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 heightBS EN ISO 11357-2:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation
2、 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 It supersedes BS ISO 11357-2:2013,which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee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
3、 its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible 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 Standa
4、rd cannot confer immunity from legal obligations.This British Standard was published under the authority of the StandardsPolicy 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
5、 ISO 11357-2:2014EUROPEAN 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 glass transition step height (ISO 11357-2:2013) Plastiques - Analy
6、se 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: Bestimmung der Glasbergangstemperatur und Glasbergangsstufenhhe (
7、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 national standard without any alteration. Up-to-date lists and bibl
8、iographical 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 version in any other language made by translation under the respon
9、sibility 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, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Repu
10、blic 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. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMA
11、LISATION 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 11357-2:2014 EEN ISO 11357-2:2014 (E)3Foreword The text of ISO 11357-
12、2:2013 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 11357-2:2014 by Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given
13、the status of a national standard, either by publication 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 ma
14、y 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 organizations of the following countries are bound to implement this European Standard: Austria
15、, 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, Sweden,
16、Switzerland, Turkey and the United Kingdom. Endorsement 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 Int
17、ernational 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 publication of an identicaltext or
18、by endorsement, at the latest by September 2014, and conflicting 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
19、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, Denmark, Estonia, Finland, Form
20、er 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.Endorsement noticeThe text of ISO 11357-2:20
21、13 has been approved by CEN as EN ISO 11357-2:2014 without any modification.BS EN ISO 11357-2:2014BS ISO 11357-2:2013ISO 11357-2:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions. 14 Principle 25 Apparatus and materials 26 Test
22、 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 Insertion of crucibles. 29.4 Temperature scan. 210 Expression of results 310.1 Determination of glass transition temperatures . 31
23、0.2 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 iiiContents PageForeword iv1 Scope . 12 Normative references 3 Terms and definitions .4 Principle 25 Apparatus and materials6 Test spe
24、cimens7 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 crucibles . 29.4 Temperature scan . 210 Expression of results 310.1 Determination of glass transition temperatures . 310.2 Deter
25、mination of glass transition step height 511 Precision .12 Test report .Bibliography 6BS EN ISO 11357-2:2014This page deliberately left blankINTERNATIONAL STANDARD ISO 11357-2:2013(E)Plastics Differential scanning calorimetry (DSC) Part 2: Determination of glass transition temperature and glass tran
26、sition step heightWARNING 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 ap
27、propriate health and safety practices and to determine the applicability of regulatory limitations prior to 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 cry
28、stalline plastics.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 the referenced document (in
29、cluding any amendments) applies.ISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General 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 amorphou
30、s polymer or in amorphous regions of a partially crystalline polymer from (or to) a viscous or rubbery condition 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: Th
31、e assigned glass transition temperature (Tg) may vary, depending on the specific property and on the method 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 c
32、rystalline polymers, the glass transition step height is proportional to the amorphous content. ISO 2013 All rights reserved 1BS EN ISO 11357-2:20144 PrincipleThe principle is specified in ISO 11357-1.The change in heat flow rate as a function of temperature is measured and the glass transition temp
33、erature 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 conditions and specimen conditioningThe test conditions and specimen conditioni
34、ng 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 specimen into the crucibleThe procedure for loading the test specimen into the c
35、rucible 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, use a mass near the higher limit.9.3 Insertion of cruciblesThe procedure
36、 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 scan rate of 20 K/min, heating the cell to a temperature high enough to era
37、se 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 specimen as received and measurements shall be taken preferably from the
38、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 deviation from the standard procedure shall be recorded in the test report (
39、see Clause 12).ISO 11357-2:2013(E) 2 ISO 2013 All rights reservedBS EN ISO 11357-2:2014ISO 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
40、a temperature scan rate of 20 K/min.NOTE In 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
41、C higher than the extrapolated end temperature (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
42、of the recorded transition. On the other hand, 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 spe
43、cimen overflow has occurred.9.4.8 Reweigh the 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
44、a lower maximum temperature.Do not reuse crucibles 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
45、Requirements for repeat testing shall be indicated by the referring standards or, if none, agreed between interested parties.10 Expression of results10.1 Determination of glass transition temperatures10.1.1 GeneralDetermine the glass transition temperature using one of the methods given in 10.1.2 to
46、 10.1.4.The type of determination of Tgshall be included in the test report (see Clause 12).10.1.2 Half-step-height methodAssign the glass transition to the temperature, T1/2,g, at which the measured DSC curve is intersected by a line that is equidistant between the two extrapolated baselines (see F
47、igure 1).10.1.3 Inflection-point methodAssign the glass transition to the temperature of inflection point, Ti,g, of the measured DSC curve in the glass transition region (see Figure 1).The point of inflection, Ti,g, is obtained either by determining the temperature of the maximum in the derivative D
48、SC signal or the temperature of the steepest slope in the transition zone. ISO 2013 All rights reserved 3BS EN ISO 11357-2:2014KeydQ/dt heat flow rate T1/2,gTgmeasured by half-step-height method (10.1.2)T temperature Ti,gTgmeasured by inflection-point method (10.1.3)(dQ/dt)1heat flow rate below TgTe
49、i,gextrapolated onset temperature of glass transition(dQ/dt)2heat flow rate above TgTef,gextrapolated end temperature of glass transitionaEndothermic direction.Figure 1 Examples of characteristic glass transition temperature determinations according to 10.1.2 and 10.1.310.1.4 Equal-areas methodAssign the glass transition to the temperature, Ta,g, obtained by drawing a vertical line such that the areas between DSC trace and baselines below and above the curve are equal, i.e. 1 + 3 = 2 (see Figure 2).9NOTE As the glass transition is a kine
