1、BSI Standards PublicationBS EN ISO 11357-2:2014BS ISO 11357-2:2013Plastics Differential scanningcalorimetry (DSC)Part 2: Determination of glass transitiontemperature and glass transition step heightCopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not
2、 for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-2:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 11357-2:2014.It is identical to ISO 11357-2:2013. It supersedes BS ISO 11357-2:2013,which is withdrawn.The
3、UK participation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee can be obtainedon request to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are respo
4、nsible for its correct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 83436 3 ICS 83.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standa
5、rdsPolicy and Strategy Committee on 30 April 2013.Amendments/corrigenda issued since publicationDate Text affected30 April 2014 This corrigendum renumbers BS ISO 11357-2:2013 asBS EN ISO 11357-2:2014Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy No
6、t for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-2 March 2014 ICS 83.080.01 English Version Plastics - Differential scanning calorimetry (DSC) - Part 2: Determination of glass transition temperature and gl
7、ass transition step height (ISO 11357-2:2013) Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 2: Dtermination de la temprature de transition vitreuse et de la hauteur de palier de transition vitreuse (ISO 11357-2:2013) Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) -Teil 2: B
8、estimmung der Glasbergangstemperatur und Glasbergangsstufenhhe (ISO 11357-2:2013) This European Standard was approved by CEN on 6 March 2014. 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 nat
9、ional 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 ve
10、rsion 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,
11、 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, Sweden, Switzerland, Turkey and United Kingdo
12、m. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 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
13、-2:2014 ECopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-EN ISO 11357-2:2014 (E)3Foreword The text of ISO 11357-2:2013 has been prepared by Technical Committee ISO/TC
14、 61 “Plastics” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 11357-2:2014 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 publicati
15、on of an identical text or by endorsement, at the latest by September 2014, and conflicting national standards 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
16、shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic,
17、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 the United Kingdom. Endorsemen
18、t notice The text of ISO 11357-2:2013 has been approved by CEN as EN ISO 11357-2:2014 without any modification. EN ISO 11357-2:2014 (E) 3ForewordThe text of ISO 11357-2:2013 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) and
19、has been taken over as EN ISO 11357-2:2014 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 identicaltext or by endorsement, at the latest by September 2014, and c
20、onflicting national standards shall bewithdrawn 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 patentrights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights.Accordin
21、g to the CEN-CENELEC 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 Yugoslav Republic of Macedonia, France, Germany, Gr
22、eece,Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.Endorsement noticeThe text of ISO 11357-2:2013 has been approved by CEN as EN ISO 11357-2:2014 wit
23、hout any modification.BS EN ISO 11357-2:2014Copyright 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 11357-2:2013ISO 11357-2:2013(E) ISO 2013 All rights reserved iiiCon
24、tents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions. 14 Principle 25 Apparatus and materials 26 Test specimens 27 Test conditions and specimen conditioning 28 Calibration 29 Procedure. 29.1 Setting up the apparatus. 29.2 Loading the test specimen into the crucible 29.3 In
25、sertion of crucibles. 29.4 Temperature scan. 210 Expression of results 310.1 Determination of glass transition temperatures . 310.2 Determination of glass transition step height 511 Precision . 512 Test report. 5Bibliography 6BS ISO 11357-2:2013ISO 11357-2:2013(E) ISO 2013 All rights reserved iiiCon
26、tents PageForeword iv1 Scope . 12 Normative references 3 Terms and definitions .4 Principle 25 Apparatus and materials6 Test specimens7 est conditions and specimen conditioning 8 Calibration 9 Procedure.9.1 Setting up the apparatus. 29.2 Loading the test specimen into the crucible 29.3 Insertion of
27、crucibles . 29.4 Temperature scan . 210 Expression of results 310.1 Determination of glass transition temperatures . 310.2 Determination of glass transition step height 511 Precision .12 Test report .Bibliography 6BS EN ISO 11357-2:2014Copyright British Standards Institution Provided by IHS under li
28、cense with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-This page deliberately left blankCopyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permit
29、ted without license from IHS-,-,-INTERNATIONAL STANDARD ISO 11357-2:2013(E)Plastics Differential scanning calorimetry (DSC) Part 2: Determination of glass transition temperature and glass transition step heightWARNING The use of this part of ISO 11357 may involve hazardous materials, operations, or
