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1、BRITISH STANDARD BS ISO 7663:2005 Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation procedures ICS 83.060 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 7663:2005 This British Standard was published under the authori
2、ty of the Standards Policy and Strategy Committee on 23 January 2006 BSI 23 January 2006 ISBN 0 580 47196 9 National foreword This British Standard reproduces verbatim ISO 7663:2005 and implements it as the UK national standard. It supersedes BS 6845:1996 which is withdrawn. The UK participation in
3、its preparation was entrusted to Technical Committee PRI/50, Rubber Raw, natural and synthetic, 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
4、 which implement 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 doe
5、s 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. aid enquirers to understand the text; present to the responsible international/Europea
6、n committee any enquiries on the interpretation, or proposals for change, and keep UK interests 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
7、 to iv, pages 1 to 9 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 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI
8、 Reference number ISO 7663:2005(E) INTERNATIONAL STANDARD ISO 7663 Fourth edition 2005-12-15 Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation procedures Caoutchoucs isobutne-isoprne halogns (BIIR et CIIR) Mthodes dvaluation BS ISO 7663:2005 Licensed Copy: sheffieldun sheffieldun, na,
9、 Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Foreword iv 1 Scope . 1 2 Normative references. 1 3 Sampling and further preparative procedures 2 4 Physical
10、 and chemical tests on raw rubber. 2 4.1 Mooney viscosity 2 4.2 Volatile matter . 2 4.3 Ash . 2 5 Preparation of test mixes. 2 5.1 Standard test formulation 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 r
11、otorless curemeter 5 7 Evaluation of tensile stress-strain properties of vulcanized test mixes. 5 8 Precision 6 8.1 General. 6 8.2 Precision details . 6 8.3 Precision results. 6 9 Test report . 7 Bibliography. 9 BS ISO 7663:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:
12、00 2006, Uncontrolled Copy, (c) BSI 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 member bod
13、y 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 Electrote
14、chnical 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 adopted by
15、 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 patent rig
16、hts. ISO shall not be held responsible for identifying any or all such patent rights. ISO 7663 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry. This fourth edition cancels and replaces the th
17、ird edition (ISO 7663:1995), which has been technically revised. BS ISO 7663:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 1 Halogenated isobutene-isoprene rubber (BIIR and CIIR) Evaluation procedures WARNING Persons using this Intern
18、ational Standard should be familiar with normal laboratory practice. This standard does not purport to address 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 nati
19、onal regulatory conditions. 1 Scope This International Standard specifies: physical and chemical tests on raw rubbers; standardized materials, a standardized test formulation, and the equipment and processing methods for evaluating the vulcanization characteristics of all types of halogenated isobut
20、ene-isoprene rubber (BIIR and CIIR). 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 latest edition of the referenced document (including any amendments
21、) applies. ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain properties ISO 247:1990, Rubber Determination of ash ISO 248:2005, Rubber, raw Determination of volatile-matter content ISO 289-1, Rubber, unvulcanized- Determinations using a shearing-disc viscometer Part
22、1: Determination of Mooney viscosity ISO 1795:2000, Rubber, raw natural and raw synthetic Sampling and further preparative procedures ISO 2393:1994, Rubber test mixes Preparation, mixing and vulcanization Equipment and procedures ISO 3417, Rubber Measurement of vulcanization characteristics with the
23、 oscillating disc curemeter ISO 6502, Rubber Guide to the use of curemeters ISO 8312, Rubber compounding ingredients Stearic acid Definition and test methods ISO/TR 9272, Rubber and rubber products Determination of precision for test method standards ISO 9298, Rubber compounding ingredients Zinc oxi
24、de Test methods ISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods BS ISO 7663:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 3 Sampling and further preparative procedures A labo
25、ratory sample of approximately 1,5 kg shall be taken in accordance with the method described in ISO 1795. Preparation of the test samples shall be in accordance with ISO 1795. 4 Physical and chemical tests on raw rubber 4.1 Mooney viscosity Prepare a test sample, without milling, in accordance with
26、the preferred procedure in ISO 1795. If milling is deemed necessary, either because of the condition of the laboratory sample (e.g. excessive porosity) or by agreement between the interested parties, it shall be performed in accordance with ISO 1795:2000, Subclause 8.3.2.2, paragraphs 1 and 2. Deter
27、mine the Mooney viscosity in accordance with ISO 289-1 on a test piece cut from the test sample which shall be as free as possible from air and pockets that may trap air against the rotor and die surface. The viscosity shall be determined as ML(1+8) at 125 C. 4.2 Volatile matter Determine the volati
28、le-matter content by hot-mill method A as specified in ISO 248:2005, Clause 4. A 450 g sized test unit may be used if required by an agreement between the interested parties. 4.3 Ash Determine the ash in accordance with one of the methods specified in ISO 247. 5 Preparation of test mixes 5.1 Standar
