BS-ISO-16564-2004.pdf
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1、BRITISH STANDARD BS ISO 16564:2004 Incorporating Amendment No. 1 Rubber, raw natural Determination of average molecular mass and molecular-mass distribution by size exclusion chromatography (SEC) ICS 83.040.10 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, Uncontro
2、lled Copy, (c) BSI BS ISO 16564:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 1 November 2004 BSI 2006 ISBN 0 580 44709 X National foreword This British Standard reproduces verbatim ISO 16564:2004, including amendment May 2006, and imp
3、lements it as the UK national standard. The start and finish of text introduced or altered by amendment is indicated in the text by tags !“. Tags indicating changes to ISO text carry the number of the amendment. For example, text altered by ISO amendment 1 is indicated in the text by !“. The UK part
4、icipation in its preparation was entrusted 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 interpretat
5、ion, or proposals for change, and keep the UK 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 imp
6、lement international publications referred to 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 purp
7、ort to include all the necessary provisions 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 pag
8、e, pages ii to iv, pages 1 to 8, and inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments 1646330 June 2006See national foreword Licensed Copy: sheffieldun sheffi
9、eldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 16564:2004(E) INTERNATIONAL STANDARD ISO 16564 First edition 2004-10-01 Rubber, raw natural Determination of average molecular mass and molecular- mass distribution by size exclusion chromatography (SEC) C
10、aoutchouc naturel brut Dtermination de la masse molculaire moyenne et de la rpartition des masses molculaires par chromatographie dexclusion strique (SEC) BS ISO 16564:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii Licensed Copy: sh
11、effieldun sheffieldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Forewordiv 1 Scope 1 2 Principle. 1 3 Materials. 1 4 Apparatus 2 5 Procedure 2 6 Calibration . 3 7 Expression of results 5 8 Precision 5 9 Test report . 6 Annex A (informative) SEC analysis of
12、 natural rubber using cyclohexane as solvent and polyisoprene standards 7 Bibliography . 8 BS ISO 16564:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, U
13、ncontrolled Copy, (c) BSI 1 Rubber, raw natural Determination of average molecular mass and molecular-mass distribution by size exclusion chromatography (SEC) WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to addre
14、ss 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 limitations prior to use. 1 Scope This International Standard specifies a method of determin
15、ing the average molecular mass and the molecular- mass distribution of raw natural rubber dissolved in tetrahydrofuran. A set of polystyrene standards is used for calibration purposes (i.e. the method is a relative one). An alternative method, using cyclohexane as solvent and polyisoprene standards,
16、 is included in an informative annex. 2 Principle Dried natural rubber is dissolved in tetrahydrofuran at room temperature. The solution is filtered to remove “gel” (slightly crosslinked rubber) and other insoluble materials. The filtrate is used to determine the molecular mass by size exclusion chr
17、omatography 1. From the chromatogram, the number-average molecular mass (Mn), the mass-average molecular mass (Mw) and a polydispersity value (Mw/Mn) are calculated. 3 Materials 3.1 The recommended solvent is HPLC-grade tetrahydrofuran (THF). If analytical-grade THF is used, 0,5 % of butylated hydro
18、xytoluene (BHT) shall be added to the solvent as an antioxidant. The BHT is strongly retained and acts as a marker for the end of the chromatogram. It also allows minor variations in run time to be corrected, as well as indicating when a serious change in the column conditions has occurred. 3.2 The
19、solvent is filtered through a polytetrafluoroethylene (PTFE) membrane (4.2) before use. 3.3 A set of polystyrene standards with proper traceability shall be used, typically covering an Mw range from 6,5 103 to 1,06 107. An example of a suitable set of polystyrene standards is given in Table 1. Table
20、 1 Polystyrene standards No. of standard Mp Mw/Mn 1 3,55 105 1,08 2 7,06 105 1,12 3 2,89 106 1,36 4 3,84 106 1,30 5 4,48 106 1,47 6 5,48 106 1,40 7 6,77 106 1,37 8 8,42 106 1,33 BS ISO 16564:2004 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:02:40 GMT+00:00 2006, Uncontrolled Copy, (c) B
21、SI 2 4 Apparatus 4.1 Size exclusion chromatograph: Suitable high-performance liquid chromatography equipment consisting of the components specified in 4.1.1 to 4.1.7. 4.1.1 Solvent reservoir, large enough to hold an adequate quantity of solvent (see 3.1). About 3 l of solvent is recommended for a co
22、mplete analysis. Refilling can result in variations in dissolved air and the inclusion of impurities. When fresh solvent is added, it takes a long time to obtain a stable baseline. 4.1.2 Automatic on-line degassing system, to prevent the formation of bubbles in the mobile phase and to ensure a stabi
23、lized liquid feed flow. 4.1.3 Pump with temperature-control equipment, capable of delivering the solvent at a sufficient rate and a suitable temperature, for example 1,0 cm3/min at 35 C. 4.1.4 Injector. 4.1.5 Columns: Columns for the SEC of natural rubber are usually packed with rigid spheres of cro
24、sslinked polystyrene gel (prepared from styrene-divinylbenzene copolymer) having a range of pore sizes. Molecular masses in the range 2 103 to 1012 can be measured, depending on the particular set of columns used. Other column packings can be used providing they are capable of separating the polymer
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