BS ISO 6502-2016 Rubber Guide to the use of curemeters《橡胶 硫化计的使用指南》.pdf

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1、BSI Standards PublicationBS ISO 6502:2016Rubber Guide to the use ofcuremetersBS ISO 6502:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 6502:2016. It supersedes BS 903-A60.1:2000 which is withdrawn.The UK participation in its preparation was entrusted to

2、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 responsible for its correct application. The

3、 British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 89437 4 ICS 83.060 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 29 F

4、ebruary 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 6502:2016 ISO 2016Rubber Guide to the use of curemetersCaoutchouc Guide pour lemploi des rhomtresINTERNATIONAL STANDARDISO6502Fourth edition2016-01-15Reference numberISO 6502:2016(E)BS ISO 6502:2016ISO 6502

5、:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 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

6、 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 officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +

7、41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 6502:2016ISO 6502:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Basic principles 25 Types of curemeter 46 Apparatus . 46.1 General . 46.2 Die cavity 46.3 Die closure 56.4 Moving member . 56.5 Movement

8、56.6 Stiffness measurement . 66.7 Heating and temperature control . 66.8 Calibration 67 Test piece 68 Vulcanization temperature 69 Conditioning 610 Test procedure 710.1 Preparation for the test . 710.2 Loading the curemeter . 711 Expression of results 712 Test report . 8Annex A (informative) Effect

9、of thermal parameters on measured cure properties 16Annex B (informative) Particular requirements for oscillating-disc curemeters 19Annex C (informative) Particular requirements for rotorless curemeters .20Bibliography .21 ISO 2016 All rights reserved iiiContents PageBS ISO 6502:2016ISO 6502:2016(E)

10、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. Each member body interested in a subject for which a te

11、chnical 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 International Electrotechnical Commission (IEC) on all matters

12、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 different types of ISO documents should be noted. This documen

13、t 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 not be held responsible for identifying any or all such

14、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 information given for the convenience of users and does n

15、ot 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) see the following URL: Foreword - Supplementary informatio

16、nThe committee responsible for this document is ISO/TC45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis.This fourth edition cancels and replaces the third edition (ISO 6502:1999), of which it constitutes a minor revision. The references have been updated.iv ISO 2016 All rights

17、reservedBS ISO 6502:2016ISO 6502:2016(E)IntroductionIn this International Standard, it became clear that a number of different curemeters were available and that significant developments had taken place, especially with the rotorless types. Rather than specify individual rotorless instruments, possi

18、bly restricting future developments, it was felt that a more general document was required. Accordingly, it was decided to provide guidance and assistance in the design and use of curemeters generally. ISO 2016 All rights reserved vBS ISO 6502:2016BS ISO 6502:2016Rubber Guide to the use of curemeter

19、sWARNING 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 establish appropriate safety and health

20、practices and to ensure compliance with any national regulatory conditions.1 ScopeThis International Standard provides guidance on the determination of vulcanization characteristics of rubber compounds by means of curemeters.2 Normative referencesThe following documents, in whole or in part, are nor

21、matively 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 1382, Rubber Vocabulary3 Terms and definitionsFor the pur

22、poses of this document, the terms and definitions given in ISO 1382 and the following apply.3.1oscillating-disc curemeterODCcuremeter consisting of a biconical disc oscillated within a temperature-controlled die cavity containing the test pieceNote 1 to entry: An oscillating-disc curemeter is also k

23、nown as an oscillating disc rheometer (ODR).3.2rotorless curemeterRCMcuremeter consisting of two dies forming a temperature-controlled cavity, one of which is moved relative to the other to apply a stress or strain to the test pieceNote 1 to entry: A rotorless curemeter is also known as a moving die

24、 rheometer (MDR).Note 2 to entry: Types of rotorless curemeter are listed in Clause 5 and illustrated in Figure 3 to Figure 7.3.3marching-modulus curetype of vulcanization during which the modulus does not reach a maximum value but, after a rapid rise, continues to rise slowly at the vulcanization t

25、emperature3.4vulcanization characteristicscharacteristics which may be taken from a vulcanization curveNote 1 to entry: See Figure 1.Note 2 to entry: More explanations are given in Clause 4.INTERNATIONAL STANDARD ISO 6502:2016(E) ISO 2016 All rights reserved 1BS ISO 6502:2016ISO 6502:2016(E)3.5stiff

26、nessmeasure of the resistance offered by rubber to deformationNote 1 to entry: Force and torque have not been defined since they have a generally accepted scientific meaning.4 Basic principlesThe properties of a rubber compound change during the course of vulcanization, and the vulcanization charact

27、eristics can be determined by measuring properties as a function of time and temperature. Vulcanization characteristics are most commonly determined using instruments known as curemeters in which a cyclic stress or strain is applied to a test piece and the associated strain or force is measured. Nor

28、mally, the test is carried out at a predetermined constant temperature and the measure of stiffness recorded continuously as a function of time.The stiffness of the rubber increases as vulcanization proceeds. Vulcanization is complete when the recorded stiffness rises to a plateau value or to a maxi

29、mum and then declines (see Figure 1). In the latter case, the decrease in stiffness is caused by reversion. In cases where the recorded stiffness continues to rise (marching-modulus cure), vulcanization is deemed to be complete after a specified time. The time required to obtain a vulcanization curv

30、e is a function of the test temperature and the characteristics of the rubber compound. Curves analogous to Figure 1 are obtained for a curemeter in which strain is measured.The following vulcanization characteristics can be taken from the measure of stiffness against time curve (Figure 1):Minimum f

