1、BSI Standards PublicationBS EN ISO 11357-7:2015Plastics Differential scanningcalorimetry (DSC)Part 7: Determination of crystallizationkineticsBS EN ISO 11357-7:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 11357-7:2015. It supersedes BS EN ISO 11357-7
2、:2013 which iswithdrawn.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 provisions
3、 of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 79981 5 ICS 83.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published u
4、nder the authority of the Standards Policy and Strategy Committee on 30 September 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-7 September 2015 ICS 83.080.01 Supersedes EN ISO 11357-7:2013English Version
5、 Plastics - Differential scanning calorimetry (DSC) - Part 7: Determination of crystallization kinetics (ISO 11357-7:2015) Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 7: Dtermination de la cintique de cristallisation (ISO 11357-7:2015) Kunststoffe - Dynamische Differenz-Thermoana
6、lyse (DSC) - Teil 7: Bestimmung der Kristallisationskinetik (ISO 11357-7:2015) This European Standard was approved by CEN on 31 July 2015. 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 nation
7、al 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 European Standard exists in three official versions (English, French, German). A versi
8、on 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 are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Cz
9、ech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
10、EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11357-7:
11、2015 EBS EN ISO 11357-7:2015EN ISO 11357-7:2015 (E) 3 European foreword This document (EN ISO 11357-7:2015) has been prepared by Technical Committee ISO/TC 61 “Plastics“in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held byNBN. This European Standard shal
12、l be given the status of a national standard, either by publication of anidentical text or by endorsement, at the latest by March 2016, and conflicting national standards shallbe withdrawn at the latest by March 2016. Attention is drawn to the possibility that some of the elements of this document m
13、ay be the subject ofpatent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patentrights. This document supersedes EN ISO 11357-7:2013. According to the CEN-CENELEC Internal Regulations, the national standards organizations of thefollowing countries are bound
14、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, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,Netherlands, Norway, Poland, Portugal, Rom
15、ania, Slovakia, Slovenia, Spain, Sweden, Switzerland,Turkey and the United Kingdom.Endorsement notice The text of ISO 11357-7:2015 has been approved by CEN as EN ISO 11357-7:2015 without anymodification. BS EN ISO 11357-7:2015ISO 11357-7:2015(E)Foreword iv1 Scope . 12 Normative references 13 Terms a
16、nd definitions . 14 Principle 25 Apparatus and materials 26 Test specimens 27 Test conditions and specimen conditioning 28 Calibration 29 Procedure. 29.1 General . 29.2 Loading the test specimen into the crucible 39.3 Insertion of the crucibles into the instrument 39.4 Melting of the polymer . 39.5
17、Isothermal crystallization . 39.6 Non-isothermal crystallization . 410 Expression of results 510.1 General . 510.2 Methods of determination of crystallization kinetics . 510.2.1 Isothermal crystallization 510.2.2 Non-isothermal crystallization 711 Precision . 812 Test report . 8Annex A (informative)
18、 Equations for crystallization kinetics of polymers 9Bibliography .11 ISO 2015 All rights reserved iiiContents PageBS EN ISO 11357-7:2015ISO 11357-7:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The
19、 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 right to be represented on that committee. International organizations, governmental and non-gove
20、rnmental, 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.The procedures used to develop this document and those intended for its further maintenance are described in
21、 the ISO/IEC Directives, Part 1. In particular the different approval 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 po
22、ssibility that some of the elements of this document may be the 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
23、 of patent declarations received (see www.iso.org/patents).Any 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 meaning of ISO specific terms and expressions related to conformity assessment, as well a
24、s information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information.The committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties.This second edition cancel
25、s and replaces the first edition (ISO 11357-7:2002), which has been technically revised with the following changes:a) values to be recorded for isothermal crystallization revised, starting time of the isothermal step (t = 0) added (10.2.1), and Figure 2 to Figure 6 revised accordingly;b) Formula (A.
