1、BSI Standards PublicationBS ISO 2476:2014Butadiene rubber (BR) Solution-polymerized types Evaluation proceduresBS ISO 2476:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 2476:2014. Itsupersedes BS ISO 2476:2009 which is withdrawn.The UK participation in i
2、ts preparation was 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
3、 a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 79384 4ICS 83.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the a
4、uthority of theStandards Policy and Strategy Committee on 28 February 2014.Amendments issued since publicationDate Text affectedBS ISO 2476:2014 ISO 2014Butadiene rubber (BR) Solution-polymerized types Evaluation proceduresCaoutchouc butadine (BR) Types polymriss en solution Mthodes dvaluationINTERN
5、ATIONAL STANDARDISO2476Sixth edition2014-03-01Reference numberISO 2476:2014(E)BS ISO 2476:2014ISO 2476:2014(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 an
6、y form or by any means, electronic or mechanical, including 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
7、 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 2476:2014ISO 2476:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Sampling and further preparative procedures . 14
8、 Physical and chemical tests on raw rubber 24.1 Mooney viscosity . 24.2 Volatile matter . 24.3 Ash . 25 Preparation of test mixes for evaluation of butadiene rubbers 25.1 Standard test formulations . 25.2 Procedure 36 Conditioning of batches . 87 Evaluation of vulcanization characteristics . 87.1 Us
9、ing an oscillating-disc curemeter 87.2 Using a rotorless curemeter 88 Evaluation of tensile stress-strain properties of vulcanized test mixes . 99 Precision . 910 Test report . 9Annex A (informative) Precision 10Bibliography .15BS ISO 2476:2014ISO 2476:2014(E)ForewordISO (the International Organizat
10、ion 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 body interested in a subject for which a technical committee has been established h
11、as 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 Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The
12、procedures used to develop this document and those intended 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 edi
13、torial rules of the ISO/IEC Directives, Part 2 (see www.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 ri
14、ghts identified during the development of the document will 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 ex
15、planation on the meaning of ISO specific terms and expressions 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 do
16、cument is ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.This sixth edition cancels and replaces the fifth edition (ISO 2476:2009), which has been technically revised with the following changes: ISO 2476 has been aligned with
17、ISO 2393:2014; 5.2.2.1 states that the laboratory internal mixer procedure is the preferred method.iv ISO 2014 All rights reservedBS ISO 2476:2014INTERNATIONAL STANDARD ISO 2476:2014(E)Butadiene rubber (BR) Solution-polymerized types Evaluation proceduresWARNING Persons using this International Stan
18、dard should be familiar with 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 appropriate safety and health practices and to ensure compliance with any na
19、tional regulatory conditions.1 ScopeThis International Standard specifies: physical and chemical tests on raw rubbers; standard materials, standard test formulations, equipment, and processing methods for evaluating the vulcanization characteristics of solution-polymerized butadiene rubbers (BR), in
20、cluding oil-extended types (OEBR), and the tensile stress-strain properties of vulcanized mixes.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 appl
21、ies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 37, Rubber, vulcanized or thermoplastic Determination of tensile stress-strain propertiesISO 247:2006, Rubber Determination of ashISO 248-1, Rubber, raw Determination of volatile-matter
22、content Part 1: Hot-mill 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: Determinati
23、on of Mooney viscosityISO 1795, 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 curemeter
24、ISO 6502, Rubber Guide 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 Take a laboratory sample of approximately 1,5 kg by the method described in ISO 1795.3.2 Prepare te
25、st samples in accordance with ISO 1795. ISO 2014 All rights reserved 1BS ISO 2476:2014ISO 2476:2014(E)4 Physical and chemical tests on raw rubber4.1 Mooney viscosityDetermine the Mooney viscosity in accordance with ISO 289-1 on a test sample prepared as indicated in ISO 1795 (preferably without mill
26、ing). If milling is necessary, maintain the mill roll surface temperature at 35 C 5 C. Record the result as ML(1 + 4) at 100 C.4.2 Volatile matterDetermine the volatile-matter content in accordance with ISO 248-1 and ISO 248-2.4.3 AshDetermine the ash in accordance with ISO 247.5 Preparation of test
27、 mixes for evaluation of butadiene rubbers5.1 Standard test formulationsTwo standard test formulations are given in Table 1. The materials used shall be national or International Standard reference materials (or, if no standard reference material is available, as agreed by the interested parties).Ta
28、ble 1 Standard test formulationsMaterialParts mass fractionNon-oil-extended Oil-extendedButadiene rubberZinc oxideIRBbStearic acidASTM 103 oilcSulfurTBBSd100,003,0060,002,0015,001,500,90100,00 + Ya3,000,6 (100 + Y)2,001,500,009 (100 + Y)Total 182,40 167,40 + 1,609YCalculated density, g/cm31,11 aY =
29、parts of oil, mass fraction, per 100 parts of base polymer in the oil-extended rubber.bUse the current industrial reference black. Dry the material for 1 h at 125 C 3 C and store in a tightly closed container.cThis oil, density 0,92 g/cm3, is produced by the Sun Refining and Marketing Company and di
