BS ISO 10638-2017 Rubber Identification of antidegradants by gas chromatography mass spectrometry《橡胶 通过气相色谱法 质谱分析法识别抗降解剂》.pdf

1、Rubber Identification of antidegradants by gas chromatography/mass spectrometryBS ISO 10638:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Rubber Identification of antidegradants by gas chromatography/mass spectrometryCaoutchouc Identification des antid

2、gradants par chromatographie en phase gazeuse/spectromtrie de masseINTERNATIONAL STANDARDISO10638Second edition2017-07Reference numberISO 10638:2017(E)National forewordThis British Standard is the UK implementation of ISO 10638:2017. It supersedes BS ISO 10638:2010, which is withdrawn.The UK partici

3、pation in its preparation was entrusted to Technical Committee PRI/22, Testing and analysis of rubber.A list of organizations represented 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 r

4、esponsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 92771 3ICS 83.040.10; 83.040.20Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authorit

5、y of the Standards Policy and Strategy Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 10638:2017 ISO 2017Rubber Identification of antidegradants by gas chromatography/mass spectrometryCaoutchouc Identification des antidgradants p

6、ar chromatographie en phase gazeuse/spectromtrie de masseINTERNATIONAL STANDARDISO10638Second edition2017-07Reference numberISO 10638:2017(E)BS ISO 10638:2017ISO 10638:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless oth

7、erwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

8、 below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 10638:2017ISO 10638:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUME

9、NT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written pe

10、rmission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 10638:2017(E)Forewo

11、rd ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Thermal-desorption method . 25.1 Reagents and materials . 25.2 Apparatus 25.3 Sampling . 25.4 Procedure 36 Solvent-extraction method. 36.1 Reagents and materials . 36.2 Apparatus 46.3 Sampling . 46.4 Proc

12、edure 47 Analysis 47.1 General . 47.2 Procedure 47.3 Important observations for analysis 58 Test report . 5Annex A (normative) Antidegradants covered by this document 6Annex B (informative) Chromatograms and mass spectra .10Annex C (informative) Determination of gas-chromatographic retention index 4

13、2Bibliography .45 ISO 2017 All rights reserved iiiContents PageBS ISO 10638:2017ISO 10638:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carr

14、ied 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 ISO, also take part in the work.

15、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, Part 1. In particular, the differe

16、nt 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 elements of this document ma

17、y 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 received (see www .iso .org/ pa

18、tents).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 voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information abo

19、ut ISOs adherence to the World Trade Organization (WTO) principles 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 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis.This

20、 second edition cancels and replaces the first edition (ISO 10638:2010), which has been technically revised with the following changes: trap coolant has been removed from the reagents; a calibration procedure for the apparatus has been added; test conditions have been added; a data analysis clause (

21、Clause 7) has been added.iv ISO 2017 All rights reservedBS ISO 10638:2017ISO 10638:2017(E)ForewordISO (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

22、 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 ISO, also take part in the work. ISO col

23、laborates 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, Part 1. In particular, the different appr

24、oval 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 elements of this document may be th

25、e 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 received (see www .iso .org/ patents).

26、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 voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs

27、 adherence to the World Trade Organization (WTO) principles 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 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis.This second

28、 edition cancels and replaces the first edition (ISO 10638:2010), which has been technically revised with the following changes: trap coolant has been removed from the reagents; a calibration procedure for the apparatus has been added; test conditions have been added; a data analysis clause (Clause

29、7) has been added.iv ISO 2017 All rights reserved ISO 10638:2017(E)IntroductionMost rubber products contain antidegradants to extend the life of the product, the type of antidegradant depending on the service conditions to which a particular product will be exposed. Doubts are increasingly being exp

30、ressed about the negative impact which rubber containing certain antidegradants can have on the environment. However, demonstrating the presence of antidegradants in rubber products is not easy.There are methods of qualitative analysis, specified in International Standards such as ISO 4645, which us

