1、BSI Standards PublicationBS ISO 289-2:2016Rubber, unvulcanized Determinations using a shearing-disc viscometerPart 2: Determination of pre-vulcanization characteristicsBS ISO 289-2:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 289-2:2016.The UK participa
2、tion in its preparation was entrusted to Technical Committee PRI/22, Testing and analysis of rubber.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are res
3、ponsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 89163 2 ICS 83.060 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Stand
4、ards Policy and Strategy Committee on 31 March 2016.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 289-2:2016 ISO 2016Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 2: Determination of pre-vulcanization characteristicsCaoutchouc non vulcanis Dtermina
5、tions utilisant un consistomtre disque de cisaillement Partie 2: Dtermination des caractristiques de prvulcanisationINTERNATIONAL STANDARDISO289-2Second edition2016-02-15Reference numberISO 289-2:2016(E)BS ISO 289-2:2016ISO 289-2:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO
6、 2016, Published in SwitzerlandAll 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 permissi
7、on. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 289-2:2016ISO 289-2:20
8、16(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Apparatus . 26 Calibration schedule . 27 Preparation of test specimen 28 Test temperature 29 Procedure. 210 Precision . 311 Test report . 3Annex A (normative) Calibration schedule . 5Annex B (informative) Pr
9、ecision results from an interlaboratory test programme . 6Bibliography 8 ISO 2016 All rights reserved iiiContents PageBS ISO 289-2:2016ISO 289-2:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The wor
10、k 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-governme
11、ntal, 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 intended for its further maintenance are described in the
12、 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. www.iso.org/directivesAttention is drawn to the possibility
13、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 will be in the Introduction and/or on the ISO list of patent
14、 declarations received. www.iso.org/patentsAny 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 expressions related to conformity assessment, as well as information ab
15、out 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, Subcommittee SC 2, Testing and analysis.This second edition cancels and
16、replaces the first edition (ISO 289-2:1994), which has been technically revised. The following changes have been incorporated: a calibration schedule has been added in Annex A; a precision clause has been moved to Annex B; the introductory statements concerning safety and environmental caution have
17、been added; the layout of the test report clause has been changed in accordance with ISO/TC 45/SC 2 internal agreements.ISO 289 consists of the following parts, under the general title Rubber, unvulcanized Determinations using a shearing-disc viscometer: Part 1: Determination of Mooney viscosity Par
18、t 2: Determination of pre-vulcanization characteristics Part 3: Determination of the Delta Mooney value for non-pigmented, oil-extended emulsion-polymerized SBR Part 4: Determination of the Mooney stress-relaxation rateiv ISO 2016 All rights reservedBS ISO 289-2:2016INTERNATIONAL STANDARD ISO 289-2:
19、2016(E)Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 2: Determination of pre-vulcanization characteristicsWARNING 1 Persons using this part of ISO 289 should be familiar with normal laboratory practice. This part of ISO 289 does not purport to address all of the safety pr
20、oblems, 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 national regulatory conditions.WARNING 2 Certain procedures specified in this part of ISO 289 might involve the use or generation of su
21、bstances, or the generation of waste, that could constitute a local environmental hazard. Reference should be made to appropriate documentation on safe handling and disposal after use.1 ScopeThis part of ISO 289 specifies a method for determining the pre-vulcanization characteristics of compounded r
22、ubber.The pre-vulcanization characteristics determined by this method provide a means of estimating how long compounded rubber can be maintained at high temperatures and remain processable.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document
23、 and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 289-1, Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determina
24、tion of Mooney viscosityISO 18899, Rubber Guide to the calibration of test equipment3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1pre-vulcanization timescorch timetime including warm-up time, for the viscosity to increase by a specified amount
25、 from the minimum valueNote 1 to entry: Expressed in minutes.4 PrincipleThe test consists of determining how the Mooney viscosity of the rubber compound changes with running time at a specified temperature relevant to the process for which the compound is to be used. The time at which the Mooney vis
26、cosity has increased by a specified number of units is recorded. ISO 2016 All rights reserved 1BS ISO 289-2:2016ISO 289-2:2016(E)5 ApparatusThe apparatus specified in ISO 289-1 shall be used. It is permissible to use the small rotor for high-viscosity compounds.6 Calibration scheduleSee Annex A.7 Pr