29、d test formulation The standard test formulation is given in Table 1. The materials shall be national or international standard reference materials (or as agreed by the interested parties). Table 1 Standard test formulation for evaluation of halogenated isobutene-isoprene rubbers Material Parts by m
30、ass Halogenated isobutene-isoprene rubber (BIIR or CIIR) 100,00 Stearic acid a, b 1,00 Industry reference black c 40,00 Zinc oxide a, d 5,00 Total146,00 a Use powder materials. b The standard reference material for stearic acid is specified in ISO 8312. Use class A. c Use the current industry refere
31、nce black. d The standard reference material for zinc oxide is specified in ISO 9298. Use the indirect (French) process. BS ISO 7663:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 5.2 Procedure 5.2.1 Equipment and procedure The equip
32、ment and procedure for the preparation, mixing and vulcanization shall be in accordance with ISO 2393:1994, Clauses 6, 7, 8 and 9. 5.2.2 Mixing procedure 5.2.2.1 General Two permitted mixing procedures are specified: method A: mill mixing; method B: miniature internal mixer (MIM) mixing. Additionall
33、y, method A and method B may be used with different mixing procedures, by agreement between the interested parties. NOTE The above procedures may not give identical results. 5.2.2.2 Method A (mill mixing procedure) The standard laboratory mill batch mass, in grams, shall be based on four times the f
34、ormulation mass, i.e. 4 146,00 g (= 584 g). The surface temperatures of the rolls shall be maintained at 40 C 5 C throughout the mixing. The vulcanization of halogenated isobutene-isoprene rubber with zinc oxide is highly sensitive to moisture. Therefore care shall be taken when conditioning the car
35、bon black. Condition the carbon black for 1 h at 125 C 3 C. The thickness of the carbon black layer shall not exceed 10 mm. Store the conditioned black in a moisture-proof container. Maintain a good rolling bank at the nip of the rolls during mixing. If this is not obtained with the nip settings spe
36、cified below, small adjustments to the mill openings may be necessary. Mix the stearic acid and the carbon black together in a suitable container before starting to mix. Duration (min) Cumulative time (min) a) Band the rubber on the slow roll with the mill opening set at 0,65 mm 1,0 1,0 b) Add the m
37、ixture of stearic acid and carbon black evenly across the mill at a uniform rate. Return any materials that drop through the mill to the batch. 9,5 10,5 c) When all the mixture of stearic acid and carbon black has been incorporated, make one 3/4 cut from each side. Do not cut the band until all visi
38、ble free black has been incorporated. 0,5 11,0 d) Add the zinc oxide. 3,0 14,0 e) When all the zinc oxide has been incorporated, make three 3/4 cuts from each side, alternately. 2,0 16,0 BS ISO 7663:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Cop
39、y, (c) BSI 4 f) Cut the batch from the mill. Set the mill opening at 0,8 mm and pass the rolled batch endwise through the mill six times. 2,0 18,0 g) Sheet the batch to a thickness of approximately 6 mm. Check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical valu
40、e by more than +0,5 %/1,5 %, discard the batch and re-mix. h) Sheet the batch to a thickness of approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring test pieces in accordance with ISO 37. i) Condition the batch for 2 h to 24 h prior to vulcanizing and
41、 curemeter testing at standard laboratory temperature and humidity as defined in ISO 23529. 5.2.2.3 Method B (miniature internal mixer procedure) A batch mass corresponding to 0,48 times the formulation mass, i.e. 0,48 146,00 (= 70,08 g) has been found to be suitable for a miniature internal mixer h
42、aving a nominal capacity of 64 cm3. Condition the carbon black as described in 5.2.2.2. Prepare the rubber by passing it once through a mill with the temperature set at 50 C 5 C and an opening of 0,5 mm. Cut the sheet into 20 mm wide strips. Mix with the head temperature of the miniature internal mi
43、xer maintained at 60 C 3 C and the unloaded rotor speed at 6,3 rad/s to 6,6 rad/s (60 rpm to 63 rpm). Duration (min) Cumulative time (min) a) Charge the stearic acid, zinc oxide and carbon black first, followed by 3/4 of the rubber, lower the ram and start the timer. 0,0 0,0 b) Allow the batch to mi
44、x, raise the ram to sweep down, if necessary. Add the rest of the rubber. 1,5 1,5 c) Allow the batch to mix. 3,5 5,0 d) Turn off the rotor, raise the ram, remove the mixing chamber and discharge the batch. Record the maximum batch temperature. The final temperature of the batch discharged after 5 mi
45、n shall not exceed 120 C. If necessary, adjust the batch mass or the head temperature so that this condition is achieved. e) Immediately pass the batch twice through a mill set at 40 C 5 C with a mill opening of 3,0 mm or compress the batch between two stainless-steel plates with a force of 100 kN f
46、or 5 s at 30 C 5 C. f) Check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than +0,5 %/1,5 %, discard the batch and remix. g) Condition the batch for 2 h to 24 h at standard laboratory temperature and humidity as defined in ISO 23529. Cut a test
47、piece for curemeter testing in accordance with either 6.1 or 6.2. h) If required, sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ring test pieces in accordance with ISO 37. Condition the batch in accordance with g) above. BS ISO 7663:2
48、005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:42:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 5 6 Evaluation of vulcanization characteristics by a curemeter test 6.1 Using an oscillating-disc curemeter Measure the following standardized test parameters: ML, MH, ts1, tc(50) and tc(90
49、) in accordance with ISO 3417, using the following test conditions: Oscillation frequency: 1,7 Hz (100 cycles per minute) Amplitude of oscillation: 1 arc NOTE An amplitude of oscillation of 3 arc is permitted as an alternative. If such an amplitude is chosen, measure ts2 instead of ts1. Selectivity: to be chosen to give at least 75 % of full-scale deflection at MH Die temperature: 160 C 0,3 C Pre-heat time: