1、BSI Standards PublicationBS ISO 2302:2014Isobutene-isoprene rubber (IIR) Evaluation procedureBS ISO 2302:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 2302:2014. Itsupersedes BS ISO 2302:2005 which is withdrawn.The UK participation in its preparation was
2、 entrusted to TechnicalCommittee PRI/50, Rubber - Raw, natural and synthetic, includinglatex and carbon black.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users
3、 are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 85477 4ICS 83.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theSta
4、ndards Policy and Strategy Committee on 31 October 2014.Amendments issued since publicationDate Text affectedBS ISO 2302:2014 ISO 2014Isobutene-isoprene rubber (IIR) Evaluation procedureCaoutchouc isobutne-isoprne (IIR) Mthode dvaluationINTERNATIONAL STANDARDISO2302Sixth edition2014-10-15Reference n
5、umberISO 2302:2014(E)BS ISO 2302:2014ISO 2302:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, includi
6、ng photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 74
7、9 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 2302:2014ISO 2302:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Sampling and further preparative procedures . 14 Physical and chemical tests on raw rubber 24.1 Mooney vi
8、scosity . 24.2 Volatile matter . 24.3 Ash . 25 Preparation of test mixes for evaluation of isobutene-isoprene rubbers 25.1 Standard test formulation . 25.2 Procedure 26 Evaluation of vulcanization characteristics by a curemeter test . 66.1 Using oscillating-disc curemeter . 66.2 Using rotorless cure
9、meter . 77 Evaluation of tensile stress-strain properties of vulcanized test mixes . 78 Precision data 79 Test report . 7Annex A (informative) Precision . 9Bibliography .11BS ISO 2302:2014ISO 2302:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of na
10、tional standards bodies (ISO member bodies). The work 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. Intern
11、ational organizations, governmental and non-governmental, 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.The procedures used to develop this document and those inten
12、ded for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.
13、iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document wi
14、ll be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and express
15、ions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommit
16、tee SC 3, Raw materials (including latex) for use in the rubber industry.This sixth edition cancels and replaces the fifth edition (ISO 2302:2005), which has been technically revised with the following changes: Clause 2 was updated. In 4.2, the method given in ISO 248-2 is now allowed. In 5.2.2.1, t
17、he addition of a statement that the mixing procedure with a laboratory internal mixer is the preferred procedure. Method B becomes “single stage mixing with a laboratory internal mixer”. In 5.2.2.2, the alternative procedure using a batch mass of two times the formulation mass has been deleted. In 5
18、.2.2.3, advice on mixing with various sizes of laboratory internal mixer is given along with a general mixing procedure. In Annex A, the precision data from ASTM D3188-95 have been used.iv ISO 2014 All rights reservedBS ISO 2302:2014INTERNATIONAL STANDARD ISO 2302:2014(E)Isobutene-isoprene rubber (I
19、IR) Evaluation procedureWARNING Users of this International Standard should be familiar with the normal laboratory practice. This International 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 appropri
20、ate safety and health practices and to ensure compliance with any national regulatory conditions.1 ScopeThis International Standard specifies physical and chemical tests on raw rubbers and standardized materials, a standardized test formulation, equipment, and processing methods for evaluating the v
21、ulcanization characteristics of all types of isobutene-isoprene rubber (IIR).2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated re
22、ferences, the latest edition of the referenced document (including any amendments) applies.ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain propertiesISO 247, Rubber Determination of ashISO 248-1, Rubber, raw Determination of volatile-matter content Part 1: Hot-mill
23、 method and oven methodISO 248-2, Rubber, raw Determination of volatile-matter content Part 2: Thermogravimetric methods using an automatic analyser with an infrared drying unitISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosityIS
24、O 1795:2007, Rubber, raw natural and raw synthetic Sampling and further preparative proceduresISO 2393, Rubber test mixes Preparation, mixing and vulcanization Equipment and proceduresISO 3417, Rubber Measurement of vulcanization characteristics with the oscillating disc curemeterISO 6502, Rubber Gu
25、ide to the use of curemetersISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods3 Sampling and further preparative procedures3.1 Selection of the sample from the lot shall be in accordance with ISO 1795.3.2 Take a laboratory sample of approximatel
26、y 1,5 kg by the method described in ISO 1795.3.3 Prepare test samples in accordance with ISO 1795. ISO 2014 All rights reserved 1BS ISO 2302:2014ISO 2302:2014(E)4 Physical and chemical tests on raw rubber4.1 Mooney viscosityPrepare a test sample in accordance with the preferred procedure in ISO 1795
27、, i.e. without milling, cutting the test sample directly from the laboratory sample. The test sample shall be as free as possible from air and pockets that may trap air against the rotor and die surface.If agreed between the interested parties or if the condition of the test sample (e.g. excessive p
28、orosity) makes milling necessary, it shall be performed in accordance with ISO 1795:2007, 7.3.2.2, paragraphs 1 and 2.Determine the Mooney viscosity in accordance with ISO 289-1 on this test portion, as ML(1+8) at 125 C.4.2 Volatile matterDetermine the volatile-matter content by the hot-mill method
29、or by the oven method as specified in ISO 248-1 or by the method specified in ISO 248-2.4.3 AshDetermine the ash in accordance with either method A or method B of ISO 247.5 Preparation of test mixes for evaluation of isobutene-isoprene rubbers5.1 Standard test formulationThe standard test formulatio
