EN ISO 11357-6-2018 Plastics - Differential scanning calorimetry (DSC) - Part 6 Determination of oxidation induction time (isothermal OIT) and oxidation inducti.pdf

1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Plastics Differential scanning calorimetry (DSC)Part 6: Determination of oxidation induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT) (ISO 11357-6:2018)BS EN ISO 11357-6:2018National forew

2、ordThis British Standard is the UK implementation of EN ISO 11357-6:2018. It is identical to ISO 11357-6:2018. It supersedes BS EN ISO 11357-6:2013, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations rep

3、resented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0

4、580 96207 3ICS 83.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STA

5、NDARDBS EN ISO 11357-6:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 11357-6April 2018ICS 83.080.01 Supersedes EN ISO 11357-6:2013EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brus

6、sels 2018 CEN Ref. No. EN ISO 11357-6:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersPlastics - Differential scanning calorimetry (DSC) - Part 6: Determination of oxidation induction time (isothermal OIT) and oxidation induction temperature

7、dynamic OIT) (ISO 11357-6:2018)Plastiques - Analyse calorimtrique diffrentielle (DSC) - Partie 6: Dtermination du temps dinduction loxydation (OIT isotherme) et de la temprature dinduction loxydation (OIT dynamique) (ISO 11357-6:2018)Kunststoffe - Dynamische Differenz-Thermoanalyse (DSC) - Teil 6:

8、Bestimmung der Oxidations-Induktionszeit (isothermische OIT) und Oxidations-Induktionstemperatur (dynamische OIT) (ISO 11357-6:2018)This European Standard was approved by CEN on 24 February 2018.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions

9、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-CENELEC Management Centre or to any CEN member.This European Standard exists in thr

10、ee 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 has the same status as the official versions.CEN members are the national standards bod

11、ies 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, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slo

12、venia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English VersionEN ISO 11357-6:2018 (E)European forewordThis document (EN ISO 11357-6:2018) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of whi

13、ch 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 October 2018, and conflicting national standards shall be withdrawn at the latest by October 2018.Attention is drawn to the possib

14、ility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights.This document supersedes EN ISO 11357-6:2013.According to the CEN-CENELEC Internal Regulations, the national standards organizations o

15、f 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, Lithuania, Luxembourg, Malta, Net

16、herlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.Endorsement noticeThe text of ISO 11357-6:2018 has been approved by CEN as EN ISO 11357-6:2018 without any modification.2BS EN ISO 11357-6:2018ISO 11357-6:2018Foreword i

17、vIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 24.1 General . 24.2 Oxidation induction time (isothermal OIT) . 24.3 Oxidation induction temperature (dynamic OIT) . 25 Apparatus and materials 35.1 General . 35.2 DSC instrument . 35.3 Crucibles . 35.4 Flowmete

18、r . 35.5 Oxygen 35.6 Air 35.7 Nitrogen 35.8 Gas-selector switch and regulators . 36 Test specimens 46.1 General . 46.2 Specimens from compression-moulded plates . 46.3 Specimens from injection-moulded plates or melt flow extrudates 46.4 Specimens from finished parts . 47 Test conditions and specimen

19、 conditioning 58 Calibration 58.1 Oxidation induction time (isothermal OIT) . 58.2 Oxidation induction temperature (dynamic OIT) . 59 Procedure. 59.1 Setting up the instrument 59.2 Loading the test specimen into the crucible 59.3 Insertion of crucibles . 59.4 Nitrogen, air and oxygen flow 59.5 Sensi

20、tivity adjustment 69.6 Performance of measurement . 69.6.1 Oxidation induction time (isothermal OIT) 69.6.2 Oxidation induction temperature (dynamic OIT) . 79.7 Cleaning . 710 Expression of results 811 Precision and bias 1012 Test report 10Bibliography .12 ISO 2018 All rights reserved iiiContents Pa

21、geBS EN ISO 11357-6:2018ISO 11357-6:2018ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member bod

22、y 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 ISO, also take part in the work. ISO collaborates closely with the International Electrote

23、chnical 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, Part 1. In particular the different approval criteria needed for the different types of IS

24、O 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 elements of this document may be the subject of patent rights. ISO shall not be held res

25、ponsible 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 received (see www.iso.org/patents).Any trade name used in this document is information give

26、n for the convenience of users and does not constitute an endorsement. For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) princi

27、ples in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties.This third edition cancels and replaces the second edition (ISO 11357-6:2008), whi

28、ch has been technically revised. The main changes compared to the previous edition are as follows: the normative references in Clause 2 have been updated; techniques for purge gas flow control have been extended.A list of all parts in the ISO 11357 series can be found on the ISO website.iv ISO 2018

29、All rights reservedBS EN ISO 11357-6:2018ISO 11357-6:2018IntroductionThe measurement of oxidation induction time or temperature described in this document provides a tool to assess the conformity of the material tested to a given formulation of plastics compounds, but it is not intended to provide t

