BS EN ISO 11358-1-2014 Plastics Thermogravimetry (TG) of polymers General principles《塑料 聚合物的热重分析法(TG) 一般原理》.pdf

1、BSI Standards PublicationBS EN ISO 11358-1:2014Plastics Thermogravimetry(TG) of polymersPart 1: General principlesBS EN ISO 11358-1:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO11358-1:2014. It supersedes BS EN ISO 11358:1997 which iswithdrawn.The UK

2、participation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsi

3、ble for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 77735 6ICS 83.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Pol

4、icy and Strategy Committee on 31 July 2014.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11358-1 July 2014 ICS 83.080.01 Supersedes EN ISO 11358:1997English Version Plastics - Thermogravimetry (TG) of polymers - Part 1: General principl

5、es (ISO 11358-1:2014) Plastiques - Thermogravimtrie (TG) des polymres - Partie 1: Principes gnraux (ISO 11358-1:2014) Kunststoffe - Thermogravimetrie (TG) von Polymeren - Teil 1: Allgemeine Grundstze (ISO 11358-1:2014) This European Standard was approved by CEN on 28 June 2014. CEN members are bound

6、 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 concerning such national standards may be obtained on application to the CEN

7、-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 responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre ha

8、s 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 Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Lu

9、xembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Bru

10、ssels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11358-1:2014 EBS EN ISO 11358-1:2014EN ISO 11358-1:2014 (E) 3 Foreword This document (EN ISO 11358-1:2014) has been prepared by Technical Committee ISO/TC 61 “Plastics”

11、 in collaboration with 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 identical text or by endorsement, at the latest by January 2015, and conflicting national sta

12、ndards shall be withdrawn at the latest by January 2015. 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. This document supersedes EN I

13、SO 11358:1997. 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, Former Yugoslav Republic of Macedon

14、ia, 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 notice The text of ISO 11358-1:2014 has been approved by CEN

15、 as EN ISO 11358-1:2014 without any modification. BS EN ISO 11358-1:2014ISO 11358-1:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Apparatus . 26 Test specimen preparation 26.1 General . 26.2 Test specimens

16、 from finished products . 36.3 Test specimen conditioning . 36.4 Test specimen mass 37 Calibration 37.1 Mass calibration . 37.2 Temperature calibration . 38 Procedure. 48.1 General . 48.2 Temperature scanning mode 48.3 Isothermal mode . 59 Expression of results 59.1 Graphical representation . 59.2 D

17、etermination of increase in mass 59.3 Determination of loss in mass . 610 Test report . 8BS EN ISO 11358-1:2014ISO 11358-1:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Interna

18、tional 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 organizations, governmental and non-governmental, in liaison with

19、ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, P

20、art 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the

21、 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. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations re

22、ceived (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs a

23、dherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical chemical properties.This first edition of ISO 11358-1 cancels and replace

24、s ISO 11358:1997, which has been technically revised.The main changes are:a) addition of ISO 472 to the Normative references clause and removal of definitions specified therein;b) revision of apparatus specifications.ISO 11358 consists of the following parts, under the general title Plastics Thermog

25、ravimetry (TG) of polymers: Part 1: General principles Part 2: Determination of activation energy Part 3: Determination of the activation energy using the Ozawa-Friedman plot and analysis of the reaction kineticsiv ISO 2014 All rights reservedBS EN ISO 11358-1:2014INTERNATIONAL STANDARD ISO 11358-1:

26、2014(E)Plastics Thermogravimetry (TG) of polymers Part 1: General principles1 ScopeThis part of ISO 11358 specifies general conditions for the analysis of polymers using thermogravimetric techniques. It is applicable to liquids or solids. Solid materials may be in the form of pellets, granules or po

27、wders. Fabricated shapes reduced to appropriate specimen size may also be analysed by this method.Thermogravimetry can be used to determine the temperature(s) and rate(s) of decomposition of polymers, and to measure at the same time the amounts of volatile matter, additives and/or fillers they conta

28、in.The thermogravimetric measurements may be carried out in dynamic mode (mass change versus temperature or time under programmed conditions) or isothermal mode (mass change versus time at constant temperature).Thermogravimetric measurements may also be carried out using different testing atmosphere

29、s, e.g. to separate decomposition in an inert atmosphere from oxidative degradation.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 und

30、ated references, the latest edition of the referenced document (including any amendments) applies.ISO 291, Plastics Standard atmospheres for conditioning and testingISO 472, Plastics VocabularyISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principles3 Terms and definit

31、ionsFor the purposes of this document, the terms and definitions given in ISO 472 and the following apply.3.1dynamic mass-change determinationtechnique for recording the variation of the mass of a test specimen with temperature T which is changing at a programmed rate3.2isothermal mass-change determ

