1、BSI Standards PublicationBS ISO 4659:2014Styrene-butadiene rubber(carbon black or carbon blackand oil masterbatches) Evaluation procedureBS ISO 4659:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 4659:2014. It supersedes BS ISO 4659:2003 which is withdraw
2、n.The UK participation in its preparation was entrusted to Technical Committee PRI/50, Rubber - Raw, natural and synthetic, including latex and carbon black.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include
3、all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 85478 1 ICS 83.060 Compliance with a British Standard cannot confer immunity from legal obligations.This British
4、 Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2014.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e d ISO 2014Styrene-butadiene rubber (carbon black or carbon black and oil masterbatches) Evaluation procedureCaoutch
5、ouc butadine-styrne (mlanges-matres avec du noir de carbone ou avec du noir de carbone et de lhuile) Mthode dvaluationINTERNATIONAL STANDARDISO 4659Sixth edition 2014-10-01Reference number ISO 4659:2014(E)BS ISO 4659:2014ISO 4659:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO
6、 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, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requ
7、ested 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 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 4659:2014ISO 4659:2014(E) ISO 2014 All r
8、ights 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 viscosity . 24.2 Volatile matter . 24.3 Ash . 25 Preparation of test mixes for evaluation . 25.1 Standard test formula
9、tion . 25.2 Procedure 26 Evaluation of vulcanization characteristics by a curemeter test . 56.1 Using an oscillating-disc curemeter 56.2 Using a rotorless curemeter 57 Evaluation of tensile stress-strain properties of vulcanized test mixes . 68 Precision . 69 Test report . 6Annex A (informative) Pre
10、cision . 7Bibliography 9BS ISO 4659:2014ISO 4659:2014(E)ForewordISO (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.
11、 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-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Interna
12、tional Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The 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 differ
13、ent 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.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
14、 not be held responsible for identifying any or all such patent rights. Details of any patent rights 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
15、 information given for the convenience of users and does not constitute an endorsement.For an explanation 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)
16、see the following URL: Foreword - Supplementary informationThe committee responsible for this document 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 4659:2003)
17、, which has been technically revised with the following changes: Clause 2 has been updated. In 4.2, the method given in ISO 248-2 is now allowed. In 5.2.2.1, addition of a statement that the mixing with a laboratory internal mixer is the preferred procedure. Method B becomes “Single stage mixing wit
18、h a laboratory internal mixer”. In 5.2.2.3, advice on mixing with various sizes of laboratory internal mixer is given along with a general mixing procedure.iv ISO 2014 All rights reservedBS ISO 4659:2014INTERNATIONAL STANDARD ISO 4659:2014(E)Styrene-butadiene rubber (carbon black or carbon black and
19、 oil masterbatches) Evaluation procedureWARNING Persons using this International Standard 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 e
20、stablish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.1 ScopeThis International Standard specifies the following: physical and chemical tests on raw rubbers; standard materials, standard test formulations, equipment, and processing methods
21、for evaluating the vulcanization characteristics of styrene-butadiene rubber masterbatches with carbon black or with carbon black and oil.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dat
22、ed references, only the edition cited applies. 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, Rubber Determination of ashISO 248-1, Rubber,
23、raw Determination of volatile-matter 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 shearin
24、g-disc viscometer Part 1: Determination 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 characteristic
25、s with the oscillating disc curemeterISO 6502, Rubber Guide to the use of curemetersISO 11235, Rubber compounding ingredients Sulfenamide accelerators Test methodsISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods3 Sampling and further preparati
26、ve procedures3.1 Selection of the sample from the lot shall be in accordance with ISO 1795.3.2 Take a laboratory sample of approximately 1,5 kg by the method described in ISO 1795. ISO 2014 All rights reserved 1BS ISO 4659:2014ISO 4659:2014(E)3.3 Prepare test samples in accordance with ISO 1795.4 Ph
27、ysical and chemical tests on raw rubber4.1 Mooney viscosityPrepare a test sample in accordance with the preferred procedure in ISO 1795, i.e. without milling.If massing is deemed necessary, use a mill with its roll surfaces maintained at a temperature of 35 C 5 C and record this fact in the test rep
28、ort.Determine the Mooney viscosity in accordance with ISO 289-1. Record the result as ML(1 + 4) at 100 C.4.2 Volatile matterDetermine the volatile-matter content by the hot-mill method 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