26、1) and Formula (A.2) are corrected;c) dated references changed to undated references.ISO 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 transit
27、ion step height Part 3: Determination of temperature 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 oxida
28、tion induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT) Part 7: Determination of crystallization kineticsiv ISO 2015 All rights reservedBS EN ISO 11357-7:2015INTERNATIONAL STANDARD ISO 11357-7:2015(E)Plastics Differential scanning calorimetry (DSC) Part 7: Determinatio
29、n of crystallization kinetics1 ScopeThis part of ISO 11357 specifies two methods (isothermal and non-isothermal) for studying the crystallization kinetics of partially crystalline polymers using differential scanning calorimetry (DSC).It is only applicable to molten polymers.NOTE These methods are n
30、ot suitable if the molecular structure of the polymer is modified during the test.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 undat
31、ed references, the latest edition of the referenced document (including any amendments) applies.ISO 472, Plastics VocabularyISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principlesISO 11357-3, Plastics Differential scanning calorimetry (DSC) Part 3: Determination of t
32、emperature and enthalpy of melting and crystallization3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472, ISO 11357-1, ISO 11357-3, and the following apply.3.1crystallization kineticsdescription of the rate of crystallization of a material taking int
33、o account the effects of variables such as time, temperature, pressure, stress, and molecular structureNote 1 to entry: These factors and also any additives, fillers, or contaminants can modify the crystallinity of the polymer at the end of crystallization.3.2relative crystallinityratio between the
34、crystallinity at a particular point in time or a particular temperature and the crystallinity at the end of crystallizationNote 1 to entry: The relative crystallinity can be expressed either as a ratio or as a percentage if multiplied by 100.Note 2 to entry: In DSC, the relative crystallinity can be
35、 determined as the ratio between the partial area of the crystallization peak, at each time or each temperature, and the total area of the peak. ISO 2015 All rights reserved 1BS EN ISO 11357-7:2015ISO 11357-7:2015(E)4 PrincipleThe principle is specified in ISO 11357-1.5 Apparatus and materials5.1 Di
36、fferential scanning calorimeter, according to ISO 11357-1.5.2 Crucibles, according to ISO 11357-1.It can be necessary to verify that the material used for the crucibles does not modify the crystallization kinetics of the polymer.5.3 Balance, according to ISO 11357-1.5.4 Calibration materials, accord
37、ing to ISO 11357-1.5.5 Purge gas, according to ISO 11357-1.6 Test specimensTest specimens shall be as specified in ISO 11357-1.7 Test conditions and specimen conditioningTest conditions and specimen conditioning shall be as specified in ISO 11357-1.8 CalibrationThe calibration shall be done in accor
38、dance with ISO 11357-1.The linearity of the temperature scale in the heating and cooling modes shall be checked using materials which do not supercool. The use of the liquid-liquid transition of liquid crystals, such as 4,4-azoxyanisole, is recommended.9 Procedure9.1 GeneralThe study of the crystall
39、ization kinetics of polymers can be done in an isothermal or a non-isothermal mode.2 ISO 2015 All rights reservedBS EN ISO 11357-7:2015ISO 11357-7:2015(E)The relative crystallinity is given by the ratio of the partial enthalpy of crystallization, at each time or each temperature, and the total entha
40、lpy of crystallization Hc, as given in Formula (1):tT tTHor or c= (1)wheretand Htare the relative crystallinity and the enthalpy of crystallization at a given time in the isothermal mode;Tand HTare the relative crystallinity and the enthalpy of crystallization at a given tempera-ture in the non-isot
41、hermal mode.9.2 Loading the test specimen into the crucibleThe loading of the test specimen shall be done as specified in ISO 11357-1.To avoid self-heating, the mass of the specimen shall be chosen based on the heat evolved by the crystallization of the material. If the object of the measurements is
42、 to compare various grades of a polymer, maintain the mass within 0,5 mg.9.3 Insertion of the crucibles into the instrumentThe crucibles shall be inserted into the instrument as specified in ISO 11357-1.9.4 Melting of the polymerPrior to isothermal or non-isothermal crystallization, all crystalline
43、elements in the sample that could modify the crystallization kinetics shall be molten completely.This is usually achieved by heating at a rate of 10 K/min or 20 K/min to a temperature of 30 K above the extrapolated end melting temperature and holding at this temperature for 3 min to 5 min.NOTE Preli
44、minary trials can be done to optimize these conditions and to prevent this step from changing the molecular structure of the polymer.9.5 Isothermal crystallizationAt the end of the melting stage, cool the specimen as quickly as possible to the selected temperature at which isothermal crystallization
45、 shall be measured.A schematic representation of an isothermal crystallization run is shown in Figure 2.The time t0, at which the selected temperature is reached, is the start of the isothermal step.Isothermal crystallization starts at initial crystallization time, ti, which is obtained by the inter
46、section point of the slope of the crystallization peak onset with a linear baseline obtained by interpolation between peak start and end.The time tfat which the isothermal step ends (i.e. the time to obtain a complete crystallization curve) depends on the crystallization rate. If not clear from the
47、DSC curve, it shall be set to five times the time taken to reach the maximum crystallization rate, tmax.Carry out at least three runs at different temperatures.The isothermal temperatures are limited by the specifications of the instrument and data shall be rejected when the crystallization starts d
48、uring cooling (see Figure 1).NOTE Limiting instrument factors can be e.g. too high thermal lag or insufficient cooling capabilities. ISO 2015 All rights reserved 3BS EN ISO 11357-7:2015ISO 11357-7:2015(E)Key1 DSC signal2 temperature plotdQ/dt heat flow ratet timeaExothermic direction.Figure 1 Bad is
49、othermal run: Crystallization started before isothermal temperature reachedKey1 DSC signal2 temperature plotdQ/dt heat flow ratet timeaExothermic direction.Figure 2 Good isothermal run9.6 Non-isothermal crystallizationAt the end of the melting stage, cool the specimen at the selected constant cooling rate to at least 10 K to 20 K below the final crystallization temperature.4 ISO 2015 All rights reservedBS EN ISO 11357-7:2015ISO 11357-7:2015(E)Carry out at least three runs at different cooling rates.NOTE It is recomm
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