BS ISO 289-1-2015 Rubber unvulcanized Determinations using a shearing-disc viscometer Determination of Mooney viscosity《未硫化橡胶 用剪切圆盘型粘度计进行测定 穆尼粘度的测定》.pdf

1、BSI Standards PublicationBS ISO 289-1:2015Rubber, unvulcanized Determinations using ashearing-disc viscometerPart 1: Determination of Mooney viscosityBS ISO 289-1:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 289-1:2015. It supersedes BS ISO 289-1:2014 w

2、hich is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/22, Physical testing of rubber.A list of organizations represented on this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 provision

3、s of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 89162 5 ICS 83.060 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published und

4、er the authority of the Standards Policy and Strategy Committee on 30 September 2015.Amendments/corrigenda issued since publicationDate Text affectedBS ISO 289-1:2015 ISO 2015Rubber, unvulcanized Determinations using a shearing-disc viscometer Part 1: Determination of Mooney viscosityCaoutchouc non

5、vulcanis Dterminations utilisant un consistomtre disque de cisaillement Partie 1: Dtermination de lindice consistomtrique MooneyINTERNATIONAL STANDARDISO289-1Fourth edition2015-09-01Reference numberISO 289-1:2015(E)BS ISO 289-1:2015ISO 289-1:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED

6、DOCUMENT ISO 2015, 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 writ

7、ten permission. 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 289-1:2015

8、ISO 289-1:2015(E)Foreword iv1 Scope . 12 Normative references 13 Principle 14 Apparatus . 14.1 Typical shearing-disc viscometer . 14.2 Dies 24.3 Rotor 24.4 Heating device . 24.5 Temperature-measurement system . 54.6 Die-closure system. 54.7 Torque-measurement device and calibration of the device . 6

9、5 Preparation of test piece 76 Temperature and duration of test 77 Procedure. 78 Expression of results 89 Precision . 810 Test report . 8Annex A (informative) Precision statement .10Annex B (informative) Heat-stable film for Mooney viscosity measurements 13Annex C (normative) Calibration schedule .1

10、6 ISO 2015 All rights reserved iiiContents PageBS ISO 289-1:2015ISO 289-1:2015(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

11、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-governmental, in liaison with ISO, also take part in the work. ISO collaborates

12、 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 ISO/IEC Directives, Part 1. In particular the different approval crite

13、ria 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.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of

14、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 declarations received (see www.iso.org/patents).Any trade name u

15、sed 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 about ISOs adherence to the WTO principles in the Technical B

16、arriers to Trade (TBT) see the following URL: Foreword - Supplementary Information The committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis.This fourth edition cancels and replaces the third edition (ISO 289-1:2014), which has been

17、 technically revised to improve the calibration schedule.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 Part 2: Determination of pre-vulcanization characteristics Part 3:

18、 Determination of the Delta Mooney value for non-pigmented, oil-extended emulsion-polymerized SBR Part 4: Determination of the Mooney stress-relaxation rateiv ISO 2015 All rights reservedBS ISO 289-1:2015INTERNATIONAL STANDARD ISO 289-1:2015(E)Rubber, unvulcanized Determinations using a shearing-dis

19、c viscometer Part 1: Determination of Mooney viscosityWARNING 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 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 part of ISO 289 specifies a method using a shearing-disc viscometer for measuring the Mooney viscosity of uncompounded or compounded rubbers.2 Normative referencesThe followi

21、ng 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 references, the latest edition of the referenced document (including any amendments) applies.ISO 1795, Rubber, r

22、aw natural and raw synthetic Sampling and further preparative proceduresISO 2393, Rubber test mixes Preparation, mixing and vulcanization Equipment and proceduresISO 6508-1, Metallic materials Rockwell hardness test Part 1: Test methodISO/TR 9272, Rubber and rubber products Determination of precisio