31、orce or torque FLor MLForce or torque at a specified time t Ftor MtScorch time (time to incipient cure) tsxTime to a percentage y of full cure from minimum force or torque tc(y)Plateau force or torque FHFor MHFMaximum force or torque (reverting cure) FHRor MHRForce or torque value attained after a s

32、pecified time (marching-modulus cure) FHor MHThe minimum force or torque FLor MLcharacterizes the stiffness of the unvulcanized compound at the curing temperature.The scorch time (time to incipient cure) tsxis a measure of the processing safety of the compound.The time tc(y) and the corresponding fo

33、rces or torques give information on the progress of cure. The optimum cure is often taken as tc(90).The highest force or torque is a measure of the stiffness of the vulcanized rubber at the curing temperature.NOTE The term F denotes force and the term M denotes torque.2 ISO 2016 All rights reservedB

34、S ISO 6502:2016ISO 6502:2016(E)12345Shear forcetorque, ForMFL orMLFt orMtFHRorMHRta) Vulcanization curve F or M = f(t)F orMxtsxtc(10)tc(50)tc(90)tHF= F FHF= M ML= F FHF= M M, y = 100ory = 10y = 50y = 90, y = 100orb) Method of evaluationKey1 sinusoidal curve2 envelope curve3 vulcanization curve with

35、steady increase to FHor MHat time teat end of test (marching-modulus cure)4 vulcanization curve with plateau at FHFor MHF(plateau cure)5 vulcanization curve with maximum FHRor MHRat time tmax(reverting cure)Figure 1 Typical vulcanization curve and method of evaluation ISO 2016 All rights reserved 3B

36、S ISO 6502:2016ISO 6502:2016(E)5 Types of curemeterThree types of curemeters have found widespread use: oscillating-disc; reciprocating-paddle; rotorless.The reciprocating-paddle type was popular, but is now much less used and is not considered further in this International Standard.Rotorless cureme

37、ters can be subdivided into three forms: reciprocating (linear strain); oscillating (torsion) unsealed cavity; oscillating (torsion) sealed cavity.Oscillating types may have a biconical die, a flat-plate die or be of top-hat section.Other geometries are possible, for example with a vibrating probe o

38、r needle.The oscillating-disc curemeter has for many years been the most widely used type of instrument, recently the rotorless type of curemeter has increased greatly in popularity. The principal advantages of the rotorless type are that the specified temperature is reached in a shorter time after

39、insertion of the test piece into the die cavity and there is better temperature distribution in the test piece (see Annex A).6 Apparatus6.1 GeneralA curemeter consists of two heated dies with means of closing them under a specified force to form a die cavity containing the test piece, a means of osc

40、illating a rotor within the cavity, or alternatively oscillating or reciprocating one of the dies relative to the other, and a means of measuring and recording the force or torque required to produce the relative movement, or the movement produced by a given applied force or torque. In addition, wit

41、h sealed rotorless torsion systems, reaction torque on the stationary die opposite the moving die may be measured.The general arrangements for oscillating-disc and rotorless curemeters are shown in Figure 2 to Figure 7.6.2 Die cavityThe dies should be manufactured from a non-deforming material. The

42、surface of the dies should minimize the effect of contamination and be hard so as to prevent wear. A minimum Rockwell hardness of 50 HRC, or equivalent, is recommended. The tolerances necessary on the dimensions of the dies will depend on the particular design, but as a general guide the dimensions

43、of the cavity should be controlled to 0,2 %.The top and bottom surfaces of the cavity should have a pattern of grooves of dimensions sufficient to prevent slippage of the rubber test piece.Holes should be provided in both the upper and lower dies to accommodate temperature sensors. The positions of

44、the sensors relative to the cavity should be controlled to ensure reproducible response.In the case of oscillating-disc instruments, one die requires a central hole to allow insertion of the die stem. A seal of suitable low, constant friction should be provided in this hole to prevent material leaki

45、ng from the cavity.4 ISO 2016 All rights reservedBS ISO 6502:2016ISO 6502:2016(E)Suitable means should be employed by design of dies or otherwise to apply pressure to the test piece throughout the test to minimize slippage between the disc and the rubber. A positive pressure is also important to exc

46、lude air which might affect the cure of, for example, peroxide-cured rubbers and to prevent any tendency for the rubber to become porous.The dimensions of the die cavity may be checked by measuring the dimensions of the vulcanized test piece. For biconical-die rotorless curemeters, particular attent

47、ion should be paid to the thin central portion, the thickness of which depends on the die gap. For oscillating-disc curemeters, the vulcanized test piece should be cut in half and checked to see that it is symmetrical. Any asymmetry indicates that the rotor height has been set incorrectly.The dimens

48、ions of the cavity and of the vulcanized test piece will not be identical because of the effect of mould shrinkage.6.3 Die closureThe dies are closed and held closed during the test by, for example, a pneumatic cylinder.A force of 11 kN 0,5 kN is recommended for oscillating-disc instruments with a m

49、ating-surface area between the dies of approximately 1 400 mm2.In unsealed rotorless instruments, the dies are not completely closed but a small clearance is left which should be between 0,05 mm and 0,2 mm. For sealed cavities, no gap should exist at the edges of the die cavity. The minimum closing force required depends on the clearance area. As a general guide, a minimum of 7 kN to 8 kN is recommended.6.4 Moving memberThe disc in an oscillating-disc instrument should be manufactured from a non-deforming material having