DIN EN ISO 11357-2-2014 Plastics - Differential scanning calorimetry (DSC) - Part 2 Determination of glass transition temperature and glass transition step height (ISO 11357-2 2013.pdf

1、July 2014Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 17.

2、200.10; 83.080.01!%2q“2159578www.din.deDDIN EN ISO 11357-2Plastics Differential scanning calorimetry (DSC) Part 2: Determination of glass transition temperature and glasstransition step height (ISO 11357-2:2013),English version EN ISO 11357-2:2014,English translation of DIN EN ISO 11357-2:2014-07Kun

3、ststoffe Dynamische Differenz-Thermoanalyse (DSC) Teil 2: Bestimmung der Glasbergangstemperatur und der Glasbergangsstufenhhe(ISO 11357-2:2013),Englische Fassung EN ISO 11357-2:2014,Englische bersetzung von DIN EN ISO 11357-2:2014-07Plastiques Analyse calorimtrique diffrentielle (DSC) Partie 2: Dter

4、mination de la temprature de transition vitreuse et de la hauteur de palierde transition vitreuse (ISO 11357-2:2013),Version anglaise EN ISO 11357-2:2014,Traduction anglaise de DIN EN ISO 11357-2:2014-07www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Docu

5、ment comprises 11 pages06.14 DIN EN ISO 11357-2:2014-07 2 A comma is used as the decimal marker. National foreword The text of ISO 11357-2:2013 has been prepared by Technical Committee ISO/TC 61 “Plastics” (Secretariat: SAC, China) and has been taken over as EN ISO 11357-2:2014 by Technical Committe

6、e CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-01-03 AA Physikalische, rheologische und analytische Prfungen. DIN EN ISO 11357 consists of the fo

7、llowing parts, under the general title Plastics Differential scanning calorimetry (DSC): Part 1: General principles Part 2: Determination of glass transition temperature and glass transition step height Part 3: Determination of temperature and enthalpy of melting and crystallization Part 4: Determin

8、ation 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 (dynamic OIT) Part 7: Determination of c

9、rystallization kinetics The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 291 DIN EN ISO 291 ISO 472 DIN EN ISO 472 ISO 11357-1 DIN EN ISO 11357-1 National Annex NA (informative) Bibliography DIN EN ISO 291, Plastics Standard atmospheres

10、for conditioning and testing DIN EN ISO 472, Plastics Vocabulary DIN EN ISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principles EN ISO 11357-2 March 2014 ICS 83.080.01 English Version Plastics - Differential scanning calorimetry (DSC) - Part 2: Determination of glass

11、 transition temperature and glass 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-

12、Thermoanalyse (DSC) -Teil 2: Bestimmung 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 Europea

13、n 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 official versions (

14、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 of Austria, Belgi

15、um, 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, Switzer

16、land, Turkey and United Kingdom. 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 EEUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALI

17、SATIONEUROPISCHES KOMITEE FR NORMUNGEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMContents Page Foreword . 3 1 Scope . 4 2 Normative references. 4 3 Terms and definitions 4 4 Principle 5 5 Apparatus and materials . 5 6 Test specimens 5 7 Test conditions and specimen conditioning . 5 8 Calibration .

18、 5 9 Procedure 5 9.1 Setting up the apparatus . 5 9.2 Loading the test specimen into the crucible . 5 9.3 Insertion of crucibles . 5 9.4 Temperature scan 5 10 Expression of results . 6 10.1 Determination of glass transition temperatures . 6 10.2 Determination of glass transition step height . 8 11 T

19、est report . 8 Bibliography 9 2DIN EN ISO 11357-2:2014-07 EN ISO 11357-2:2014 (E) Foreword The text of ISO 11357-2:2013 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 Technica

20、l 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 September 2014, and conflicting national standards shall be withdrawn at

21、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 shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the n

22、ational 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, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

23、Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, 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. 3DIN EN ISO 11357-2:2

24、014-07EN ISO 11357-2:2014 (E)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 e

25、stablish appropriate 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 pa

26、rtially crystalline 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 d

27、ocument (including 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

28、an amorphous 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 t

29、o entry: The 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

30、partially crystalline polymers, the glass transition step height is proportional to the amorphous content.4DIN EN ISO 11357-2:2014-07 EN ISO 11357-2:2014 (E) 4 PrincipleThe principle is specified in ISO 11357-1.The change in heat flow rate as a function of temperature is measured and the glass trans

31、ition 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 conditions and specimen conditioningThe test conditions and specimen

32、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 specimen into the crucibleThe procedure for loading the test specimen

33、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, use a mass near the higher limit.9.3 Insertion of cruciblesThe

34、 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 scan rate of 20 K/min, heating the cell to a temperature high eno

35、ugh 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 specimen as received and measurements shall be taken preferably

36、 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 deviation from the standard procedure shall be recorded in the tes

37、t report (see Clause 12).5DIN EN ISO 11357-2:2014-07EN ISO 11357-2:2014 (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

38、/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 C higher than the extrapolated

39、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 of the recorded transition. On

40、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 specimen overflow has occurred.9.4

41、.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 a lower maximum temperature.Do

42、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 Requirements for repeat testing

43、 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 10.1.4.The type of determinati

44、on 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 Figure 1).10.1.3 Inflection-poin

45、t 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 DSC signal or the temperature of

46、 the steepest slope in the transition zone.6DIN EN ISO 11357-2:2014-07 EN ISO 11357-2:2014 (E) KeydQ/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 TgTei,gextrapolated onset temperatur

47、e 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 te

48、mperature, 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 kinetic phenomenon, the glass transition temperature depends on the actual used cooling rate

49、and annealing conditions below Tg. Unperturbed glass transitions are obtained only if cooling and subsequent heating rate are the same and no significant physical ageing occurred due to annealing below Tg. If a sample is cooled significantly slower or annealed below Tg, enthalpy relaxations can occur resulting in endotherm peaks just above Tg. Peaks due to enthalpy relaxation will disappear by extrapolating to zero heating rates. The equal