27、eparation of test specimenPrepare the two discs comprising the test specimen from a sheet of rubber compound, using the procedure for preparation of test pieces described in ISO 289-1.8 Test temperatureChoose a test temperature relevant to the process for which the compound is to be used.9 Procedure
28、Use the procedure described in ISO 289-1. The pre-heating time shall be 1 min, and the test shall be continued until the viscosity reaches the specified number of units above the minimum. When a large rotor is used, the increase is specified as five units and when a small rotor is used, the increase
29、 is specified as three units. The corresponding pre-vulcanization times are designated t5and t3, respectively. A typical trace obtained with the large rotor is shown in Figure 1.2 ISO 2016 All rights reservedBS ISO 289-2:2016ISO 289-2:2016(E)Key1 rotor started2 minimum viscosity valueX time (in minu
30、tes)Y Mooney viscosity (in Mooney units)Figure 1 Determination of the pre-vulcanization or scorch time using the large rotor (increase in viscosity = 5 units)10 PrecisionSee Annex B.11 Test reportThe test report shall include the following information:a) sample details:1) full description of the sam
31、ple and its origin;2) details of compounded rubbers, if applicable;b) details of the preparation of the test pieces,c) a reference to this part of ISO 289, i.e. ISO 289-2;d) a description of the apparatus used, including the model used, the manufacturer of the apparatus and the rotor size (large or
32、small), ISO 2016 All rights reserved 3BS ISO 289-2:2016ISO 289-2:2016(E)e) test details:1) the test temperature;2) the die-closing force, if other than 11,5 kN;3) details of any procedures not specified in this part of ISO 289;f) test results:1) the minimum viscosity, in Mooney units;2) the pre-vulc
33、anization or scorch time (t5or t3), in minutes;g) date(s) of test.4 ISO 2016 All rights reservedBS ISO 289-2:2016ISO 289-2:2016(E)Annex A (normative) Calibration scheduleA.1 InspectionBefore any calibration is undertaken, the condition of the items to be calibrated shall be ascertained by inspection
34、 and recorded in any calibration report or certificate. It shall be reported whether calibration was carried out in the “as-received” condition or after rectification of any abnormality or fault.It shall be ascertained that the apparatus is generally fit for the intended purpose, including any param
35、eters specified as approximate and for which the apparatus does not therefore need to be formally calibrated. If such parameters are liable to change, then the need for periodic checks shall be written into the detailed calibration procedures.A.2 ScheduleVerification/calibration of the test apparatu
36、s is a mandatory part of this International Standard. However, the frequency of calibration and procedures used are, unless otherwise stated, at the discretion of the individual laboratory, using ISO 18899 for guidance.The calibration schedule is given in ISO 289-1. ISO 2016 All rights reserved 5BS
37、ISO 289-2:2016ISO 289-2:2016(E)Annex B (informative) Precision results from an interlaboratory test programmeB.1 GeneralThe following interlaboratory test programme (ITP) was initially carried out in 1987.All calculations to provide repeatability and reproducibility values were performed in accordan
38、ce with ISO/TR 92721. Precision concepts and nomenclature are also given in ISO/TR 9272.B.2 Programme detailsDuplicate test pieces of the following compounded rubbers were sent to all participating laboratories: chloroprene (CR), EPDM (highly loaded), fluororubber (FKM) and SBR 1500 including 50 par
39、ts per hundred (mass of rubber) N550 black1).Pre-vulcanization characteristic determinations (single measurement) were made on two separate days (one week apart), one determination on each day. The test conditions were as follows: for CR and EPDM compounds 120 C and the small rotor; for FKM compound
40、 150 C and the large rotor; for SBR compound 170 C and the small rotor. A total of 16 laboratories participated.This ITP corresponds to a type 1 precision evaluation, with no preparation or processing steps in the participating laboratories.B.3 Precision resultsB.3.1 The precision results are given
41、in Table B.1.1) Designation according to ASTM D1765-89, Standard classification System for carbon blacks used in rubber products.6 ISO 2016 All rights reservedBS ISO 289-2:2016ISO 289-2:2016(E)Table B.1 Precision of pre-vulcanization characteristic determinationsRubber material AverageWithin lab Bet
42、ween labr (r) R (R)Minimum viscosity (Mooney torque units)SBRCRFKMEPDM22,022,346,160,31,031,282,811,944,705,756,113,233,064,967, 2011,1013,922,215,618,4Pooled values 37,7 1,88 4,99 7,23 19,2Pre-vulcanization time (min)SBRCRFKMEPDM5,2314,808,9720,800,341,821,275,326,4112,3014,2025,502,557, 553,8811,6
43、048,850,943,355,5Pooled values 12,50 2,89 23,10 7,28 58,1B.3.2 The symbols used in Table B.1 are defined as follows:r repeatability (in Mooney units);(r) repeatability (in percent of mean level);R reproducibility (in Mooney units);(R) reproducibility (in percent of mean level). ISO 2016 All rights r
44、eserved 7BS ISO 289-2:2016ISO 289-2:2016(E)Bibliography1 ISO/TR 9272, Rubber and rubber products Determination of precision for test method standards8 ISO 2016 All rights reservedBS ISO 289-2:2016BS ISO 289-2:2016ISO 289-2:2016(E) ISO 2016 All rights reservedICS 83.060Price based on 8 pagesThis page
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