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1、BRITISH STANDARD BS ISO 2303:2003 Isoprene rubber (IR) Non-oil-extended, solution-polymerized types Evaluation procedure ICS 83.060 ? BS ISO 2303:2003 This British Standards was published under the authority of the Standards Policy and Strategy Committee on 24 January 2003 BSI 24 January 2003 ISBN 0
2、 580 41141 9 National foreword This British Standard reproduces verbatim ISO 2303:2003 and implements it as the UK national standard. It supersedes BS 5474:1991 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/50, Rubber-raw, natural and synthetic,
3、 including latex and carbon black, which has the responsibility to: 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 to in this document may be found in the BS
4、I 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 of a contract. Users are responsible for
5、its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK inter
6、ests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 10, an inside back cover and a back cover. The BSI copyright date displa
7、yed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Reference number ISO 2303:2003(E) INTERNATIONAL STANDARD ISO 2303 Fourth edition 2003-01-15 Isoprene rubber (IR) Non-oil-extended, solution-polymerized types Evaluation procedu
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13、i Contents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Sampling and sample preparation 2 4 Physical and chemical tests on raw rubber . 2 4.1 Mooney viscosity 2 4.2 Volatile matter 2 4.3 Ash 2 5 Preparation of the test mixes for evaluation of Isoprene rubbers. 2 5.1 Standard test formulatio
14、n. 2 5.2 Procedure. 3 6 Evaluation of vulcanization characteristics by a curemeter test. 5 6.1 Using an oscillating disc curemeter 5 6.2 Using a rotorless curemeter 5 7 Evaluation of tensile stress-strain properties of vulcanized test mixes . 6 8 Precision 6 8.1 General. 6 8.2 Precision details 6 8.
15、3 Precision results . 6 9 Test report 7 Annex A (informative) Alternative mixing method by internal mixer-mill mixing procedure . 8 BS ISO 2303:2003 iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The wo
16、rk of preparing 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-governm
17、ental, in liaison 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 3. The
18、main task of technical 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.
19、Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 2303 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Sub
20、committee SC 3, Raw materials (including latex) for use in the rubber industry. This fourth edition cancels and replaces the third edition (ISO 2303:1990), which has been technically revised. Annex A of this International Standard is for information only. BS ISO 2303:2003 INTENRATIONAL TSANDADR IS:3
21、032 O3002(E) 1 Isoprene rubber (IR) Non-oil-extended, solution-polymerized types Evaluation procedure WARNING Persons using this International Standard should be familiar with normal laboratory practices. This International Standard does not purport to address all of the safety problems, if any, ass
22、ociated 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, for general purpose non-oil-extended, solution-polymerized polyisoprene rub
23、bers (IR): physical and chemical tests on raw rubbers; standard materials, standard test formulation, equipment and processing methods for evaluating the vulcanization characteristics. Two mill-mixing procedures are described in this International Standard and an internal mixer-mill mixing procedure
24、 is described in annex A. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply.
25、However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO
26、and IEC maintain registers of currently valid International Standards. ISO 37:1994, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain properties ISO 247:1990, Rubber Determination of ash ISO 248:1991, Rubbers, raw Determination of volatile-matter content ISO 289-1:1994, Rubb
27、er, unvulcanized Determinations using a shearing-disc viscometer Determination of Mooney viscosity ISO 471:1995, Rubber Temperatures, humidities and times for conditioning and testing ISO 1795:2000, Rubber, raw natural and raw synthetic Sampling and further preparative procedures ISO 2393:1994, Rubb
28、er test mixes Preparation, mixing and vulcanization Equipment and procedures ISO 3417:1991, Rubber Measurement of vulcanization characteristics with the oscillating disc curemeter BS ISO 2303:2003 2 ISO 6472:1), Rubber compounding ingredients Abbreviations ISO 6502:1999, Rubber Guide to the use of c
29、uremeters ISO/TR 9272:1986, Rubber and rubber products Determination of precision for test method standards ISO 11235:1999, Rubber compounding ingredients Sulfenamide accelerators Test methods 3 Sampling and sample preparation 3.1 A laboratory sample of approximately 1,5 kg shall be taken by the met
30、hod described in ISO 1795. 3.2 Preparation of the test portion shall be in accordance with ISO 1795. 4 Physical and chemical tests on raw rubber 4.1 Mooney viscosity The Mooney viscosity shall be determined in accordance with ISO 289-1 on a test portion prepared as described in ISO 1795 (without mas
31、sing). The result shall be recorded as ML(1 + 4) at 100 C. 4.2 Volatile matter The volatile matter content shall be determined in accordance with ISO 248. 4.3 Ash The ash content shall be deternined in accordance with ISO 247. 5 Preparation of the test mixes for evaluation of Isoprene rubbers 5.1 St