32、inationtechnique for recording the variation of the mass of a test specimen with time t at constant temperature T3.3Curie temperaturetemperature at which a ferromagnetic material passes from the ferromagnetic state to the paramagnetic state or vice versa ISO 2014 All rights reserved 1BS EN ISO 11358

33、-1:2014ISO 11358-1:2014(E)4 PrincipleA test specimen is heated at specified rates with a controlled temperature programme, and the change in mass is measured as a function of temperature. Alternatively, the specimen is kept at a given constant temperature and the change in mass is measured as a func

34、tion of time over a given period.During measurement the test specimen is held in a controlled inert or oxidising atmosphere.In general, the reactions which cause the mass of a test specimen to change are decomposition or oxidation reactions or the volatilisation of a component. The change in mass is

35、 recorded as a thermogravimetric (TG) curve.The change in mass of a material as a function of temperature and the extent of this change are indicators of the thermal stability of the material. TG data can therefore be used to evaluate the relative thermal stability of polymers of the same generic fa

36、mily and polymer-polymer or polymer-additive interactions, using measurements made under the same test conditions.NOTE TG data may be used for process control, process development and material evaluation. Long-term thermal stability is a complex function of service and environmental conditions. TG d

37、ata alone may not be able to describe the long-term thermal stability of a polymer.5 ApparatusA number of commercial instruments suitable for thermogravimetric measurements are available. The basic apparatus consists of the following.5.1 Thermobalance, meeting the following requirements: capability

38、to generate constant heating and cooling rates suitable for intended measurements; capability to maintain the test temperature constant (to within 0,3 K or less for the duration of measurement); capability to maintain a constant purge gas flow rate controllable to within 10 % over a range of flow ra

39、tes (e.g. 10 ml/min to 150 ml/min); temperature and mass range in line with experimental requirements; recording device capable of automatically recording the measured curve of mass versus temperature and time; measurement of temperature signals with an accuracy of 2 K or better; measurement of time

40、 with an accuracy of 1 s or better; measurement of mass with an accuracy of 20 g or better.5.2 Purge gas, dry air or oxygen (oxidizing conditions) or a suitable inert gas with an oxygen content of 0,001 % by volume or less (non-oxidizing conditions). In either case, the water content of the purge ga

41、s shall be less than 0,001 % by mass.6 Test specimen preparation6.1 GeneralTest specimens may be liquids or solids. Solids may be in the form of powders, pellets, granules or cut pieces. For finished products, the test specimen shall be in the form normally found in use.2 ISO 2014 All rights reserve

42、dBS EN ISO 11358-1:2014ISO 11358-1:2014(E)6.2 Test specimens from finished productsCut the test specimen to appropriate size for the specimen holder. Microtomes or razor blades are suitable for this purpose.NOTE Test specimen size and shape are generally dependent on the sample holder. Surface area

43、affects the overall results. For instance, in comparing a test specimen of large surface area with a test specimen of smaller surface area, both having the same mass, the smaller surface area test specimen normally changes at a slower rate.6.3 Test specimen conditioningUnless otherwise specified in

44、a material specification or product standard, test specimens shall be conditioned, prior to measurement, at one of the standard atmospheres specified in ISO 291, or by any other method specified by agreement between the interested parties.6.4 Test specimen massPreferably, the mass of the test specim

45、en shall be in the range of 10 mg to 100 mg.7 Calibration7.1 Mass calibrationWithout any gas flow through the thermobalance (to prevent any disturbance through buoyancy and/or convection effects), calibrate the thermobalance as follows, using calibrated masses in the range of 10 mg to 100 mg:Record

46、the temperature at which the mass calibration was carried out.Zero the thermobalance. Place the calibration weight on the thermobalance and measure the corresponding mass change. If necessary, adjust the thermobalance so that the measured mass is equal to the calibration mass.If mass calibration is

47、done by procedures included in the instrument control software or by external service providers a valid calibration certificate may be acceptable to demonstrate adequate mass calibration.7.2 Temperature calibrationCarry out the temperature calibration using the same atmosphere, rate of gas flow and

48、heating rate as shall be used in the procedure specified in Clause 8.If the thermobalance is not coupled with another thermoanalytical method, use the following procedure.a) Choose two or more calibration materials with a Curie temperature near the temperature range to be examined. If possible, choo

49、se the calibration materials in such a way that the temperature range to be examined lies between the Curie temperatures of two of them.b) Start heating at the same heating rate as will be used in the procedure specified in Clause 8 and carry out a calibration based on the start temperature TA, mid-point temperature TCand end temperature TBfor the Curie temperature transition.NOTE 1 The Curie point is the temperature at which a ferromagnetic material becomes paramagnetic on heating. The effect is reversible. Applying a magnetic fie