30、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 appropriate health and safety practices and to determine the applicability of regulatory limitations prior to
31、use.1 ScopeThis part of ISO 11357 specifies methods for the determination of the glass transition temperature and the step height related to the glass transition of amorphous and partially crystalline plastics.2 Normative referencesThe following documents, in whole or in part, are normatively refere
32、nced in this document and are indispensable for its application. For dated 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: Genera
33、l principles3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 11357-1 and the following apply.3.1glass transitionreversible change in an amorphous polymer or in amorphous regions of a partially crystalline polymer from (or to) a viscous or rubbery condi
34、tion to (or from) a hard and relatively brittle one3.2glass transition temperatureTgcharacteristic value of the temperature range over which the glass transition takes placeNote 1 to entry: The assigned glass transition temperature (Tg) may vary, depending on the specific property and on the method
35、and conditions selected to measure it.3.3glass transition step heightcp(Tg)difference in specific heat capacity at TgNote 1 to entry: See Figure 1 and Figure 2.Note 2 to entry: For partially crystalline polymers, the glass transition step height is proportional to the amorphous content. ISO 2013 All
36、 rights reserved 1BS EN ISO 11357-2:2014Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or networking permitted without license from IHS-,-,-4 PrincipleThe principle is specified in ISO 11357-1.The change in heat flow r
37、ate as a function of temperature is measured and the glass transition temperature and step height are determined from the curve thus obtained.5 Apparatus and materialsThe apparatus and materials are specified in ISO 11357-1.6 Test specimensThe test specimens are specified in ISO 11357-1.7 Test condi
38、tions and specimen conditioningThe test conditions and specimen conditioning are specified in ISO 11357-1.8 CalibrationThe calibration is specified in ISO 11357-1.9 Procedure9.1 Setting up the apparatusThe procedure for setting up the apparatus is specified in ISO 11357-1.9.2 Loading the test specim
39、en into the crucibleThe procedure for loading the test specimen into the crucible is specified in ISO 11357-1.Determine the mass of the test specimen to the nearest 0,1 mg. Unless otherwise specified in the materials standard, use a mass of between 5 mg and 20 mg. For partially crystalline materials
40、, use a mass near the higher limit.9.3 Insertion of cruciblesThe procedure for inserting the crucibles is specified in ISO 11357-1.9.4 Temperature scan9.4.1 Allow 5 min for nitrogen pre-purge prior to beginning the heating cycle.9.4.2 Perform and record a preliminary thermal cycle at a temperature s
41、can rate of 20 K/min, heating the cell to a temperature high enough to erase the test materials previous thermal history.DSC measurements on polymers are greatly affected by the thermal history and morphology of the sample and the test specimen. A first heating scan shall be performed using the test
42、 specimen as received and measurements shall be taken preferably from the second heating scan (see ISO 11357-1). In cases where the material 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 scan. This de
43、viation from the standard procedure shall be recorded in the test report (see Clause 12).ISO 11357-2:2013(E) 2 ISO 2013 All rights reservedBS EN ISO 11357-2:2014Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Not for ResaleNo reproduction or network
44、ing permitted without license from IHS-,-,-ISO 11357-2:2013(E)9.4.3 Hold the temperature for 5 min unless a shorter time is required due to sample decomposition.9.4.4 Cool down to approximately 50 C below the anticipated glass transition temperature using a temperature scan rate of 20 K/min.NOTE In
45、particular cases, e.g. if cold crystallization is to be measured, quench cooling might have to be used.9.4.5 Hold the temperature for 5 min.9.4.6 Perform and record a second heating cycle at a temperature scan rate of 20 K/min, heating to approximately 30 C higher than the extrapolated end temperatu
46、re (Tef,g).NOTE Other heating or cooling rates can be used by agreement between the interested parties. Preferably, the same scan rates are intended to be used for heating and cooling cycles. In particular, high scanning rates result in better sensitivity of the recorded transition. On the other han
47、d, low scanning rates provide better resolution. Appropriate selection of rate is important to the observation of subtle transitions.9.4.7 Bring the apparatus to ambient temperature and remove the crucible to determine if deformation of the crucible or specimen overflow has occurred.9.4.8 Reweigh th
48、e crucible with the test specimen to within 0,1 mg.9.4.9 If any loss of mass has occurred, a chemical change should be suspected. Open the crucible and inspect the test specimen. If the specimen has degraded, discard the test results and retest, selecting a lower maximum temperature.Do not reuse cru
49、cibles showing signs of deterioration for another measurement.If the test specimen overflows during measurement, clean the specimen holder assembly, following the instrument manufacturers instructions, and verify that the calibration is still valid.9.4.10 Requirements for repeat testing shall be indicated by the refe