32、andard test formulation The standard test formulation is given in Table 1. The materials shall be national or International Standard reference materials. If no standard reference material is available, the materials to be used shall be agreed by the concerned parties. 1) To be published. (Revision o
33、f ISO 6472:1994) BS ISO 2303:2003 3 Table 1 Standard test formulation for evaluation of IR rubbers Material Parts by mass Isoprene rubber (IR) 100,00 Stearic acid 2,00 Zinc oxide 5,00 Sulfur 2,25 Industry Reference Black (N330) 35,00 TBBS a 0,70 Total 144,95 a TBBS or N-tert-butyl-2-benzothiazole su
34、lfenamide in accordance with ISO 6472. This shall be supplied in powder form having an initial insoluble matter content, in accordance with ISO 11235, of less than 0,3 %. The material shall be stored at room temperature in a closed container and insoluble matter shall be checked every 6 months. If t
35、his is found to exceed 0,75 %, the material shall be discarded. TBBS may be purified by reprocessing, e.g. by recrystallization; the procedure for this is beyond the scope of this International Standard. 5.2 Procedure 5.2.1 Equipment and procedure Equipment and procedure for the preparation, mixing
36、and vulcanization shall be in accordance with ISO 2393. 5.2.2 Mill mixing procedures 5.2.2.1 General Two mill mixing procedures are specified, A and B. The mixing time is shorter in method B than in method A. The two methods do not necessarily give identical results. In laboratory cross checks or in
37、 a series of evaluations the same procedure shall be used in all cases. In both methods the standard laboratory mill batch mass, in grams, shall be based on four times the formula mass. The surface temperature of the rolls shall be maintained at 70 C 5 C throughout the mixing. A good rolling bank at
38、 the nip of the rolls shall be maintained during mixing. If this is not obtained with the nip settings specified in 5.2.2.2 and 5.2.2.3, small adjustments to the mill openings may be necessary. 5.2.2.2 Procedure A Duration Cumulative time (min) (min) a) Pass the rubber between the mill-rolls twice w
39、ithout banding, with the mill opening set at 0,5 mm for approximately 2 min and weigh the rubber. 2 2 b) Band the rubber with the mill opening set at 1,4 mm and make two 3/4 cuts from each side. 2 4 BS ISO 2303:2003 4 NOTE Some types of isoprene rubber go to the back roll, in which case the stearic
40、acid should be added and after its incorporation the rubber can usually be transferred to the front roll. In addition, certain tougher types of isoprene rubber may require slightly longer breakdown before the addition of other materials in order to obtain a good rolling bank. c) Set the mill opening
41、 to 1,7 mm and add the stearic acid. Make one 3/4 cut from each side. 2 6 d) Add the zinc oxide and the sulfur. Make two 3/4 cuts from each side. 3 9 e) Add the carbon black evenly across the mill at a uniform rate. When approximately half the black has been incorporated, open the mill to 1,9 mm and
42、 make one 3/4 cut from each side, then add the remainder of the carbon black. Be certain to add the black that has dropped into the mill pan. When all the black has been incorporated, make one 3/4 cut from each side. 13 22 f) Add the TBBS with the mill opening still at 1,9 mm. Make three 3/4 cuts fr
43、om each side. 3 25 g) Cut the batch from the mill. Set the mill opening to 0,8 mm and pass the rolled batch endwise through the rolls six times. 3 28 Total time 28 h) Sheet the batch to an approximate thickness of 6 mm and check-weigh the batch (see ISO 2393). If the mass of the batch differs from t
44、he theoretical value by more than 0,5 1,5 + % discard the batch and re-mix. Remove sufficient material for curemeter testing. i) Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. j) Condition
45、 the batch for 2 h to 24 h after mixing and prior to vulcanizing, if possible at standard temperature and humidity as defined in ISO 471. 5.2.2.3 Procedure B Duration Cumulative time (min) (min) a) Pass the rubber between the rolls twice without banding, with the mill opening set at 0,5 mm 0,1 mm, t
46、hen band the rubber between the rolls with the mill opening gradually increased to 1,4 mm. 2 2 b) Add the stearic acid. Make one 3/4 cut from each side. 2 4 c) Add the sulfur and the zinc oxide. Make two 3/4 cuts from each side. 3 7 d) Add half of the carbon black. Make two 3/4 cuts from each side.
47、3 10 e) Add the remaining half of the carbon black and the black that has dropped into the mill pan. Make three 3/4 cuts from each side. 5 15 f) Add the TBBS. Make three 3/4 cuts from each side. 3 18 g) Cut the batch from the mill. Set the mill opening to 0,5 mm 0,1 mm and pass the rolled batch endw
48、ise through the rolls six times. 2 20 Total time 20 BS ISO 2303:2003 5 h) Sheet the batch to approximately 2,2 mm for preparing test slabs or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. i) Cut the batch from the mill and check-weigh the batch (see ISO 2
49、393). If the mass of the batch differs from the theoretical value by more than 0,5 1,5 + % discard the batch and re-mix. j) Condition the batch for 2 h to 24 h after mixing and prior to vulcanizing if possible at standard temperature and humidity as defined in ISO 471. 6 Evaluation of vulcanization characteristics by a curemeter test Warning Formation of nitrosamines is possible during the cure. 6.1 Using an oscillating disc curemete