23、n for test method standardsISO 18899:2013, Rubber Guide to the calibration of test equipmentISO 23529, Rubber General procedures for preparing and conditioning test pieces for physical test methods3 PrincipleThe torque which has to be applied under specified conditions in order to rotate a metal dis

24、c in a cylindrical chamber formed from mating dies filled with rubber is measured. The resistance offered by the rubber to this rotation is expressed in arbitrary units as the Mooney viscosity of the test piece.4 Apparatus4.1 Typical shearing-disc viscometerA typical shearing-disc viscometer (see Fi

25、gure 1), consisting ofa) two dies to form a cylindrical cavity,b) a rotor,c) a means for maintaining the dies at a constant temperature,d) a means for maintaining a specified closure pressure, ISO 2015 All rights reserved 1BS ISO 289-1:2015ISO 289-1:2015(E)e) a means for rotating the rotor at consta

26、nt angular velocity, andf) a means for indicating the torque required to rotate the rotor.The rotor and die cavity have the dimensions shown in Table 1.Table 1 Dimensions of essential parts of the apparatusPartDimensionmmRotor diameter 38,10 0,03Rotor thickness 5,54 0,03Die cavity diameter 50,9 0,1D

27、ie cavity depth 10,59 0,03NOTE Normally, a rotor with these dimensions is called a large rotor.It is permissible to use a smaller rotor where high viscosity makes this necessary. This small rotor shall have the same dimensions as the large rotor except that the diameter shall be 30,48 mm 0,03 mm. Re

28、sults obtained with the small rotor are not identical with those obtained using the large rotor.4.2 DiesThe two dies forming the cavity shall be formed from non-deforming unplated hardened steel of minimum Rockwell hardness 60 HRC (see ISO 6508-1). The dimensions of the cavity are given in Figure 1

29、and shall be measured from the highest surfaces. For good heat transfer, each die should preferably be made from only one piece of steel. The flat surfaces shall have radial V-grooves to prevent slippage. The grooves shall be spaced radially at 20 intervals and shall extend from an outer circle of d

30、iameter 47 mm to an inner circle of diameter 7 mm for the upper die and to within 1,5 mm of the hole in the lower die. Each groove shall form a 90 angle in the die surface with the bisector of the angle perpendicular to the surface and shall be 1,0 mm 0,1 mm wide at the surface (see Figure 2).4.3 Ro

31、torThe rotor shall be fabricated from non-deforming unplated hardened steel of minimum Rockwell hardness 60 HRC. The rotor surfaces shall have rectangular-section grooves 0,80 mm 0,02 mm wide, of uniform depth 0,30 mm 0,05 mm, and spaced 1,60 mm 0,04 mm apart (distance between central axes). The fla

32、t surfaces of the rotor shall have two sets of such grooves at right angles to each other (see Figure 3). The edge of the rotor shall have vertical grooves of the same dimensions. The large rotor shall have 75 vertical grooves and the small rotor shall have 60. The rotor is fastened at right angles

33、to a shaft having a diameter of 10 mm 1 mm and a length such that, in the closed die cavity, the clearance above the rotor does not differ from that below by more than 0,25 mm. The rotor shaft shall bear on the spindle which turns the rotor shaft not on the wall of the die cavity. The clearance at t

34、he point where the rotor shaft enters the cavity shall be small enough to prevent the rubber from leaving the cavity. A grommet, O-ring, or other sealing device can be used as a seal at this point.The eccentricity or runout of the rotor while turning in the viscometer shall not exceed 0,1 mm.The ang

35、ular velocity of the rotor shall be 0,209 rad/s 0,002 rad/s (2,00 r/min 0,02 r/min).4.4 Heating deviceThe dies are mounted on, or form part of, platens equipped with a heating device capable of maintaining the temperature of the platens and that of the dies to within 0,5 C of the test temperature. A

36、fter 2 ISO 2015 All rights reservedBS ISO 289-1:2015ISO 289-1:2015(E)insertion of the test piece, the devices shall be capable of returning the temperature of the dies to within 0,5 C of the test temperature within 4 min.NOTE Older machines might not comply with these requirements and might give les

