571.6 Test

35、specimenThe test specimen shall be in accordance with ISO 113571.7 Test conditions and specimen conditioningThe test conditions and specimen conditioning shall be in accordance with ISO 113571.8 CalibrationCalibration shall be in accordance with ISO 113571.9 Procedure9.1 Setting up the apparatusThe

36、setting up of the apparatus shall be in accordance with ISO 113571.9.2 Loading the test specimen into the crucibleThe loading of the test specimen shall be in accordance with ISO 113571.Unless otherwise specified in the material standard, preferably use a mass of 5 mg to 10 mg for the measurement. I

37、n the case of high or low heats of transition, masses lower or higher than 5 mg to 10 mg, respectively, may be used. In case of polymer compounds the mass shall refer to the matrix polymer.9.3 Insertion of cruciblesThe insertion shall be in accordance with ISO 113571.9.4 Temperature scan9.4.1 Heatin

38、g and cooling rates other than those recommended here may be used by agreement between the interested parties. In particular, high scanning rates result in larger effects of the recorded transition. On the other hand, low scanning rates provide higher resolution in temperature and may be appropriate

39、 in the resolution of closely overlapping transitions.9.4.2 Allow 5 min for a nitrogen prepurge prior to beginning the heating cycle.2 ISO 2018 All rights reservedBS EN ISO 113573:2018ISO 11357-3:20189.4.3 Perform and record a first heating run, heating the cell to a temperature high enough to erase

40、 the test materials previous thermal history, typically 30 K above the extrapolated end melting temperature, Tef,m. Preferred heating rates for the first heating run are 10 K/min or 20 K/min, but also higher heating rates may be used to delete the thermal and mechanical history of a sample within th

41、e first heating run.DSC measurements on polymers are greatly affected by the thermal history and morphology of the sample and the test specimen. It is important that the preliminary heat cycle be performed and the measurements be taken from the second heat scan (see ISO 113571). In cases where the m

42、aterial is reactive or where it is desired to evaluate the properties of a specially preconditioned specimen, data may be taken during the first heating cycle. This deviation from the standard procedure shall be recorded in the test report.9.4.4 Hold the temperature for 5 min.NOTE Longer times can b

43、e acceptable or needed provided degradation of the polymer does not result.9.4.5 Perform and record a cooling run at preferably 10 K/min or 20 K/min to approximately 50 K below the extrapolated end crystallization temperature, Tef,cor lower if required by the polymer to be measured.NOTE Because of s

44、upercooling, crystallization does not occur until a sufficient temperature gradient is available, usually significantly below the melting temperature.If glass transitions are to be evaluated, too, cooling shall be done 50 K below the glass transition temperature or lower if required by the polymer t

45、o be measured.9.4.6 Hold the temperature for 5 min.NOTE It is important to create a defined thermal history in order to evaluate correct results.9.4.7 Perform and record a second heating run at preferably the same heating rate as the cooling run (see 9.4.5) to approximately 30 K higher than the extr

46、apolated end melting temperature, Tef,m.9.4.8 Bring the apparatus to ambient temperature and remove the crucibles to determine if deformation of the crucible or specimen overflow has occurred.9.4.9 Reweigh the crucible with the test specimen, unless it is known that the material will suffer no loss

47、in mass during the experiment.In case of significant weight loss repetition of measurements with stronger dried specimens shall be considered.10 Expression of results10.1 Determination of transition temperaturesScale the plot so that the peak covers at least 25 % of full scale. Construct a baseline

48、to the peak (see Figure 1) by joining the peak initiation temperature, Ti,m, and end temperature, Tf,m, at which the peak (endothermic peak for fusion, exothermic peak for crystallization) begins to deviate from the relatively straight baseline. If multiple peaks are present, a baseline shall be dra

49、wn, covering all peaks. If possible, the evaluation shall then be divided between each peak, in order to get the most accurate enthalpy. Suitable peak separation techniques may be used and shall then be mentioned in the test report.For a melting transition curve, measure and report the peak melting temperature, Tp,m, for each peak.Reporting onset of melting is acceptable if requested. ISO 2018 All rights reserved 3BS EN ISO 113573:2018ISO 11357-3:2018For a crystallization transition curve, mea