BS 7164-12-1991 Chemical tests for raw and vulcanized rubber - Determination of bound styrene content of raw styrene-butadiene rubber emulsion polymerized refractive index method《生.pdf
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1、BRITISH STANDARD This Standard is confirmed.See the BSI Catalogue for details. August 1997. BS 7164-12: 1991 ISO 2453:1991 Incorporating Technical Corrigendum No. 1 Chemical tests for raw and vulcanized rubber Part 12: Determination of bound styrene content of raw styrene-butadiene rubber, emulsion
2、polymerized: refractive index method ICS.83.040.10 BS 7164-12:1991 This British Standard, having been prepared under the direction of the Plastics and Rubber Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 31 October 1991 BSI 28 November
3、2003 The following BSI references relate to the work on this standard: Committee reference PRM/23 Draft for comment 84/38407 DC ISBN 0 580 20156 2 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Plastics and Rubber Standards Policy Commi
4、ttee (PRM/-) to Technical Committee PRM/23, upon which the following bodies were represented: Institute of Water and Environmental Management Laboratory of the Government Chemist Ministry of Defence Royal Society of Chemistry Rubber and Plastics Research Association Amendments issued since publicati
5、on Amd. No. Date Comments 14801 Technical Corrigendum No. 1 28 November 2003 Change to Table 1BS 7164-12:1991 BSI 28 November 2003 i Contents Page Committees responsible Inside front cover National foreword ii 1S c o p e 1 2 Significance of the test 1 3 Principle 1 4R e a g e n t s 1 5A p p a r a t
6、u s 1 6 Preparation of test pieces 2 7 Procedure 3 8 Expression of results 3 9 Test report 4 Annex A (informative) Other International Standards relating to the styrene content of styrene-butadiene rubbers 6 Table 1 Values of refractive index at 25 C and percentage, by mass, of bound styrene 5BS 716
7、4-12:1991 ii BSI 28 November 2003 National foreword This part of BS 7164 has been prepared under the direction of the Plastics and Rubber Standards Policy Committee and is identical with ISO 2453:1991 “Rubber, raw styrene-butadiene, emulsion-polymerized Determination of bound styrene content Refract
8、ive index method”, including Technical Corrigendum August 2003, published by the International Organization for Standardization (ISO). BS 7164 rationalizes all the methods that deal with chemical analysis of raw, compounded and vulcanized rubber, some of which have previously been published in BS 90
9、3, BS 1673 and BS 5923. Relevant parts of those standards will be withdrawn or deleted by amendment, as appropriate, when superseded by Parts and Sections of BS 7164. This part of BS 7164 supersedes BS 1673-5.1:1963 which is withdrawn. Annex A of this standard is for information only. Cross-referenc
10、es The British Standards which implement international or European 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 St
11、andards Online. This publication does not purport 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 co
12、ver, an inside front cover, pages i and ii, pages 1 to 7 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.BS 7164-12:1991 BSI 28 November 2003 1 1 Scope This International Standard specifies a method for determining the bound styrene c
13、ontent of emulsion-polymerized styrene-butadiene (SBR) rubbers by correlation with the measured refractive index of an extracted sample according to a table of refractive indices versus percentages by mass of styrene. The method is also applicable to extracted oil-extended emulsion-polymerized SBR a
14、s long as it produces a film suitable for refractive index measurements. It is not applicable to solution-polymerized SBR. 2 Significance of the test The bound styrene test is a measure of the bound monomeric composition of the rubber. It is used as a check on the accuracy of monomer charging and al
15、so as a guide to the uniformity of the product, since the bound styrene content affects the physical properties. 3 Principle Extraction of a test piece with ethanol-toluene azeotrope (ETA), followed by drying and pressing between sheets of aluminium foil to provide sheeted rubber having a thickness
16、of not more than 0,50 mm. Calculation of the bound styrene content from the refractive index obtained at 25 C on this thinly sheeted rubber. 4 Reagents 4.1 Ethanol-toluene azeotrope (ETA) Mix 7 volumes of absolute ethanol with 3 volumes of toluene. Alternatively, mix 7 volumes of commercial grade et
17、hanol with 3 volumes of toluene, and boil the mixture with anhydrous calcium oxide (quicklime) under reflux for 4 h. Then distil the azeotrope and collect the fraction with a boiling range not exceeding 1 C, for use in the test. 4.2 Acidified ETA Add 10 cm 3of concentrated hydrochloric acid approxim
18、ately 35 % (m/m) to a portion of ETA (4.1) and make the solution up to 1 000 cm 3with ETA. NOTE 1 Acidified ETA is used for alum-coagulated polymers. 4.3 -Bromonaphthalene 5 Apparatus 5.1 Spiders, consisting of 13 mm squares of sheet aluminium or stainless steel having a nickel-chromium wire leg abo
19、ut 38 mm long attached to each corner. When the extracting solvent is ETA acidified with hydrochloric acid, the spider and the legs shall be made of tantalum. 5.2 Reflux condenser 5.3 Abbe-type refractometer, having fourth-decimal-place accuracy and whose refracting prism can be placed in a nearly h
20、orizontal position for measurement of the refractive index of solids. An Amici-type compensating prism for achromatization is necessary unless a sodium-vapour lamp is used as a light source. The refractometer shall be maintained at a temperature of 25 C0 , 1 C, obtained by the use of a constant temp
21、erature room or by circulating constant temperature water through the instrument. 5.4 Vacuum oven, capable of being evacuated to a pressure of 1 300 Pa 1)and of maintaining a temperature of 100 C5 C. 5.5 Aluminium foil, between 0,025 mm and 0,08 mm thick, having good tear strength. 5.6 Glass referen
22、ce, for checking adjustment of the refractometer. The glass reference shall be calibrated for use at 25 C. 1) 10 3 Pa = 10 3 N/m 2 = 7,5 mmHg.BS 7164-12:1991 2 BSI 28 November 2003 5.7 Hydraulic press, that can be maintained at a temperature of 100 C and can attain a total force of up to 100 kN on t
23、he platens. 5.8 Pressing plates, (optional apparatus), measuring 210 mm 210 mm 3 mm, with a wooden handle. One of the plates shall have a 150 mm square area in the centre milled out to a depth not to exceed 0,65 mm. 5.9 Scissors, small and sharp. 5.10 Light source, which shall be collimated to provi
24、de a beam at grazing incidence to the prism. If an incandescent light source is used, such as a flashlight bulb, it shall be of low intensity. A sodium-vapour lamp may also be used. The light source requirement is that a clear, sharp line with good contrast can be observed in the telescope of the re
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