37、s reproducible results.Dimensions in millimetresKey1 die cavity2 rotor3 temperature sensor4 sealing deviceFigure 1 Typical shearing-disc viscometer ISO 2015 All rights reserved 3BS ISO 289-1:2015ISO 289-1:2015(E)Dimensions in millimetresKeyaSection through groove.Figure 2 Die with radial V-groovesDi

38、mensions in millimetresKeyaR at edge of groove 0,1 mm.Figure 3 Rotor with rectangular-section grooves4 ISO 2015 All rights reservedBS ISO 289-1:2015ISO 289-1:2015(E)4.5 Temperature-measurement system4.5.1 The test temperature is defined as the steady-state temperature of the closed dies with the rot

39、or in place and the cavity empty. This temperature is measured by two thermocouple measurement probes which can be inserted into the cavity for this purpose as shown in Figure 4. These measurement probes are also used to check the temperature of the test piece as described in 7.2.4.5.2 In order to c

40、ontrol the supply of heat to the dies, a temperature sensor shall be present in each die to measure the die temperature. The sensor shall be located for the best possible heat contact with the dies, i.e. heat gaps and other heat resistance shall be excluded. The axes of the sensors shall be at a dis

41、tance of 3 mm to 5 mm from the working surface of the dies and 15 mm to 20 mm from the rotational axis of the rotor (see Figure 1).4.5.3 Both the thermocouple measurement probes and the temperature sensors shall be capable of indicating temperature to an accuracy of 0,25 C.4.6 Die-closure systemThe

42、dies could be closed and held closed by hydraulic, pneumatic, or mechanical means. A force of 11,5 kN 0,5 kN shall be maintained on the dies during the test.A greater force can be required to close the dies when rubbers of high viscosity are tested. At least 10 s before starting the viscometer, the

43、force shall be reduced in such cases to 11,5 kN 0,5 kN and maintained at this level throughout the test.For all types of closing device, a piece of soft tissue paper not thicker than 0,04 mm placed between the mating surfaces shall show a continuous pattern of uniform intensity when the dies are clo

44、sed. A non-uniform pattern indicates incorrect adjustment of the die closure, worn or faulty mating surfaces, or distortion of the dies. Any of these conditions might result in leakage and erroneous results. ISO 2015 All rights reserved 5BS ISO 289-1:2015ISO 289-1:2015(E)Dimensions in millimetresKey

45、1 measurement probe, withdrawn2 measurement probe, inserted3 stop connected to apparatus4 stop connected to measurement probeFigure 4 Measurement-probe design4.7 Torque-measurement device and calibration of the deviceThe torque required to turn the rotor is recorded or indicated on a linear scale gr

46、aduated in Mooney units. The reading shall be zero when the machine is run empty and 100 0,5 when a torque of 8,30 Nm 0,02 Nm is applied to the rotor shaft. Therefore, a torque of 0,083 Nm is equivalent to one Mooney unit. The scale shall be capable of being read to 0,5 Mooney units. Variation from

47、zero shall be less than 0,5 Mooney units when the machine is running with the rotor in place and the dies closed and empty.If the viscometer is equipped with a rotor-ejection spring, the zero calibration shall be made with the dies open so that the rotor is not pressing against the upper die.The vis

48、cometer shall be calibrated while the machine is running at the test temperature. A suitable method for the calibration of most machines is as follows.The scale is calibrated to a reading of 100 by applying certified masses fastened with flexible wire to an appropriate rotor. During calibration, the

49、 rotor is turned at 0,209 rad/s and the platens are at the specified test temperature.NOTE In order to check linearity, intermediate masses can be used to give scale readings of 25 Mooney units, 50 Mooney units, and 75 Mooney units, respectively. In addition, a sample of butyl rubber of certified Mooney viscosity can be used to check whether or not the machine is working correctly. Measurement can be carried out at 100 C or 125 C for 8 min.6 ISO 2015 All ri