29、 accordance with ISO 247.5 Preparation of test mixes for evaluation5.1 Standard test formulationThe standard test formulation is given in Table 1.The materials used shall be national or international standard reference materials. If no standard reference material is available, the materials to be us
30、ed shall be agreed between the interested parties.5.2 Procedure5.2.1 Equipment and procedureEquipment and procedure for the preparation, mixing, and vulcanization shall be in accordance with ISO 2393.5.2.2 Mixing procedure5.2.2.1 GeneralTwo alternative mixing procedures are specified, but in accorda
31、nce with ISO 2393, the laboratory internal mixer procedure is preferred: Method A: Mixing with a laboratory mill; Method B: Single-stage mixing using a laboratory internal mixer the preferred method.2 ISO 2014 All rights reservedBS ISO 4659:2014ISO 4659:2014(E)Table 1 Standard test formulation for e
32、valuation of masterbatches of styrene-butadiene rubbersMaterial Parts by massMasterbatchZinc oxideSulfurStearic acidTBBS c100 + xa+ yb3,001,751,501,25Total 107,50 + x + yax is the number of parts of carbon black to 100 parts of rubber in the masterbatch.by is the number of parts of oil to 100 parts
33、of rubber in the masterbatch.cN-tert-butyl-benzothiazole-2-sulfenamide. This shall be supplied in powder form having an initial insoluble-matter content, determined in accordance with ISO 11235, of less than 0,3 %. The material shall be stored at room temperature in a closed container and the insolu
34、ble matter shall be checked every 6 months. If this is found to exceed 0,75 %, the TBBS shall be discarded or recrystallized.5.2.2.2 Method A Mixing with a laboratory millThe standard laboratory mill batch mass factor shall be selected to the nearest 0,5 to give as large a total mass as possible tha
35、t does not exceed 525 g. The surface temperature of the rolls shall be maintained at 50 C 5 C throughout the mixing.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
36、 may be necessary.Duration (min)Cumulative time (min)a) Band the masterbatch with the mill opening set at 1,4 mm. 2,0 2,0b) Add the sulfur slowly and evenly across the masterbatch. 2,0 4,0c) Add the stearic acid. Make one 3/4 cut from each side. 2,0 6,0d) Add the zinc oxide and the TBBS. 3,0 9,0e) M
37、ake three 3/4 cuts from each side. 2,0 11,0f) Cut the batch from the mill. Set the mill opening to 0,8 mm and pass the rolled batch endwise between the rolls six times.2,0 13,0Total time 13,0 13,0g) Sheet the batch to approximately 6 mm and determine the mass of the batch (see ISO 2393). If the mass
38、 of the batch differs from the theoretical value by more than +1505,%, discard the batch and re-mix.h) Remove sufficient material for curemeter testing.i) Sheet the batch to approximately 2,2 mm for preparing test sheets or to the appropriate thickness for preparing ISO ring specimens in accordance
39、with ISO 37.j) Leave the batch for 2 h to 24 h after mixing, if possible at standard temperature and humidity as defined in ISO 23529. ISO 2014 All rights reserved 3BS ISO 4659:2014ISO 4659:2014(E)5.2.2.3 Method B Single stage mixing using a laboratory internal mixerFor laboratory internal mixers ha
40、ving nominal capacities of 65 cm3to about 2 000 cm3, the batch 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 id
41、entical mixes. At the beginning of each series of test mixes, a 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 temperatu
42、re control conditions shall 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 mas
43、s or the mixer starting temperature so that this condition is metIn the following procedure, compounding materials other than masterbatch, 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 blend
44、s may be made using one of the following: a mortar 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 blende
45、r has been found suitable for this method).CAUTION If the mixing periods are longer than 3 s, the stearic acid may melt, thus preventing good dispersion.NOTE The following is a general mixing procedure for the laboratory internal mixer.Duration (min)Cumulative time (min)a) Load the mixing chamber wi
46、th the masterbatch, lower the ram and start the timer.b) Masticate the masterbatch. 0,5 0,5c) Raise the ram and add the pre-blended zinc oxide, sulfur, stearic acid and TBBS. Sweep in any powder round the mouth of the mixing chamber, taking care to avoid any losses. Lower the ram.0,5 1,0d) Allow the
47、 batch to mix. 5,0 6,0Total time 6,0 6,0e) Turn off the rotors, raise the ram, open the mixing chamber and discharge the batch. Record the maximum batch temperature indicated, if desired.f) Pass the batch through a laboratory mill set at 50 C 5 C, once with the mill opening set at 0,5 mm then twice
48、with the mill opening set at 3 mm.g) Check-weigh the batch and record the mass. If it differs from the theoretical value by more than +1505,%, discard the batch.h) Leave the batch for 2 h to 24 h after mixing and prior to vulcanizing, if possible at standard tem-perature and humidity as defined in I
49、SO 23529.4 ISO 2014 All rights reservedBS ISO 4659:2014ISO 4659:2014(E)For a laboratory internal mixer having a nominal mixing capacity of 65 cm3, a batch mass corresponding to 0,47 times the formulation mass (i.e. 0,47 156,75 = 73,67 g) has been found to be suitable.Prepare the masterbatch by passing it through a laboratory mill once with the roll temperature set at 50 C 5 C and with an opening that will give an approximately 5 mm thick sheet. Cut i
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