30、he concentration of antioxidant. Different antioxidants can have different oxidation induction times or temperatures. Due to interaction of the antioxidant with other substances in the formulation, different oxidation induction times or temperatures can result even with products having the same type

31、 and concentration of antioxidant. ISO 2018 All rights reserved vBS EN ISO 11357-6:2018This page deliberately left blankPlastics Differential scanning calorimetry (DSC) Part 6: Determination of oxidation induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT) (ISO 11357-6:2

32、018)1 ScopeThis document specifies methods for the determination of oxidation induction time (isothermal OIT) and oxidation induction temperature (dynamic OIT) of polymeric materials by means of differential scanning calorimetry (DSC). It is applicable to polyolefin resins that are in a fully stabil

33、ized or compounded form, either as raw materials or finished products. It can be applicable to other plastics.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, onl

34、y the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 293, Plastics Compression moulding of test specimens of thermoplastic materialsISO 294-3, Plastics Injection moulding of test specimens of thermoplastic materials

35、 Part 3: Small platesISO 472, Plastics VocabularyISO 8986-2, Plastics Polybutene-1 (PB-1) moulding and extrusion materials Part 2: Preparation of test specimens and determination of propertiesISO 11357-1, Plastics Differential scanning calorimetry (DSC) Part 1: General principlesISO 17855-2, Plastic

36、s Polyethylene (PE) moulding and extrusion materials Part 2: Preparation of test specimens and determination of propertiesISO 19069-2, Plastics Polypropylene (PP) moulding and extrusion materials Part 2: Preparation of test specimens and determination of properties3 Terms and definitionsFor the purp

37、oses of this document, the terms and definitions given in ISO 472 and ISO 11357-1 and the following apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at http:/www.electropedia.org/ ISO Online browsing platform: avai

38、lable at https:/www.iso.org/obpINTERNATIONAL STANDARD ISO 11357-6:2018 ISO 2018 All rights reserved 1BS EN ISO 11357-6:2018ISO 11357-6:20183.1oxidation induction timeisothermal OITrelative measure of a stabilized materials resistance to oxidative decomposition, determined by the calorimetric measure

39、ment of the time interval to the onset of exothermic oxidation of the material at a specified temperature in an oxygen or air atmosphere, under atmospheric pressureNote 1 to entry: It is expressed in minutes (min).3.2oxidation induction temperaturedynamic OITrelative measure of a stabilized material

40、s resistance to oxidative decomposition, determined by the calorimetric measurement of the temperature of the onset of exothermic oxidation of the material when subjected to a specified heating rate in an oxygen or air atmosphere, under atmospheric pressureNote 1 to entry: It is expressed in degrees

41、 Celsius (C).Note 2 to entry: The oxidation induction temperature is also called oxidation onset temperature (OOT).4 Principle4.1 GeneralThe time for which, or the temperature up to which, an antioxidant stabilizer system present in a test specimen inhibits oxidation is measured while the specimen i

42、s held isothermally at a specified temperature or heated at a constant rate in an oxygen or air atmosphere. The oxidation induction time or temperature is an assessment of the level (or degree) of stabilization of the material tested. Higher test temperatures will result in shorter oxidation inducti

43、on times; faster heating rates will result in higher oxidation induction temperatures. The oxidation induction time and temperature are also dependent on the surface area of the specimen available for oxidation. It should be noted that tests carried out in pure oxygen will result in a lower oxidatio

44、n induction time or temperature than tests performed under normal atmospheric-air conditions.NOTE The oxidation induction time or temperature can be indicative of the effective antioxidant level present in the test specimen. Caution should be exercised in data interpretation, however, since oxidatio

45、n reaction kinetics are a function of temperature and the inherent properties of the additives contained in the sample. For example, oxidation induction time or temperature results are often used to select optimum resin formulations. Volatile antioxidants or differences in activation energies of oxi

46、dation reactions can generate poor oxidation induction time or temperature results, even though the antioxidants can perform adequately at the intended temperature of use of the finished product.4.2 Oxidation induction time (isothermal OIT)The specimen and a reference material are heated at a consta

47、nt rate in an inert gaseous environment (a flow of nitrogen). When the specified temperature has been reached, the atmosphere is changed to oxygen or air maintained at the same flow rate. The specimen is then held at constant temperature until the oxidative reaction is displayed on the thermal curve

48、 The isothermal OIT is the time interval between the initiation of oxygen or air flow and the onset of the oxidative reaction. The onset of oxidation is indicated by an abrupt increase in the specimens evolved heat and may be observed by a differential scanning calorimeter (DSC). The isothermal OIT

49、 is determined in accordance with 9.6.1.4.3 Oxidation induction temperature (dynamic OIT)The specimen and a reference material are heated at a constant rate in an oxygen or air atmosphere until the oxidative reaction is displayed on the thermal curve. The dynamic OIT is the temperature of the onset of the oxidative reaction. The onset of oxidation is indicated by an abrupt increase in the specimens evolved heat and may be observed by a differential scanning calorimeter (DSC). The dynamic OIT is determined in accordance