30、n 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 parties concerned.Table 1 Standard test formulationMaterial Parts by massIsobutene-isoprene rubber (II
31、R) 100,00Stearic acida1,00Industry reference blackb50,00Zinc oxidea3,00Sulfura1,75Tetramethylthiuram disulfide(TMTD)a1,00Total 156,75aPowder materials shall be used (standard curing ingredients used in the industry).bThe current industry reference black shall be used.5.2 Procedure5.2.1 Equipment and
32、 procedureThe equipment and procedure for the preparation, mixing, and vulcanization shall be in accordance with ISO 2393.2 ISO 2014 All rights reservedBS ISO 2302:2014ISO 2302:2014(E)5.2.2 Mixing procedures5.2.2.1 GeneralThree alternative mixing procedures are specified, but in accordance with ISO
33、2393, the laboratory internal mixer procedure is preferred. method A: mill mixing; method B: single-stage mixing using a laboratory internal mixer (the preferred procedure); method C: two-stage mixing using a laboratory internal mixer for initial mixing and a mill for final mixing.NOTE These procedu
34、res might not give identical results.5.2.2.2 Method A Mixing with a laboratory millThe standard laboratory mill-batch mass, in grams, shall be based on four times the formulation mass (i.e. 4 156,75 g = 627 g). The surface temperature of the rolls shall be maintained at 45 C 5 C throughout the mixin
35、g.A good rolling bank at the nip of the rolls shall be maintained during mixing. If this is not obtained with the nip settings specified hereunder, small adjustments to the mill openings may be necessary.Duration (min)Cumulative time (min)a) Band the rubber with the mill opening set at 0,65 mm. 1,0
36、1,0b) Mix the carbon black and the stearic acid, and add evenly across the mill rolls at a uniform rate. Increase the mill opening at intervals to maintain a constant rolling bank. When all the carbon black has been incorporated, make a 3/4 cut from each side.Do not cut the batch while free carbon b
37、lack is evident in the bank or on the milling surface. Be certain to return to the batch any materials that drop through the mill.10,0 11,0c) Add the zinc oxide, the sulfur, and the TMTD. 3,0 14,0d) Make three alternating 3/4 cuts from each side. 2,0 16,0e) Cut the batch from the mill. Set the mill
38、opening to 0,8 mm and pass the rolled batch endwise through the mill six times.2,0 18,0f)Sheet the batch to approximately 6 mm and check-weigh the batch (see ISO 2393). If the mass of the batch differs from the theoretical value by more than +1,50,5%, discard the batch and re-mix.g) Remove sufficien
39、t material for curemeter testing.h) Sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring or dumbbell test pieces in accordance with ISO 37.i) After mixing, condition the batch for at least 2 h but not more than 24 h, if possible at
40、standard laboratory temperature and humidity as defined in ISO 23529. ISO 2014 All rights reserved 3BS ISO 2302:2014ISO 2302:2014(E)5.2.2.3 Method B Single stage mixing using a laboratory internal mixerFor laboratory internal mixers having a nominal capacities of 65 cm3to about 2 000 cm3, the batch
41、mass shall be equal to the nominal mixer capacity, in cubic centimetres, multiplied by the density of the compound. For each batch mixed, the laboratory internal mixer conditions shall be the same during the preparation of a series of identical mixes. At the beginning of each series of test mixes, a
42、 machine-conditioning batch shall be mixed using the same formulation as the mixes under test. The laboratory internal mixer shall be allowed to cool down to 60 C between the end of one test batch and the start of the next. The temperature control conditions shall not be altered during the mixing of
43、 a series of test batches.The mixing technique shall be such as to obtain a good dispersion of all the ingredients.The temperature of the batch discharged on completion of mixing shall not exceed 120 C. If necessary, adjust the batch mass or the mixer head starting temperature so that this condition
44、 is metIn the following procedure, compounding materials other than rubber and carbon black, may be added to the batch more precisely and with greater ease if they are previously blended together in the proportions required by the formulation. Such blends may be made using one of the following: a mo
45、rtar and pestle; a double-cone mixer (mix for 10 min with the intensifier bar turning); a blender (mix for five periods of 3 s each, scraping the inside of the blender to dislodge material stuck to the sides after each 3 s period) (a “Waring”-type blender has been found suitable for this method).CAU
46、TION If the mixing periods are longer than 3 s, the stearic acid may melt, thus preventing good dispersion.A general mixing procedure for the laboratory internal mixer is as follows:Duration (min)Cumulative time (min)a) Load the rubber, lower the ram, and allow the rubber to be masticated. 0,5 0,5b)
47、 Raise the ram and add the zinc oxide, sulfur, stearic acid and TMTD, tak-ing care to avoid any loss. Then add the carbon black. Sweep down the mixer throat and lower the ram.1,0 1,5c) Allow the batch to mix. 2,0 3,5d) Raise the ram, clean the mixer throat and the top of the ram, and lower the ram.0
48、,5 4,0e) Allow the batch to mix. 1,0 5,0f) Discharge the batch and immediately check the temperature with a suitable measuring device.g) The final temperature of the discharged batch after the cumulative mixing time of 5 min shall not exceed 120 C. If it does, discard the batch and repeat the proced
49、ure with a different batch mass or starting temperature.h) Pass the batch through a mill set at 50 C 5 C twice with a 3,0 mm mill opening.i)Check the batch mass (see ISO 2393) and record. If it differs from the theoretical value by more than +1505,%, discard the batch and re-mix.4 ISO 2014 All rights reservedBS ISO 2302:2014ISO 2302:2014(E)j) Cut out a test piece for determining the vulcanization characteristics in accordance with ISO 3417 or ISO 6502, if required. Condition the te
