BS-ISO-21561-2005.pdf
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1、BRITISH STANDARD BS ISO 21561:2005 Styrene-butadiene rubber (SBR) Determination of the microstructure of solution-polymerized SBR ICS 83.060 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 21561:2005 This British Standard was publis
2、hed under the authority of the Standards Policy and Strategy Committee on 4 January 2006 BSI 4 January 2006 ISBN 0 580 47395 3 National foreword This British Standard reproduces verbatim ISO 21561:2005 and implements it as the UK national standard. The UK participation in its preparation was entrust
3、ed to Technical Committee PRI/23, Test methods for rubber and non-black compounding ingredients, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep U
4、K interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred t
5、o in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions
6、of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 15 and a back
7、cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 21561:2005
8、(E) INTERNATIONAL STANDARD ISO 21561 First edition 2005-12-01 Styrene-butadiene rubber (SBR) Determination of the microstructure of solution-polymerized SBR Caoutchouc styrne-butadine (SBR) Dtermination de la microstructure du SBR polymris en solution BS ISO 21561:2005 Licensed Copy: sheffieldun she
9、ffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 21561:2005 iii Contents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 NMR method (absolute met
10、hod) . 1 4 IR method (relative method) 4 5 Precision 10 6 Test report . 11 Annex A (informative) Procedure for sample-film preparation and measurement of microstructure by FT IR spectrophotometry 12 Bibliography . 15 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Unc
11、ontrolled Copy, (c) BSI BS ISO 21561:2005 iv Foreword ISO (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 memb
12、er 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 collaborates closely with the International Ele
13、ctrotechnical 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 technical committees is to prepare International Standards. Draft International Standards adop
14、ted 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 drawn to the possibility that some of the elements of this document may be the subject of pate
15、nt rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 21561 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Un
16、controlled Copy, (c) BSI 1 Styrene-butadiene rubber (SBR) Determination of the microstructure of solution-polymerized SBR WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all the safety problems, if any, a
17、ssociated 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 conditions. 1 Scope This International Standard specifies procedures for the quantitative determination of the microstructure of the
18、 butadiene units and the content of styrene units in solution-polymerized SBR (S-SBR) by 1H-NMR spectrometry as an absolute method and by IR spectrometry as a relative method. The styrene content is expressed in mass % relative to the whole polymer. The 1,4-trans, 1,4-cis and 1,2-vinyl contents are
19、expressed in mol % relative to the butadiene units. NOTE IR spectrometry can also give absolute values of microstructure by calibration with S-SBRs of known absolute microstructure obtained by 1H-NMR spectrometry. 2 Normative references The following referenced documents are indispensable for the ap
20、plication 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 1407, Rubber Determination of solvent extract ISO 1795, Rubber, raw natural and raw synthetic Sampling and f
21、urther preparative procedures 3 NMR method (absolute method) 3.1 Principle 3.1.1 A small quantity of an extracted S-SBR is dissolved in deuterated-chloroform. 3.1.2 A 1H-NMR spectrum of the sample solution is measured at a 15 ppm sweep width. The peak areas of the 1,4-bond (the sum of the 1,4-trans
22、bond and 1,4-cis bond) and the 1,2-vinyl bond of the butadiene portion are determined along with the peak area of styrene. The microstructure of the butadiene portion and the styrene content are then calculated using theoretical formulae. 3.2 Reagents 3.2.1 Deuterated chloroform, CDCl3, containing 0
23、,03 % of tetramethyl silane (TMS) as internal standard. The purity of the CDCl3 itself shall be 99,8 %. 3.2.2 Anhydrous ethanol-toluene azeotrope (ETA). BS ISO 21561:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:49:52 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 3.2.3 Acetone. 3.3 A
24、pparatus 3.3.1 1H-NMR spectrometer: Fourier transform nuclear magnetic resonance (FT-NMR) spectrometer with a resonance frequency of 150 MHz or higher. 3.3.2 Extraction apparatus, as described in ISO 1407. 3.3.3 Vacuum oven, operated at 50 C to 60 C. 3.3.4 Analytical balance, accurate to 0,1 mg. 3.4
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