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1、a Date: 22 March 2007 Origin: International Latest date for receipt of comments: 30 June 2007 Project no.: 2007/00245 Responsible committee: PRI/23 Test methods for rubber and non-black compounding ingredients Interested committees: Title: Draft BS ISO 9924-3 Rubber and rubber products Determination
2、 of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rubbers, halogenated rubbers and polysiloxane rubbers after extraction Supersession information: If this document is published as a standard, the UK implementation of it will supersede NONE and partiall
3、y supersede NONE . If you are aware of a current national standard which may be affected, please notify the secretary (contact details below). WARNING: THIS IS A DRAFT AND MUST NOT BE REGARDED OR USED AS A BRITISH STANDARD. THIS DRAFT IS NOT CURRENT BEYOND 30 June 2007. This draft is issued to allow
4、 comments from interested parties; all comments will be given consideration prior to publication. No acknowledgement will normally be sent. See overleaf for information on commenting. No copying is allowed, in any form, without prior written permission from BSI except as permitted under the Copyrigh
5、t, Designs and Patent Act 1988 or for circulation within a nominating organization for briefing purposes. Electronic circulation is limited to dissemination by e-mail within such an organization by committee members. Further copies of this draft may be purchased from BSI Customer Services, Tel: +44(
6、0) 20 8996 9001 or email ordersbsi-. British, International and foreign standards are also available from BSI Customer Services. British Standards on CD or Online are available from British Standards Publishing Sales Limited. Tel: 01344 404409 or email bsonlinetechindex.co.uk. Information on the co-
7、operating organizations represented on the committees referenced above may be obtained from the responsible committee secretary. Cross-references The British Standards which implement International or European publications referred to in this draft may be found via the British Standards Online Servi
8、ce on the BSI web site http:/www.bsi-. Direct tel: 020 8996 7009 Responsible Committee Secretary: Committee Service Centre (BSI) E-mail: cscbsi- Draft for Public Comment Head Office 389 Chiswick High Road London W4 4AL Telephone: +44(0)20 8996 9000 Fax: +44(0)20 8996 7001 Form 36 Version 7.0 DPC: 07
9、/30161736 DC Licensed Copy: London South Bank University, London South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled Copy, (c) BSI b Introduction This draft standard is based on international discussions in which the UK has taken an active part. Your comments on this draft are in
10、vited and will assist in the preparation of the consequent standard. Comments submitted will be reviewed by the relevant BSI committee before sending the consensus UK vote and comments to the international secretariat, which will then decide appropriate action on the draft and the comments received.
11、 If no comments are received to the contrary, then the UK will approve this draft. If the international standard is approved, it is possible the text will be published as an identical British Standard. UK Vote Please indicate whether you consider the UK should submit a negative (with reasons) or pos
12、itive vote on this draft. Submission The guidance given below is intended to ensure that all comments receive efficient and appropriate attention by the responsible BSI committee. Annotated drafts are not acceptable and will be rejected. All comments must be submitted, preferably electronically, to
13、the Responsible Committee Secretary at the address given on the front cover. Comments should be compatible with Version 6.0 or Version 97 of Microsoft Word for Windows, if possible; otherwise comments in ASCII text format are acceptable. Any comments not submitted electronically should still adhere
14、to these format requirements. All comments submitted should be presented as given in the example below. Further information on submitting comments and how to obtain a blank electronic version of a comment form are available from the BSI web site at:http:/www.bsi- Template for comments and secretaria
15、t observations Date: xx/xx/200x Document: ISO/DIS xxxxx 1 2 (3) 4 5 (6) (7) MB Clause No./ Subclause No./ Annex (e.g. 3.1) Paragraph/ Figure/Table/ Note (e.g. Table 1) Type of com- ment Comment (justification for change) by the MB Proposed change by the MB Secretariat observations on each comment su
16、bmitted 3.1 Definition 1 ed Definition is ambiguous and needs clarifying. Amend to read . so that the mains connector to which no connection . 6.4 Paragraph 2 te The use of the UV photometer as an alternative cannot be supported as serious problems have been encountered in its use in the UK. Delete
17、reference to UV photometer. Microsoft and MS-DOS are registered trademarks, and Windows is a trademark of Microsoft Corporation. Licensed Copy: London South Bank University, London South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled Copy, (c) BSI THIS DOCUMENT IS A DRAFT CIRCULAT
18、ED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH. IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT INTERNATIONAL STANDARDS MAY ON OCCASI
19、ON HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS. DRAFT INTERNATIONAL STANDARD ISO/DIS 9924-3 International Organization for Standardization, 2007 INTERNATIONAL ORGANIZATION FOR STANDARDIZATION ORGANISATION INTERNATIO
20、NALE DE NORMALISATION ISO/TC 45/SC 2 Voting begins on: 2007-02-26 Secretariat: SIS Voting terminates on: 2007-07-26 Rubber and rubber products Determination of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rubbers, halogenated rubbers and polysiloxane
21、rubbers after extraction Caoutchouc et produits base de caoutchouc Dtermination de la composition des vulcanisats et des mlanges non vulcaniss par thermogravimtrie Partie 3: Caoutchoucs hydrocarbons, caoutchoucs halogns et caoutchoucs polysiloxanes aprs extraction ICS 83.060 To expedite distribution
22、, this document is circulated as received from the committee secretariat. ISO Central Secretariat work of editing and text composition will be undertaken at publication stage. Pour acclrer la distribution, le prsent document est distribu tel quil est parvenu du secrtariat du comit. Le travail de rda
23、ction et de composition de texte sera effectu au Secrtariat central de lISO au stade de publication. Licensed Copy: London South Bank University, London South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 9924-3 ii ISO 2007 All rights reserved PDF disclaimer
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26、e; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. Copyright notice Thi
27、s ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted under the applicable laws of the users country, neither this ISO draft nor any extract from it may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electroni
28、c, photocopying, recording or otherwise, without prior written permission being secured. Requests for permission to reproduce should be addressed to either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 2
29、2 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Reproduction may be subject to royalty payments or a licensing agreement. Violators may be prosecuted. Licensed Copy: London South Bank University, London South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled
30、 Copy, (c) BSI ISO/DIS 9924-3 ISO 2006 All rights reserved iii Contents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle .2 4 Reagent.2 5 Apparatus.2 6 Preparation of samples.2 6.1 Conditioning of samples.2 6.2 Extraction of samples.2 6.3 Test piece.3 7 Procedure.3 7.1 General .3 7.2 De
31、scription of the various procedures .3 7.3 Test procedures.3 8 Expression of the results .4 8.1 Recordings (thermograms) 4 8.2 Calculation of the mass change from curves.4 8.3 Interpretation .5 8.3.1 General .5 8.3.2 Rubbers with hydrocarbon rubbers (Figures B.2 and B.3).5 8.3.3 Rubbers with nitroge
32、nous hydrocarbon chain (Figure B.4).5 8.3.4 Rubbers with halogenated hydrocarbon chain (figure B.5)5 8.3.5 Rubbers with hydrocarbon, nitrogenous and oxygenated chain.5 8.3.6 Rubbers with hydrocarbon and sulphurated chain.5 8.3.7 Rubbers with polysiloxane chain 6 8.4 Expression of the results .6 8.4.
33、1 Result obtained from the TGA curve.6 8.4.2 Calculated percentages of material.6 9 Test report7 10 Precision 7 Annex A (informative) Recommended procedure .8 Annex B (informative) Examples of thermogram 9 Annex C (Informative) Precision 14 DRAFT 2007 Licensed Copy: London South Bank University, Lon
34、don South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 9924-3 iv ISO 2006 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing
35、 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 organizations, governmental and non-governmental, in liais
36、on 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 in the ISO/IEC Directives, Part 2. The main task of te
37、chnical 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 % of the member bodies casting a vote. Attention is dr
38、awn 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 9924-3 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and
39、 analysis. ISO 9924 consists of the following parts, under the general title Rubber and rubber products Determination of composition of vulcanizates and uncured compounds by thermogravimetry: Part 1: Butadiene, ethylene-propylene copolymer and terpolymer, isobutene-isoprene, isoprene and styrene-but
40、adiene rubbers Part 2: Acrylonitrile-butadiene and halobutyl rubbers Part 3: Hydrocarbon, halogenated and polysiloxane rubbers after extraction. DRAFT 2007 Licensed Copy: London South Bank University, London South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled Copy, (c) BSI DRAFT
41、INTERNATIONAL STANDARD ISO/DIS 9924-3 ISO 2006 All rights reserved 1 WARNING Persons using this part of ISO 9924 should be familiar with normal laboratory practice. This part of ISO 9924 does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility
42、 of the user to establish appropriate safety and health practices to ensure compliance with any regulatory conditions. CAUTION Certain procedures specified in this International Standard may involve the use or generation of substances, or the generation of waste, that could constitute a local enviro
43、nmental hazard. Reference should be made to appropriate documentation on safe handling and disposal after use. 1 Scope This part of ISO 9924 specifies a thermogravimetric method for the determination of the main constituents of rubber compounds such as elastomer (s), carbon black and mineral filler.
44、 It allows the “fingerprint“ of the tested material to be established. However, the obtained result does not correspond still exactly to the theoretical formula of the rubber. This method applies to raw or compounded rubbers, vulcanised or not after preliminary extraction. This method applies to rub
45、bers with hydrocarbon chains (NR, BR, SBR, IIR, EPDM, ACM, AEM, etc.) used singly or in combination in formulations. In the latter case, the polymer content will correspond to the total rubber, and it will not usually be possible to determine individual polymers. This method applies to rubbers with
46、halogenated, hydrocarbon chains (CR, CSM, FKM, CM, CO, ECO, etc.) or nitrogen containing (NBR, HNBR, NBR / PVC, etc.), as well as to their mixtures. However, these rubbers often form carbonaceous residues which interfere with the analysis. An appropriate procedure will minimize these interferences.
47、This method also applies to rubbers with polysiloxane chain (VMQ, etc.) and to rubbers not listed above. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the
48、 latest edition of the referenced document (including any amendments) applies. ISO 1407, Rubber - Determination of solvent extract ISO 23529, DRAFT 2007 Rubber and rubber products Determination of the composition of vulcanizates and uncured compounds by thermogravimetry Part 3: Hydrocarbon rubbers,
49、halogenated rubbers and polysiloxane rubbers after extraction Licensed Copy: London South Bank University, London South Bank University, Mon Apr 02 00:22:55 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ISO/DIS 9924-3 2 ISO 2006 All rights reserved 3 Principle A weighed test portion placed in the pan of a thermogravimetric analyser, is heated, following a pre-se