EN ISO 11357-3-2013 en Plastics - Differential scanning calorimetry (DSC) - Part 3 Determination of temperature and enthalpy of melting and crystallization《塑料 差示扫描量热法(DSC) 第3部分 熔化和.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 11357-3:2013Plastics Differential scanning calorimetry (DSC)Part 3: Determination of temperatureand enthalpy of melting and crystallization (ISO 11357-3:2011)BS EN ISO

2、11357-3:2013National forewordThis British Standard is the UK implementation of EN ISO 11357-3:2013. It is identical to ISO 11357-3:2011. It supersedes BS ISO 11357-3:2011,which is withdrawn.The UK participation in its preparation was entrusted toTechnical Committee PRI/21, Testing of plastics.A list

3、 of organizations represented on this committee can be obtainedon 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 2013. Published by BSI Standards Li

4、mited 2013 ISBN 978 0 580 78958 8 ICS 83.080.01 Compliance with a British Standard cannot confer immunityfrom legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2011. Amendments/corrigenda issued since publicationDate Te

5、xt affected30 April 2013 This corrigendum renumbers BS ISO 11357-3:2011 as BS EN ISO 11357-3:2013BRITISH STANDARDEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-3 January 2013 ICS 83.080.01 English Version Plastics - Differential scanning calorimetry (DSC) - Part 3: Determination of t

6、emperature and enthalpy of melting and crystallization (ISO 11357-3:2011) Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 3: Dtermination de la temprature et de lenthalpie de fusion et de cristallisation (ISO 11357-3:2011) Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil

7、 3: Bestimmung der Schmelz- und Kristallisationstemperatur und der Schmelz- und Kristallisationsenthalpie (ISO 11357-3:2011) This European Standard was approved by CEN on 22 December 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for gi

8、ving 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 European Standard exists in three of

9、ficial 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 are the national standards bodies

10、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, Romania, Slovakia, Slovenia, Spain

11、, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN nati

12、onal Members. Ref. No. EN ISO 11357-3:2013: EForeword The text of ISO 11357-3:2011 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 11357-3:2013 by Technical Committee CEN/TC 249 “Plastics” the

13、 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 July 2013, and conflicting national standards shall be withdrawn at the latest by July 2013. Attention is draw

14、n 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 Internal Regulations, the national standards organisations of the followin

15、g 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, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norw

16、ay, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 11357-3:2011 has been approved by CEN as a EN ISO 11357-3:2013 without any modification. BS EN ISO 11357-3:2013 EN ISO 11357-3:2013 (E)Reference numberISO

17、11357-3:2011(E)ISO 2011INTERNATIONAL STANDARD ISO11357-3Second edition2011-05-01Plastics Differential scanning calorimetry (DSC) Part 3: Determination of temperature and enthalpy of melting and crystallization Plastiques Analyse calorimtrique diffrentielle (DSC) Partie 3: Dtermination de la tempratu

18、re et de lenthalpie de fusion et de cristallisation COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without pe

19、rmission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii BS EN ISO 11357-3:2013

20、 ISO 11357-3:2011 (E) ISO 2013iiiForeword ISO (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 committees. Each member body inte

21、rested 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 International Electrotechnica

22、l Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the t

23、echnical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. I

24、SO shall not be held responsible for identifying any or all such patent rights. ISO 11357-3 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties. This second edition cancels and replaces the first edition (ISO 11357-3:1999), which has been technica

25、lly revised. It also incorporates the Amendment, ISO 11357-3:1999/Amd 1:2005. The most important changes are the following: a specification of the preferred scanning rates of 10 K/min or 20 K/min has been given; Figure 1 has been updated to better reflect the profile of a real melting peak and y-axi

26、s directions specified in ISO 11357-1. 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 Part 3: Determination of temperature and enthalpy of melting an

27、d 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 oxidation induction time (isothermal OIT) and oxidation induction temperature (dynam

28、ic OIT) Part 7: Determination of crystallization kinetics BS EN ISO 11357-3:2013 ISO 11357-3:2011 (E) ISO 2013BS EN ISO 11357-3:2013 ISO 11357-3:2011 (E) ISO 2013INTERNATIONAL STANDARD1Plastics Differential scanning calorimetry (DSC) Part 3: Determination of temperature and enthalpy of melting and c

29、rystallization WARNING The use of this part of ISO 11357 may involve hazardous materials, operations or equipment. This part of ISO 11357 does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this part of ISO 11357 to establish approp

30、riate health and safety practices and to determine the applicability of regulatory limitations prior to use. 1 Scope This part of ISO 11357 specifies a method for the determination of the temperatures and enthalpies of melting and crystallization of crystalline or partially crystalline plastics. 2 N

31、ormative references The following referenced documents are indispensable for the application 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, Plastics Vocabulary

