1、BS EN ISO11357-1:2009ICS 83.080.01NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Differentialscanning calorimetry(DSC)Part 1: General principles (ISO11357-1:2009)Copyright European Committee for Standardization Provided by IHS under license with CENNot
2、 for ResaleNo reproduction or networking permitted without license from IHS-,-,-This British Standardwas published underthe authority of theStandards Policy andStrategy Committee on 30November 2009 BSI 2009ISBN 978 0 580 63088 0Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 113
3、57-1:2009National forewordThis British Standard is the UK implementation of EN ISO11357-1:2009. It supersedes BS EN ISO 11357-1:1997 which iswithdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this c
4、ommittee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.Copyright European Committee f
5、or Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11357-1 October 2009 ICS 83.080.01 Supersedes EN ISO 11357-1:1997English Version Plastics - Differentia
6、l scanning calorimetry (DSC) - Part 1: General principles (ISO 11357-1:2009) Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 1: Principes gnraux (ISO 11357-1:2009) Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 1: Allgemeine Grundlagen (ISO 11357-1:2009) This European
7、Standard was approved by CEN on 17 September 2009. 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 bibliographical references conc
8、erning such national standards may be obtained on application to the CEN 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 responsibility of a CEN member into its o
9、wn language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithu
10、ania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 C
11、EN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11357-1:2009: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS
12、-,-,-BS EN ISO 11357-1:2009EN ISO 11357-1:2009 (E) 3 Foreword This document (EN ISO 11357-1:2009) 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 by NBN. This European Standard shall be gi
13、ven the status of a national standard, either by publication of an identical text or by endorsement, at the latest by April 2010, and conflicting national standards shall be withdrawn at the latest by April 2010. Attention is drawn to the possibility that some of the elements of this document may be
14、 the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 11357-1:1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to
15、 implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switze
16、rland and the United Kingdom. Endorsement notice The text of ISO 11357-1:2009 has been approved by CEN as a EN ISO 11357-1:2009 without any modification. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted witho
17、ut license from IHS-,-,-BS EN ISO 11357-1:2009ISO 11357-1:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Normative references1 3 Terms and definitions .2 4 Basic principles .8 4.1 General .8 4.2 Heat-flux DSC.8 4.3 Power-compensation DSC8 5 Apparatus and
18、materials.9 6 Specimen10 7 Test conditions and specimen conditioning 11 7.1 Test conditions 11 7.2 Conditioning of specimens 11 8 Calibration11 8.1 General .11 8.2 Calibration materials .12 8.3 Temperature calibration12 8.4 Heat calibration14 8.5 Heat flow rate calibration15 9 Procedure.17 9.1 Setti
19、ng up the apparatus 17 9.2 Loading the specimen into the crucible17 9.3 Insertion of crucibles into the instrument 18 9.4 Performing measurements.18 9.5 Post-run checks.20 10 Test report21 Annex A (normative) Extended, high-precision, temperature calibration11.22 Annex B (normative) Extended, high-p
20、recision, heat calibration24 Annex C (informative) Recommended calibration materials26 Annex D (informative) Interaction of calibration materials with different crucible materials .29 Annex E (informative) General recommendations.30 Bibliography31 Copyright European Committee for Standardization Pro
21、vided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-1:2009ISO 11357-1:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national stand
22、ards bodies (ISO member bodies). The 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 orga
23、nizations, governmental and non-governmental, 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. International Standards are drafted in accordance with the rules given
24、in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75
25、% 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. ISO shall not be held responsible for identifying any or all such patent rights. ISO 11357-1 was prepared by Technical Committee ISO/TC 61, Pla
26、stics, Subcommittee SC 5, Physical-chemical properties. This second edition cancels and replaces the first edition (ISO 11357-1:1997), which has been technically revised. The most important changes are the following: an indication has been given of the preferred graphical representation of DSC diagr
27、ams in accordance with thermodynamic requirements; an additional, more precise, method of temperature calibration, providing an accuracy of 0,3 K over an extended temperature range, has been included; an additional, more precise, procedure for enthalpy calibration, providing an accuracy of 0,5 %, ha
28、s been included; a procedure for heat flow rate calibration has been included; information has been included on interactions between calibration materials and the crucibles. ISO 11357 consists of the following parts, under the general title Plastics Differential scanning calorimetry (DSC): Part 1: G
29、eneral principles Part 2: Determination of glass transition temperature 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
30、 and degree of conversion Part 6: Determination of oxidation induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT) Part 7: Determination of crystallization kinetics Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo rep
31、roduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-1:2009ISO 11357-1:2009(E) ISO 2009 All rights reserved vIntroduction ISO 11357 describes thermoanalytical DSC test methods which can be used for quality assurance purposes, for routine checks of raw materials and finished
32、 products or for the determination of comparable data needed for data sheets or databases. The procedures given in ISO 11357 apply as long as product standards or standards describing special atmospheres for conditioning of specimens do not specify otherwise. Copyright European Committee for Standar
33、dization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-1:2009Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without
34、 license from IHS-,-,-BS EN ISO 11357-1:2009INTERNATIONAL STANDARD ISO 11357-1:2009(E) ISO 2009 All rights reserved 1Plastics Differential scanning calorimetry (DSC) Part 1: General principles SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applica
35、ble. This document does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory requirements. 1 Scope ISO 11357 specifies several differe
36、ntial scanning calorimetry (DSC) methods for the thermal analysis of polymers and polymer blends, such as thermoplastics (polymers, moulding compounds and other moulding materials, with or without fillers, fibres or reinforcements); thermosets (uncured or cured materials, with or without fillers, fi
37、bres or reinforcements); elastomers (with or without fillers, fibres or reinforcements). ISO 11357 is intended for the observation and measurement of various properties of, and phenomena associated with, the above-mentioned materials, such as physical transitions (glass transition, phase transitions
38、 such as melting and crystallization, polymorphic transitions, etc.); chemical reactions (polymerization, crosslinking and curing of elastomers and thermosets, etc.); the stability to oxidation; the heat capacity. This part of ISO 11357 specifies a number of general aspects of differential scanning
39、calorimetry, such as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report common to all following parts. Details on performing specific methods are given in subsequent parts of ISO 11357 (see Foreword). 2 Normative references The following refer
40、enced 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 291, Plastics Standard atmospheres for conditioning and testing
41、Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 11357-1:2009ISO 11357-1:2009(E) 2 ISO 2009 All rights reservedISO 472, Plastics Vocabulary ISO 80000-5, Quantities and u
42、nits Part 5: Thermodynamics 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 472 and ISO 80000-5 and the following apply. 3.1 differential scanning calorimetry DSC technique in which the difference between the rate of flow of heat into a specimen cruc
43、ible containing the specimen and that into a reference crucible is derived as a function of temperature and/or time while the specimen and reference are subjected to the same controlled temperature programme in a specified atmosphere using a symmetrical measurement system NOTE 1 It is common practic
44、e to record, for each measurement run, a curve in which temperature or time is plotted as the abscissa and heat flow rate difference as the ordinate. The endothermic and/or exothermic direction is indicated on the DSC curve. NOTE 2 According to the principles of thermodynamics, energy absorbed by a
45、system is considered positive while energy released is negative. This approach implies that the endothermic direction points upwards in the ordinate and the exothermic direction downwards (see Figures 1 and 2). It also has the advantage that the direction of thermal effects in plots of heat flow rat
46、e and specific heat are consistent. 3.2 calibration material material for which one or more of the thermal properties are sufficiently homogeneous and well established to be used for the calibration of a DSC instrument or for the assessment of a measurement method 3.3 reference crucible crucible use
47、d on the reference side of the symmetrical crucible holder assembly NOTE 1 Normally the reference crucible is empty. NOTE 2 In special cases, such as the measurement of highly filled or reinforced polymers or specimens having a heat capacity comparable to that of the crucible, a suitable material ca
48、n be used inside the reference crucible. This reference material should be thermally inactive over the temperature and time range of interest and its heat capacity should be similar to that of the specimen. In the case of filled or reinforced products, the pure filler or reinforcement can be used, for example. 3.4 heat flow rate quantity of heat transferred per unit time (dQ/dt), expressed in watts (W) or milliwatts (mW) NOTE The total quantity of heat transferred, Q, corresponds to the time integral of the heat flow rate: dddQQtt=(1) Cop