30、stributed by R.E. Carroll, Inc., 1570 North Olden Avenue Ext, Trenton, NJ 08638-3204, USA. Overseas requests should be directed to Sunoco Overseas, Inc., 1801 Market Street, Philadelphia, PA 19103-1699, USA. This is an example of a suitable product available commercially. This information is given f
31、or convenience of users of this document and does not constitute an endorsement by ISO of this product. Alternative oils can be used, but might give slightly different results.dN-tert-butylbenzothiazole-2-sulfenamide. This is supplied in powder form having an initial insoluble-matter content, determ
32、ined in accordance with ISO 11235, of less than 0,3 %. The material shall be stored at room temperature in a closed container and the insoluble matter checked every 6 months. If this is found to exceed 0,75 %, the material shall be discarded or recrystallized.2 ISO 2014 All rights reservedBS ISO 247
33、6:2014ISO 2476:2014(E)5.2 Procedure5.2.1 GeneralThe equipment and procedure for the preparation, mixing, and vulcanization shall be in accordance with ISO 2393.5.2.2 Mixing procedures5.2.2.1 GeneralFive mixing procedures are specified, a procedure using a laboratory internal mixer is preferred. meth
34、od A1: single-stage mixing using a laboratory internal mixer; method A2: two-stage mixing using a laboratory internal mixer for both initial and final mixing; method B: two-stage mixing using a laboratory internal mixer for initial mixing and a mill for final mixing.The smaller laboratory internal m
35、ixers do not provide enough compound for the final mill mixing since a batch mass of four times the formula mass is required. In these cases, the laboratory internal mixer should be used for the final mixing. The mixer head starting temperature or the batch mass can be adjusted, so that the final te
36、mperature of the discharged batch does not exceed 120 C. method C1 and C2: mill mixing.NOTE 1 These procedures can give different results.NOTE 2 Mill mixing of solution-polymerized butadiene rubbers is more difficult than with other rubbers, and mixing is best accomplished by using an internal mixer
37、. With some types of butadiene rubber, it is not possible to obtain a satisfactory mix using a mill-mixing procedure.5.2.2.2 Method A1 Single-stage mixing using a laboratory internal mixerFor laboratory internal mixers having nominal capacities of 65 cm3to about 2 000 cm3, the batch mass shall be eq
38、ual 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 machine-conditi
39、oning batch shall be mixed using the same formulation as the mixes under test. The laboratory internal mixer shall be allowed to cool down to a specified temperature (60 C has been found to be suitable) between the end of one test batch and the start of the next. The temperature control conditions s
40、hall not be altered during the mixing of 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 sta
41、rting temperature so that this condition is met.NOTE 1 The mixing conditions given in Table A.7 for various sizes of laboratory internal mixer might be helpful.NOTE 2 A general mixing procedure for the laboratory internal mixer is as follows: ISO 2014 All rights reserved 3BS ISO 2476:2014ISO 2476:20
42、14(E)Duration (min)Cumulative time (min)a) Charge the chamber with the rubber. Lower the ram. b) Masticate the rubber. 1,0 1,0c) Raise the ram and add the zinc oxide, the oil, the stearic acid, and half of the carbon black. Then sweep the orifice and lower the ram.1,0 2,0d) Raise the ram and add the
43、 TBBS, the sulfur, and the rest of the carbon black. Then sweep the orifice and lower the ram.1,0 3,0e) Allow the batch to mix. 6,0 9,0f) Turn off the motor, raise the ram, remove or open the mixing chamber, and discharge the batch. Record the maximum batch temperature.With some types of mixer, the
44、rotors might need to be turning in order to discharge the batch.Immediately after discharging the mixed batch, pass it through a mill at 50 C 5 C once at a 0,5 mm mill opening, and then twice at a 3,0 mm mill opening.Determine the batch mass and record it. If it differs from the theoretical value by
45、 more than +0,5 % or 1,5 %, discard the batch.Prepare a test piece for determining the vulcanization characteristics in accordance with ISO 3417 or ISO 6502, if required. Condition the test piece for 2 h to 24 h, if possible at a standard temperature and humidity as defined in ISO 23529 before testi
46、ng.If required, sheet the batch to approximately 2,2 mm for preparing test sheets or the appropriate thickness for preparing ring pieces in accordance with ISO 37. To obtain a grain effect, pass the lengthwise-folded batch in the same direction four times between mill rolls set at an opening between
47、 2,1 mm and 2,5 mm and a temperature of 50 C 5 C.5.2.2.3 Method A2 Two-stage mixing using a laboratory internal mixer for both initial and final mixing5.2.2.3.1 Stage 1 Initial mixing procedureSee 5.2.2.2.The final temperature of the batch shall not exceed 170 C. If necessary, adjust the batch mass
48、or the mixer head starting temperature so that this condition is met.NOTE A general mixing procedure for initial mixing using a laboratory mixer is as follows:4 ISO 2014 All rights reservedBS ISO 2476:2014ISO 2476:2014(E)Duration (min)Cumulative time (min)a) Adjust the temperature to 50 C 5 C and th
49、e rotor speed and ram pressure of the laboratory internal mixer so that the batch will be discharged under the conditions outlined in e) below. Close the discharge gate, start the motor, and raise the ram. b) Load one-half of the rubber, followed by the zinc oxide, the carbon black, the oil (omit from oil-extended BR), the stearic acid, and the balance of the rub-ber. Lower the ram.0,5 0,5c) Allow the batch to mix. 3,0 3,5d) Raise the ram and clean the mixer t