32、ISO 11357-1:2009, Plastics Differential scanning calorimetry (DSC) Part 1: General principles 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 472 and ISO 11357-1 and the following apply. 3.1 melting transition stage between a fully crystalline or par

33、tially crystalline solid state and an amorphous liquid of variable viscosity NOTE The transition, also referred to as “fusion”, is characterised by an endothermic peak in the DSC curve. 3.2 crystallization transition stage between an amorphous liquid state and a fully crystalline or partially crysta

34、lline solid state NOTE The transition is characterised by an exothermic peak in the DSC curve. An exception to this definition is the case of liquid crystals, where the term “amorphous liquid” should be replaced by “ordered liquid”. BS EN ISO 11357-3:2013 ISO 11357-3:2011 (E) ISO 20132 3.3 enthalpy

35、of fusion heat required to melt a material at constant pressure NOTE It is expressed in kilojoules per kilogram (kJ/kg). 3.4 enthalpy of crystallization heat released by the crystallization of a material at constant pressure NOTE It is expressed in kilojoules per kilogram (kJ/kg). 4 Principle See IS

36、O 11357-1:2009, Clause 4. 5 Apparatus and materials Apparatus and materials shall be in accordance with ISO 11357-1:2009, Clause 5. 6 Test specimen The test specimen shall be in accordance with ISO 11357-1:2009, Clause 6. 7 Test conditions and specimen conditioning The test conditions and specimen c

37、onditioning shall be in accordance with ISO 11357-1:2009, Clause 7. 8 Calibration Calibration shall be in accordance with ISO 11357-1:2009, Clause 8. 9 Procedure 9.1 Setting up the apparatus The setting up of the apparatus shall be in accordance with ISO 11357-1:2009, 9.1. 9.2 Loading the test speci

38、men into the crucible The loading of the test specimen shall be in accordance with ISO 11357-1:2009, 9.2. Unless otherwise specified in the material standard, preferably use a mass of 5 mg to 10 mg for the measurement. In the case of high or low heats of transition, masses higher or lower than 5 mg

39、to 10 mg may be used. 9.3 Insertion of crucibles The insertion shall be in accordance with ISO 11357-1:2009, 9.3. BS EN ISO 11357-3:2013 ISO 11357-3:2011 (E) ISO 201339.4 Temperature scan 9.4.1 Heating and cooling rates other than those recommended here may be used by agreement between the intereste

40、d parties. In particular, high scanning rates result in better sensitivity of the recorded transition. On the other hand, low scanning rates provide better resolution in temperature and may be appropriate in the resolution of closely overlapping transitions. 9.4.2 Allow 5 min for a nitrogen pre-purg

41、e prior to beginning the heating cycle. 9.4.3 Perform and record a first heating run, preferably at a rate of 10 K/min or 20 K/min, heating the cell to a temperature high enough to erase the test materials previous thermal history, typically 30 C above the extrapolated end melting temperature, Tefm.

42、 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 11357-1:2009, Annex E). In cases where the mater

43、ial is reactive or where it is desired to evaluate the properties of a specially pre-conditioned 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 may be

44、 acceptable or needed provided degradation of the polymer does not result. 9.4.5 Perform and record a cooling run at preferably the same rate used for the first and second heatings to approximately 50 C below the extrapolated end crystallization temperature, Tefc. NOTE Because of supercooling, cryst

45、allization does not occur until a sufficient temperature gradient is available, usually significantly below the melting temperature. 9.4.6 Hold the temperature for 5 min. 9.4.7 Perform and record a second heating run at preferably the same heating rate as the first heating and cooling runs (see 9.4.

46、1) to approximately 30 C higher than the extrapolated end melting temperature, Tefm. NOTE It is important to create a defined thermal history in order to evaluate correct results. 9.4.8 Bring the apparatus to ambient temperature and remove the crucibles to determine if deformation of the crucible or

47、 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 in mass during the experiment. 10 Expression of results 10.1 Determination of transition temperatures Scale the plot so that the peak covers at least 25 % of

48、full scale. Construct a baseline to the peak (see Figure 1) by joining the peak initiation temperature, Tim, and end temperature, Tfm, at which the peak (endothermic peak for fusion, exothermic peak for crystallization) begins to deviate from the relatively straight baseline. If multiple peaks are p

49、resent, a baseline should be drawn, covering all peaks. The evaluation should then be divided between each peak, in order to get the most correct enthalpy. For a melting transition curve, measure and report the peak melting temperature, Tpm, for each peak. Reporting onset of melting is acceptable if requested. BS EN ISO 11357-3:2013 ISO 11357-3:2011 (E) ISO 20134 For a crystallization transition curve, measure and report for each peak: the extrapolated onset crystallization temperature, Teic; the peak cryst