31、e thin-layer chromatography. This requires a highly skilled operator with a great amount of knowledge and experience, as well as the use of standard reference materials.The gas chromatography/mass spectrometry technique specified in this document is an efficient method suitable for identifying antid

32、egradants contained in rubber products, as well as in the raw-rubber and the unvulcanized-rubber compounds used to make such products. ISO 2017 All rights reserved vBS ISO 10638:2017Rubber Identification of antidegradants by gas chromatography/mass spectrometryWARNING 1 Persons using this document s

33、hould be familiar with normal laboratory practice. This document does not purport to address all of the safety problems, 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 national regulatory co

34、nditions.WARNING 2 Certain procedures specified in this document might involve the use or generation of substances, or the generation of waste, that could constitute a local environmental hazard. Reference should be made to appropriate documentation on safe handling and disposal after use.1 ScopeThi

35、s document specifies a method using gas chromatography/mass spectrometry, for the identification of antidegradants in raw rubbers, latices, unvulcanized-rubber compounds and vulcanized-rubber products. It is applicable to the 31 types of antidegradant listed in Annex A. The method specified is quali

36、tative and is not intended for quantitative analysis.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, only the edition cited applies. For undated references, the

37、latest edition of the referenced document (including any amendments) applies.ISO 123, Rubber latex SamplingISO 124, Latex, rubber Determination of total solids contentISO 1407:2011, Rubber Determination of solvent extractISO 1795, Rubber, raw natural and raw synthetic Sampling and further preparativ

38、e procedures3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h

39、t t p :/ www .iso .org/ obp4 PrincipleAntidegradants are recovered from samples by thermal desorption or solvent extraction. For thermal-desorption method, the fume generated from heating test samples is to be analysed after being separated through the gas chromatograph/mass spectrometer which is co

40、nnected to a heating and desorbing device. For solvent-extraction method, the extract of test samples obtained by solvent extraction process is to be separated and analysed by the gas chromatograph/mass spectrometer. The type of antidegradant recovered is identified by the mass spectrum that is prod

41、uced after passing the antidegradant through a gas chromatograph and mass spectrometer connected in tandem. The retention index can be used as a supplementary means of identification if necessary.INTERNATIONAL STANDARD ISO 10638:2017(E) ISO 2017 All rights reserved 1BS ISO 10638:2017Rubber Identific

42、ation of antidegradants by gas chromatography/mass spectrometryWARNING 1 Persons using this document should be familiar with normal laboratory practice. This document does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to esta

43、blish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.WARNING 2 Certain procedures specified in this document might involve the use or generation of substances, or the generation of waste, that could constitute a local environmental hazard. Re

44、ference should be made to appropriate documentation on safe handling and disposal after use.1 ScopeThis document specifies a method using gas chromatography/mass spectrometry, for the identification of antidegradants in raw rubbers, latices, unvulcanized-rubber compounds and vulcanized-rubber produc

45、ts. It is applicable to the 31 types of antidegradant listed in Annex A. The method specified is qualitative and is not intended for quantitative analysis.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirement

46、s 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 123, Rubber latex SamplingISO 124, Latex, rubber Determination of total solids contentISO 1407:2011, Rubber Determina

47、tion of solvent extractISO 1795, Rubber, raw natural and raw synthetic Sampling and further preparative procedures3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Elect

48、ropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp4 PrincipleAntidegradants are recovered from samples by thermal desorption or solvent extraction. For thermal-desorption method, the fume generated from heating test sampl

49、es is to be analysed after being separated through the gas chromatograph/mass spectrometer which is connected to a heating and desorbing device. For solvent-extraction method, the extract of test samples obtained by solvent extraction process is to be separated and analysed by the gas chromatograph/mass spectrometer. The type of antidegradant recovered is identified by the mass spectrum that is produced after passing the antidegradant through a gas chromatograph and mass spectrometer connected